#============================================================================== data_global #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Michael Rose' _publ_contact_author_address ; Division of Chemistry and Chemical Engineering, California Institute of Technology, 1200 E California Blvd, Pasdena, CA 91125 USA ; _publ_contact_author_email mrose@caltech.edu _publ_contact_author_fax '+1 626 459 2935' _publ_contact_author_phone '+1 626 395 2846' _publ_requested_journal 'Inorganic Chemistry' _publ_requested_category FM _publ_section_abstract ; Here we report the syntheses and X-ray structures of a series of cobalt(II) and nickel(II) complexes derived from RNP2 ligands (where R = OMeBz, HBz, BrBz, Ph) bearing ethylene linkers between a single N and two P donors. In the X-ray structures, the CoII complexes generally adopt a tetrahedral configuration of general formula [(NP2)Co(I)2], wherein the two phosphorous donors are bound to the metal center but the central N-donor remains unbound. We have found one case of structural isomerism within a single crystal structure: the CoII complex derived from BzNP2 displays dual coordination modes: one in the tetrahedral complex [(BzNP2)Co(I)2]; and the other in a square pyramidal variant, [(BzNP2)Co(I)2]. In contrast, the NiII complexes adopt a square planar geometry in which the P(Et)N(Et)P donors in the backbone of the ligand are coordinated to the metal center, resulting in cationic species of formula [(RNP2)Ni(I)]+ with iodide as counterion. All NiII complexes exhibit sharp 1H and 31P spectra in the diamagnetic region. The CoII complexes are high-spin (S = 3/2) in the solid state as determined by SQUID measurements from 4 to 300 K. Solution EPR experiments reveal a high-spin/low-spin CoII equilibrium that is dependent on solvent and ligand substituent. ; #============================================================================== # TITLE AND AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Dong, Qingchen' ; Division of Chemistry and Chemical Engineering, California Institute of Technology, 1200 E California Blvd, Pasdena, CA 91125 USA ; 'Rose, Michael J.' ; Division of Chemistry and Chemical Engineering, California Institute of Technology, 1200 E California Blvd, Pasdena, CA 91125 USA ; 'Wong, Raymond' ; Department of Chemistry, Hong Kong Baptist University, Waterloo Rd Hong Kong, P.R. China ; 'Gray, Harry B.' ; Division of Chemistry and Chemical Engineering, California Institute of Technology, 1200 E California Blvd, Pasdena, CA 91125 USA ; #============================================================================== data_dqc03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 Co I2 N P2, C4 H8 O' _chemical_formula_sum 'C39 H43 Co I2 N O P2' _chemical_formula_weight 916.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.1301(5) _cell_length_b 14.3870(7) _cell_length_c 28.7247(14) _cell_angle_alpha 90.00 _cell_angle_beta 94.000(2) _cell_angle_gamma 90.00 _cell_volume 3763.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 33.98 _exptl_crystal_description Blade _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 2.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6471 _exptl_absorpt_correction_T_max 0.7470 _exptl_absorpt_process_details 'SADABS v2008/2, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 12 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 143020 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 35.49 _reflns_number_total 17137 _reflns_number_gt 13900 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17137 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0424 _refine_ls_wR_factor_gt 0.0411 _refine_ls_goodness_of_fit_ref 1.663 _refine_ls_restrained_S_all 1.663 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.836131(19) -0.024085(13) 0.321736(6) 0.01385(4) Uani 1 1 d . . . I1 I 0.716491(10) -0.072727(7) 0.241791(3) 0.01937(2) Uani 1 1 d . . . I2 I 1.006968(10) -0.144682(7) 0.362399(3) 0.02088(2) Uani 1 1 d . . . P1 P 0.95832(4) 0.11383(2) 0.303088(12) 0.01414(7) Uani 1 1 d . . . P2 P 0.63677(4) -0.00202(2) 0.368430(12) 0.01369(7) Uani 1 1 d . . . N1 N 0.65593(12) 0.20266(8) 0.33193(4) 0.0145(2) Uani 1 1 d . . . C1 C 0.83707(14) 0.19582(10) 0.27000(5) 0.0180(3) Uani 1 1 d . . . H1A H 0.8727 0.2599 0.2763 0.022 Uiso 1 1 calc R . . H1B H 0.8426 0.1837 0.2362 0.022 Uiso 1 1 calc R . . C2 C 0.67623(14) 0.18911(10) 0.28205(5) 0.0166(3) Uani 1 1 d . . . H2A H 0.6182 0.2365 0.2639 0.020 Uiso 1 1 calc R . . H2B H 0.6374 0.1272 0.2725 0.020 Uiso 1 1 calc R . . C3 C 0.50785(14) 0.17176(9) 0.34264(5) 0.0158(3) Uani 1 1 d . . . H3A H 0.4346 0.2018 0.3205 0.019 Uiso 1 1 calc R . . H3B H 0.4888 0.1930 0.3744 0.019 Uiso 1 1 calc R . . C4 C 0.48624(14) 0.06623(9) 0.33996(5) 0.0154(3) Uani 1 1 d . . . H4A H 0.4739 0.0479 0.3067 0.018 Uiso 1 1 calc R . . H4B H 0.3943 0.0503 0.3545 0.018 Uiso 1 1 calc R . . C5 C 0.67150(15) 0.30266(9) 0.34310(5) 0.0181(3) Uani 1 1 d . . . H5A H 0.5939 0.3373 0.3246 0.022 Uiso 1 1 calc R . . H5B H 0.7675 0.3244 0.3333 0.022 Uiso 1 1 calc R . . C6 C 0.66166(15) 0.32590(10) 0.39389(5) 0.0195(3) Uani 1 1 d . . . C7 C 0.76383(17) 0.29178(10) 0.42776(5) 0.0235(3) Uani 1 1 d . . . H7 H 0.8402 0.2520 0.4190 0.028 Uiso 1 1 calc R . . C8 C 0.7549(2) 0.31547(11) 0.47414(6) 0.0318(4) Uani 1 1 d . . . H8 H 0.8255 0.2920 0.4970 0.038 Uiso 1 1 calc R . . C9 C 0.6437(2) 0.37316(12) 0.48749(6) 0.0373(4) Uani 1 1 d . . . H9 H 0.6374 0.3887 0.5194 0.045 Uiso 1 1 calc R . . C10 C 0.54174(19) 0.40809(12) 0.45399(6) 0.0360(4) Uani 1 1 d . . . H10 H 0.4656 0.4480 0.4629 0.043 Uiso 1 1 calc R . . C11 C 0.55110(17) 0.38464(11) 0.40745(6) 0.0273(3) Uani 1 1 d . . . H11 H 0.4813 0.4089 0.3846 0.033 Uiso 1 1 calc R . . C12 C 1.04995(14) 0.17588(9) 0.35231(5) 0.0152(3) Uani 1 1 d . . . C13 C 1.09037(15) 0.26933(10) 0.35023(5) 0.0203(3) Uani 1 1 d . . . H13 H 1.0647 0.3045 0.3229 0.024 Uiso 1 1 calc R . . C14 C 1.16784(16) 0.31092(11) 0.38789(6) 0.0248(3) Uani 1 1 d . . . H14 H 1.1966 0.3742 0.3861 0.030 Uiso 1 1 calc R . . C15 C 1.20357(16) 0.26039(11) 0.42827(6) 0.0257(3) Uani 1 1 d . . . H15 H 1.2550 0.2894 0.4542 0.031 Uiso 1 1 calc R . . C16 C 1.16435(16) 0.16782(11) 0.43071(5) 0.0231(3) Uani 1 1 d . . . H16 H 1.1890 0.1332 0.4583 0.028 Uiso 1 1 calc R . . C17 C 1.08887(15) 0.12547(10) 0.39272(5) 0.0184(3) Uani 1 1 d . . . H17 H 1.0636 0.0616 0.3943 0.022 Uiso 1 1 calc R . . C18 C 1.10798(14) 0.09717(10) 0.26486(5) 0.0155(3) Uani 1 1 d . . . C19 C 1.16915(15) 0.00923(10) 0.26066(5) 0.0176(3) Uani 1 1 d . . . H19 H 1.1285 -0.0425 0.2758 0.021 Uiso 1 1 calc R . . C20 C 1.29000(15) -0.00281(11) 0.23432(5) 0.0209(3) Uani 1 1 d . . . H20 H 1.3322 -0.0628 0.2317 0.025 Uiso 1 1 calc R . . C21 C 1.34900(15) 0.07219(11) 0.21186(5) 0.0217(3) Uani 1 1 d . . . H21 H 1.4317 0.0636 0.1940 0.026 Uiso 1 1 calc R . . C22 C 1.28776(15) 0.15954(11) 0.21538(5) 0.0216(3) Uani 1 1 d . . . H22 H 1.3277 0.2108 0.1997 0.026 Uiso 1 1 calc R . . C23 C 1.16749(15) 0.17213(10) 0.24191(5) 0.0196(3) Uani 1 1 d . . . H23 H 1.1256 0.2322 0.2444 0.024 Uiso 1 1 calc R . . C24 C 0.65919(15) 0.04103(9) 0.42799(5) 0.0151(3) Uani 1 1 d . . . C25 C 0.79434(16) 0.03358(10) 0.45369(5) 0.0199(3) Uani 1 1 d . . . H25 H 0.8758 0.0069 0.4398 0.024 Uiso 1 1 calc R . . C26 C 0.81009(17) 0.06505(11) 0.49944(5) 0.0243(3) Uani 1 1 d . . . H26 H 0.9022 0.0593 0.5168 0.029 Uiso 1 1 calc R . . C27 C 0.69271(17) 0.10472(10) 0.51997(5) 0.0236(3) Uani 1 1 d . . . H27 H 0.7038 0.1263 0.5513 0.028 Uiso 1 1 calc R . . C28 C 0.55898(17) 0.11275(11) 0.49456(5) 0.0230(3) Uani 1 1 d . . . H28 H 0.4784 0.1406 0.5084 0.028 Uiso 1 1 calc R . . C29 C 0.54136(15) 0.08071(10) 0.44926(5) 0.0186(3) Uani 1 1 d . . . H29 H 0.4484 0.0857 0.4324 0.022 Uiso 1 1 calc R . . C30 C 0.56024(14) -0.11832(9) 0.37478(5) 0.0159(3) Uani 1 1 d . . . C31 C 0.63177(16) -0.17996(10) 0.40649(5) 0.0198(3) Uani 1 1 d . . . H31 H 0.7154 -0.1595 0.4253 0.024 Uiso 1 1 calc R . . C32 C 0.58221(16) -0.27036(10) 0.41086(5) 0.0235(3) Uani 1 1 d . . . H32 H 0.6314 -0.3113 0.4327 0.028 Uiso 1 1 calc R . . C33 C 0.46084(17) -0.30133(10) 0.38340(5) 0.0239(3) Uani 1 1 d . . . H33 H 0.4264 -0.3632 0.3864 0.029 Uiso 1 1 calc R . . C34 C 0.39075(16) -0.24140(10) 0.35165(5) 0.0226(3) Uani 1 1 d . . . H34 H 0.3080 -0.2626 0.3327 0.027 Uiso 1 1 calc R . . C35 C 0.43912(15) -0.15059(10) 0.34695(5) 0.0198(3) Uani 1 1 d . . . H35 H 0.3899 -0.1104 0.3248 0.024 Uiso 1 1 calc R . . O41 O 0.17205(14) 0.53365(9) 0.41353(4) 0.0403(3) Uani 1 1 d . . . C42 C 0.06448(18) 0.51197(12) 0.44593(6) 0.0336(4) Uani 1 1 d . . . H42A H 0.0996 0.5314 0.4778 0.040 Uiso 1 1 calc R . . H42B H 0.0454 0.4442 0.4461 0.040 Uiso 1 1 calc R . . C43 C -0.0717(2) 0.56341(18) 0.43036(10) 0.0743(9) Uani 1 1 d . . . H43A H -0.0703 0.6277 0.4427 0.089 Uiso 1 1 calc R . . H43B H -0.1606 0.5311 0.4398 0.089 Uiso 1 1 calc R . . C44 C -0.0627(3) 0.5620(2) 0.37828(11) 0.1195(15) Uani 1 1 d . . . H44A H -0.1000 0.5025 0.3647 0.143 Uiso 1 1 calc R . . H44B H -0.1189 0.6140 0.3632 0.143 Uiso 1 1 calc R . . C45 C 0.0988(3) 0.57257(15) 0.37295(8) 0.0655(7) Uani 1 1 d . . . H45A H 0.1270 0.5395 0.3447 0.079 Uiso 1 1 calc R . . H45B H 0.1247 0.6391 0.3701 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01221(9) 0.01481(9) 0.01462(8) -0.00058(7) 0.00165(7) 0.00057(7) I1 0.01888(5) 0.02209(5) 0.01690(4) -0.00541(4) -0.00045(3) 0.00374(4) I2 0.01844(5) 0.01864(5) 0.02536(5) 0.00286(4) 0.00010(4) 0.00428(4) P1 0.01249(16) 0.01557(16) 0.01460(16) -0.00001(13) 0.00255(13) 0.00088(13) P2 0.01230(16) 0.01607(17) 0.01274(15) -0.00053(12) 0.00121(12) 0.00025(13) N1 0.0129(5) 0.0159(6) 0.0149(5) 0.0002(4) 0.0023(4) 0.0009(4) C1 0.0170(7) 0.0208(7) 0.0165(6) 0.0039(5) 0.0037(5) 0.0030(5) C2 0.0143(6) 0.0205(7) 0.0150(6) 0.0021(5) 0.0016(5) 0.0035(5) C3 0.0134(6) 0.0173(6) 0.0167(6) 0.0005(5) 0.0015(5) 0.0022(5) C4 0.0115(6) 0.0197(7) 0.0148(6) -0.0006(5) 0.0000(5) 0.0000(5) C5 0.0179(7) 0.0154(7) 0.0215(7) 0.0011(5) 0.0047(5) 0.0006(5) C6 0.0199(7) 0.0158(7) 0.0234(7) -0.0034(5) 0.0062(6) -0.0052(5) C7 0.0286(8) 0.0196(7) 0.0224(7) -0.0014(6) 0.0035(6) -0.0031(6) C8 0.0447(11) 0.0258(9) 0.0247(8) -0.0017(7) 0.0005(7) -0.0126(8) C9 0.0489(11) 0.0378(10) 0.0269(9) -0.0155(7) 0.0148(8) -0.0209(9) C10 0.0322(9) 0.0348(10) 0.0429(11) -0.0222(8) 0.0158(8) -0.0097(8) C11 0.0213(8) 0.0263(8) 0.0349(9) -0.0104(7) 0.0050(7) -0.0042(6) C12 0.0117(6) 0.0179(6) 0.0165(6) -0.0026(5) 0.0050(5) 0.0001(5) C13 0.0197(7) 0.0202(7) 0.0214(7) 0.0000(6) 0.0049(6) -0.0019(6) C14 0.0253(8) 0.0201(7) 0.0295(8) -0.0052(6) 0.0049(6) -0.0063(6) C15 0.0207(8) 0.0307(9) 0.0256(8) -0.0086(7) -0.0001(6) -0.0050(6) C16 0.0211(8) 0.0283(8) 0.0197(7) -0.0010(6) -0.0005(6) -0.0010(6) C17 0.0168(7) 0.0181(7) 0.0204(7) -0.0003(5) 0.0018(5) -0.0007(5) C18 0.0125(6) 0.0193(7) 0.0147(6) -0.0024(5) 0.0015(5) 0.0002(5) C19 0.0163(7) 0.0204(7) 0.0161(6) -0.0022(5) 0.0007(5) 0.0006(5) C20 0.0188(7) 0.0254(8) 0.0182(7) -0.0061(6) -0.0004(5) 0.0063(6) C21 0.0143(7) 0.0355(9) 0.0156(6) -0.0039(6) 0.0025(5) 0.0029(6) C22 0.0191(7) 0.0267(8) 0.0196(7) -0.0006(6) 0.0057(6) -0.0028(6) C23 0.0177(7) 0.0200(7) 0.0216(7) -0.0019(5) 0.0051(6) 0.0010(6) C24 0.0173(7) 0.0154(6) 0.0127(6) 0.0003(5) 0.0010(5) -0.0016(5) C25 0.0181(7) 0.0240(7) 0.0173(7) -0.0006(5) -0.0006(5) 0.0015(6) C26 0.0258(8) 0.0283(8) 0.0177(7) 0.0009(6) -0.0057(6) -0.0015(6) C27 0.0343(9) 0.0232(8) 0.0135(6) -0.0014(5) 0.0026(6) -0.0034(7) C28 0.0272(8) 0.0252(8) 0.0173(7) -0.0021(6) 0.0068(6) 0.0010(6) C29 0.0169(7) 0.0223(7) 0.0166(6) -0.0003(5) 0.0021(5) -0.0002(6) C30 0.0154(7) 0.0183(7) 0.0147(6) -0.0011(5) 0.0058(5) 0.0002(5) C31 0.0180(7) 0.0226(7) 0.0191(7) 0.0013(6) 0.0039(5) 0.0006(6) C32 0.0270(8) 0.0215(8) 0.0229(7) 0.0041(6) 0.0078(6) 0.0032(6) C33 0.0288(8) 0.0176(7) 0.0267(8) -0.0019(6) 0.0134(6) -0.0049(6) C34 0.0225(8) 0.0232(8) 0.0227(7) -0.0044(6) 0.0053(6) -0.0071(6) C35 0.0190(7) 0.0216(7) 0.0188(7) -0.0013(6) 0.0025(5) -0.0008(6) O41 0.0493(8) 0.0352(7) 0.0378(7) -0.0028(6) 0.0120(6) -0.0127(6) C42 0.0379(10) 0.0356(10) 0.0273(9) -0.0041(7) 0.0032(7) -0.0061(8) C43 0.0283(11) 0.0814(19) 0.112(2) 0.0542(17) -0.0017(12) -0.0032(11) C44 0.118(3) 0.123(3) 0.104(2) 0.082(2) -0.088(2) -0.081(2) C45 0.125(2) 0.0361(12) 0.0369(12) 0.0101(10) 0.0158(13) -0.0026(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P1 2.3563(4) . yes Co1 P2 2.3566(4) . yes Co1 I2 2.5599(2) . yes Co1 I1 2.5703(2) . yes P1 C12 1.8251(14) . ? P1 C18 1.8275(13) . ? P1 C1 1.8368(14) . ? P2 C24 1.8175(14) . ? P2 C30 1.8273(14) . ? P2 C4 1.8345(13) . ? N1 C2 1.4704(16) . ? N1 C3 1.4759(16) . ? N1 C5 1.4786(17) . ? C1 C2 1.5352(18) . ? C3 C4 1.5322(19) . ? C5 C6 1.5057(19) . ? C6 C7 1.390(2) . ? C6 C11 1.393(2) . ? C7 C8 1.383(2) . ? C8 C9 1.386(2) . ? C9 C10 1.386(3) . ? C10 C11 1.387(2) . ? C12 C17 1.3935(19) . ? C12 C13 1.3965(19) . ? C13 C14 1.386(2) . ? C14 C15 1.389(2) . ? C15 C16 1.382(2) . ? C16 C17 1.390(2) . ? C18 C19 1.3915(19) . ? C18 C23 1.3938(19) . ? C19 C20 1.3916(19) . ? C20 C21 1.385(2) . ? C21 C22 1.382(2) . ? C22 C23 1.3914(19) . ? C24 C29 1.3958(18) . ? C24 C25 1.3971(19) . ? C25 C26 1.388(2) . ? C26 C27 1.382(2) . ? C27 C28 1.383(2) . ? C28 C29 1.3792(19) . ? C30 C35 1.3979(19) . ? C30 C31 1.3998(19) . ? C31 C32 1.386(2) . ? C32 C33 1.388(2) . ? C33 C34 1.380(2) . ? C34 C35 1.389(2) . ? O41 C45 1.418(3) . ? O41 C42 1.4338(19) . ? C42 C43 1.488(3) . ? C43 C44 1.504(4) . ? C44 C45 1.501(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Co1 P2 114.376(14) . . yes P1 Co1 I2 113.041(12) . . yes P2 Co1 I2 107.566(12) . . yes P1 Co1 I1 101.807(11) . . yes P2 Co1 I1 104.371(11) . . yes I2 Co1 I1 115.503(8) . . yes C12 P1 C18 102.01(6) . . ? C12 P1 C1 108.30(7) . . ? C18 P1 C1 102.84(6) . . ? C12 P1 Co1 115.75(5) . . ? C18 P1 Co1 114.32(5) . . ? C1 P1 Co1 112.37(5) . . ? C24 P2 C30 103.70(6) . . ? C24 P2 C4 105.60(6) . . ? C30 P2 C4 104.77(6) . . ? C24 P2 Co1 122.74(5) . . ? C30 P2 Co1 104.44(4) . . ? C4 P2 Co1 113.75(4) . . ? C2 N1 C3 110.04(10) . . ? C2 N1 C5 108.88(10) . . ? C3 N1 C5 108.87(10) . . ? C2 C1 P1 113.22(9) . . ? N1 C2 C1 113.52(11) . . ? N1 C3 C4 113.87(10) . . ? C3 C4 P2 114.72(9) . . ? N1 C5 C6 114.52(11) . . ? C7 C6 C11 118.87(14) . . ? C7 C6 C5 121.16(13) . . ? C11 C6 C5 119.94(14) . . ? C8 C7 C6 120.36(15) . . ? C7 C8 C9 120.51(17) . . ? C8 C9 C10 119.64(16) . . ? C9 C10 C11 119.84(16) . . ? C10 C11 C6 120.77(16) . . ? C17 C12 C13 118.94(13) . . ? C17 C12 P1 117.85(10) . . ? C13 C12 P1 123.09(11) . . ? C14 C13 C12 120.28(14) . . ? C13 C14 C15 120.22(14) . . ? C16 C15 C14 120.02(14) . . ? C15 C16 C17 119.90(14) . . ? C16 C17 C12 120.63(13) . . ? C19 C18 C23 119.37(12) . . ? C19 C18 P1 119.52(10) . . ? C23 C18 P1 121.00(10) . . ? C20 C19 C18 119.90(13) . . ? C21 C20 C19 120.34(13) . . ? C22 C21 C20 120.12(13) . . ? C21 C22 C23 119.81(14) . . ? C22 C23 C18 120.45(13) . . ? C29 C24 C25 118.64(13) . . ? C29 C24 P2 120.79(10) . . ? C25 C24 P2 120.56(10) . . ? C26 C25 C24 120.31(13) . . ? C27 C26 C25 120.42(14) . . ? C26 C27 C28 119.45(14) . . ? C29 C28 C27 120.71(14) . . ? C28 C29 C24 120.46(13) . . ? C35 C30 C31 118.44(13) . . ? C35 C30 P2 122.66(11) . . ? C31 C30 P2 118.73(11) . . ? C32 C31 C30 120.87(14) . . ? C31 C32 C33 120.17(14) . . ? C34 C33 C32 119.35(14) . . ? C33 C34 C35 121.08(14) . . ? C34 C35 C30 120.07(14) . . ? C45 O41 C42 108.33(15) . . ? O41 C42 C43 106.99(16) . . ? C42 C43 C44 100.9(2) . . ? C45 C44 C43 102.84(18) . . ? O41 C45 C44 106.64(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 35.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.106 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.101 #===END data_dqc04 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 I N Ni P2, C H2 Cl2, I' _chemical_formula_sum 'C36 H37 Cl2 I2 N Ni P2' _chemical_formula_weight 929.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.9712(4) _cell_length_b 24.7251(10) _cell_length_c 16.2706(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.804(2) _cell_angle_gamma 90.00 _cell_volume 3601.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9723 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 39.30 _exptl_crystal_description Blade _exptl_crystal_colour 'Deep purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1832 _exptl_absorpt_coefficient_mu 2.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6569 _exptl_absorpt_correction_T_max 0.7481 _exptl_absorpt_process_details 'SADABS v2008/2, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 14 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 181997 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 40.81 _reflns_number_total 23057 _reflns_number_gt 18234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23057 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0426 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.675 _refine_ls_restrained_S_all 1.675 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I2 I 0.774067(9) 0.827720(3) 0.923959(5) 0.01948(2) Uani 1 1 d . . . Ni1 Ni 0.245863(15) 0.997675(5) 0.756005(8) 0.00964(2) Uani 1 1 d . . . I1 I 0.393950(8) 1.004770(3) 0.633459(4) 0.01522(2) Uani 1 1 d . . . P1 P 0.19404(3) 0.911629(11) 0.733184(16) 0.01078(5) Uani 1 1 d . . . P2 P 0.20217(3) 1.085880(11) 0.770927(17) 0.01150(5) Uani 1 1 d . . . N1 N 0.17365(10) 0.98768(4) 0.86780(5) 0.01017(15) Uani 1 1 d . . . C1 C 0.14835(13) 0.88907(4) 0.83512(6) 0.01298(19) Uani 1 1 d . . . H1A H 0.0749 0.8592 0.8304 0.016 Uiso 1 1 calc R . . H1B H 0.2393 0.8760 0.8668 0.016 Uiso 1 1 calc R . . C2 C 0.08291(12) 0.93728(4) 0.87811(6) 0.01224(19) Uani 1 1 d . . . H2A H -0.0206 0.9435 0.8552 0.015 Uiso 1 1 calc R . . H2B H 0.0792 0.9292 0.9375 0.015 Uiso 1 1 calc R . . C3 C 0.08177(12) 1.03432(4) 0.89564(6) 0.01270(19) Uani 1 1 d . . . H3A H 0.0701 1.0311 0.9555 0.015 Uiso 1 1 calc R . . H3B H -0.0190 1.0328 0.8669 0.015 Uiso 1 1 calc R . . C4 C 0.15343(13) 1.08829(4) 0.87815(6) 0.01382(19) Uani 1 1 d . . . H4A H 0.2440 1.0939 0.9153 0.017 Uiso 1 1 calc R . . H4B H 0.0827 1.1182 0.8864 0.017 Uiso 1 1 calc R . . C5 C 0.32308(12) 0.98419(4) 0.91737(6) 0.01176(18) Uani 1 1 d . . . H5A H 0.3814 0.9545 0.8944 0.014 Uiso 1 1 calc R . . H5B H 0.3783 1.0182 0.9090 0.014 Uiso 1 1 calc R . . C6 C 0.31846(12) 0.97495(4) 1.00896(6) 0.01225(18) Uani 1 1 d . . . C7 C 0.33403(14) 0.92272(5) 1.04097(7) 0.0185(2) Uani 1 1 d . . . H7 H 0.3425 0.8930 1.0045 0.022 Uiso 1 1 calc R . . C8 C 0.33734(15) 0.91355(6) 1.12548(8) 0.0241(3) Uani 1 1 d . . . H8 H 0.3452 0.8777 1.1463 0.029 Uiso 1 1 calc R . . C9 C 0.32914(13) 0.95668(6) 1.17911(7) 0.0234(3) Uani 1 1 d . . . H9 H 0.3331 0.9506 1.2369 0.028 Uiso 1 1 calc R . . C10 C 0.31510(12) 1.00877(6) 1.14828(7) 0.0196(2) Uani 1 1 d . . . H10 H 0.3094 1.0384 1.1851 0.024 Uiso 1 1 calc R . . C11 C 0.30927(12) 1.01799(5) 1.06370(7) 0.0145(2) Uani 1 1 d . . . H11 H 0.2990 1.0539 1.0432 0.017 Uiso 1 1 calc R . . C12 C 0.02096(12) 0.91236(4) 0.66855(6) 0.01236(18) Uani 1 1 d . . . C13 C 0.02172(13) 0.93266(5) 0.58818(7) 0.0143(2) Uani 1 1 d . . . H13 H 0.1137 0.9426 0.5667 0.017 Uiso 1 1 calc R . . C14 C -0.11025(13) 0.93836(5) 0.53981(7) 0.0160(2) Uani 1 1 d . . . H14 H -0.1082 0.9513 0.4849 0.019 Uiso 1 1 calc R . . C15 C -0.24609(13) 0.92512(5) 0.57149(7) 0.0179(2) Uani 1 1 d . . . H15 H -0.3370 0.9301 0.5390 0.021 Uiso 1 1 calc R . . C16 C -0.24795(13) 0.90465(5) 0.65070(7) 0.0187(2) Uani 1 1 d . . . H16 H -0.3405 0.8953 0.6722 0.022 Uiso 1 1 calc R . . C17 C -0.11572(13) 0.89763(5) 0.69904(7) 0.0151(2) Uani 1 1 d . . . H17 H -0.1180 0.8828 0.7528 0.018 Uiso 1 1 calc R . . C18 C 0.31300(12) 0.85927(4) 0.69518(7) 0.01349(19) Uani 1 1 d . . . C19 C 0.28417(14) 0.83564(5) 0.61782(7) 0.0200(2) Uani 1 1 d . . . H19 H 0.2019 0.8478 0.5829 0.024 Uiso 1 1 calc R . . C20 C 0.37518(16) 0.79441(5) 0.59171(8) 0.0253(3) Uani 1 1 d . . . H20 H 0.3551 0.7784 0.5390 0.030 Uiso 1 1 calc R . . C21 C 0.49502(16) 0.77670(5) 0.64254(9) 0.0254(3) Uani 1 1 d . . . H21 H 0.5568 0.7484 0.6248 0.031 Uiso 1 1 calc R . . C22 C 0.52533(15) 0.80001(5) 0.71915(8) 0.0225(2) Uani 1 1 d . . . H22 H 0.6079 0.7877 0.7537 0.027 Uiso 1 1 calc R . . C23 C 0.43541(13) 0.84137(5) 0.74561(7) 0.0171(2) Uani 1 1 d . . . H23 H 0.4571 0.8575 0.7980 0.021 Uiso 1 1 calc R . . C24 C 0.02901(12) 1.10228(4) 0.71125(7) 0.01371(19) Uani 1 1 d . . . C25 C -0.04657(13) 1.06293(5) 0.66393(7) 0.0152(2) Uani 1 1 d . . . H25 H -0.0072 1.0273 0.6624 0.018 Uiso 1 1 calc R . . C26 C -0.17940(13) 1.07520(5) 0.61876(7) 0.0182(2) Uani 1 1 d . . . H26 H -0.2302 1.0481 0.5864 0.022 Uiso 1 1 calc R . . C27 C -0.23746(14) 1.12697(5) 0.62101(8) 0.0225(2) Uani 1 1 d . . . H27 H -0.3277 1.1355 0.5899 0.027 Uiso 1 1 calc R . . C28 C -0.16356(15) 1.16642(6) 0.66890(10) 0.0290(3) Uani 1 1 d . . . H28 H -0.2041 1.2018 0.6710 0.035 Uiso 1 1 calc R . . C29 C -0.03099(14) 1.15437(5) 0.71368(8) 0.0232(3) Uani 1 1 d . . . H29 H 0.0192 1.1816 0.7461 0.028 Uiso 1 1 calc R . . C30 C 0.32021(12) 1.14436(4) 0.75777(7) 0.0147(2) Uani 1 1 d . . . C31 C 0.36176(14) 1.17902(5) 0.82321(8) 0.0221(2) Uani 1 1 d . . . H31 H 0.3316 1.1713 0.8769 0.026 Uiso 1 1 calc R . . C32 C 0.44724(16) 1.22474(6) 0.80986(10) 0.0287(3) Uani 1 1 d . . . H32 H 0.4761 1.2480 0.8547 0.034 Uiso 1 1 calc R . . C33 C 0.49039(15) 1.23663(5) 0.73211(10) 0.0277(3) Uani 1 1 d . . . H33 H 0.5488 1.2679 0.7234 0.033 Uiso 1 1 calc R . . C34 C 0.44833(15) 1.20274(5) 0.66652(9) 0.0257(3) Uani 1 1 d . . . H34 H 0.4775 1.2111 0.6129 0.031 Uiso 1 1 calc R . . C35 C 0.36392(14) 1.15675(5) 0.67885(8) 0.0203(2) Uani 1 1 d . . . H35 H 0.3358 1.1337 0.6338 0.024 Uiso 1 1 calc R . . C41 C 0.39038(18) 0.75008(6) 0.94181(11) 0.0372(4) Uani 1 1 d . . . H41A H 0.3654 0.7442 0.8823 0.045 Uiso 1 1 calc R . . H41B H 0.4847 0.7709 0.9479 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.41436(5) 0.686974(16) 0.99208(3) 0.04074(9) Uani 1 1 d . . . Cl2 Cl 0.24493(6) 0.787298(15) 0.98473(3) 0.04417(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I2 0.02749(4) 0.01502(3) 0.01633(3) -0.00115(3) 0.00437(3) -0.00344(3) Ni1 0.01001(6) 0.01066(6) 0.00840(5) 0.00052(4) 0.00183(4) 0.00040(5) I1 0.01373(3) 0.02045(4) 0.01180(3) 0.00149(2) 0.00312(2) 0.00001(3) P1 0.01187(12) 0.01133(12) 0.00918(11) 0.00006(9) 0.00102(9) 0.00020(10) P2 0.01215(13) 0.01128(12) 0.01117(11) 0.00098(9) 0.00164(9) 0.00092(10) N1 0.0091(4) 0.0122(4) 0.0092(3) -0.0001(3) 0.0008(3) -0.0002(3) C1 0.0146(5) 0.0133(5) 0.0110(4) 0.0014(3) 0.0002(4) -0.0014(4) C2 0.0111(5) 0.0145(5) 0.0111(4) 0.0001(3) 0.0016(3) -0.0029(4) C3 0.0121(5) 0.0143(5) 0.0120(4) -0.0007(3) 0.0028(4) 0.0015(4) C4 0.0163(5) 0.0131(5) 0.0122(4) -0.0009(4) 0.0012(4) 0.0013(4) C5 0.0100(4) 0.0146(5) 0.0107(4) 0.0000(3) 0.0005(3) -0.0004(4) C6 0.0092(4) 0.0166(5) 0.0109(4) 0.0006(3) -0.0003(3) -0.0007(4) C7 0.0207(6) 0.0176(5) 0.0167(5) 0.0021(4) -0.0023(4) -0.0016(4) C8 0.0224(6) 0.0285(7) 0.0208(6) 0.0114(5) -0.0039(5) -0.0033(5) C9 0.0131(5) 0.0442(8) 0.0127(5) 0.0065(5) 0.0000(4) -0.0030(5) C10 0.0106(5) 0.0350(7) 0.0134(5) -0.0050(4) 0.0013(4) 0.0001(5) C11 0.0109(5) 0.0190(5) 0.0135(4) -0.0015(4) 0.0001(4) 0.0007(4) C12 0.0129(5) 0.0122(5) 0.0119(4) -0.0010(3) 0.0004(4) 0.0003(4) C13 0.0137(5) 0.0169(5) 0.0126(4) 0.0000(4) 0.0017(4) -0.0008(4) C14 0.0173(5) 0.0186(5) 0.0120(4) 0.0007(4) -0.0006(4) 0.0001(4) C15 0.0147(5) 0.0215(6) 0.0169(5) -0.0007(4) -0.0022(4) 0.0011(4) C16 0.0138(5) 0.0245(6) 0.0178(5) -0.0003(4) 0.0024(4) -0.0024(4) C17 0.0164(5) 0.0166(5) 0.0125(4) 0.0005(4) 0.0018(4) -0.0017(4) C18 0.0149(5) 0.0112(5) 0.0147(4) -0.0006(4) 0.0034(4) -0.0004(4) C19 0.0228(6) 0.0194(6) 0.0178(5) -0.0053(4) 0.0004(4) 0.0029(5) C20 0.0317(7) 0.0203(6) 0.0243(6) -0.0077(5) 0.0046(5) 0.0041(5) C21 0.0303(7) 0.0162(6) 0.0309(7) -0.0009(5) 0.0103(6) 0.0075(5) C22 0.0213(6) 0.0188(6) 0.0275(6) 0.0040(5) 0.0033(5) 0.0069(5) C23 0.0176(5) 0.0157(5) 0.0181(5) 0.0006(4) 0.0021(4) 0.0014(4) C24 0.0131(5) 0.0150(5) 0.0132(4) 0.0015(4) 0.0024(4) 0.0021(4) C25 0.0160(5) 0.0152(5) 0.0143(5) 0.0010(4) 0.0013(4) 0.0026(4) C26 0.0159(5) 0.0229(6) 0.0156(5) -0.0008(4) 0.0001(4) 0.0001(4) C27 0.0148(6) 0.0260(6) 0.0261(6) 0.0027(5) -0.0025(5) 0.0052(5) C28 0.0219(6) 0.0197(6) 0.0442(8) -0.0014(6) -0.0061(6) 0.0080(5) C29 0.0199(6) 0.0166(6) 0.0324(7) -0.0033(5) -0.0040(5) 0.0034(5) C30 0.0131(5) 0.0123(5) 0.0189(5) 0.0027(4) 0.0016(4) 0.0014(4) C31 0.0237(6) 0.0172(6) 0.0254(6) -0.0005(4) 0.0015(5) -0.0030(5) C32 0.0281(7) 0.0184(6) 0.0393(8) -0.0019(5) 0.0004(6) -0.0055(5) C33 0.0208(6) 0.0153(6) 0.0476(9) 0.0060(5) 0.0066(6) -0.0012(5) C34 0.0218(6) 0.0216(6) 0.0349(7) 0.0108(5) 0.0114(5) 0.0030(5) C35 0.0198(6) 0.0180(5) 0.0236(6) 0.0048(4) 0.0057(5) 0.0027(4) C41 0.0359(9) 0.0306(8) 0.0444(9) 0.0141(7) -0.0025(7) -0.0084(7) Cl1 0.0494(2) 0.03104(19) 0.0401(2) 0.01186(16) -0.00975(18) -0.00070(17) Cl2 0.0704(3) 0.02196(18) 0.0399(2) 0.00503(15) 0.0020(2) -0.00089(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9864(8) . yes Ni1 P1 2.2039(3) . yes Ni1 P2 2.2319(3) . yes Ni1 I1 2.47444(16) . yes P1 C18 1.8124(11) . ? P1 C12 1.8167(12) . ? P1 C1 1.8222(10) . ? P2 C30 1.8132(12) . ? P2 C24 1.8222(12) . ? P2 C4 1.8273(11) . ? N1 C3 1.5047(14) . ? N1 C2 1.5039(14) . ? N1 C5 1.5205(14) . ? C1 C2 1.5196(15) . ? C3 C4 1.5162(16) . ? C5 C6 1.5108(14) . ? C6 C11 1.3937(15) . ? C6 C7 1.3960(16) . ? C7 C8 1.3920(17) . ? C8 C9 1.383(2) . ? C9 C10 1.3848(19) . ? C10 C11 1.3925(16) . ? C12 C17 1.4010(15) . ? C12 C13 1.4012(15) . ? C13 C14 1.3846(17) . ? C14 C15 1.3934(16) . ? C15 C16 1.3856(17) . ? C16 C17 1.3900(17) . ? C18 C19 1.3961(16) . ? C18 C23 1.3984(17) . ? C19 C20 1.3901(17) . ? C20 C21 1.383(2) . ? C21 C22 1.384(2) . ? C22 C23 1.3886(17) . ? C24 C25 1.3892(16) . ? C24 C29 1.3975(17) . ? C25 C26 1.3914(17) . ? C26 C27 1.3834(18) . ? C27 C28 1.389(2) . ? C28 C29 1.3852(19) . ? C30 C35 1.4013(16) . ? C30 C31 1.3980(17) . ? C31 C32 1.3913(18) . ? C32 C33 1.379(2) . ? C33 C34 1.389(2) . ? C34 C35 1.3881(18) . ? C41 Cl1 1.7682(15) . ? C41 Cl2 1.7771(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P1 87.49(3) . . yes N1 Ni1 P2 87.23(3) . . yes P1 Ni1 P2 157.662(13) . . yes N1 Ni1 I1 166.37(3) . . yes P1 Ni1 I1 92.936(8) . . yes P2 Ni1 I1 97.234(8) . . yes C18 P1 C12 108.03(5) . . ? C18 P1 C1 105.37(5) . . ? C12 P1 C1 107.14(5) . . ? C18 P1 Ni1 128.65(4) . . ? C12 P1 Ni1 104.51(4) . . ? C1 P1 Ni1 101.53(4) . . ? C30 P2 C24 104.09(5) . . ? C30 P2 C4 105.39(5) . . ? C24 P2 C4 104.59(5) . . ? C30 P2 Ni1 131.16(4) . . ? C24 P2 Ni1 108.01(4) . . ? C4 P2 Ni1 100.98(4) . . ? C3 N1 C2 106.87(8) . . ? C3 N1 C5 111.41(8) . . ? C2 N1 C5 111.02(8) . . ? C3 N1 Ni1 113.50(6) . . ? C2 N1 Ni1 114.65(6) . . ? C5 N1 Ni1 99.39(6) . . ? C2 C1 P1 107.21(7) . . ? N1 C2 C1 111.72(8) . . ? N1 C3 C4 111.74(8) . . ? C3 C4 P2 106.37(7) . . ? C6 C5 N1 116.80(8) . . ? C11 C6 C7 118.47(10) . . ? C11 C6 C5 121.43(10) . . ? C7 C6 C5 119.95(10) . . ? C8 C7 C6 120.95(11) . . ? C9 C8 C7 119.94(12) . . ? C10 C9 C8 119.73(11) . . ? C9 C10 C11 120.46(11) . . ? C10 C11 C6 120.43(11) . . ? C17 C12 C13 118.82(10) . . ? C17 C12 P1 121.80(8) . . ? C13 C12 P1 119.14(8) . . ? C14 C13 C12 120.67(10) . . ? C13 C14 C15 120.11(10) . . ? C16 C15 C14 119.65(11) . . ? C15 C16 C17 120.62(10) . . ? C16 C17 C12 120.09(10) . . ? C19 C18 C23 119.20(10) . . ? C19 C18 P1 121.90(9) . . ? C23 C18 P1 118.89(8) . . ? C20 C19 C18 120.33(12) . . ? C21 C20 C19 119.89(12) . . ? C20 C21 C22 120.34(11) . . ? C21 C22 C23 120.17(12) . . ? C22 C23 C18 120.06(11) . . ? C25 C24 C29 119.11(11) . . ? C25 C24 P2 120.46(8) . . ? C29 C24 P2 120.43(9) . . ? C24 C25 C26 120.63(11) . . ? C27 C26 C25 119.90(12) . . ? C26 C27 C28 119.87(12) . . ? C29 C28 C27 120.35(12) . . ? C28 C29 C24 120.14(12) . . ? C35 C30 C31 119.16(11) . . ? C35 C30 P2 118.93(9) . . ? C31 C30 P2 121.82(9) . . ? C32 C31 C30 120.07(12) . . ? C33 C32 C31 120.50(13) . . ? C32 C33 C34 119.85(12) . . ? C35 C34 C33 120.40(12) . . ? C34 C35 C30 120.00(12) . . ? Cl1 C41 Cl2 110.19(9) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 40.81 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.477 _refine_diff_density_min -1.508 _refine_diff_density_rms 0.119 #===END data_dqc05 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H34 Br Co I2 N P2' _chemical_formula_sum 'C35 H34 Br Co I2 N P2' _chemical_formula_weight 923.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5306(4) _cell_length_b 11.7513(5) _cell_length_c 15.7593(7) _cell_angle_alpha 98.758(2) _cell_angle_beta 93.890(2) _cell_angle_gamma 101.072(2) _cell_volume 1703.35(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9262 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 38.11 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 3.609 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5978 _exptl_absorpt_correction_T_max 0.7482 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 21 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 139410 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 41.70 _reflns_number_total 23322 _reflns_number_gt 18290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23322 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0445 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0393 _refine_ls_wR_factor_gt 0.0381 _refine_ls_goodness_of_fit_ref 1.433 _refine_ls_restrained_S_all 1.433 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.087234(14) 0.652957(11) 0.722110(9) 0.01040(3) Uani 1 1 d . . . I1 I -0.285729(7) 0.697947(6) 0.817350(5) 0.01500(2) Uani 1 1 d . . . I2 I -0.136469(8) 0.444632(6) 0.633914(4) 0.01684(2) Uani 1 1 d . . . Br1 Br 0.550439(13) 1.376502(10) 0.828404(10) 0.02854(3) Uani 1 1 d . . . P1 P 0.12537(3) 0.63740(2) 0.803510(17) 0.01084(5) Uani 1 1 d . . . P2 P -0.05544(3) 0.79477(2) 0.626795(17) 0.01084(5) Uani 1 1 d . . . N1 N 0.27283(9) 0.78060(7) 0.66932(6) 0.01254(15) Uani 1 1 d . . . C1 C 0.26373(11) 0.59916(9) 0.73482(7) 0.01492(19) Uani 1 1 d . . . H1A H 0.3594 0.6271 0.7680 0.018 Uiso 1 1 calc R . . H1B H 0.2477 0.5125 0.7192 0.018 Uiso 1 1 calc R . . C2 C 0.26290(11) 0.65260(9) 0.65267(7) 0.01488(19) Uani 1 1 d . . . H2A H 0.3448 0.6353 0.6211 0.018 Uiso 1 1 calc R . . H2B H 0.1733 0.6150 0.6152 0.018 Uiso 1 1 calc R . . C3 C 0.23801(11) 0.82199(9) 0.58880(7) 0.01438(18) Uani 1 1 d . . . H3A H 0.3004 0.7951 0.5455 0.017 Uiso 1 1 calc R . . H3B H 0.2605 0.9091 0.5995 0.017 Uiso 1 1 calc R . . C4 C 0.08105(11) 0.77958(9) 0.55108(6) 0.01379(18) Uani 1 1 d . . . H4A H 0.0669 0.6955 0.5250 0.017 Uiso 1 1 calc R . . H4B H 0.0636 0.8236 0.5040 0.017 Uiso 1 1 calc R . . C5 C 0.42042(11) 0.83797(9) 0.70580(7) 0.0169(2) Uani 1 1 d . . . H5A H 0.4869 0.8209 0.6622 0.020 Uiso 1 1 calc R . . H5B H 0.4454 0.8023 0.7563 0.020 Uiso 1 1 calc R . . C6 C 0.44525(11) 0.96953(9) 0.73370(7) 0.01441(18) Uani 1 1 d . . . C7 C 0.34582(11) 1.02440(10) 0.77540(7) 0.0164(2) Uani 1 1 d . . . H7 H 0.2563 0.9785 0.7845 0.020 Uiso 1 1 calc R . . C8 C 0.37502(11) 1.14503(10) 0.80394(7) 0.0178(2) Uani 1 1 d . . . H8 H 0.3059 1.1818 0.8317 0.021 Uiso 1 1 calc R . . C9 C 0.50693(11) 1.21115(9) 0.79129(7) 0.0171(2) Uani 1 1 d . . . C10 C 0.60866(11) 1.15922(10) 0.75112(8) 0.0186(2) Uani 1 1 d . . . H10 H 0.6991 1.2052 0.7436 0.022 Uiso 1 1 calc R . . C11 C 0.57653(11) 1.03874(10) 0.72196(7) 0.0176(2) Uani 1 1 d . . . H11 H 0.6454 1.0026 0.6934 0.021 Uiso 1 1 calc R . . C12 C 0.20900(11) 0.76344(9) 0.88602(7) 0.01384(18) Uani 1 1 d . . . C13 C 0.13212(12) 0.85072(10) 0.90823(7) 0.0191(2) Uani 1 1 d . . . H13 H 0.0430 0.8480 0.8762 0.023 Uiso 1 1 calc R . . C14 C 0.18401(14) 0.94252(11) 0.97703(8) 0.0292(3) Uani 1 1 d . . . H14 H 0.1308 1.0021 0.9914 0.035 Uiso 1 1 calc R . . C15 C 0.31237(15) 0.94638(12) 1.02391(8) 0.0333(3) Uani 1 1 d . . . H15 H 0.3467 1.0076 1.0717 0.040 Uiso 1 1 calc R . . C16 C 0.39161(15) 0.86108(12) 1.00151(8) 0.0319(3) Uani 1 1 d . . . H16 H 0.4810 0.8646 1.0335 0.038 Uiso 1 1 calc R . . C17 C 0.34106(12) 0.77058(10) 0.93265(8) 0.0230(2) Uani 1 1 d . . . H17 H 0.3967 0.7131 0.9171 0.028 Uiso 1 1 calc R . . C18 C 0.09956(11) 0.51562(8) 0.86438(6) 0.01237(17) Uani 1 1 d . . . C19 C -0.03858(11) 0.46161(9) 0.87858(7) 0.01355(18) Uani 1 1 d . . . H19 H -0.1197 0.4874 0.8560 0.016 Uiso 1 1 calc R . . C20 C -0.05738(12) 0.36981(9) 0.92592(7) 0.0158(2) Uani 1 1 d . . . H20 H -0.1515 0.3326 0.9351 0.019 Uiso 1 1 calc R . . C21 C 0.06082(13) 0.33271(9) 0.95960(7) 0.0176(2) Uani 1 1 d . . . H21 H 0.0476 0.2711 0.9928 0.021 Uiso 1 1 calc R . . C22 C 0.19819(12) 0.38499(10) 0.94512(7) 0.0181(2) Uani 1 1 d . . . H22 H 0.2790 0.3589 0.9679 0.022 Uiso 1 1 calc R . . C23 C 0.21741(11) 0.47554(9) 0.89732(7) 0.01611(19) Uani 1 1 d . . . H23 H 0.3116 0.5107 0.8869 0.019 Uiso 1 1 calc R . . C24 C -0.01907(10) 0.95027(8) 0.67257(6) 0.01172(17) Uani 1 1 d . . . C25 C -0.06533(11) 0.98610(9) 0.75257(7) 0.01335(18) Uani 1 1 d . . . H25 H -0.1121 0.9289 0.7835 0.016 Uiso 1 1 calc R . . C26 C -0.04348(12) 1.10488(9) 0.78722(7) 0.0166(2) Uani 1 1 d . . . H26 H -0.0755 1.1285 0.8417 0.020 Uiso 1 1 calc R . . C27 C 0.02486(11) 1.18922(9) 0.74267(7) 0.0160(2) Uani 1 1 d . . . H27 H 0.0393 1.2704 0.7664 0.019 Uiso 1 1 calc R . . C28 C 0.07207(11) 1.15446(9) 0.66320(7) 0.01530(19) Uani 1 1 d . . . H28 H 0.1195 1.2120 0.6327 0.018 Uiso 1 1 calc R . . C29 C 0.05009(11) 1.03589(9) 0.62816(7) 0.01425(18) Uani 1 1 d . . . H29 H 0.0822 1.0127 0.5737 0.017 Uiso 1 1 calc R . . C30 C -0.21653(11) 0.77589(9) 0.55095(7) 0.01389(18) Uani 1 1 d . . . C31 C -0.28055(13) 0.66255(10) 0.50832(8) 0.0239(2) Uani 1 1 d . . . H31 H -0.2420 0.5972 0.5203 0.029 Uiso 1 1 calc R . . C32 C -0.39991(14) 0.64485(11) 0.44873(8) 0.0278(3) Uani 1 1 d . . . H32 H -0.4426 0.5675 0.4202 0.033 Uiso 1 1 calc R . . C33 C -0.45714(12) 0.73910(11) 0.43053(8) 0.0214(2) Uani 1 1 d . . . H33 H -0.5391 0.7267 0.3898 0.026 Uiso 1 1 calc R . . C34 C -0.39408(12) 0.85182(10) 0.47216(7) 0.0193(2) Uani 1 1 d . . . H34 H -0.4322 0.9169 0.4593 0.023 Uiso 1 1 calc R . . C35 C -0.27518(11) 0.87002(9) 0.53264(7) 0.01526(19) Uani 1 1 d . . . H35 H -0.2338 0.9474 0.5616 0.018 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01048(6) 0.00982(6) 0.01061(6) 0.00122(5) 0.00034(4) 0.00202(4) I1 0.01179(3) 0.01582(3) 0.01913(3) 0.00503(2) 0.00423(2) 0.00455(2) I2 0.02235(3) 0.01119(3) 0.01486(3) -0.00168(2) -0.00002(2) 0.00197(2) Br1 0.01677(5) 0.01796(5) 0.04711(8) -0.00293(5) 0.00320(5) 0.00088(4) P1 0.00993(11) 0.01063(11) 0.01239(11) 0.00335(9) 0.00126(9) 0.00197(8) P2 0.01253(11) 0.01020(11) 0.00950(10) 0.00088(9) 0.00013(8) 0.00259(8) N1 0.0111(4) 0.0129(4) 0.0142(4) 0.0045(3) 0.0011(3) 0.0024(3) C1 0.0135(4) 0.0152(4) 0.0187(5) 0.0063(4) 0.0052(4) 0.0055(4) C2 0.0154(4) 0.0145(4) 0.0160(5) 0.0035(4) 0.0047(4) 0.0044(4) C3 0.0144(4) 0.0169(5) 0.0133(4) 0.0055(4) 0.0036(3) 0.0038(4) C4 0.0166(4) 0.0155(4) 0.0100(4) 0.0019(3) 0.0019(3) 0.0051(4) C5 0.0114(4) 0.0185(5) 0.0215(5) 0.0059(4) 0.0009(4) 0.0030(4) C6 0.0111(4) 0.0177(5) 0.0148(4) 0.0060(4) -0.0008(3) 0.0018(3) C7 0.0104(4) 0.0205(5) 0.0170(5) 0.0038(4) 0.0016(4) -0.0002(4) C8 0.0120(4) 0.0222(5) 0.0179(5) 0.0007(4) 0.0006(4) 0.0029(4) C9 0.0135(4) 0.0168(5) 0.0199(5) 0.0030(4) -0.0016(4) 0.0018(4) C10 0.0112(4) 0.0198(5) 0.0248(6) 0.0062(4) 0.0031(4) 0.0008(4) C11 0.0112(4) 0.0209(5) 0.0218(5) 0.0056(4) 0.0031(4) 0.0037(4) C12 0.0131(4) 0.0141(4) 0.0128(4) 0.0050(4) 0.0006(3) -0.0025(3) C13 0.0161(5) 0.0174(5) 0.0208(5) -0.0011(4) 0.0042(4) -0.0016(4) C14 0.0277(6) 0.0241(6) 0.0279(6) -0.0090(5) 0.0126(5) -0.0071(5) C15 0.0364(7) 0.0344(7) 0.0160(5) -0.0049(5) 0.0057(5) -0.0189(6) C16 0.0287(7) 0.0356(7) 0.0228(6) 0.0129(5) -0.0116(5) -0.0158(5) C17 0.0188(5) 0.0206(5) 0.0270(6) 0.0101(5) -0.0070(4) -0.0037(4) C18 0.0146(4) 0.0110(4) 0.0119(4) 0.0030(3) 0.0028(3) 0.0022(3) C19 0.0144(4) 0.0118(4) 0.0136(4) 0.0001(3) 0.0025(3) 0.0017(3) C20 0.0200(5) 0.0120(4) 0.0137(4) 0.0002(4) 0.0063(4) -0.0008(4) C21 0.0291(6) 0.0115(4) 0.0129(4) 0.0040(4) 0.0055(4) 0.0033(4) C22 0.0234(5) 0.0170(5) 0.0163(5) 0.0051(4) 0.0019(4) 0.0078(4) C23 0.0152(5) 0.0157(5) 0.0185(5) 0.0051(4) 0.0027(4) 0.0039(4) C24 0.0129(4) 0.0104(4) 0.0117(4) 0.0014(3) 0.0001(3) 0.0028(3) C25 0.0149(4) 0.0124(4) 0.0130(4) 0.0030(3) 0.0023(3) 0.0024(3) C26 0.0204(5) 0.0141(4) 0.0147(5) -0.0009(4) 0.0031(4) 0.0043(4) C27 0.0198(5) 0.0102(4) 0.0170(5) 0.0004(4) 0.0003(4) 0.0029(4) C28 0.0183(5) 0.0121(4) 0.0154(5) 0.0043(4) 0.0000(4) 0.0019(4) C29 0.0169(5) 0.0140(4) 0.0122(4) 0.0026(4) 0.0012(3) 0.0039(4) C30 0.0137(4) 0.0158(4) 0.0120(4) 0.0027(4) 0.0001(3) 0.0027(3) C31 0.0279(6) 0.0161(5) 0.0242(6) 0.0017(4) -0.0109(5) 0.0026(4) C32 0.0288(6) 0.0217(6) 0.0269(6) 0.0018(5) -0.0128(5) -0.0028(5) C33 0.0156(5) 0.0281(6) 0.0193(5) 0.0079(5) -0.0042(4) 0.0007(4) C34 0.0150(5) 0.0244(5) 0.0210(5) 0.0093(4) 0.0013(4) 0.0064(4) C35 0.0143(4) 0.0169(5) 0.0153(5) 0.0039(4) 0.0027(4) 0.0037(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P1 2.3761(3) . yes Co1 P2 2.3990(3) . yes Co1 I2 2.56501(17) . yes Co1 I1 2.57659(17) . yes Br1 C9 1.8977(11) . ? P1 C1 1.8400(10) . ? P1 C12 1.8274(10) . ? P1 C18 1.8285(11) . ? P2 C24 1.8169(10) . ? P2 C30 1.8369(11) . ? P2 C4 1.8392(10) . ? N1 C3 1.4663(14) . ? N1 C2 1.4705(13) . ? N1 C5 1.4737(13) . ? C1 C2 1.5228(15) . ? C3 C4 1.5305(14) . ? C5 C6 1.5093(15) . ? C6 C11 1.3955(14) . ? C6 C7 1.3913(15) . ? C7 C8 1.3879(15) . ? C8 C9 1.3893(15) . ? C9 C10 1.3805(16) . ? C10 C11 1.3877(16) . ? C12 C13 1.3876(16) . ? C12 C17 1.3951(16) . ? C13 C14 1.3964(16) . ? C14 C15 1.375(2) . ? C15 C16 1.385(2) . ? C16 C17 1.3862(18) . ? C18 C19 1.3959(14) . ? C18 C23 1.3970(15) . ? C19 C20 1.3933(15) . ? C20 C21 1.3853(17) . ? C21 C22 1.3849(16) . ? C22 C23 1.3860(16) . ? C24 C29 1.3996(15) . ? C24 C25 1.3950(14) . ? C25 C26 1.3896(14) . ? C26 C27 1.3876(16) . ? C27 C28 1.3888(15) . ? C28 C29 1.3886(14) . ? C30 C35 1.3900(15) . ? C30 C31 1.3991(15) . ? C31 C32 1.3870(17) . ? C32 C33 1.3836(18) . ? C33 C34 1.3864(16) . ? C34 C35 1.3915(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Co1 P2 115.373(10) . . yes P1 Co1 I2 96.395(8) . . yes P2 Co1 I2 109.637(9) . . yes P1 Co1 I1 112.875(9) . . yes P2 Co1 I1 107.468(8) . . yes I2 Co1 I1 115.006(6) . . yes C1 P1 C12 108.25(5) . . ? C1 P1 C18 101.18(5) . . ? C12 P1 C18 102.84(5) . . ? C1 P1 Co1 112.57(4) . . ? C12 P1 Co1 116.87(4) . . ? C18 P1 Co1 113.57(3) . . ? C24 P2 C30 103.62(5) . . ? C24 P2 C4 105.00(5) . . ? C30 P2 C4 100.58(5) . . ? C24 P2 Co1 118.87(3) . . ? C30 P2 Co1 111.08(3) . . ? C4 P2 Co1 115.54(4) . . ? C3 N1 C2 110.05(8) . . ? C3 N1 C5 109.89(8) . . ? C2 N1 C5 108.63(8) . . ? C2 C1 P1 112.66(7) . . ? N1 C2 C1 112.99(8) . . ? N1 C3 C4 114.26(8) . . ? C3 C4 P2 116.36(7) . . ? N1 C5 C6 115.23(9) . . ? C11 C6 C7 118.31(10) . . ? C11 C6 C5 118.91(9) . . ? C7 C6 C5 122.67(9) . . ? C8 C7 C6 121.18(10) . . ? C7 C8 C9 118.94(10) . . ? C10 C9 C8 121.32(10) . . ? C10 C9 Br1 118.40(8) . . ? C8 C9 Br1 120.27(8) . . ? C9 C10 C11 118.83(10) . . ? C10 C11 C6 121.41(10) . . ? C13 C12 C17 118.63(10) . . ? C13 C12 P1 118.38(8) . . ? C17 C12 P1 122.75(9) . . ? C12 C13 C14 120.84(11) . . ? C15 C14 C13 119.78(13) . . ? C14 C15 C16 120.04(11) . . ? C17 C16 C15 120.27(12) . . ? C16 C17 C12 120.40(12) . . ? C19 C18 C23 119.16(10) . . ? C19 C18 P1 120.26(8) . . ? C23 C18 P1 120.58(8) . . ? C20 C19 C18 119.96(10) . . ? C21 C20 C19 120.14(10) . . ? C20 C21 C22 120.30(10) . . ? C23 C22 C21 119.79(11) . . ? C22 C23 C18 120.63(10) . . ? C29 C24 C25 118.88(9) . . ? C29 C24 P2 121.60(7) . . ? C25 C24 P2 119.49(8) . . ? C26 C25 C24 120.41(10) . . ? C27 C26 C25 120.34(10) . . ? C26 C27 C28 119.70(9) . . ? C29 C28 C27 120.18(10) . . ? C28 C29 C24 120.48(9) . . ? C35 C30 C31 118.72(10) . . ? C35 C30 P2 122.62(8) . . ? C31 C30 P2 118.64(8) . . ? C32 C31 C30 120.47(11) . . ? C33 C32 C31 120.44(11) . . ? C32 C33 C34 119.52(10) . . ? C33 C34 C35 120.32(11) . . ? C30 C35 C34 120.52(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 41.70 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.636 _refine_diff_density_min -1.796 _refine_diff_density_rms 0.124 #===END data_dqc06 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H34 Br I N Ni P2, I' _chemical_formula_sum 'C35 H34 Br I2 N Ni P2' _chemical_formula_weight 922.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9678(6) _cell_length_b 12.1991(12) _cell_length_c 13.2965(7) _cell_angle_alpha 103.056(4) _cell_angle_beta 108.995(3) _cell_angle_gamma 102.700(4) _cell_volume 1695.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9207 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 41.45 _exptl_crystal_description Block _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 3.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6620 _exptl_absorpt_correction_T_max 0.7482 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 18 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 124870 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 41.90 _reflns_number_total 23459 _reflns_number_gt 18790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Patterson method' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23459 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0475 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0529 _refine_ls_wR_factor_gt 0.0520 _refine_ls_goodness_of_fit_ref 2.002 _refine_ls_restrained_S_all 2.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.104943(15) 0.259296(14) 0.259892(14) 0.00951(3) Uani 1 1 d . . . I1 I 0.085518(8) 0.044874(7) 0.207502(8) 0.01358(2) Uani 1 1 d . . . Br1 Br -0.390701(16) 0.318153(17) -0.183091(16) 0.03526(5) Uani 1 1 d . . . P1 P 0.29898(3) 0.30996(3) 0.27270(3) 0.01083(6) Uani 1 1 d . . . P2 P -0.08641(3) 0.22204(3) 0.25354(3) 0.01077(6) Uani 1 1 d . . . N1 N 0.12885(10) 0.43184(9) 0.31579(9) 0.01184(19) Uani 1 1 d . . . C1 C 0.35653(12) 0.46988(12) 0.35267(11) 0.0143(2) Uani 1 1 d . . . H1A H 0.4395 0.4908 0.4137 0.017 Uiso 1 1 calc R . . H1B H 0.3638 0.5177 0.3027 0.017 Uiso 1 1 calc R . . C2 C 0.26161(12) 0.49382(12) 0.40151(11) 0.0146(2) Uani 1 1 d . . . H2A H 0.2735 0.4659 0.4675 0.018 Uiso 1 1 calc R . . H2B H 0.2761 0.5804 0.4273 0.018 Uiso 1 1 calc R . . C3 C 0.04647(13) 0.45471(12) 0.37773(12) 0.0152(2) Uani 1 1 d . . . H3A H 0.0457 0.5375 0.3884 0.018 Uiso 1 1 calc R . . H3B H 0.0831 0.4470 0.4531 0.018 Uiso 1 1 calc R . . C4 C -0.08732(13) 0.37172(12) 0.31868(12) 0.0149(2) Uani 1 1 d . . . H4A H -0.1361 0.4004 0.2604 0.018 Uiso 1 1 calc R . . H4B H -0.1266 0.3698 0.3736 0.018 Uiso 1 1 calc R . . C5 C 0.11262(13) 0.48907(12) 0.22423(12) 0.0149(2) Uani 1 1 d . . . H5A H 0.1305 0.5751 0.2596 0.018 Uiso 1 1 calc R . . H5B H 0.1768 0.4805 0.1939 0.018 Uiso 1 1 calc R . . C6 C -0.01186(12) 0.44354(11) 0.12670(11) 0.0125(2) Uani 1 1 d . . . C7 C -0.03699(14) 0.34849(13) 0.03276(12) 0.0167(3) Uani 1 1 d . . . H7 H 0.0235 0.3095 0.0324 0.020 Uiso 1 1 calc R . . C8 C -0.14906(15) 0.30988(14) -0.06032(13) 0.0207(3) Uani 1 1 d . . . H8 H -0.1657 0.2450 -0.1241 0.025 Uiso 1 1 calc R . . C9 C -0.23574(13) 0.36778(14) -0.05830(13) 0.0213(3) Uani 1 1 d . . . C10 C -0.21264(14) 0.46367(14) 0.03286(14) 0.0213(3) Uani 1 1 d . . . H10 H -0.2730 0.5029 0.0324 0.026 Uiso 1 1 calc R . . C11 C -0.10055(13) 0.50155(13) 0.12456(13) 0.0172(3) Uani 1 1 d . . . H11 H -0.0836 0.5680 0.1870 0.021 Uiso 1 1 calc R . . C12 C 0.40705(12) 0.24678(11) 0.35264(11) 0.0123(2) Uani 1 1 d . . . C13 C 0.50167(13) 0.21976(13) 0.32319(12) 0.0173(3) Uani 1 1 d . . . H13 H 0.5115 0.2338 0.2587 0.021 Uiso 1 1 calc R . . C14 C 0.58189(14) 0.17215(14) 0.38848(13) 0.0216(3) Uani 1 1 d . . . H14 H 0.6466 0.1539 0.3684 0.026 Uiso 1 1 calc R . . C15 C 0.56772(14) 0.15127(13) 0.48242(13) 0.0215(3) Uani 1 1 d . . . H15 H 0.6221 0.1181 0.5263 0.026 Uiso 1 1 calc R . . C16 C 0.47400(14) 0.17878(14) 0.51235(13) 0.0211(3) Uani 1 1 d . . . H16 H 0.4647 0.1649 0.5771 0.025 Uiso 1 1 calc R . . C17 C 0.39377(13) 0.22652(13) 0.44795(12) 0.0162(3) Uani 1 1 d . . . H17 H 0.3298 0.2454 0.4688 0.019 Uiso 1 1 calc R . . C18 C 0.31890(12) 0.30140(12) 0.14196(11) 0.0126(2) Uani 1 1 d . . . C19 C 0.22470(12) 0.22620(12) 0.03932(11) 0.0134(2) Uani 1 1 d . . . H19 H 0.1516 0.1746 0.0378 0.016 Uiso 1 1 calc R . . C20 C 0.23813(13) 0.22705(13) -0.06048(12) 0.0168(3) Uani 1 1 d . . . H20 H 0.1732 0.1772 -0.1303 0.020 Uiso 1 1 calc R . . C21 C 0.34583(14) 0.30025(13) -0.05863(12) 0.0182(3) Uani 1 1 d . . . H21 H 0.3546 0.3006 -0.1271 0.022 Uiso 1 1 calc R . . C22 C 0.44113(13) 0.37320(13) 0.04361(13) 0.0178(3) Uani 1 1 d . . . H22 H 0.5157 0.4218 0.0449 0.021 Uiso 1 1 calc R . . C23 C 0.42751(12) 0.37509(13) 0.14362(12) 0.0157(2) Uani 1 1 d . . . H23 H 0.4919 0.4264 0.2131 0.019 Uiso 1 1 calc R . . C24 C -0.21825(12) 0.16158(12) 0.11910(11) 0.0127(2) Uani 1 1 d . . . C25 C -0.21510(13) 0.08181(13) 0.02750(12) 0.0158(3) Uani 1 1 d . . . H25 H -0.1422 0.0599 0.0346 0.019 Uiso 1 1 calc R . . C26 C -0.31814(13) 0.03421(13) -0.07419(13) 0.0183(3) Uani 1 1 d . . . H26 H -0.3153 -0.0199 -0.1364 0.022 Uiso 1 1 calc R . . C27 C -0.42499(13) 0.06540(13) -0.08526(13) 0.0192(3) Uani 1 1 d . . . H27 H -0.4953 0.0327 -0.1549 0.023 Uiso 1 1 calc R . . C28 C -0.42916(13) 0.14423(13) 0.00534(14) 0.0200(3) Uani 1 1 d . . . H28 H -0.5027 0.1652 -0.0024 0.024 Uiso 1 1 calc R . . C29 C -0.32689(13) 0.19295(13) 0.10740(13) 0.0168(3) Uani 1 1 d . . . H29 H -0.3303 0.2473 0.1691 0.020 Uiso 1 1 calc R . . C30 C -0.12608(12) 0.13286(12) 0.33673(11) 0.0125(2) Uani 1 1 d . . . C31 C -0.21278(13) 0.01905(12) 0.28590(12) 0.0157(2) Uani 1 1 d . . . H31 H -0.2557 -0.0114 0.2065 0.019 Uiso 1 1 calc R . . C32 C -0.23621(15) -0.04977(13) 0.35183(14) 0.0213(3) Uani 1 1 d . . . H32 H -0.2949 -0.1274 0.3172 0.026 Uiso 1 1 calc R . . C33 C -0.17443(15) -0.00561(14) 0.46756(14) 0.0233(3) Uani 1 1 d . . . H33 H -0.1908 -0.0528 0.5122 0.028 Uiso 1 1 calc R . . C34 C -0.08859(15) 0.10770(15) 0.51834(14) 0.0241(3) Uani 1 1 d . . . H34 H -0.0465 0.1382 0.5978 0.029 Uiso 1 1 calc R . . C35 C -0.06397(13) 0.17679(14) 0.45326(12) 0.0189(3) Uani 1 1 d . . . H35 H -0.0047 0.2541 0.4883 0.023 Uiso 1 1 calc R . . I2 I 0.258638(8) 0.391185(8) 0.661343(7) 0.01570(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00999(7) 0.00869(7) 0.01060(7) 0.00336(6) 0.00523(6) 0.00235(5) I1 0.01229(4) 0.00976(3) 0.01890(4) 0.00370(3) 0.00711(3) 0.00339(3) Br1 0.02148(8) 0.03850(10) 0.03077(9) 0.02562(8) -0.00646(7) -0.00799(7) P1 0.00961(13) 0.01185(14) 0.01003(15) 0.00406(12) 0.00358(11) 0.00146(11) P2 0.01211(14) 0.01052(14) 0.01284(15) 0.00502(12) 0.00747(12) 0.00437(11) N1 0.0148(5) 0.0104(5) 0.0104(5) 0.0042(4) 0.0052(4) 0.0030(4) C1 0.0132(5) 0.0125(5) 0.0125(6) 0.0047(5) 0.0016(4) 0.0000(4) C2 0.0166(6) 0.0129(6) 0.0099(6) 0.0026(5) 0.0026(5) 0.0014(5) C3 0.0220(6) 0.0120(6) 0.0150(6) 0.0032(5) 0.0113(5) 0.0070(5) C4 0.0196(6) 0.0127(6) 0.0195(7) 0.0071(5) 0.0132(5) 0.0080(5) C5 0.0161(6) 0.0135(6) 0.0146(6) 0.0078(5) 0.0048(5) 0.0024(5) C6 0.0140(5) 0.0129(5) 0.0130(6) 0.0066(5) 0.0067(5) 0.0042(4) C7 0.0208(6) 0.0175(6) 0.0161(6) 0.0079(5) 0.0091(5) 0.0086(5) C8 0.0262(7) 0.0193(7) 0.0134(6) 0.0059(5) 0.0070(6) 0.0020(6) C9 0.0148(6) 0.0245(7) 0.0208(7) 0.0157(6) 0.0013(5) -0.0007(5) C10 0.0159(6) 0.0239(7) 0.0299(8) 0.0165(6) 0.0094(6) 0.0085(6) C11 0.0195(6) 0.0160(6) 0.0194(7) 0.0077(5) 0.0095(5) 0.0071(5) C12 0.0113(5) 0.0121(5) 0.0117(6) 0.0037(4) 0.0036(4) 0.0019(4) C13 0.0153(6) 0.0225(7) 0.0168(7) 0.0079(5) 0.0079(5) 0.0069(5) C14 0.0170(6) 0.0257(7) 0.0240(8) 0.0077(6) 0.0078(6) 0.0110(6) C15 0.0197(7) 0.0199(7) 0.0229(8) 0.0090(6) 0.0027(6) 0.0091(6) C16 0.0244(7) 0.0233(7) 0.0156(7) 0.0100(6) 0.0059(6) 0.0070(6) C17 0.0178(6) 0.0182(6) 0.0141(6) 0.0069(5) 0.0070(5) 0.0059(5) C18 0.0108(5) 0.0144(6) 0.0121(6) 0.0056(5) 0.0041(4) 0.0025(4) C19 0.0118(5) 0.0151(6) 0.0127(6) 0.0039(5) 0.0044(4) 0.0046(5) C20 0.0190(6) 0.0195(6) 0.0120(6) 0.0046(5) 0.0049(5) 0.0088(5) C21 0.0241(7) 0.0247(7) 0.0158(7) 0.0114(6) 0.0127(6) 0.0144(6) C22 0.0171(6) 0.0219(7) 0.0225(7) 0.0132(6) 0.0124(5) 0.0081(5) C23 0.0126(5) 0.0185(6) 0.0153(6) 0.0070(5) 0.0053(5) 0.0025(5) C24 0.0120(5) 0.0138(6) 0.0145(6) 0.0069(5) 0.0064(5) 0.0043(4) C25 0.0127(5) 0.0187(6) 0.0180(7) 0.0064(5) 0.0070(5) 0.0071(5) C26 0.0175(6) 0.0193(7) 0.0163(7) 0.0050(5) 0.0060(5) 0.0044(5) C27 0.0140(6) 0.0196(7) 0.0213(7) 0.0092(6) 0.0035(5) 0.0030(5) C28 0.0135(6) 0.0207(7) 0.0292(8) 0.0126(6) 0.0082(6) 0.0076(5) C29 0.0160(6) 0.0175(6) 0.0218(7) 0.0084(5) 0.0105(5) 0.0081(5) C30 0.0130(5) 0.0139(6) 0.0157(6) 0.0076(5) 0.0089(5) 0.0063(4) C31 0.0192(6) 0.0135(6) 0.0175(7) 0.0056(5) 0.0108(5) 0.0050(5) C32 0.0238(7) 0.0161(6) 0.0292(8) 0.0109(6) 0.0154(6) 0.0049(6) C33 0.0246(7) 0.0270(8) 0.0288(8) 0.0200(7) 0.0150(7) 0.0100(6) C34 0.0233(7) 0.0322(8) 0.0180(7) 0.0138(6) 0.0076(6) 0.0057(6) C35 0.0169(6) 0.0217(7) 0.0176(7) 0.0096(6) 0.0064(5) 0.0027(5) I2 0.01677(4) 0.01600(4) 0.01248(4) 0.00501(3) 0.00399(3) 0.00403(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9887(11) . yes Ni1 P2 2.2039(4) . yes Ni1 P1 2.2062(4) . yes Ni1 I1 2.4871(3) . yes Br1 C9 1.8995(14) . ? P1 C18 1.8135(14) . ? P1 C12 1.8194(13) . ? P1 C1 1.8456(14) . ? P2 C24 1.8126(14) . ? P2 C30 1.8140(14) . ? P2 C4 1.8398(13) . ? N1 C3 1.5079(17) . ? N1 C2 1.5161(17) . ? N1 C5 1.5155(17) . ? C1 C2 1.529(2) . ? C3 C4 1.521(2) . ? C5 C6 1.5042(19) . ? C6 C7 1.3939(19) . ? C6 C11 1.3957(18) . ? C7 C8 1.389(2) . ? C8 C9 1.381(2) . ? C9 C10 1.383(2) . ? C10 C11 1.381(2) . ? C12 C13 1.3924(18) . ? C12 C17 1.396(2) . ? C13 C14 1.394(2) . ? C14 C15 1.384(2) . ? C15 C16 1.387(2) . ? C16 C17 1.389(2) . ? C18 C23 1.3988(19) . ? C18 C19 1.3975(19) . ? C19 C20 1.390(2) . ? C20 C21 1.387(2) . ? C21 C22 1.392(2) . ? C22 C23 1.387(2) . ? C24 C25 1.3937(19) . ? C24 C29 1.4054(18) . ? C25 C26 1.390(2) . ? C26 C27 1.385(2) . ? C27 C28 1.384(2) . ? C28 C29 1.388(2) . ? C30 C35 1.393(2) . ? C30 C31 1.3954(19) . ? C31 C32 1.393(2) . ? C32 C33 1.384(2) . ? C33 C34 1.387(2) . ? C34 C35 1.390(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P2 88.80(3) . . yes N1 Ni1 P1 87.18(3) . . yes P2 Ni1 P1 175.916(15) . . yes N1 Ni1 I1 174.92(3) . . yes P2 Ni1 I1 92.165(11) . . yes P1 Ni1 I1 91.784(11) . . yes C18 P1 C12 107.95(6) . . ? C18 P1 C1 105.17(6) . . ? C12 P1 C1 105.37(6) . . ? C18 P1 Ni1 116.12(4) . . ? C12 P1 Ni1 118.77(5) . . ? C1 P1 Ni1 101.78(4) . . ? C24 P2 C30 104.86(6) . . ? C24 P2 C4 106.12(6) . . ? C30 P2 C4 106.37(6) . . ? C24 P2 Ni1 120.00(5) . . ? C30 P2 Ni1 116.72(4) . . ? C4 P2 Ni1 101.51(5) . . ? C3 N1 C2 105.81(10) . . ? C3 N1 C5 111.70(10) . . ? C2 N1 C5 106.43(10) . . ? C3 N1 Ni1 111.10(8) . . ? C2 N1 Ni1 108.38(8) . . ? C5 N1 Ni1 112.99(8) . . ? C2 C1 P1 106.72(9) . . ? N1 C2 C1 111.72(10) . . ? N1 C3 C4 114.28(11) . . ? C3 C4 P2 108.76(9) . . ? C6 C5 N1 117.84(11) . . ? C7 C6 C11 118.61(13) . . ? C7 C6 C5 120.57(12) . . ? C11 C6 C5 120.62(12) . . ? C8 C7 C6 121.04(13) . . ? C9 C8 C7 118.67(14) . . ? C8 C9 C10 121.64(14) . . ? C8 C9 Br1 120.36(12) . . ? C10 C9 Br1 117.99(11) . . ? C11 C10 C9 119.08(13) . . ? C10 C11 C6 120.93(13) . . ? C13 C12 C17 119.59(12) . . ? C13 C12 P1 122.80(11) . . ? C17 C12 P1 117.61(10) . . ? C12 C13 C14 119.93(14) . . ? C15 C14 C13 120.28(13) . . ? C14 C15 C16 119.91(13) . . ? C15 C16 C17 120.22(14) . . ? C16 C17 C12 120.06(13) . . ? C23 C18 C19 119.68(13) . . ? C23 C18 P1 119.46(10) . . ? C19 C18 P1 120.79(10) . . ? C20 C19 C18 119.90(13) . . ? C21 C20 C19 120.31(13) . . ? C20 C21 C22 119.93(13) . . ? C23 C22 C21 120.23(14) . . ? C22 C23 C18 119.92(13) . . ? C25 C24 C29 119.21(12) . . ? C25 C24 P2 121.09(10) . . ? C29 C24 P2 119.68(10) . . ? C26 C25 C24 120.30(12) . . ? C27 C26 C25 120.26(13) . . ? C26 C27 C28 119.86(14) . . ? C27 C28 C29 120.61(13) . . ? C28 C29 C24 119.76(13) . . ? C35 C30 C31 119.55(13) . . ? C35 C30 P2 119.14(10) . . ? C31 C30 P2 121.23(11) . . ? C32 C31 C30 119.87(14) . . ? C33 C32 C31 120.34(14) . . ? C32 C33 C34 119.91(15) . . ? C33 C34 C35 120.20(15) . . ? C34 C35 C30 120.13(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 41.90 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 5.994 _refine_diff_density_min -6.087 _refine_diff_density_rms 0.146 #===END data_dqc07 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 Co I2 N P2' _chemical_formula_sum 'C35 H35 Co I2 N P2' _chemical_formula_weight 844.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.1550(6) _cell_length_b 13.1354(5) _cell_length_c 36.1275(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.612(2) _cell_angle_gamma 90.00 _cell_volume 6622.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9747 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 41.54 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3320 _exptl_absorpt_coefficient_mu 2.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6654 _exptl_absorpt_correction_T_max 0.7485 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 17 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 151325 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -68 _diffrn_reflns_limit_l_max 69 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 43.38 _reflns_number_total 43586 _reflns_number_gt 39771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.012(5) _refine_ls_number_reflns 43586 _refine_ls_number_parameters 857 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0588 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.372 _refine_ls_restrained_S_all 1.371 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.223284(14) 0.394434(16) 0.413460(6) 0.01140(3) Uani 1 1 d . . . I1 I 0.052513(7) 0.326289(8) 0.409665(3) 0.01564(2) Uani 1 1 d . . . I2 I 0.335615(8) 0.365491(9) 0.475906(3) 0.01784(2) Uani 1 1 d . . . P1A P 0.30485(3) 0.29769(3) 0.373972(11) 0.01146(6) Uani 1 1 d . . . P2A P 0.22487(3) 0.57309(3) 0.404758(11) 0.01196(6) Uani 1 1 d . . . N1A N 0.39302(9) 0.51344(10) 0.36074(4) 0.0134(2) Uani 1 1 d . . . C1A C 0.45025(11) 0.42431(13) 0.35411(5) 0.0149(3) Uani 1 1 d . . . H1A1 H 0.5176 0.4419 0.3603 0.018 Uiso 1 1 calc R . . H1A2 H 0.4371 0.4077 0.3276 0.018 Uiso 1 1 calc R . . C2A C 0.43163(10) 0.32986(13) 0.37655(5) 0.0146(2) Uani 1 1 d . . . H2A1 H 0.4595 0.3406 0.4027 0.018 Uiso 1 1 calc R . . H2A2 H 0.4642 0.2723 0.3675 0.018 Uiso 1 1 calc R . . C3A C 0.42077(10) 0.55112(13) 0.39933(4) 0.0147(2) Uani 1 1 d . . . H3A1 H 0.4821 0.5854 0.4014 0.018 Uiso 1 1 calc R . . H3A2 H 0.4288 0.4935 0.4164 0.018 Uiso 1 1 calc R . . C4A C 0.34787(10) 0.62448(12) 0.41146(4) 0.0145(2) Uani 1 1 d . . . H4A1 H 0.3478 0.6871 0.3972 0.017 Uiso 1 1 calc R . . H4A2 H 0.3677 0.6410 0.4378 0.017 Uiso 1 1 calc R . . C5A C 0.25610(11) 0.28239(12) 0.32465(4) 0.0133(2) Uani 1 1 d . . . C6A C 0.16030(11) 0.30622(15) 0.31163(5) 0.0186(3) Uani 1 1 d . . . H6A H 0.1223 0.3317 0.3281 0.022 Uiso 1 1 calc R . . C7A C 0.12143(12) 0.29199(17) 0.27404(5) 0.0232(4) Uani 1 1 d . . . H7A H 0.0574 0.3076 0.2656 0.028 Uiso 1 1 calc R . . C8A C 0.17752(13) 0.25466(15) 0.24918(5) 0.0211(3) Uani 1 1 d . . . H8A H 0.1513 0.2454 0.2240 0.025 Uiso 1 1 calc R . . C9A C 0.27270(14) 0.23117(15) 0.26187(5) 0.0205(3) Uani 1 1 d . . . H9A H 0.3104 0.2060 0.2452 0.025 Uiso 1 1 calc R . . C10A C 0.31230(11) 0.24494(14) 0.29942(5) 0.0174(3) Uani 1 1 d . . . H10A H 0.3764 0.2292 0.3077 0.021 Uiso 1 1 calc R . . C11A C 0.30885(10) 0.16919(11) 0.39302(4) 0.0123(2) Uani 1 1 d . . . C12A C 0.39051(11) 0.13184(13) 0.41647(5) 0.0177(3) Uani 1 1 d . . . H12A H 0.4461 0.1708 0.4208 0.021 Uiso 1 1 calc R . . C13A C 0.38865(12) 0.03681(14) 0.43329(5) 0.0200(3) Uani 1 1 d . . . H13A H 0.4433 0.0123 0.4486 0.024 Uiso 1 1 calc R . . C14A C 0.30608(13) -0.02170(14) 0.42737(5) 0.0201(3) Uani 1 1 d . . . H14A H 0.3052 -0.0851 0.4388 0.024 Uiso 1 1 calc R . . C15A C 0.22460(12) 0.01462(14) 0.40431(5) 0.0200(3) Uani 1 1 d . . . H15A H 0.1689 -0.0242 0.4005 0.024 Uiso 1 1 calc R . . C16A C 0.22624(11) 0.10916(13) 0.38697(5) 0.0157(3) Uani 1 1 d . . . H16A H 0.1718 0.1325 0.3712 0.019 Uiso 1 1 calc R . . C17A C 0.16161(11) 0.62227(12) 0.36024(4) 0.0140(2) Uani 1 1 d . . . C18A C 0.18361(12) 0.71558(13) 0.34489(5) 0.0177(3) Uani 1 1 d . . . H18A H 0.2337 0.7549 0.3573 0.021 Uiso 1 1 calc R . . C19A C 0.13125(12) 0.74976(15) 0.31132(5) 0.0211(3) Uani 1 1 d . . . H19A H 0.1461 0.8119 0.3014 0.025 Uiso 1 1 calc R . . C20A C 0.05635(12) 0.69094(16) 0.29250(5) 0.0219(3) Uani 1 1 d . . . H20A H 0.0215 0.7136 0.2699 0.026 Uiso 1 1 calc R . . C21A C 0.03369(12) 0.59853(15) 0.30750(5) 0.0198(3) Uani 1 1 d . . . H21A H -0.0161 0.5592 0.2949 0.024 Uiso 1 1 calc R . . C22A C 0.08537(11) 0.56481(13) 0.34136(5) 0.0162(3) Uani 1 1 d . . . H22A H 0.0691 0.5035 0.3516 0.019 Uiso 1 1 calc R . . C23A C 0.17181(11) 0.64329(12) 0.43983(4) 0.0144(2) Uani 1 1 d . . . C24A C 0.16044(14) 0.74910(14) 0.43747(5) 0.0210(3) Uani 1 1 d . . . H24A H 0.1770 0.7841 0.4171 0.025 Uiso 1 1 calc R . . C25A C 0.12460(15) 0.80212(15) 0.46531(6) 0.0255(4) Uani 1 1 d . . . H25A H 0.1179 0.8725 0.4637 0.031 Uiso 1 1 calc R . . C26A C 0.09875(14) 0.75026(17) 0.49551(6) 0.0251(4) Uani 1 1 d . . . H26A H 0.0750 0.7860 0.5142 0.030 Uiso 1 1 calc R . . C27A C 0.10816(14) 0.64540(16) 0.49794(5) 0.0235(3) Uani 1 1 d . . . H27A H 0.0899 0.6108 0.5181 0.028 Uiso 1 1 calc R . . C28A C 0.14502(13) 0.59163(14) 0.47026(5) 0.0191(3) Uani 1 1 d . . . H28A H 0.1518 0.5213 0.4721 0.023 Uiso 1 1 calc R . . C29A C 0.40759(11) 0.59489(13) 0.33373(5) 0.0156(3) Uani 1 1 d . . . H29A H 0.4747 0.6142 0.3377 0.019 Uiso 1 1 calc R . . H29B H 0.3705 0.6543 0.3382 0.019 Uiso 1 1 calc R . . C30A C 0.37770(11) 0.55996(13) 0.29375(5) 0.0160(3) Uani 1 1 d . . . C31A C 0.44511(12) 0.54262(15) 0.27069(5) 0.0205(3) Uani 1 1 d . . . H31A H 0.5090 0.5592 0.2791 0.025 Uiso 1 1 calc R . . C32A C 0.41824(14) 0.50062(17) 0.23504(5) 0.0242(3) Uani 1 1 d . . . H32A H 0.4642 0.4881 0.2200 0.029 Uiso 1 1 calc R . . C33A C 0.32259(14) 0.47758(15) 0.22213(5) 0.0233(3) Uani 1 1 d . . . H33A H 0.3044 0.4488 0.1985 0.028 Uiso 1 1 calc R . . C34A C 0.25445(12) 0.49752(14) 0.24454(5) 0.0206(3) Uani 1 1 d . . . H34A H 0.1902 0.4839 0.2356 0.025 Uiso 1 1 calc R . . C35A C 0.28140(12) 0.53762(14) 0.28020(5) 0.0180(3) Uani 1 1 d . . . H35A H 0.2353 0.5498 0.2952 0.022 Uiso 1 1 calc R . . Co2 Co 0.309254(18) 0.90885(2) 0.144723(7) 0.01145(5) Uani 0.8057(5) 1 d P A 1 I3 I 0.245014(9) 1.089821(12) 0.156112(4) 0.01519(3) Uani 0.8057(5) 1 d P A 1 I4 I 0.48938(3) 0.94171(3) 0.184814(8) 0.01709(4) Uani 0.8057(5) 1 d P A 1 P1B P 0.24778(3) 0.84711(4) 0.191905(12) 0.01552(7) Uani 1 1 d . . . P2B P 0.33885(3) 0.93573(4) 0.087001(12) 0.01601(7) Uani 1 1 d . . . N1B N 0.33386(11) 0.75761(13) 0.13252(5) 0.0138(3) Uani 0.8057(5) 1 d P A 1 C1B C 0.36080(14) 0.69895(16) 0.16844(5) 0.0155(3) Uani 0.8057(5) 1 d P A 1 H1B1 H 0.3664 0.6272 0.1628 0.019 Uiso 0.8057(5) 1 calc PR A 1 H1B2 H 0.4225 0.7223 0.1815 0.019 Uiso 0.8057(5) 1 calc PR A 1 C2B C 0.28686(15) 0.71310(15) 0.19307(5) 0.0236(3) Uani 1 1 d . A . H2B1 H 0.3134 0.6939 0.2186 0.028 Uiso 0.8057(5) 1 calc PR A 1 H2B2 H 0.2323 0.6695 0.1845 0.028 Uiso 0.8057(5) 1 calc PR A 1 H2B3 H 0.3542 0.7095 0.2040 0.028 Uiso 0.1943(5) 1 calc PR A 2 H2B4 H 0.2512 0.6747 0.2090 0.028 Uiso 0.1943(5) 1 calc PR A 2 C3B C 0.41719(16) 0.75072(19) 0.11230(6) 0.0165(3) Uani 0.8057(5) 1 d P A 1 H3B1 H 0.4251 0.6807 0.1048 0.020 Uiso 0.8057(5) 1 calc PR A 1 H3B2 H 0.4750 0.7710 0.1290 0.020 Uiso 0.8057(5) 1 calc PR A 1 C4B C 0.40354(14) 0.81783(15) 0.07802(5) 0.0233(3) Uani 1 1 d . A . H4B1 H 0.3673 0.7815 0.0569 0.028 Uiso 0.8057(5) 1 calc PR A 1 H4B2 H 0.4655 0.8353 0.0717 0.028 Uiso 0.8057(5) 1 calc PR A 1 H4B3 H 0.3801 0.7916 0.0531 0.028 Uiso 0.1943(5) 1 calc PR A 2 H4B4 H 0.4718 0.8303 0.0804 0.028 Uiso 0.1943(5) 1 calc PR A 2 C5B C 0.11725(12) 0.83503(14) 0.18288(5) 0.0186(3) Uani 1 1 d . A . C6B C 0.06053(12) 0.90272(15) 0.15885(5) 0.0204(3) Uani 1 1 d . . . H6B H 0.0890 0.9566 0.1481 0.024 Uiso 1 1 calc R A . C7B C -0.03918(13) 0.88972(16) 0.15085(6) 0.0238(3) Uani 1 1 d . A . H7B H -0.0768 0.9355 0.1352 0.029 Uiso 1 1 calc R . . C8B C -0.08137(13) 0.80879(16) 0.16628(6) 0.0241(4) Uani 1 1 d . . . H8B H -0.1473 0.7993 0.1605 0.029 Uiso 1 1 calc R A . C9B C -0.02615(14) 0.74186(17) 0.19027(6) 0.0255(4) Uani 1 1 d . A . H9B H -0.0551 0.6880 0.2008 0.031 Uiso 1 1 calc R . . C10B C 0.07301(13) 0.75480(16) 0.19873(5) 0.0224(3) Uani 1 1 d . . . H10B H 0.1098 0.7098 0.2150 0.027 Uiso 1 1 calc R A . C11B C 0.27473(12) 0.88819(13) 0.24070(4) 0.0152(3) Uani 1 1 d . A . C12B C 0.35041(12) 0.84462(15) 0.26548(5) 0.0186(3) Uani 1 1 d . . . H12B H 0.3878 0.7943 0.2570 0.022 Uiso 1 1 calc R A . C13B C 0.36995(13) 0.87619(16) 0.30274(5) 0.0218(3) Uani 1 1 d . A . H13B H 0.4201 0.8465 0.3191 0.026 Uiso 1 1 calc R . . C14B C 0.31520(13) 0.95146(15) 0.31565(5) 0.0213(3) Uani 1 1 d . . . H14B H 0.3283 0.9722 0.3406 0.026 Uiso 1 1 calc R A . C15B C 0.24011(14) 0.99601(15) 0.29092(5) 0.0211(3) Uani 1 1 d . A . H15B H 0.2033 1.0468 0.2994 0.025 Uiso 1 1 calc R . . C16B C 0.22022(13) 0.96476(14) 0.25376(5) 0.0184(3) Uani 1 1 d . . . H16B H 0.1703 0.9950 0.2375 0.022 Uiso 1 1 calc R A . C17B C 0.23006(13) 0.93469(14) 0.05148(5) 0.0197(3) Uani 1 1 d . A . C18B C 0.14763(14) 0.98145(15) 0.06000(5) 0.0237(4) Uani 1 1 d . . . H18B H 0.1491 1.0110 0.0835 0.028 Uiso 1 1 calc R A . C19B C 0.06321(15) 0.98459(17) 0.03383(6) 0.0275(4) Uani 1 1 d . A . H19B H 0.0089 1.0164 0.0397 0.033 Uiso 1 1 calc R . . C20B C 0.06136(16) 0.93934(16) -0.00132(6) 0.0283(4) Uani 1 1 d . . . H20B H 0.0053 0.9409 -0.0189 0.034 Uiso 1 1 calc R A . C21B C 0.14151(18) 0.89266(16) -0.01010(5) 0.0288(4) Uani 1 1 d . A . H21B H 0.1395 0.8624 -0.0335 0.035 Uiso 1 1 calc R . . C22B C 0.22603(16) 0.89068(16) 0.01608(5) 0.0250(4) Uani 1 1 d . . . H22B H 0.2803 0.8597 0.0099 0.030 Uiso 1 1 calc R A . C23B C 0.40920(14) 1.03819(15) 0.07088(5) 0.0207(3) Uani 1 1 d . A . C24B C 0.43690(19) 1.0340(2) 0.03566(6) 0.0347(5) Uani 1 1 d . . . H24B H 0.4206 0.9779 0.0202 0.042 Uiso 1 1 calc R A . C25B C 0.4894(2) 1.1143(2) 0.02349(7) 0.0429(7) Uani 1 1 d . A . H25B H 0.5065 1.1116 -0.0002 0.051 Uiso 1 1 calc R . . C26B C 0.51597(18) 1.19731(19) 0.04631(7) 0.0339(5) Uani 1 1 d . . . H26B H 0.5512 1.2500 0.0381 0.041 Uiso 1 1 calc R A . C27B C 0.48989(18) 1.20165(19) 0.08150(7) 0.0339(5) Uani 1 1 d . A . H27B H 0.5072 1.2578 0.0968 0.041 Uiso 1 1 calc R . . C28B C 0.43791(16) 1.12269(18) 0.09421(7) 0.0293(4) Uani 1 1 d . . . H28B H 0.4221 1.1257 0.1182 0.035 Uiso 1 1 calc R A . C29B C 0.24356(16) 0.71412(17) 0.10958(6) 0.0152(3) Uani 0.8057(5) 1 d P A 1 H29C H 0.2326 0.7485 0.0855 0.018 Uiso 0.8057(5) 1 calc PR A 1 H29D H 0.1902 0.7308 0.1222 0.018 Uiso 0.8057(5) 1 calc PR A 1 C30B C 0.24149(14) 0.60036(16) 0.10236(6) 0.0159(3) Uani 0.8057(5) 1 d P A 1 C31B C 0.28653(17) 0.55900(19) 0.07417(6) 0.0201(4) Uani 0.8057(5) 1 d P A 1 H31B H 0.3189 0.6016 0.0600 0.024 Uiso 0.8057(5) 1 calc PR A 1 C32B C 0.28347(19) 0.4541(2) 0.06705(7) 0.0241(4) Uani 0.8057(5) 1 d P A 1 H32B H 0.3137 0.4275 0.0482 0.029 Uiso 0.8057(5) 1 calc PR A 1 C33B C 0.2355(2) 0.3902(2) 0.08797(8) 0.0247(5) Uani 0.8057(5) 1 d P A 1 H33B H 0.2345 0.3204 0.0836 0.030 Uiso 0.8057(5) 1 calc PR A 1 C34B C 0.18858(18) 0.4308(2) 0.11559(7) 0.0219(4) Uani 0.8057(5) 1 d P A 1 H34B H 0.1557 0.3881 0.1296 0.026 Uiso 0.8057(5) 1 calc PR A 1 C35B C 0.19098(15) 0.53491(18) 0.12223(6) 0.0187(4) Uani 0.8057(5) 1 d P A 1 H35B H 0.1582 0.5615 0.1403 0.022 Uiso 0.8057(5) 1 calc PR A 1 Co2C Co 0.31837(8) 0.97489(9) 0.15216(3) 0.0139(2) Uani 0.1943(5) 1 d P A 2 I3C I 0.21730(5) 1.13619(6) 0.156003(19) 0.02233(15) Uani 0.1943(5) 1 d P A 2 I4C I 0.49380(18) 0.96274(15) 0.18321(7) 0.0399(5) Uani 0.1943(5) 1 d P A 2 N1C N 0.2839(8) 0.7203(7) 0.1179(2) 0.0226(16) Uani 0.1943(5) 1 d P A 2 C1C C 0.2724(13) 0.6642(10) 0.1540(4) 0.045(4) Uani 0.1943(5) 1 d P A 2 H1C1 H 0.2080 0.6364 0.1499 0.054 Uiso 0.1943(5) 1 calc PR A 2 H1C2 H 0.3156 0.6064 0.1559 0.054 Uiso 0.1943(5) 1 calc PR A 2 C3C C 0.3786(9) 0.7311(9) 0.1131(3) 0.028(2) Uani 0.1943(5) 1 d P A 2 H3C1 H 0.4021 0.6646 0.1073 0.033 Uiso 0.1943(5) 1 calc PR A 2 H3C2 H 0.4155 0.7523 0.1369 0.033 Uiso 0.1943(5) 1 calc PR A 2 C29C C 0.2187(8) 0.6633(8) 0.0886(4) 0.031(2) Uani 0.1943(5) 1 d P A 2 H29E H 0.1535 0.6760 0.0924 0.037 Uiso 0.1943(5) 1 calc PR A 2 H29F H 0.2252 0.6917 0.0644 0.037 Uiso 0.1943(5) 1 calc PR A 2 C30C C 0.2317(8) 0.5532(9) 0.0868(3) 0.0262(19) Uani 0.1943(5) 1 d P A 2 C31C C 0.2952(9) 0.5065(10) 0.0676(3) 0.029(2) Uani 0.1943(5) 1 d P A 2 H31C H 0.3313 0.5487 0.0547 0.034 Uiso 0.1943(5) 1 calc PR A 2 C32C C 0.3117(11) 0.4013(9) 0.0655(4) 0.033(2) Uani 0.1943(5) 1 d P A 2 H32C H 0.3563 0.3751 0.0518 0.040 Uiso 0.1943(5) 1 calc PR A 2 C33C C 0.2584(11) 0.3390(11) 0.0846(4) 0.041(4) Uani 0.1943(5) 1 d P A 2 H33C H 0.2680 0.2690 0.0848 0.050 Uiso 0.1943(5) 1 calc PR A 2 C34C C 0.1903(11) 0.3809(11) 0.1037(4) 0.035(3) Uani 0.1943(5) 1 d P A 2 H34C H 0.1520 0.3385 0.1155 0.042 Uiso 0.1943(5) 1 calc PR A 2 C35C C 0.1793(10) 0.4832(10) 0.1051(5) 0.041(3) Uani 0.1943(5) 1 d P A 2 H35C H 0.1347 0.5088 0.1189 0.050 Uiso 0.1943(5) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01171(7) 0.00989(8) 0.01259(8) -0.00001(6) 0.00201(6) -0.00053(6) I1 0.01317(3) 0.01505(4) 0.01936(4) 0.00000(3) 0.00459(3) -0.00254(3) I2 0.01914(4) 0.02111(5) 0.01231(4) 0.00120(3) -0.00014(3) 0.00075(4) P1A 0.01064(13) 0.01040(15) 0.01299(15) -0.00012(12) 0.00091(11) 0.00062(12) P2A 0.01240(13) 0.00994(16) 0.01345(15) -0.00020(11) 0.00187(11) -0.00067(12) N1A 0.0129(4) 0.0121(5) 0.0150(5) 0.0015(4) 0.0018(4) -0.0001(4) C1A 0.0130(5) 0.0149(7) 0.0171(6) -0.0008(5) 0.0031(4) -0.0016(5) C2A 0.0112(5) 0.0146(6) 0.0175(6) 0.0002(5) 0.0007(4) -0.0004(5) C3A 0.0125(5) 0.0148(6) 0.0163(6) -0.0002(5) 0.0014(4) -0.0010(5) C4A 0.0128(5) 0.0140(6) 0.0167(6) -0.0015(5) 0.0025(4) -0.0029(5) C5A 0.0143(5) 0.0127(6) 0.0126(6) -0.0004(4) 0.0011(4) 0.0007(5) C6A 0.0126(5) 0.0270(9) 0.0158(6) 0.0000(6) 0.0019(5) 0.0022(6) C7A 0.0160(6) 0.0331(10) 0.0186(7) 0.0031(6) -0.0024(5) -0.0005(6) C8A 0.0251(7) 0.0226(8) 0.0142(6) 0.0003(5) -0.0012(5) -0.0048(6) C9A 0.0269(7) 0.0216(8) 0.0133(6) -0.0026(5) 0.0040(5) -0.0011(6) C10A 0.0160(6) 0.0197(7) 0.0164(6) -0.0035(5) 0.0022(5) 0.0026(5) C11A 0.0147(5) 0.0097(5) 0.0120(5) -0.0008(4) 0.0012(4) 0.0008(5) C12A 0.0144(5) 0.0139(7) 0.0232(7) 0.0027(5) -0.0015(5) 0.0019(5) C13A 0.0191(6) 0.0164(7) 0.0230(8) 0.0036(6) -0.0012(5) 0.0022(6) C14A 0.0222(7) 0.0140(7) 0.0235(8) 0.0041(5) 0.0022(6) 0.0014(6) C15A 0.0171(6) 0.0180(7) 0.0248(8) 0.0019(6) 0.0030(5) -0.0035(6) C16A 0.0136(5) 0.0126(6) 0.0200(7) 0.0007(5) 0.0008(5) 0.0002(5) C17A 0.0140(5) 0.0130(6) 0.0150(6) 0.0022(4) 0.0025(4) 0.0006(5) C18A 0.0176(6) 0.0146(7) 0.0210(7) 0.0039(5) 0.0036(5) -0.0016(5) C19A 0.0191(6) 0.0220(8) 0.0227(8) 0.0104(6) 0.0044(5) 0.0017(6) C20A 0.0171(6) 0.0291(9) 0.0196(7) 0.0098(6) 0.0036(5) 0.0025(6) C21A 0.0141(5) 0.0246(8) 0.0198(7) 0.0039(6) -0.0001(5) -0.0013(6) C22A 0.0147(5) 0.0158(7) 0.0179(7) 0.0021(5) 0.0024(5) -0.0013(5) C23A 0.0144(5) 0.0131(6) 0.0155(6) -0.0010(5) 0.0018(4) 0.0004(5) C24A 0.0263(7) 0.0146(7) 0.0231(8) -0.0007(6) 0.0075(6) 0.0013(6) C25A 0.0312(9) 0.0157(8) 0.0308(9) -0.0055(7) 0.0085(7) 0.0044(7) C26A 0.0233(7) 0.0292(10) 0.0227(8) -0.0095(7) 0.0029(6) 0.0052(7) C27A 0.0257(8) 0.0261(9) 0.0200(8) -0.0014(6) 0.0076(6) 0.0047(7) C28A 0.0217(7) 0.0189(8) 0.0173(7) -0.0002(5) 0.0049(5) 0.0008(6) C29A 0.0158(5) 0.0143(6) 0.0172(6) 0.0009(5) 0.0040(5) -0.0038(5) C30A 0.0157(5) 0.0153(7) 0.0166(6) 0.0021(5) 0.0020(5) -0.0013(5) C31A 0.0173(6) 0.0251(9) 0.0193(7) 0.0008(6) 0.0040(5) -0.0001(6) C32A 0.0251(7) 0.0302(10) 0.0174(7) -0.0004(6) 0.0042(6) 0.0020(7) C33A 0.0291(8) 0.0211(8) 0.0175(7) -0.0003(6) -0.0024(6) 0.0020(7) C34A 0.0204(7) 0.0157(7) 0.0237(8) 0.0036(6) -0.0020(6) -0.0024(6) C35A 0.0156(6) 0.0179(7) 0.0199(7) 0.0025(5) 0.0013(5) -0.0019(5) Co2 0.01114(9) 0.01286(11) 0.01044(10) -0.00002(8) 0.00208(7) -0.00213(8) I3 0.01474(5) 0.01341(6) 0.01781(5) -0.00267(4) 0.00386(4) -0.00354(5) I4 0.01222(6) 0.02109(12) 0.01644(7) 0.00119(7) -0.00207(5) -0.00305(7) P1B 0.01659(15) 0.01574(18) 0.01382(16) -0.00192(13) 0.00135(12) -0.00259(14) P2B 0.02046(17) 0.01496(18) 0.01222(16) -0.00054(13) 0.00164(13) 0.00038(15) N1B 0.0143(6) 0.0144(7) 0.0129(6) 0.0013(5) 0.0031(5) -0.0002(5) C1B 0.0175(7) 0.0160(8) 0.0130(7) 0.0018(6) 0.0024(6) 0.0000(6) C2B 0.0306(8) 0.0214(8) 0.0179(7) -0.0024(6) 0.0011(6) 0.0030(7) C3B 0.0141(7) 0.0189(10) 0.0172(8) 0.0008(7) 0.0051(6) 0.0011(7) C4B 0.0279(8) 0.0195(8) 0.0227(8) 0.0006(6) 0.0050(6) 0.0047(7) C5B 0.0177(6) 0.0197(7) 0.0177(7) -0.0026(5) 0.0008(5) -0.0060(6) C6B 0.0186(6) 0.0206(8) 0.0215(7) -0.0023(6) 0.0022(5) -0.0043(6) C7B 0.0189(7) 0.0227(9) 0.0277(9) -0.0032(7) -0.0016(6) -0.0020(6) C8B 0.0184(6) 0.0242(9) 0.0291(9) -0.0087(7) 0.0023(6) -0.0091(6) C9B 0.0218(7) 0.0253(9) 0.0296(9) -0.0038(7) 0.0047(6) -0.0101(7) C10B 0.0199(7) 0.0239(9) 0.0231(8) 0.0004(6) 0.0024(6) -0.0056(6) C11B 0.0186(6) 0.0162(7) 0.0113(6) 0.0015(5) 0.0036(4) -0.0042(5) C12B 0.0177(6) 0.0220(8) 0.0160(6) 0.0007(5) 0.0021(5) -0.0005(6) C13B 0.0217(7) 0.0260(9) 0.0167(7) 0.0029(6) 0.0001(5) -0.0041(7) C14B 0.0266(7) 0.0242(8) 0.0128(6) -0.0020(5) 0.0027(5) -0.0086(7) C15B 0.0261(7) 0.0188(8) 0.0188(7) -0.0035(6) 0.0045(6) -0.0036(6) C16B 0.0228(7) 0.0164(7) 0.0155(6) -0.0005(5) 0.0022(5) -0.0020(6) C17B 0.0264(7) 0.0154(7) 0.0154(7) -0.0010(5) -0.0024(5) 0.0016(6) C18B 0.0265(8) 0.0234(9) 0.0180(7) -0.0026(6) -0.0057(6) 0.0028(7) C19B 0.0259(8) 0.0270(10) 0.0260(9) 0.0000(7) -0.0062(7) 0.0034(7) C20B 0.0336(9) 0.0246(9) 0.0213(8) 0.0057(7) -0.0108(7) -0.0085(8) C21B 0.0442(11) 0.0231(9) 0.0151(7) -0.0006(6) -0.0064(7) -0.0079(8) C22B 0.0343(9) 0.0230(9) 0.0156(7) -0.0027(6) -0.0017(6) -0.0004(7) C23B 0.0274(8) 0.0203(8) 0.0163(7) 0.0017(5) 0.0093(6) 0.0006(6) C24B 0.0482(13) 0.0381(13) 0.0219(9) -0.0082(8) 0.0180(9) -0.0170(11) C25B 0.0604(16) 0.0481(15) 0.0262(11) -0.0042(10) 0.0243(11) -0.0240(13) C26B 0.0406(12) 0.0276(11) 0.0367(12) 0.0046(9) 0.0158(9) -0.0080(9) C27B 0.0377(11) 0.0287(11) 0.0390(12) -0.0088(9) 0.0169(9) -0.0117(9) C28B 0.0320(9) 0.0301(11) 0.0295(10) -0.0077(8) 0.0162(8) -0.0077(8) C29B 0.0158(7) 0.0146(8) 0.0153(8) 0.0001(6) 0.0026(6) -0.0021(7) C30B 0.0185(7) 0.0156(8) 0.0128(7) -0.0014(6) 0.0000(6) -0.0024(7) C31B 0.0263(9) 0.0201(10) 0.0142(8) -0.0025(7) 0.0045(7) -0.0038(8) C32B 0.0304(11) 0.0191(11) 0.0227(10) -0.0067(8) 0.0042(8) -0.0010(10) C33B 0.0293(11) 0.0165(10) 0.0265(11) -0.0035(8) -0.0009(9) -0.0026(9) C34B 0.0265(10) 0.0191(10) 0.0191(9) 0.0006(8) 0.0009(7) -0.0074(9) C35B 0.0213(8) 0.0194(9) 0.0155(8) -0.0005(6) 0.0034(6) -0.0055(7) Co2C 0.0196(5) 0.0130(5) 0.0092(4) -0.0002(3) 0.0022(3) -0.0016(4) I3C 0.0209(2) 0.0187(3) 0.0269(3) -0.0109(2) 0.0028(2) 0.0012(2) I4C 0.0271(6) 0.0378(10) 0.0515(7) 0.0150(6) -0.0027(4) 0.0004(6) N1C 0.035(5) 0.020(4) 0.011(3) -0.005(2) 0.000(3) 0.006(4) C1C 0.082(11) 0.028(6) 0.027(6) 0.001(4) 0.015(6) -0.029(7) C3C 0.029(5) 0.023(5) 0.032(5) 0.008(4) 0.007(4) -0.001(4) C29C 0.029(5) 0.015(4) 0.053(7) 0.003(4) 0.021(5) 0.001(4) C30C 0.027(4) 0.025(5) 0.024(5) 0.006(4) -0.001(3) 0.006(4) C31C 0.041(6) 0.021(5) 0.018(4) 0.003(4) -0.012(4) 0.001(5) C32C 0.052(7) 0.017(5) 0.032(6) -0.005(4) 0.008(5) -0.002(5) C33C 0.048(7) 0.028(6) 0.038(7) 0.010(5) -0.021(6) -0.014(6) C34C 0.044(7) 0.034(7) 0.024(5) 0.001(4) -0.007(5) -0.007(5) C35C 0.037(6) 0.021(6) 0.069(10) -0.007(6) 0.020(6) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P1A 2.3523(5) . yes Co1 P2A 2.3683(5) . yes Co1 I1 2.5598(2) . yes Co1 I2 2.5621(2) . yes P1A C5A 1.8113(15) . ? P1A C11A 1.8201(16) . ? P1A C2A 1.8308(15) . ? P2A C17A 1.8235(15) . ? P2A C23A 1.8270(17) . ? P2A C4A 1.8452(15) . ? N1A C1A 1.466(2) . ? N1A C3A 1.470(2) . ? N1A C29A 1.485(2) . ? C1A C2A 1.529(2) . ? C3A C4A 1.529(2) . ? C5A C6A 1.395(2) . ? C5A C10A 1.396(2) . ? C6A C7A 1.390(2) . ? C7A C8A 1.384(3) . ? C8A C9A 1.384(3) . ? C9A C10A 1.390(2) . ? C11A C16A 1.397(2) . ? C11A C12A 1.403(2) . ? C12A C13A 1.390(2) . ? C13A C14A 1.385(3) . ? C14A C15A 1.389(2) . ? C15A C16A 1.393(2) . ? C17A C22A 1.398(2) . ? C17A C18A 1.402(2) . ? C18A C19A 1.386(2) . ? C19A C20A 1.394(3) . ? C20A C21A 1.389(3) . ? C21A C22A 1.389(2) . ? C23A C28A 1.397(2) . ? C23A C24A 1.400(2) . ? C24A C25A 1.387(3) . ? C25A C26A 1.386(3) . ? C26A C27A 1.385(3) . ? C27A C28A 1.395(3) . ? C29A C30A 1.507(2) . ? C30A C31A 1.386(2) . ? C30A C35A 1.400(2) . ? C31A C32A 1.394(3) . ? C32A C33A 1.390(3) . ? C33A C34A 1.384(3) . ? C34A C35A 1.385(3) . ? Co2 N1B 2.0769(18) . yes Co2 P1B 2.1945(5) . yes Co2 P2B 2.2228(5) . yes Co2 I3 2.6023(3) . yes Co2 I4 2.7480(4) . yes P1B C11B 1.8219(16) . ? P1B C5B 1.8287(17) . ? P1B C2B 1.844(2) . ? P1B Co2C 2.5211(13) . ? P2B C23B 1.826(2) . ? P2B C17B 1.8327(17) . ? P2B C4B 1.855(2) . ? P2B Co2C 2.4736(12) . ? N1B C3B 1.491(3) . ? N1B C1B 1.502(2) . ? N1B C29B 1.514(3) . ? C1B C2B 1.494(3) . ? C2B C1C 1.532(13) . ? C3B C4B 1.506(3) . ? C4B C3C 1.782(12) . ? C5B C10B 1.397(3) . ? C5B C6B 1.399(3) . ? C6B C7B 1.403(2) . ? C7B C8B 1.381(3) . ? C8B C9B 1.382(3) . ? C9B C10B 1.396(2) . ? C11B C16B 1.397(3) . ? C11B C12B 1.399(2) . ? C12B C13B 1.391(2) . ? C13B C14B 1.384(3) . ? C14B C15B 1.398(3) . ? C15B C16B 1.387(2) . ? C17B C22B 1.396(3) . ? C17B C18B 1.398(3) . ? C18B C19B 1.395(2) . ? C19B C20B 1.398(3) . ? C20B C21B 1.372(4) . ? C21B C22B 1.396(3) . ? C23B C24B 1.394(3) . ? C23B C28B 1.412(3) . ? C24B C25B 1.403(3) . ? C25B C26B 1.380(4) . ? C26B C27B 1.383(3) . ? C27B C28B 1.393(3) . ? C29B C30B 1.516(3) . ? C30B C35B 1.392(3) . ? C30B C31B 1.398(3) . ? C31B C32B 1.401(4) . ? C32B C33B 1.382(4) . ? C33B C34B 1.394(4) . ? C34B C35B 1.388(3) . ? Co2C P1B 2.5211(13) . yes Co2C P2B 2.4736(12) . yes Co2C N1C 3.5715(90) . yes Co2C I4C 2.553(3) . yes Co2C I3C 2.5731(14) . yes N1C C3C 1.388(16) . yes N1C C29C 1.484(16) . yes N1C C1C 1.532(15) . yes C29C C30C 1.461(15) . ? C30C C31C 1.368(18) . ? C30C C35C 1.413(18) . ? C31C C32C 1.406(17) . ? C32C C33C 1.375(19) . ? C33C C34C 1.39(2) . ? C34C C35C 1.355(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1A Co1 P2A 115.998(17) . . yes P1A Co1 I1 109.471(12) . . yes P2A Co1 I1 111.665(13) . . yes P1A Co1 I2 99.124(12) . . yes P2A Co1 I2 104.222(12) . . yes I1 Co1 I2 115.908(9) . . yes C5A P1A C11A 104.58(7) . . ? C5A P1A C2A 106.55(7) . . ? C11A P1A C2A 103.09(7) . . ? C5A P1A Co1 120.77(5) . . ? C11A P1A Co1 105.02(5) . . ? C2A P1A Co1 114.87(6) . . ? C17A P2A C23A 103.58(7) . . ? C17A P2A C4A 107.44(7) . . ? C23A P2A C4A 102.27(7) . . ? C17A P2A Co1 117.00(5) . . ? C23A P2A Co1 113.20(6) . . ? C4A P2A Co1 112.01(5) . . ? C1A N1A C3A 110.89(12) . . ? C1A N1A C29A 109.06(13) . . ? C3A N1A C29A 109.65(13) . . ? N1A C1A C2A 114.35(13) . . ? C1A C2A P1A 114.50(10) . . ? N1A C3A C4A 113.45(12) . . ? C3A C4A P2A 113.52(11) . . ? C6A C5A C10A 119.13(14) . . ? C6A C5A P1A 119.75(13) . . ? C10A C5A P1A 121.11(11) . . ? C7A C6A C5A 120.23(16) . . ? C8A C7A C6A 120.34(16) . . ? C9A C8A C7A 119.76(16) . . ? C8A C9A C10A 120.39(17) . . ? C9A C10A C5A 120.15(15) . . ? C16A C11A C12A 118.74(14) . . ? C16A C11A P1A 119.47(11) . . ? C12A C11A P1A 121.55(12) . . ? C13A C12A C11A 120.28(15) . . ? C14A C13A C12A 120.50(15) . . ? C13A C14A C15A 119.77(16) . . ? C14A C15A C16A 120.09(16) . . ? C15A C16A C11A 120.61(14) . . ? C22A C17A C18A 118.92(14) . . ? C22A C17A P2A 117.67(12) . . ? C18A C17A P2A 123.37(12) . . ? C19A C18A C17A 120.52(16) . . ? C18A C19A C20A 119.96(17) . . ? C21A C20A C19A 120.03(16) . . ? C20A C21A C22A 120.04(16) . . ? C21A C22A C17A 120.51(16) . . ? C28A C23A C24A 119.12(16) . . ? C28A C23A P2A 119.84(13) . . ? C24A C23A P2A 121.01(13) . . ? C25A C24A C23A 120.42(18) . . ? C26A C25A C24A 120.03(19) . . ? C27A C26A C25A 120.22(18) . . ? C26A C27A C28A 120.11(19) . . ? C27A C28A C23A 120.08(18) . . ? N1A C29A C30A 111.27(13) . . ? C31A C30A C35A 118.90(16) . . ? C31A C30A C29A 120.97(14) . . ? C35A C30A C29A 119.98(15) . . ? C30A C31A C32A 120.73(17) . . ? C33A C32A C31A 119.76(18) . . ? C34A C33A C32A 119.84(17) . . ? C33A C34A C35A 120.37(16) . . ? C34A C35A C30A 120.36(17) . . ? N1B Co2 P1B 85.05(5) . . yes N1B Co2 P2B 83.58(5) . . yes P1B Co2 P2B 161.57(2) . . yes N1B Co2 I3 169.34(5) . . yes P1B Co2 I3 91.170(16) . . yes P2B Co2 I3 97.403(16) . . yes N1B Co2 I4 95.07(5) . . yes P1B Co2 I4 95.853(16) . . yes P2B Co2 I4 99.550(17) . . yes I3 Co2 I4 95.229(12) . . yes C11B P1B C5B 103.91(8) . . ? C11B P1B C2B 104.31(8) . . ? C5B P1B C2B 102.22(9) . . ? C11B P1B Co2 126.58(6) . . ? C5B P1B Co2 114.42(6) . . ? C2B P1B Co2 102.37(7) . . ? C11B P1B Co2C 108.36(6) . . ? C5B P1B Co2C 116.16(7) . . ? C2B P1B Co2C 120.18(8) . . ? Co2 P1B Co2C 20.83(3) . . ? C23B P2B C17B 102.78(9) . . ? C23B P2B C4B 104.36(9) . . ? C17B P2B C4B 104.65(9) . . ? C23B P2B Co2 127.91(6) . . ? C17B P2B Co2 112.82(7) . . ? C4B P2B Co2 101.97(6) . . ? C23B P2B Co2C 107.88(7) . . ? C17B P2B Co2C 116.72(7) . . ? C4B P2B Co2C 118.67(7) . . ? Co2 P2B Co2C 21.52(3) . . ? C3B N1B C1B 106.54(15) . . ? C3B N1B C29B 111.93(16) . . ? C1B N1B C29B 110.41(16) . . ? C3B N1B Co2 109.67(14) . . ? C1B N1B Co2 109.55(12) . . ? C29B N1B Co2 108.72(12) . . ? C2B C1B N1B 110.39(16) . . ? C1B C2B C1C 53.1(7) . . ? C1B C2B P1B 110.03(15) . . ? C1C C2B P1B 112.7(6) . . ? N1B C3B C4B 111.36(17) . . ? C3B C4B C3C 19.1(4) . . ? C3B C4B P2B 110.13(14) . . ? C3C C4B P2B 104.3(4) . . ? C10B C5B C6B 118.95(16) . . ? C10B C5B P1B 120.08(14) . . ? C6B C5B P1B 120.91(14) . . ? C5B C6B C7B 120.26(18) . . ? C8B C7B C6B 119.89(19) . . ? C9B C8B C7B 120.35(17) . . ? C8B C9B C10B 120.18(19) . . ? C9B C10B C5B 120.34(19) . . ? C16B C11B C12B 119.04(15) . . ? C16B C11B P1B 120.13(12) . . ? C12B C11B P1B 120.83(14) . . ? C13B C12B C11B 120.31(17) . . ? C14B C13B C12B 120.43(17) . . ? C13B C14B C15B 119.52(17) . . ? C16B C15B C14B 120.30(18) . . ? C15B C16B C11B 120.38(16) . . ? C22B C17B C18B 118.41(16) . . ? C22B C17B P2B 123.07(15) . . ? C18B C17B P2B 118.51(13) . . ? C19B C18B C17B 121.05(18) . . ? C18B C19B C20B 119.1(2) . . ? C21B C20B C19B 120.59(17) . . ? C20B C21B C22B 119.98(19) . . ? C21B C22B C17B 120.8(2) . . ? C24B C23B C28B 118.63(19) . . ? C24B C23B P2B 120.90(16) . . ? C28B C23B P2B 120.46(15) . . ? C23B C24B C25B 120.1(2) . . ? C26B C25B C24B 120.8(2) . . ? C25B C26B C27B 119.6(2) . . ? C26B C27B C28B 120.6(2) . . ? C27B C28B C23B 120.3(2) . . ? N1B C29B C30B 117.14(17) . . ? C35B C30B C31B 118.1(2) . . ? C35B C30B C29B 121.1(2) . . ? C31B C30B C29B 120.7(2) . . ? C30B C31B C32B 120.8(2) . . ? C33B C32B C31B 120.0(2) . . ? C32B C33B C34B 119.7(3) . . ? C35B C34B C33B 120.0(2) . . ? C34B C35B C30B 121.3(2) . . ? P2B Co2C P1B 121.61(5) . . yes P2B Co2C I4C 98.35(7) . . yes P1B Co2C I4C 99.04(6) . . yes P2B Co2C I3C 112.16(5) . . yes P1B Co2C I3C 103.93(5) . . yes I4C Co2C I3C 122.44(7) . . yes C3C N1C C29C 117.5(9) . . ? C3C N1C C1C 113.5(10) . . ? C29C N1C C1C 102.9(9) . . ? C2B C1C N1C 124.5(9) . . ? N1C C3C C4B 117.7(8) . . ? C30C C29C N1C 117.7(10) . . ? C31C C30C C35C 112.7(11) . . ? C31C C30C C29C 124.5(11) . . ? C35C C30C C29C 122.9(11) . . ? C30C C31C C32C 126.7(12) . . ? C33C C32C C31C 116.6(14) . . ? C32C C33C C34C 119.9(14) . . ? C35C C34C C33C 120.4(14) . . ? C34C C35C C30C 123.7(14) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 43.38 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.524 _refine_diff_density_min -1.064 _refine_diff_density_rms 0.114 #===END data_dqc08 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H29 Co I2 N P2, C4 H8 O' _chemical_formula_sum 'C36 H37 Co I2 N O P2' _chemical_formula_weight 874.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9884(4) _cell_length_b 11.7808(5) _cell_length_c 15.8303(7) _cell_angle_alpha 101.126(2) _cell_angle_beta 93.187(2) _cell_angle_gamma 103.450(2) _cell_volume 1767.75(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9674 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 44.95 _exptl_crystal_description Block _exptl_crystal_colour Brown/green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 2.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6758 _exptl_absorpt_correction_T_max 0.7494 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 27 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 200055 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 47.91 _reflns_number_total 33282 _reflns_number_gt 25010 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 33282 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 2.236 _refine_ls_restrained_S_all 2.236 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 1.138849(13) 0.376059(11) 0.272351(8) 0.01323(2) Uani 1 1 d . . . I1 I 1.328160(7) 0.331343(7) 0.181356(4) 0.02307(2) Uani 1 1 d . . . I2 I 1.170950(7) 0.587654(5) 0.360345(4) 0.01792(1) Uani 1 1 d . . . P1 P 1.09344(3) 0.26106(2) 0.376340(14) 0.01308(4) Uani 1 1 d . . . P2 P 0.91054(3) 0.33864(2) 0.209816(15) 0.01420(4) Uani 1 1 d . . . N1 N 0.81305(9) 0.23847(8) 0.34557(5) 0.01688(14) Uani 1 1 d . . . C1 C 0.92639(10) 0.27999(9) 0.41491(6) 0.01554(15) Uani 1 1 d . . . H1A H 0.9051 0.2358 0.4603 0.019 Uiso 1 1 calc R . . H1B H 0.9351 0.3638 0.4395 0.019 Uiso 1 1 calc R . . C2 C 0.79444(10) 0.32762(9) 0.29692(6) 0.01768(16) Uani 1 1 d . . . H2A H 0.8121 0.4048 0.3363 0.021 Uiso 1 1 calc R . . H2B H 0.6991 0.3074 0.2715 0.021 Uiso 1 1 calc R . . C3 C 1.06887(11) 0.10052(8) 0.34520(6) 0.01627(15) Uani 1 1 d . . . C4 C 1.00277(17) 0.04187(10) 0.26325(7) 0.0312(3) Uani 1 1 d . . . H4 H 0.9770 0.0856 0.2249 0.037 Uiso 1 1 calc R . . C5 C 0.9752(2) -0.08176(11) 0.23864(8) 0.0394(4) Uani 1 1 d . . . H5 H 0.9275 -0.1207 0.1848 0.047 Uiso 1 1 calc R . . C6 C 1.01852(16) -0.14734(10) 0.29394(8) 0.0305(3) Uani 1 1 d . . . H6 H 1.0025 -0.2298 0.2766 0.037 Uiso 1 1 calc R . . C7 C 1.08581(13) -0.08933(10) 0.37511(7) 0.0234(2) Uani 1 1 d . . . H7 H 1.1154 -0.1330 0.4122 0.028 Uiso 1 1 calc R . . C8 C 1.10926(11) 0.03391(9) 0.40142(6) 0.01856(17) Uani 1 1 d . . . H8 H 1.1520 0.0720 0.4566 0.022 Uiso 1 1 calc R . . C9 C 1.21758(10) 0.30873(8) 0.47144(6) 0.01572(15) Uani 1 1 d . . . C10 C 1.18096(12) 0.32304(11) 0.55575(6) 0.0244(2) Uani 1 1 d . . . H10 H 1.0881 0.3098 0.5654 0.029 Uiso 1 1 calc R . . C11 C 1.28308(14) 0.35708(12) 0.62547(7) 0.0288(2) Uani 1 1 d . . . H11 H 1.2583 0.3670 0.6817 0.035 Uiso 1 1 calc R . . C12 C 1.42126(13) 0.37625(11) 0.61173(7) 0.0272(2) Uani 1 1 d . . . H12 H 1.4892 0.3989 0.6586 0.033 Uiso 1 1 calc R . . C13 C 1.45837(13) 0.36170(13) 0.52795(8) 0.0321(3) Uani 1 1 d . . . H13 H 1.5512 0.3738 0.5185 0.039 Uiso 1 1 calc R . . C14 C 1.35701(12) 0.32904(12) 0.45816(7) 0.0259(2) Uani 1 1 d . . . H14 H 1.3824 0.3206 0.4021 0.031 Uiso 1 1 calc R . . C15 C 0.84495(12) 0.20425(9) 0.12645(6) 0.02071(19) Uani 1 1 d . . . C16 C 0.71633(19) 0.12610(13) 0.12406(9) 0.0443(4) Uani 1 1 d . . . H16 H 0.6592 0.1405 0.1672 0.053 Uiso 1 1 calc R . . C17 C 0.6734(3) 0.02603(15) 0.05664(10) 0.0616(6) Uani 1 1 d . . . H17 H 0.5885 -0.0278 0.0557 0.074 Uiso 1 1 calc R . . C18 C 0.7566(2) 0.00658(13) -0.00868(10) 0.0532(5) Uani 1 1 d . . . H18 H 0.7267 -0.0595 -0.0541 0.064 Uiso 1 1 calc R . . C19 C 0.8831(2) 0.08415(14) -0.00698(9) 0.0463(4) Uani 1 1 d . . . H19 H 0.9383 0.0708 -0.0514 0.056 Uiso 1 1 calc R . . C20 C 0.92909(15) 0.18304(12) 0.06128(7) 0.0300(2) Uani 1 1 d . . . H20 H 1.0158 0.2346 0.0631 0.036 Uiso 1 1 calc R . . C21 C 0.86913(10) 0.45635(8) 0.16208(6) 0.01567(15) Uani 1 1 d . . . C22 C 0.73555(11) 0.47334(10) 0.15687(7) 0.02033(18) Uani 1 1 d . . . H22 H 0.6651 0.4241 0.1787 0.024 Uiso 1 1 calc R . . C23 C 0.70750(12) 0.56391(10) 0.11907(7) 0.02326(19) Uani 1 1 d . . . H23 H 0.6187 0.5760 0.1167 0.028 Uiso 1 1 calc R . . C24 C 0.81133(13) 0.63605(10) 0.08493(7) 0.0231(2) Uani 1 1 d . . . H24 H 0.7922 0.6959 0.0592 0.028 Uiso 1 1 calc R . . C25 C 0.94370(13) 0.61861(10) 0.08925(7) 0.0249(2) Uani 1 1 d . . . H25 H 1.0133 0.6665 0.0658 0.030 Uiso 1 1 calc R . . C26 C 0.97331(11) 0.52992(10) 0.12841(7) 0.02058(18) Uani 1 1 d . . . H26 H 1.0629 0.5198 0.1321 0.025 Uiso 1 1 calc R . . C27 C 0.69816(10) 0.14684(9) 0.35606(6) 0.01667(16) Uani 1 1 d . . . C28 C 0.72124(12) 0.05143(10) 0.39059(7) 0.02131(18) Uani 1 1 d . . . H28 H 0.8115 0.0486 0.4060 0.026 Uiso 1 1 calc R . . C29 C 0.61124(13) -0.03926(10) 0.40221(7) 0.0247(2) Uani 1 1 d . . . H29 H 0.6287 -0.1009 0.4265 0.030 Uiso 1 1 calc R . . C30 C 0.47628(13) -0.03884(11) 0.37799(8) 0.0269(2) Uani 1 1 d . . . H30 H 0.4029 -0.0996 0.3858 0.032 Uiso 1 1 calc R . . C31 C 0.45242(12) 0.05362(12) 0.34187(8) 0.0280(2) Uani 1 1 d . . . H31 H 0.3621 0.0538 0.3243 0.034 Uiso 1 1 calc R . . C32 C 0.56139(11) 0.14662(11) 0.33137(7) 0.02320(19) Uani 1 1 d . . . H32 H 0.5430 0.2086 0.3079 0.028 Uiso 1 1 calc R . . O40 O 0.43774(10) 0.22909(8) 0.90384(6) 0.03130(18) Uani 1 1 d . . . C41 C 0.49596(19) 0.19929(15) 0.82468(9) 0.0416(3) Uani 1 1 d . . . H41A H 0.4682 0.2419 0.7828 0.050 Uiso 1 1 calc R . . H41B H 0.4649 0.1142 0.8006 0.050 Uiso 1 1 calc R . . C42 C 0.6520(2) 0.23563(19) 0.84625(11) 0.0503(4) Uani 1 1 d . . . H42A H 0.6865 0.1705 0.8606 0.060 Uiso 1 1 calc R . . H42B H 0.6982 0.2620 0.7986 0.060 Uiso 1 1 calc R . . C43 C 0.67106(17) 0.33792(17) 0.92434(10) 0.0437(4) Uani 1 1 d . . . H43A H 0.7555 0.3465 0.9610 0.052 Uiso 1 1 calc R . . H43B H 0.6729 0.4128 0.9069 0.052 Uiso 1 1 calc R . . C44 C 0.54471(14) 0.29880(13) 0.96940(8) 0.0308(2) Uani 1 1 d . . . H44A H 0.5638 0.2516 1.0104 0.037 Uiso 1 1 calc R . . H44B H 0.5173 0.3677 1.0005 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01559(5) 0.01231(5) 0.01233(4) 0.00257(4) 0.00266(4) 0.00427(4) I1 0.02073(3) 0.02699(3) 0.02127(3) 0.00127(2) 0.00897(2) 0.00707(2) I2 0.01908(3) 0.01377(3) 0.01956(3) -0.00121(2) -0.00046(2) 0.00589(2) P1 0.01560(10) 0.01289(9) 0.01141(8) 0.00263(7) 0.00147(7) 0.00477(8) P2 0.01624(10) 0.01345(10) 0.01323(9) 0.00388(7) 0.00212(7) 0.00335(8) N1 0.0153(3) 0.0196(4) 0.0159(3) 0.0078(3) 0.0004(2) 0.0016(3) C1 0.0169(4) 0.0171(4) 0.0125(3) 0.0029(3) 0.0022(3) 0.0039(3) C2 0.0169(4) 0.0210(4) 0.0180(4) 0.0082(3) 0.0040(3) 0.0065(3) C3 0.0218(4) 0.0141(4) 0.0140(3) 0.0033(3) 0.0030(3) 0.0062(3) C4 0.0611(9) 0.0169(4) 0.0159(4) 0.0015(3) -0.0058(5) 0.0141(5) C5 0.0771(11) 0.0175(5) 0.0202(5) -0.0019(4) -0.0080(6) 0.0127(6) C6 0.0523(8) 0.0145(4) 0.0252(5) 0.0035(4) 0.0036(5) 0.0100(5) C7 0.0311(5) 0.0170(4) 0.0254(5) 0.0098(4) 0.0031(4) 0.0082(4) C8 0.0210(4) 0.0173(4) 0.0185(4) 0.0066(3) 0.0009(3) 0.0050(3) C9 0.0180(4) 0.0146(4) 0.0147(3) 0.0031(3) -0.0004(3) 0.0047(3) C10 0.0220(5) 0.0347(6) 0.0149(4) 0.0004(4) -0.0002(3) 0.0086(4) C11 0.0313(6) 0.0364(6) 0.0159(4) -0.0016(4) -0.0037(4) 0.0103(5) C12 0.0281(5) 0.0244(5) 0.0249(5) 0.0032(4) -0.0100(4) 0.0025(4) C13 0.0182(5) 0.0448(7) 0.0318(6) 0.0134(5) -0.0039(4) 0.0017(5) C14 0.0189(5) 0.0381(6) 0.0213(4) 0.0098(4) 0.0012(3) 0.0057(4) C15 0.0318(5) 0.0143(4) 0.0148(4) 0.0035(3) -0.0024(3) 0.0041(4) C16 0.0577(10) 0.0331(7) 0.0242(5) 0.0027(5) -0.0004(6) -0.0202(6) C17 0.0935(15) 0.0318(7) 0.0332(7) 0.0039(6) -0.0102(8) -0.0300(9) C18 0.0998(15) 0.0203(6) 0.0291(6) -0.0063(5) -0.0175(8) 0.0096(7) C19 0.0724(11) 0.0411(8) 0.0250(6) -0.0112(5) -0.0064(6) 0.0309(8) C20 0.0363(6) 0.0324(6) 0.0208(4) -0.0036(4) -0.0015(4) 0.0160(5) C21 0.0190(4) 0.0142(4) 0.0137(3) 0.0032(3) 0.0011(3) 0.0039(3) C22 0.0199(4) 0.0223(4) 0.0208(4) 0.0082(3) 0.0025(3) 0.0063(4) C23 0.0242(5) 0.0245(5) 0.0236(4) 0.0070(4) -0.0001(4) 0.0102(4) C24 0.0318(6) 0.0166(4) 0.0215(4) 0.0059(3) -0.0019(4) 0.0067(4) C25 0.0275(5) 0.0206(5) 0.0280(5) 0.0123(4) 0.0025(4) 0.0027(4) C26 0.0200(4) 0.0198(4) 0.0234(4) 0.0092(3) 0.0035(3) 0.0040(3) C27 0.0161(4) 0.0193(4) 0.0142(3) 0.0040(3) 0.0042(3) 0.0028(3) C28 0.0202(4) 0.0231(5) 0.0206(4) 0.0089(3) 0.0014(3) 0.0019(4) C29 0.0281(5) 0.0223(5) 0.0225(4) 0.0087(4) 0.0039(4) 0.0000(4) C30 0.0241(5) 0.0265(5) 0.0262(5) 0.0055(4) 0.0084(4) -0.0027(4) C31 0.0165(4) 0.0343(6) 0.0332(5) 0.0092(5) 0.0079(4) 0.0036(4) C32 0.0174(4) 0.0266(5) 0.0282(5) 0.0094(4) 0.0074(4) 0.0064(4) O40 0.0361(5) 0.0295(4) 0.0282(4) 0.0012(3) 0.0031(3) 0.0120(4) C41 0.0606(10) 0.0405(8) 0.0252(5) 0.0031(5) 0.0081(6) 0.0177(7) C42 0.0568(10) 0.0649(11) 0.0368(7) 0.0105(7) 0.0214(7) 0.0265(9) C43 0.0374(8) 0.0596(10) 0.0332(7) 0.0057(6) 0.0090(6) 0.0123(7) C44 0.0330(6) 0.0411(7) 0.0219(5) 0.0066(4) 0.0034(4) 0.0160(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P1 2.3257(3) . yes Co1 P2 2.3426(3) . yes Co1 I1 2.53009(16) . yes Co1 I2 2.54861(17) . yes P1 C9 1.8060(9) . ? P1 C3 1.8141(10) . ? P1 C1 1.8549(10) . ? P2 C15 1.8145(10) . ? P2 C21 1.8170(10) . ? P2 C2 1.8547(10) . ? N1 C27 1.4226(13) . ? N1 C2 1.4552(13) . ? N1 C1 1.4571(12) . ? C3 C8 1.3956(14) . ? C3 C4 1.3939(14) . ? C4 C5 1.3897(16) . ? C5 C6 1.3874(19) . ? C6 C7 1.3860(17) . ? C7 C8 1.3906(15) . ? C9 C14 1.3921(15) . ? C9 C10 1.3926(14) . ? C10 C11 1.3904(15) . ? C11 C12 1.3822(19) . ? C12 C13 1.3863(19) . ? C13 C14 1.3872(16) . ? C15 C20 1.3884(17) . ? C15 C16 1.3894(19) . ? C16 C17 1.393(2) . ? C17 C18 1.380(3) . ? C18 C19 1.372(3) . ? C19 C20 1.3949(17) . ? C21 C26 1.3923(14) . ? C21 C22 1.3948(15) . ? C22 C23 1.3936(16) . ? C23 C24 1.3854(17) . ? C24 C25 1.3845(18) . ? C25 C26 1.3917(16) . ? C27 C32 1.3992(15) . ? C27 C28 1.3997(15) . ? C28 C29 1.3910(15) . ? C29 C30 1.3822(19) . ? C30 C31 1.384(2) . ? C31 C32 1.3959(16) . ? O40 C44 1.4258(16) . ? O40 C41 1.4276(17) . ? C41 C42 1.517(3) . ? C42 C43 1.519(2) . ? C43 C44 1.507(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Co1 P2 97.364(10) . . yes P1 Co1 I1 114.001(9) . . yes P2 Co1 I1 120.871(8) . . yes P1 Co1 I2 102.545(8) . . yes P2 Co1 I2 100.275(8) . . yes I1 Co1 I2 118.297(6) . . yes C9 P1 C3 105.47(4) . . ? C9 P1 C1 105.66(4) . . ? C3 P1 C1 104.24(5) . . ? C9 P1 Co1 114.54(3) . . ? C3 P1 Co1 119.34(3) . . ? C1 P1 Co1 106.35(3) . . ? C15 P2 C21 104.11(4) . . ? C15 P2 C2 106.36(5) . . ? C21 P2 C2 103.49(5) . . ? C15 P2 Co1 117.66(4) . . ? C21 P2 Co1 115.84(3) . . ? C2 P2 Co1 108.14(3) . . ? C27 N1 C2 120.68(8) . . ? C27 N1 C1 117.51(8) . . ? C2 N1 C1 114.74(8) . . ? N1 C1 P1 112.17(6) . . ? N1 C2 P2 112.65(7) . . ? C8 C3 C4 119.25(9) . . ? C8 C3 P1 122.29(7) . . ? C4 C3 P1 118.42(8) . . ? C3 C4 C5 120.22(11) . . ? C6 C5 C4 120.31(11) . . ? C7 C6 C5 119.68(10) . . ? C6 C7 C8 120.34(10) . . ? C3 C8 C7 120.15(9) . . ? C14 C9 C10 119.22(9) . . ? C14 C9 P1 117.09(7) . . ? C10 C9 P1 123.68(8) . . ? C11 C10 C9 120.04(11) . . ? C12 C11 C10 120.40(11) . . ? C11 C12 C13 119.85(10) . . ? C14 C13 C12 120.01(12) . . ? C13 C14 C9 120.48(11) . . ? C20 C15 C16 119.92(11) . . ? C20 C15 P2 116.48(9) . . ? C16 C15 P2 123.58(10) . . ? C15 C16 C17 119.65(16) . . ? C18 C17 C16 120.10(17) . . ? C17 C18 C19 120.41(12) . . ? C18 C19 C20 120.14(15) . . ? C15 C20 C19 119.75(14) . . ? C26 C21 C22 119.32(9) . . ? C26 C21 P2 118.90(8) . . ? C22 C21 P2 121.78(8) . . ? C21 C22 C23 120.11(10) . . ? C24 C23 C22 120.27(11) . . ? C23 C24 C25 119.72(10) . . ? C24 C25 C26 120.41(11) . . ? C21 C26 C25 120.15(10) . . ? C32 C27 C28 118.04(9) . . ? C32 C27 N1 122.45(10) . . ? C28 C27 N1 119.49(9) . . ? C29 C28 C27 120.97(10) . . ? C30 C29 C28 120.74(11) . . ? C29 C30 C31 118.77(10) . . ? C30 C31 C32 121.24(11) . . ? C27 C32 C31 120.20(11) . . ? C44 O40 C41 109.57(11) . . ? O40 C41 C42 106.67(12) . . ? C43 C42 C41 102.19(13) . . ? C44 C43 C42 102.19(14) . . ? O40 C44 C43 106.81(10) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 47.91 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 6.670 _refine_diff_density_min -2.149 _refine_diff_density_rms 0.142 #===END data_dqc09 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H29 I2 N Ni P2' _chemical_formula_sum 'C32 H29 I2 N Ni P2' _chemical_formula_weight 802.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3909(5) _cell_length_b 24.7658(11) _cell_length_c 12.8704(6) _cell_angle_alpha 90.00 _cell_angle_beta 112.745(2) _cell_angle_gamma 90.00 _cell_volume 3054.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9736 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 42.16 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 2.784 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6079 _exptl_absorpt_correction_T_max 0.7483 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 20 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 181248 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0211 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 42.39 _reflns_number_total 21774 _reflns_number_gt 18089 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21774 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0385 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.749 _refine_ls_restrained_S_all 1.749 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.497473(12) 0.306527(5) 0.855759(10) 0.01060(2) Uani 1 1 d . . . I1 I 0.575143(7) 0.224375(2) 0.982516(5) 0.01466(1) Uani 1 1 d . . . I2 I 0.422386(7) 0.352571(2) 0.998728(5) 0.01505(1) Uani 1 1 d . . . P1 P 0.57406(2) 0.266165(9) 0.74005(2) 0.01098(4) Uani 1 1 d . . . P2 P 0.44872(2) 0.380912(9) 0.75820(2) 0.01106(4) Uani 1 1 d . . . N1 N 0.53681(8) 0.34882(3) 0.58808(7) 0.01253(12) Uani 1 1 d . . . C1 C 0.51231(10) 0.29086(4) 0.59345(8) 0.01300(14) Uani 1 1 d . . . H1A H 0.5601 0.2714 0.5536 0.016 Uiso 1 1 calc R . . H1B H 0.4132 0.2836 0.5560 0.016 Uiso 1 1 calc R . . C2 C 0.43172(10) 0.38051(4) 0.60943(8) 0.01347(14) Uani 1 1 d . . . H2A H 0.3403 0.3665 0.5629 0.016 Uiso 1 1 calc R . . H2B H 0.4365 0.4175 0.5861 0.016 Uiso 1 1 calc R . . C3 C 0.76153(9) 0.27280(4) 0.78482(8) 0.01327(14) Uani 1 1 d . . . C4 C 0.83350(10) 0.30680(4) 0.87473(8) 0.01540(15) Uani 1 1 d . . . H4 H 0.7858 0.3248 0.9123 0.018 Uiso 1 1 calc R . . C5 C 0.97714(11) 0.31384(4) 0.90845(9) 0.02093(19) Uani 1 1 d . . . H5 H 1.0249 0.3372 0.9673 0.025 Uiso 1 1 calc R . . C6 C 1.04869(11) 0.28585(5) 0.85396(10) 0.0232(2) Uani 1 1 d . . . H6 H 1.1450 0.2895 0.8784 0.028 Uiso 1 1 calc R . . C7 C 0.97740(11) 0.25247(5) 0.76314(10) 0.0217(2) Uani 1 1 d . . . H7 H 1.0258 0.2342 0.7265 0.026 Uiso 1 1 calc R . . C8 C 0.83402(10) 0.24640(4) 0.72710(9) 0.01768(17) Uani 1 1 d . . . H8 H 0.7859 0.2249 0.6649 0.021 Uiso 1 1 calc R . . C9 C 0.53108(9) 0.19495(4) 0.71434(8) 0.01269(14) Uani 1 1 d . . . C10 C 0.63194(10) 0.15443(4) 0.75129(9) 0.01709(16) Uani 1 1 d . . . H10 H 0.7252 0.1634 0.7904 0.021 Uiso 1 1 calc R . . C11 C 0.59295(11) 0.10056(4) 0.72956(10) 0.02070(18) Uani 1 1 d . . . H11 H 0.6604 0.0736 0.7541 0.025 Uiso 1 1 calc R . . C12 C 0.45407(11) 0.08674(4) 0.67148(9) 0.01915(17) Uani 1 1 d . . . H12 H 0.4287 0.0507 0.6563 0.023 Uiso 1 1 calc R . . C13 C 0.35302(10) 0.12688(4) 0.63602(9) 0.01677(16) Uani 1 1 d . . . H13 H 0.2598 0.1177 0.5974 0.020 Uiso 1 1 calc R . . C14 C 0.39099(10) 0.18082(4) 0.65820(8) 0.01452(15) Uani 1 1 d . . . H14 H 0.3229 0.2076 0.6356 0.017 Uiso 1 1 calc R . . C15 C 0.58638(9) 0.43040(3) 0.82286(8) 0.01267(14) Uani 1 1 d . . . C16 C 0.70152(10) 0.43186(4) 0.79131(9) 0.01596(16) Uani 1 1 d . . . H16 H 0.7051 0.4088 0.7355 0.019 Uiso 1 1 calc R . . C17 C 0.81004(11) 0.46777(4) 0.84347(10) 0.01901(18) Uani 1 1 d . . . H17 H 0.8863 0.4685 0.8226 0.023 Uiso 1 1 calc R . . C18 C 0.80561(10) 0.50267(4) 0.92646(9) 0.01769(17) Uani 1 1 d . . . H18 H 0.8782 0.5269 0.9604 0.021 Uiso 1 1 calc R . . C19 C 0.69241(10) 0.50127(4) 0.95870(9) 0.01656(16) Uani 1 1 d . . . H19 H 0.6896 0.5244 1.0147 0.020 Uiso 1 1 calc R . . C20 C 0.58356(10) 0.46534(4) 0.90720(9) 0.01538(16) Uani 1 1 d . . . H20 H 0.5081 0.4645 0.9291 0.018 Uiso 1 1 calc R . . C21 C 0.28242(10) 0.41437(4) 0.72861(8) 0.01381(15) Uani 1 1 d . . . C22 C 0.26457(11) 0.46886(4) 0.69866(10) 0.01884(18) Uani 1 1 d . . . H22 H 0.3416 0.4900 0.7061 0.023 Uiso 1 1 calc R . . C23 C 0.13171(12) 0.49157(5) 0.65777(10) 0.0236(2) Uani 1 1 d . . . H23 H 0.1200 0.5279 0.6382 0.028 Uiso 1 1 calc R . . C24 C 0.01674(11) 0.45996(5) 0.64613(10) 0.0245(2) Uani 1 1 d . . . H24 H -0.0720 0.4751 0.6185 0.029 Uiso 1 1 calc R . . C25 C 0.03379(11) 0.40574(5) 0.67561(10) 0.0231(2) Uani 1 1 d . . . H25 H -0.0435 0.3847 0.6679 0.028 Uiso 1 1 calc R . . C26 C 0.16612(10) 0.38277(4) 0.71660(9) 0.01742(16) Uani 1 1 d . . . H26 H 0.1773 0.3464 0.7360 0.021 Uiso 1 1 calc R . . C27 C 0.56407(9) 0.36478(4) 0.49132(8) 0.01274(14) Uani 1 1 d . . . C28 C 0.68486(10) 0.34544(4) 0.48061(9) 0.01666(16) Uani 1 1 d . . . H28 H 0.7450 0.3227 0.5354 0.020 Uiso 1 1 calc R . . C29 C 0.71542(11) 0.36015(4) 0.38817(9) 0.01927(18) Uani 1 1 d . . . H29 H 0.7957 0.3470 0.3815 0.023 Uiso 1 1 calc R . . C30 C 0.62704(11) 0.39431(4) 0.30603(9) 0.01975(18) Uani 1 1 d . . . H30 H 0.6477 0.4040 0.2444 0.024 Uiso 1 1 calc R . . C31 C 0.50760(11) 0.41385(4) 0.31670(9) 0.01939(18) Uani 1 1 d . . . H31 H 0.4481 0.4368 0.2620 0.023 Uiso 1 1 calc R . . C32 C 0.47620(10) 0.39929(4) 0.40887(8) 0.01573(16) Uani 1 1 d . . . H32 H 0.3961 0.4127 0.4154 0.019 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01264(5) 0.00856(4) 0.01095(5) 0.00018(3) 0.00494(4) -0.00043(4) I1 0.01838(3) 0.01176(2) 0.01322(2) 0.00247(2) 0.00542(2) -0.00001(2) I2 0.01952(3) 0.01430(2) 0.01311(2) -0.00113(2) 0.00826(2) 0.00005(2) P1 0.01230(9) 0.00867(9) 0.01123(9) 0.00000(7) 0.00371(8) 0.00077(7) P2 0.01290(9) 0.00860(8) 0.01278(9) -0.00011(7) 0.00618(8) -0.00028(7) N1 0.0162(3) 0.0098(3) 0.0127(3) 0.0006(2) 0.0069(3) 0.0014(2) C1 0.0160(4) 0.0102(3) 0.0120(3) 0.0001(3) 0.0045(3) 0.0006(3) C2 0.0166(4) 0.0112(3) 0.0130(4) 0.0013(3) 0.0062(3) 0.0022(3) C3 0.0132(3) 0.0121(3) 0.0139(4) 0.0014(3) 0.0046(3) -0.0004(3) C4 0.0170(4) 0.0137(4) 0.0138(4) 0.0016(3) 0.0041(3) -0.0021(3) C5 0.0191(4) 0.0210(5) 0.0182(4) 0.0043(3) 0.0023(4) -0.0076(4) C6 0.0145(4) 0.0293(5) 0.0250(5) 0.0105(4) 0.0068(4) -0.0036(4) C7 0.0172(4) 0.0267(5) 0.0240(5) 0.0067(4) 0.0110(4) 0.0029(4) C8 0.0165(4) 0.0192(4) 0.0178(4) 0.0003(3) 0.0071(3) 0.0018(3) C9 0.0154(4) 0.0098(3) 0.0122(3) 0.0000(3) 0.0045(3) 0.0007(3) C10 0.0159(4) 0.0111(4) 0.0200(4) -0.0010(3) 0.0022(3) 0.0016(3) C11 0.0203(4) 0.0116(4) 0.0252(5) -0.0013(3) 0.0034(4) 0.0033(3) C12 0.0236(5) 0.0119(4) 0.0192(4) -0.0024(3) 0.0052(4) -0.0030(3) C13 0.0168(4) 0.0153(4) 0.0164(4) 0.0003(3) 0.0044(3) -0.0035(3) C14 0.0142(4) 0.0132(4) 0.0152(4) 0.0015(3) 0.0046(3) 0.0010(3) C15 0.0138(3) 0.0095(3) 0.0152(4) 0.0007(3) 0.0062(3) -0.0006(3) C16 0.0170(4) 0.0147(4) 0.0186(4) -0.0017(3) 0.0095(3) -0.0016(3) C17 0.0166(4) 0.0192(4) 0.0243(5) -0.0018(4) 0.0112(4) -0.0037(3) C18 0.0153(4) 0.0149(4) 0.0213(4) -0.0007(3) 0.0055(4) -0.0035(3) C19 0.0184(4) 0.0128(4) 0.0189(4) -0.0026(3) 0.0077(4) -0.0006(3) C20 0.0161(4) 0.0127(4) 0.0194(4) -0.0024(3) 0.0092(3) -0.0012(3) C21 0.0144(4) 0.0131(4) 0.0148(4) 0.0001(3) 0.0066(3) 0.0012(3) C22 0.0185(4) 0.0137(4) 0.0255(5) 0.0021(3) 0.0098(4) 0.0019(3) C23 0.0235(5) 0.0185(5) 0.0288(5) 0.0039(4) 0.0101(4) 0.0079(4) C24 0.0165(4) 0.0308(6) 0.0251(5) 0.0021(4) 0.0069(4) 0.0082(4) C25 0.0146(4) 0.0286(5) 0.0255(5) -0.0002(4) 0.0071(4) -0.0017(4) C26 0.0157(4) 0.0174(4) 0.0193(4) 0.0002(3) 0.0069(3) -0.0018(3) C27 0.0139(4) 0.0123(3) 0.0115(3) -0.0009(3) 0.0044(3) -0.0017(3) C28 0.0160(4) 0.0172(4) 0.0168(4) 0.0016(3) 0.0063(3) 0.0024(3) C29 0.0186(4) 0.0217(5) 0.0206(4) -0.0012(4) 0.0110(4) -0.0007(3) C30 0.0230(5) 0.0227(5) 0.0165(4) 0.0003(3) 0.0108(4) -0.0041(4) C31 0.0206(4) 0.0223(5) 0.0143(4) 0.0048(3) 0.0057(4) 0.0001(4) C32 0.0148(4) 0.0180(4) 0.0139(4) 0.0024(3) 0.0050(3) 0.0008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 P2 2.1760(3) . yes Ni1 P1 2.1833(3) . yes Ni1 I2 2.53083(14) . yes Ni1 I1 2.53658(15) . yes P1 C3 1.8127(9) . ? P1 C9 1.8180(9) . ? P1 C1 1.8465(9) . ? P2 C21 1.8190(9) . ? P2 C15 1.8222(9) . ? P2 C2 1.8537(9) . ? N1 C27 1.4353(11) . ? N1 C2 1.4547(11) . ? N1 C1 1.4640(12) . ? C3 C4 1.3921(14) . ? C3 C8 1.4069(13) . ? C4 C5 1.3948(14) . ? C5 C6 1.3886(17) . ? C6 C7 1.3888(18) . ? C7 C8 1.3868(14) . ? C9 C10 1.3952(13) . ? C9 C14 1.3965(13) . ? C10 C11 1.3909(14) . ? C11 C12 1.3872(15) . ? C12 C13 1.3888(15) . ? C13 C14 1.3908(14) . ? C15 C20 1.3972(13) . ? C15 C16 1.4048(12) . ? C16 C17 1.3885(14) . ? C17 C18 1.3886(15) . ? C18 C19 1.3908(13) . ? C19 C20 1.3896(14) . ? C21 C22 1.3961(14) . ? C21 C26 1.3972(13) . ? C22 C23 1.3919(15) . ? C23 C24 1.3871(17) . ? C24 C25 1.3881(17) . ? C25 C26 1.3898(15) . ? C27 C32 1.3933(13) . ? C27 C28 1.3990(13) . ? C28 C29 1.3933(14) . ? C29 C30 1.3878(16) . ? C30 C31 1.3875(15) . ? C31 C32 1.3939(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ni1 P1 93.381(10) . . yes P2 Ni1 I2 88.260(8) . . yes P1 Ni1 I2 176.719(9) . . yes P2 Ni1 I1 174.479(9) . . yes P1 Ni1 I1 87.835(8) . . yes I2 Ni1 I1 90.267(5) . . yes C3 P1 C9 107.70(4) . . ? C3 P1 C1 101.59(4) . . ? C9 P1 C1 99.87(4) . . ? C3 P1 Ni1 111.84(3) . . ? C9 P1 Ni1 116.08(3) . . ? C1 P1 Ni1 118.10(3) . . ? C21 P2 C15 107.68(4) . . ? C21 P2 C2 94.74(4) . . ? C15 P2 C2 102.69(4) . . ? C21 P2 Ni1 119.79(3) . . ? C15 P2 Ni1 109.84(3) . . ? C2 P2 Ni1 119.97(3) . . ? C27 N1 C2 115.45(7) . . ? C27 N1 C1 114.03(7) . . ? C2 N1 C1 111.29(7) . . ? N1 C1 P1 112.02(6) . . ? N1 C2 P2 114.79(6) . . ? C4 C3 C8 119.66(9) . . ? C4 C3 P1 119.01(7) . . ? C8 C3 P1 121.26(7) . . ? C3 C4 C5 120.04(9) . . ? C6 C5 C4 119.86(10) . . ? C5 C6 C7 120.44(10) . . ? C8 C7 C6 120.04(10) . . ? C7 C8 C3 119.88(10) . . ? C10 C9 C14 119.43(8) . . ? C10 C9 P1 122.45(7) . . ? C14 C9 P1 118.10(7) . . ? C11 C10 C9 119.96(9) . . ? C12 C11 C10 120.43(9) . . ? C11 C12 C13 119.82(9) . . ? C12 C13 C14 120.11(9) . . ? C13 C14 C9 120.21(9) . . ? C20 C15 C16 118.99(9) . . ? C20 C15 P2 121.52(7) . . ? C16 C15 P2 119.42(7) . . ? C17 C16 C15 120.00(9) . . ? C16 C17 C18 120.55(9) . . ? C17 C18 C19 119.83(9) . . ? C20 C19 C18 120.00(9) . . ? C19 C20 C15 120.62(8) . . ? C22 C21 C26 119.60(9) . . ? C22 C21 P2 120.81(7) . . ? C26 C21 P2 118.62(7) . . ? C23 C22 C21 120.09(10) . . ? C24 C23 C22 119.99(10) . . ? C23 C24 C25 120.19(10) . . ? C24 C25 C26 120.17(10) . . ? C25 C26 C21 119.96(10) . . ? C32 C27 C28 118.93(8) . . ? C32 C27 N1 122.60(8) . . ? C28 C27 N1 118.47(8) . . ? C29 C28 C27 120.26(9) . . ? C30 C29 C28 120.51(9) . . ? C31 C30 C29 119.41(9) . . ? C30 C31 C32 120.44(10) . . ? C27 C32 C31 120.45(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 42.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.386 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.112 #===END data_dqc10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H33 Co I2 N P2' _chemical_formula_sum 'C34 H33 Co I2 N P2' _chemical_formula_weight 830.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.7095(6) _cell_length_b 14.2590(7) _cell_length_c 19.3910(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3237.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9025 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 40.43 _exptl_crystal_description Block _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 2.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6258 _exptl_absorpt_correction_T_max 0.7488 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 14 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 202158 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 44.82 _reflns_number_total 26395 _reflns_number_gt 23504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.012(4) _refine_ls_number_reflns 26395 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0326 _refine_ls_wR_factor_gt 0.0316 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.849567(9) 0.185684(8) 0.800146(6) 0.01112(2) Uani 1 1 d . . . I1 I 1.050540(4) 0.165036(4) 0.852776(3) 0.01814(1) Uani 1 1 d . . . I2 I 0.768271(5) 0.045138(4) 0.736110(3) 0.01726(1) Uani 1 1 d . . . P1 P 0.732248(18) 0.219765(14) 0.895299(11) 0.01021(3) Uani 1 1 d . . . P2 P 0.872865(18) 0.311763(16) 0.724024(12) 0.01277(4) Uani 1 1 d . . . N1 N 0.80021(5) 0.42987(5) 0.85463(4) 0.01201(11) Uani 1 1 d . . . C1 C 0.86392(7) 0.38507(6) 0.91055(5) 0.01288(13) Uani 1 1 d . . . H1A H 0.8895 0.4341 0.9432 0.015 Uiso 1 1 calc R . . H1B H 0.9330 0.3552 0.8910 0.015 Uiso 1 1 calc R . . C2 C 0.79610(7) 0.31065(6) 0.95068(5) 0.01313(13) Uani 1 1 d . . . H2A H 0.7345 0.3422 0.9769 0.016 Uiso 1 1 calc R . . H2B H 0.8476 0.2801 0.9844 0.016 Uiso 1 1 calc R . . C3 C 0.87717(7) 0.47777(6) 0.80507(5) 0.01429(14) Uani 1 1 d . . . H3A H 0.9286 0.5201 0.8311 0.017 Uiso 1 1 calc R . . H3B H 0.8303 0.5171 0.7739 0.017 Uiso 1 1 calc R . . C4 C 0.94991(7) 0.41191(6) 0.76129(5) 0.01505(13) Uani 1 1 d . . . H4A H 1.0131 0.3876 0.7902 0.018 Uiso 1 1 calc R . . H4B H 0.9844 0.4485 0.7233 0.018 Uiso 1 1 calc R . . C5 C 0.58308(7) 0.25031(6) 0.88041(5) 0.01216(13) Uani 1 1 d . . . C6 C 0.52812(7) 0.32503(6) 0.91243(5) 0.01677(15) Uani 1 1 d . . . H6 H 0.5684 0.3625 0.9448 0.020 Uiso 1 1 calc R . . C7 C 0.41418(7) 0.34537(7) 0.89737(6) 0.02103(18) Uani 1 1 d . . . H7 H 0.3777 0.3972 0.9189 0.025 Uiso 1 1 calc R . . C8 C 0.35418(7) 0.29020(7) 0.85107(6) 0.02079(17) Uani 1 1 d . . . H8 H 0.2770 0.3047 0.8403 0.025 Uiso 1 1 calc R . . C9 C 0.40702(8) 0.21360(8) 0.82046(6) 0.02117(18) Uani 1 1 d . . . H9 H 0.3654 0.1747 0.7896 0.025 Uiso 1 1 calc R . . C10 C 0.52127(7) 0.19363(7) 0.83489(5) 0.01763(16) Uani 1 1 d . . . H10 H 0.5572 0.1413 0.8137 0.021 Uiso 1 1 calc R . . C11 C 0.72213(7) 0.11854(6) 0.95221(4) 0.01253(13) Uani 1 1 d . . . C12 C 0.65315(7) 0.12073(7) 1.01096(5) 0.01623(15) Uani 1 1 d . . . H12 H 0.6073 0.1742 1.0204 0.019 Uiso 1 1 calc R . . C13 C 0.65178(7) 0.04454(8) 1.05557(5) 0.02009(17) Uani 1 1 d . . . H13 H 0.6060 0.0465 1.0960 0.024 Uiso 1 1 calc R . . C14 C 0.71677(8) -0.03441(7) 1.04141(5) 0.02046(17) Uani 1 1 d . . . H14 H 0.7159 -0.0861 1.0723 0.025 Uiso 1 1 calc R . . C15 C 0.78310(9) -0.03822(7) 0.98222(5) 0.02125(17) Uani 1 1 d . . . H15 H 0.8264 -0.0929 0.9721 0.026 Uiso 1 1 calc R . . C16 C 0.78598(8) 0.03842(7) 0.93766(5) 0.01813(16) Uani 1 1 d . . . H16 H 0.8316 0.0361 0.8972 0.022 Uiso 1 1 calc R . . C17 C 0.74677(7) 0.36021(6) 0.68255(5) 0.01481(14) Uani 1 1 d . . . C18 C 0.75245(8) 0.44252(6) 0.64330(5) 0.01799(15) Uani 1 1 d . . . H18 H 0.8241 0.4717 0.6353 0.022 Uiso 1 1 calc R . . C19 C 0.65361(9) 0.48158(7) 0.61611(5) 0.02251(18) Uani 1 1 d . . . H19 H 0.6579 0.5380 0.5902 0.027 Uiso 1 1 calc R . . C20 C 0.54814(10) 0.43849(8) 0.62657(6) 0.0258(2) Uani 1 1 d . . . H20 H 0.4808 0.4653 0.6077 0.031 Uiso 1 1 calc R . . C21 C 0.54188(9) 0.35616(8) 0.66469(6) 0.0272(2) Uani 1 1 d . . . H21 H 0.4702 0.3264 0.6717 0.033 Uiso 1 1 calc R . . C22 C 0.64091(8) 0.31722(7) 0.69274(6) 0.02095(17) Uani 1 1 d . . . H22 H 0.6363 0.2611 0.7190 0.025 Uiso 1 1 calc R . . C23 C 0.96653(7) 0.27491(6) 0.65378(5) 0.01617(15) Uani 1 1 d . . . C24 C 1.08484(9) 0.26816(8) 0.66407(6) 0.02325(19) Uani 1 1 d . . . H24 H 1.1173 0.2880 0.7065 0.028 Uiso 1 1 calc R . . C25 C 1.15468(9) 0.23256(8) 0.61235(6) 0.0268(2) Uani 1 1 d . . . H25 H 1.2347 0.2281 0.6196 0.032 Uiso 1 1 calc R . . C26 C 1.10779(10) 0.20352(7) 0.55016(6) 0.0259(2) Uani 1 1 d . . . H26 H 1.1557 0.1794 0.5148 0.031 Uiso 1 1 calc R . . C27 C 0.99088(10) 0.20973(7) 0.53965(6) 0.0249(2) Uani 1 1 d . . . H27 H 0.9586 0.1899 0.4971 0.030 Uiso 1 1 calc R . . C28 C 0.92080(9) 0.24513(7) 0.59155(5) 0.01986(17) Uani 1 1 d . . . H28 H 0.8407 0.2489 0.5842 0.024 Uiso 1 1 calc R . . C29 C 0.70858(7) 0.49044(6) 0.87518(5) 0.01243(13) Uani 1 1 d . . . C30 C 0.69323(8) 0.52089(6) 0.94278(5) 0.01560(15) Uani 1 1 d . . . H30 H 0.7462 0.5028 0.9774 0.019 Uiso 1 1 calc R . . C31 C 0.60050(8) 0.57793(7) 0.95998(5) 0.02002(17) Uani 1 1 d . . . H31 H 0.5899 0.5971 1.0065 0.024 Uiso 1 1 calc R . . C32 C 0.52386(8) 0.60671(8) 0.90990(6) 0.02267(19) Uani 1 1 d . . . H32 H 0.4616 0.6464 0.9216 0.027 Uiso 1 1 calc R . . C33 C 0.53922(8) 0.57684(7) 0.84254(5) 0.02136(18) Uani 1 1 d . . . H33 H 0.4872 0.5965 0.8078 0.026 Uiso 1 1 calc R . . C34 C 0.62978(7) 0.51854(7) 0.82519(5) 0.01675(15) Uani 1 1 d . . . H34 H 0.6382 0.4976 0.7790 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01078(4) 0.01157(4) 0.01101(5) -0.00057(4) 0.00066(4) 0.00034(3) I1 0.01197(2) 0.01763(2) 0.02483(3) -0.00419(2) -0.00364(2) 0.00275(2) I2 0.01699(2) 0.01725(2) 0.01754(2) -0.00697(2) -0.00345(2) 0.00195(2) P1 0.01074(7) 0.01004(8) 0.00985(8) 0.00031(6) 0.00007(7) 0.00077(7) P2 0.01338(8) 0.01264(9) 0.01228(9) 0.00014(7) 0.00158(7) -0.00120(7) N1 0.0122(2) 0.0117(3) 0.0121(3) 0.0013(2) -0.0002(2) -0.0005(2) C1 0.0126(3) 0.0127(3) 0.0134(3) -0.0006(3) -0.0023(3) 0.0001(3) C2 0.0156(3) 0.0123(3) 0.0115(3) -0.0001(3) -0.0020(2) 0.0006(3) C3 0.0157(3) 0.0124(3) 0.0148(4) 0.0005(3) 0.0016(3) -0.0023(3) C4 0.0143(3) 0.0146(3) 0.0163(3) -0.0010(3) 0.0019(3) -0.0030(3) C5 0.0116(3) 0.0127(3) 0.0122(3) 0.0020(3) 0.0012(2) 0.0005(2) C6 0.0130(3) 0.0134(4) 0.0239(4) -0.0025(3) 0.0030(3) -0.0007(3) C7 0.0132(3) 0.0149(4) 0.0350(6) -0.0019(4) 0.0047(3) 0.0012(3) C8 0.0120(3) 0.0224(4) 0.0279(5) 0.0035(4) 0.0001(3) 0.0012(3) C9 0.0145(3) 0.0265(5) 0.0225(5) -0.0048(4) -0.0030(3) -0.0004(3) C10 0.0146(3) 0.0205(4) 0.0178(4) -0.0042(3) -0.0015(3) 0.0026(3) C11 0.0136(3) 0.0125(3) 0.0116(3) 0.0013(2) -0.0010(3) 0.0000(3) C12 0.0136(3) 0.0199(4) 0.0152(4) 0.0041(3) 0.0017(3) 0.0023(3) C13 0.0152(3) 0.0267(4) 0.0184(4) 0.0093(4) 0.0013(3) -0.0021(3) C14 0.0247(4) 0.0162(4) 0.0205(4) 0.0068(3) -0.0039(3) -0.0062(3) C15 0.0344(5) 0.0115(3) 0.0179(4) 0.0010(3) -0.0031(4) 0.0034(3) C16 0.0264(4) 0.0140(4) 0.0139(4) 0.0003(3) 0.0009(3) 0.0046(3) C17 0.0174(3) 0.0140(3) 0.0130(3) -0.0011(3) 0.0001(3) -0.0003(3) C18 0.0229(4) 0.0161(3) 0.0149(3) 0.0006(3) 0.0026(3) 0.0006(3) C19 0.0327(5) 0.0200(4) 0.0148(4) 0.0013(3) 0.0000(4) 0.0075(4) C20 0.0258(4) 0.0275(5) 0.0241(5) -0.0016(4) -0.0070(4) 0.0076(4) C21 0.0190(4) 0.0296(5) 0.0330(6) 0.0028(4) -0.0071(4) -0.0027(4) C22 0.0186(4) 0.0191(4) 0.0252(5) 0.0036(3) -0.0034(3) -0.0026(3) C23 0.0205(4) 0.0123(3) 0.0157(4) 0.0008(3) 0.0054(3) -0.0004(3) C24 0.0212(4) 0.0290(5) 0.0196(5) -0.0002(4) 0.0053(3) 0.0018(4) C25 0.0229(4) 0.0292(5) 0.0284(6) 0.0020(4) 0.0113(4) 0.0043(4) C26 0.0350(5) 0.0173(4) 0.0255(5) 0.0019(4) 0.0151(4) 0.0053(4) C27 0.0372(5) 0.0178(4) 0.0196(5) -0.0039(3) 0.0068(4) 0.0014(4) C28 0.0255(4) 0.0154(4) 0.0187(4) -0.0024(3) 0.0040(3) 0.0002(3) C29 0.0126(3) 0.0114(3) 0.0133(3) 0.0006(2) -0.0005(2) -0.0010(2) C30 0.0179(3) 0.0143(3) 0.0146(4) -0.0006(3) -0.0023(3) 0.0019(3) C31 0.0239(4) 0.0186(4) 0.0175(4) -0.0014(3) 0.0029(3) 0.0041(3) C32 0.0197(4) 0.0232(5) 0.0251(5) 0.0045(4) 0.0037(3) 0.0077(3) C33 0.0172(4) 0.0259(4) 0.0210(4) 0.0061(3) -0.0016(3) 0.0045(3) C34 0.0165(3) 0.0205(4) 0.0133(4) 0.0021(3) -0.0014(3) 0.0005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P2 2.3420(3) . yes Co1 P1 2.3511(3) . yes Co1 I2 2.54249(15) . yes Co1 I1 2.58189(16) . yes P1 C11 1.8208(8) . ? P1 C5 1.8232(8) . ? P1 C2 1.8417(9) . ? P2 C17 1.8177(9) . ? P2 C23 1.8260(9) . ? P2 C4 1.8371(9) . ? N1 C29 1.4338(11) . ? N1 C1 1.4630(11) . ? N1 C3 1.4841(11) . ? C1 C2 1.5369(12) . ? C3 C4 1.5258(13) . ? C5 C6 1.3910(12) . ? C5 C10 1.3986(13) . ? C6 C7 1.3962(13) . ? C7 C8 1.3851(15) . ? C8 C9 1.3887(15) . ? C9 C10 1.3961(13) . ? C11 C16 1.3941(12) . ? C11 C12 1.3969(12) . ? C12 C13 1.3889(13) . ? C13 C14 1.3862(15) . ? C14 C15 1.3870(15) . ? C15 C16 1.3935(13) . ? C17 C22 1.3969(13) . ? C17 C18 1.4004(13) . ? C18 C19 1.3884(14) . ? C19 C20 1.3942(17) . ? C20 C21 1.3891(16) . ? C21 C22 1.3959(14) . ? C23 C28 1.3867(14) . ? C23 C24 1.4030(14) . ? C24 C25 1.3901(15) . ? C25 C26 1.3884(18) . ? C26 C27 1.3868(17) . ? C27 C28 1.3932(14) . ? C29 C30 1.3926(13) . ? C29 C34 1.3969(12) . ? C30 C31 1.3970(13) . ? C31 C32 1.3845(15) . ? C32 C33 1.3856(16) . ? C33 C34 1.3889(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Co1 P1 113.829(9) . . yes P2 Co1 I2 109.928(8) . . yes P1 Co1 I2 109.113(7) . . yes P2 Co1 I1 103.326(7) . . yes P1 Co1 I1 104.237(8) . . yes I2 Co1 I1 116.386(5) . . yes C11 P1 C5 102.89(4) . . ? C11 P1 C2 103.35(4) . . ? C5 P1 C2 108.25(4) . . ? C11 P1 Co1 110.47(3) . . ? C5 P1 Co1 119.00(3) . . ? C2 P1 Co1 111.46(3) . . ? C17 P2 C23 105.50(4) . . ? C17 P2 C4 106.11(4) . . ? C23 P2 C4 102.84(4) . . ? C17 P2 Co1 118.42(3) . . ? C23 P2 Co1 108.61(3) . . ? C4 P2 Co1 113.95(3) . . ? C29 N1 C1 116.02(7) . . ? C29 N1 C3 110.92(6) . . ? C1 N1 C3 111.79(6) . . ? N1 C1 C2 114.41(7) . . ? C1 C2 P1 113.60(6) . . ? N1 C3 C4 114.58(7) . . ? C3 C4 P2 115.03(6) . . ? C6 C5 C10 119.01(8) . . ? C6 C5 P1 123.75(7) . . ? C10 C5 P1 117.24(6) . . ? C5 C6 C7 120.52(9) . . ? C8 C7 C6 120.16(9) . . ? C7 C8 C9 119.85(8) . . ? C8 C9 C10 120.12(9) . . ? C9 C10 C5 120.30(9) . . ? C16 C11 C12 119.57(8) . . ? C16 C11 P1 119.48(7) . . ? C12 C11 P1 120.94(6) . . ? C13 C12 C11 119.81(8) . . ? C14 C13 C12 120.37(9) . . ? C13 C14 C15 120.21(9) . . ? C14 C15 C16 119.73(9) . . ? C15 C16 C11 120.28(9) . . ? C22 C17 C18 119.13(8) . . ? C22 C17 P2 119.44(7) . . ? C18 C17 P2 121.36(7) . . ? C19 C18 C17 120.20(9) . . ? C18 C19 C20 120.42(9) . . ? C21 C20 C19 119.77(10) . . ? C20 C21 C22 119.98(10) . . ? C21 C22 C17 120.49(9) . . ? C28 C23 C24 118.96(9) . . ? C28 C23 P2 120.35(7) . . ? C24 C23 P2 120.44(8) . . ? C25 C24 C23 120.22(10) . . ? C26 C25 C24 120.20(10) . . ? C27 C26 C25 119.93(10) . . ? C26 C27 C28 119.90(11) . . ? C23 C28 C27 120.80(10) . . ? C30 C29 C34 118.58(8) . . ? C30 C29 N1 123.09(8) . . ? C34 C29 N1 118.31(8) . . ? C29 C30 C31 120.44(8) . . ? C32 C31 C30 120.59(9) . . ? C31 C32 C33 119.08(9) . . ? C32 C33 C34 120.76(9) . . ? C33 C34 C29 120.53(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 44.82 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.922 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.089 #===END data_dqc14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H37 I N Ni O P2, I' _chemical_formula_sum 'C36 H37 I2 N Ni O P2' _chemical_formula_weight 874.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9939(5) _cell_length_b 12.7222(5) _cell_length_c 12.9714(9) _cell_angle_alpha 105.152(2) _cell_angle_beta 100.967(2) _cell_angle_gamma 110.363(2) _cell_volume 1702.42(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9633 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 47.47 _exptl_crystal_description Block _exptl_crystal_colour Purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 2.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6661 _exptl_absorpt_correction_T_max 0.7495 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 27 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 186659 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 47.94 _reflns_number_total 32429 _reflns_number_gt 26434 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 32429 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0502 _refine_ls_wR_factor_gt 0.0497 _refine_ls_goodness_of_fit_ref 2.336 _refine_ls_restrained_S_all 2.336 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.083245(9) 0.739966(9) 0.270403(9) 0.00928(2) Uani 1 1 d . . . I1 I 0.079085(5) 0.698865(5) 0.072131(5) 0.01493(1) Uani 1 1 d . . . I2 I 0.700982(5) 0.831619(5) 0.555698(5) 0.01731(1) Uani 1 1 d . . . P1 P 0.274155(18) 0.75098(2) 0.329267(18) 0.01065(3) Uani 1 1 d . . . P2 P -0.081437(18) 0.779308(19) 0.239728(18) 0.01034(3) Uani 1 1 d . . . O1 O -0.37329(6) 0.24329(6) 0.16876(6) 0.01985(12) Uani 1 1 d . . . N1 N 0.08089(6) 0.76492(6) 0.42899(6) 0.01034(10) Uani 1 1 d . . . C1 C 0.20629(7) 0.86376(7) 0.50253(7) 0.01302(12) Uani 1 1 d . . . H1A H 0.2111 0.8774 0.5823 0.016 Uiso 1 1 calc R . . H1B H 0.2141 0.9387 0.4891 0.016 Uiso 1 1 calc R . . C2 C 0.31583(7) 0.83541(8) 0.48088(7) 0.01480(13) Uani 1 1 d . . . H2A H 0.3332 0.7870 0.5251 0.018 Uiso 1 1 calc R . . H2B H 0.3920 0.9108 0.5042 0.018 Uiso 1 1 calc R . . C3 C -0.01910(7) 0.80333(8) 0.45634(7) 0.01249(12) Uani 1 1 d . . . H3A H 0.0107 0.8549 0.5366 0.015 Uiso 1 1 calc R . . H3B H -0.0951 0.7315 0.4441 0.015 Uiso 1 1 calc R . . C4 C -0.05213(7) 0.87180(7) 0.38427(7) 0.01263(12) Uani 1 1 d . . . H4A H 0.0179 0.9513 0.4055 0.015 Uiso 1 1 calc R . . H4B H -0.1276 0.8835 0.3934 0.015 Uiso 1 1 calc R . . C5 C 0.28842(7) 0.61014(8) 0.31224(7) 0.01223(12) Uani 1 1 d . . . C6 C 0.34930(7) 0.58679(8) 0.40093(8) 0.01565(14) Uani 1 1 d . . . H6 H 0.3936 0.6487 0.4724 0.019 Uiso 1 1 calc R . . C7 C 0.34483(8) 0.47199(9) 0.38414(8) 0.01852(16) Uani 1 1 d . . . H7 H 0.3844 0.4557 0.4450 0.022 Uiso 1 1 calc R . . C8 C 0.28283(8) 0.38148(9) 0.27890(9) 0.01881(16) Uani 1 1 d . . . H8 H 0.2791 0.3034 0.2683 0.023 Uiso 1 1 calc R . . C9 C 0.22642(8) 0.40576(9) 0.18939(8) 0.01804(15) Uani 1 1 d . . . H9 H 0.1865 0.3450 0.1169 0.022 Uiso 1 1 calc R . . C10 C 0.22852(8) 0.51924(8) 0.20604(8) 0.01554(14) Uani 1 1 d . . . H10 H 0.1890 0.5351 0.1449 0.019 Uiso 1 1 calc R . . C11 C 0.39375(7) 0.83791(8) 0.28094(7) 0.01252(12) Uani 1 1 d . . . C12 C 0.49219(8) 0.80765(9) 0.26570(8) 0.01811(16) Uani 1 1 d . . . H12 H 0.4953 0.7378 0.2770 0.022 Uiso 1 1 calc R . . C13 C 0.58588(8) 0.88028(10) 0.23391(9) 0.02189(18) Uani 1 1 d . . . H13 H 0.6524 0.8592 0.2228 0.026 Uiso 1 1 calc R . . C14 C 0.58263(8) 0.98288(9) 0.21847(8) 0.01993(16) Uani 1 1 d . . . H14 H 0.6470 1.0321 0.1970 0.024 Uiso 1 1 calc R . . C15 C 0.48510(8) 1.01405(9) 0.23428(8) 0.01941(16) Uani 1 1 d . . . H15 H 0.4835 1.0850 0.2246 0.023 Uiso 1 1 calc R . . C16 C 0.38999(8) 0.94096(8) 0.26432(8) 0.01675(14) Uani 1 1 d . . . H16 H 0.3224 0.9612 0.2735 0.020 Uiso 1 1 calc R . . C17 C -0.22973(7) 0.64986(7) 0.19484(7) 0.01295(13) Uani 1 1 d . . . C18 C -0.31610(7) 0.64461(8) 0.25425(8) 0.01631(14) Uani 1 1 d . . . H18 H -0.2972 0.7094 0.3210 0.020 Uiso 1 1 calc R . . C19 C -0.42997(8) 0.54418(9) 0.21519(10) 0.02250(19) Uani 1 1 d . . . H19 H -0.4880 0.5399 0.2563 0.027 Uiso 1 1 calc R . . C20 C -0.45920(8) 0.45033(9) 0.11672(10) 0.0253(2) Uani 1 1 d . . . H20 H -0.5374 0.3824 0.0903 0.030 Uiso 1 1 calc R . . C21 C -0.37425(9) 0.45536(9) 0.05662(9) 0.02354(19) Uani 1 1 d . . . H21 H -0.3951 0.3917 -0.0116 0.028 Uiso 1 1 calc R . . C22 C -0.25879(8) 0.55372(8) 0.09647(8) 0.01834(15) Uani 1 1 d . . . H22 H -0.1995 0.5557 0.0569 0.022 Uiso 1 1 calc R . . C23 C -0.10566(7) 0.86912(8) 0.15679(7) 0.01321(13) Uani 1 1 d . . . C24 C -0.21249(8) 0.82318(9) 0.06444(8) 0.01808(15) Uani 1 1 d . . . H24 H -0.2728 0.7430 0.0429 0.022 Uiso 1 1 calc R . . C25 C -0.23100(10) 0.89461(10) 0.00358(9) 0.02413(19) Uani 1 1 d . . . H25 H -0.3033 0.8626 -0.0599 0.029 Uiso 1 1 calc R . . C26 C -0.14438(10) 1.01199(11) 0.03546(10) 0.0263(2) Uani 1 1 d . . . H26 H -0.1575 1.0608 -0.0055 0.032 Uiso 1 1 calc R . . C27 C -0.03813(11) 1.05822(10) 0.12754(11) 0.0287(2) Uani 1 1 d . . . H27 H 0.0211 1.1390 0.1496 0.034 Uiso 1 1 calc R . . C28 C -0.01774(9) 0.98708(9) 0.18776(9) 0.02224(18) Uani 1 1 d . . . H28 H 0.0559 1.0188 0.2498 0.027 Uiso 1 1 calc R . . C29 C 0.06436(7) 0.65473(7) 0.45982(7) 0.01234(12) Uani 1 1 d . . . H29A H 0.1388 0.6379 0.4582 0.015 Uiso 1 1 calc R . . H29B H 0.0606 0.6724 0.5378 0.015 Uiso 1 1 calc R . . C30 C -0.05079(7) 0.54407(7) 0.38386(7) 0.01189(12) Uani 1 1 d . . . C31 C -0.16323(7) 0.50954(8) 0.40993(7) 0.01352(13) Uani 1 1 d . . . H31 H -0.1673 0.5560 0.4784 0.016 Uiso 1 1 calc R . . C32 C -0.26886(7) 0.40822(8) 0.33703(7) 0.01453(13) Uani 1 1 d . . . H32 H -0.3447 0.3865 0.3555 0.017 Uiso 1 1 calc R . . C33 C -0.26384(8) 0.33844(8) 0.23695(7) 0.01511(13) Uani 1 1 d . . . C34 C -0.15166(8) 0.36841(9) 0.21181(8) 0.01933(16) Uani 1 1 d . . . H34 H -0.1467 0.3195 0.1452 0.023 Uiso 1 1 calc R . . C35 C -0.04705(8) 0.47050(8) 0.28497(8) 0.01735(15) Uani 1 1 d . . . H35 H 0.0292 0.4908 0.2672 0.021 Uiso 1 1 calc R . . C36 C -0.37487(10) 0.17649(9) 0.06052(9) 0.02437(18) Uani 1 1 d . . . H36A H -0.3501 0.2305 0.0191 0.037 Uiso 1 1 calc R . . H36B H -0.4594 0.1138 0.0187 0.037 Uiso 1 1 calc R . . H36C H -0.3162 0.1394 0.0697 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00914(3) 0.01035(4) 0.00838(4) 0.00340(3) 0.00292(3) 0.00398(3) I1 0.01692(2) 0.01983(3) 0.00990(2) 0.00589(2) 0.00496(2) 0.00893(2) I2 0.01947(2) 0.01455(2) 0.01715(3) 0.00609(2) 0.00658(2) 0.00549(2) P1 0.00928(7) 0.01243(9) 0.01033(9) 0.00470(7) 0.00332(6) 0.00406(6) P2 0.01003(7) 0.01001(8) 0.01075(9) 0.00359(7) 0.00305(6) 0.00415(6) O1 0.0190(3) 0.0140(3) 0.0162(3) 0.0035(2) 0.0023(2) -0.0017(2) N1 0.0106(2) 0.0096(3) 0.0104(3) 0.0035(2) 0.0036(2) 0.0035(2) C1 0.0126(3) 0.0113(3) 0.0108(3) 0.0017(3) 0.0026(2) 0.0022(2) C2 0.0116(3) 0.0174(4) 0.0113(3) 0.0029(3) 0.0020(2) 0.0040(3) C3 0.0140(3) 0.0129(3) 0.0123(3) 0.0047(3) 0.0062(2) 0.0062(3) C4 0.0146(3) 0.0109(3) 0.0124(3) 0.0032(3) 0.0046(2) 0.0058(3) C5 0.0106(3) 0.0138(3) 0.0138(3) 0.0068(3) 0.0045(2) 0.0050(2) C6 0.0147(3) 0.0178(4) 0.0150(4) 0.0083(3) 0.0036(3) 0.0062(3) C7 0.0187(3) 0.0209(4) 0.0212(4) 0.0130(4) 0.0065(3) 0.0099(3) C8 0.0185(3) 0.0166(4) 0.0257(5) 0.0113(4) 0.0086(3) 0.0087(3) C9 0.0186(3) 0.0160(4) 0.0190(4) 0.0050(3) 0.0046(3) 0.0083(3) C10 0.0164(3) 0.0169(4) 0.0144(4) 0.0057(3) 0.0038(3) 0.0085(3) C11 0.0108(3) 0.0134(3) 0.0124(3) 0.0051(3) 0.0037(2) 0.0035(2) C12 0.0136(3) 0.0223(4) 0.0248(4) 0.0141(4) 0.0093(3) 0.0089(3) C13 0.0143(3) 0.0302(5) 0.0267(5) 0.0163(4) 0.0105(3) 0.0089(3) C14 0.0145(3) 0.0240(4) 0.0165(4) 0.0103(3) 0.0041(3) 0.0008(3) C15 0.0208(4) 0.0147(4) 0.0201(4) 0.0082(3) 0.0060(3) 0.0032(3) C16 0.0174(3) 0.0136(4) 0.0195(4) 0.0067(3) 0.0071(3) 0.0055(3) C17 0.0111(3) 0.0112(3) 0.0152(3) 0.0049(3) 0.0021(2) 0.0040(2) C18 0.0119(3) 0.0168(4) 0.0210(4) 0.0087(3) 0.0054(3) 0.0053(3) C19 0.0118(3) 0.0220(4) 0.0345(6) 0.0156(4) 0.0059(3) 0.0048(3) C20 0.0141(3) 0.0169(4) 0.0363(6) 0.0122(4) -0.0036(3) 0.0006(3) C21 0.0217(4) 0.0130(4) 0.0239(5) 0.0026(3) -0.0041(3) 0.0026(3) C22 0.0186(3) 0.0133(4) 0.0178(4) 0.0023(3) 0.0020(3) 0.0050(3) C23 0.0137(3) 0.0134(3) 0.0145(3) 0.0064(3) 0.0051(3) 0.0066(3) C24 0.0184(3) 0.0180(4) 0.0176(4) 0.0078(3) 0.0021(3) 0.0081(3) C25 0.0263(4) 0.0295(5) 0.0230(5) 0.0153(4) 0.0051(4) 0.0159(4) C26 0.0336(5) 0.0292(5) 0.0309(6) 0.0213(5) 0.0150(4) 0.0196(4) C27 0.0313(5) 0.0202(5) 0.0364(6) 0.0178(5) 0.0101(4) 0.0075(4) C28 0.0203(4) 0.0176(4) 0.0261(5) 0.0119(4) 0.0043(3) 0.0033(3) C29 0.0131(3) 0.0121(3) 0.0119(3) 0.0060(3) 0.0037(2) 0.0043(2) C30 0.0126(3) 0.0112(3) 0.0118(3) 0.0054(3) 0.0041(2) 0.0038(2) C31 0.0148(3) 0.0128(3) 0.0135(3) 0.0055(3) 0.0062(3) 0.0048(3) C32 0.0139(3) 0.0139(3) 0.0157(4) 0.0068(3) 0.0058(3) 0.0040(3) C33 0.0163(3) 0.0117(3) 0.0131(3) 0.0052(3) 0.0027(3) 0.0014(3) C34 0.0209(4) 0.0153(4) 0.0156(4) 0.0016(3) 0.0086(3) 0.0020(3) C35 0.0167(3) 0.0155(4) 0.0167(4) 0.0033(3) 0.0085(3) 0.0032(3) C36 0.0303(5) 0.0157(4) 0.0158(4) 0.0029(3) 0.0027(4) 0.0013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.0051(7) . yes Ni1 P2 2.1916(2) . yes Ni1 P1 2.2139(2) . yes Ni1 I1 2.4739(2) . yes P1 C11 1.8094(8) . ? P1 C5 1.8192(8) . ? P1 C2 1.8492(9) . ? P2 C17 1.8113(8) . ? P2 C23 1.8171(8) . ? P2 C4 1.8252(9) . ? O1 C33 1.3651(10) . ? O1 C36 1.4313(12) . ? N1 C1 1.5047(10) . ? N1 C3 1.5107(9) . ? N1 C29 1.5146(10) . ? C1 C2 1.5337(10) . ? C3 C4 1.5214(11) . ? C5 C6 1.3982(11) . ? C5 C10 1.4013(12) . ? C6 C7 1.3994(12) . ? C7 C8 1.3923(14) . ? C8 C9 1.3912(12) . ? C9 C10 1.3932(12) . ? C11 C12 1.3953(10) . ? C11 C16 1.3974(11) . ? C12 C13 1.3925(12) . ? C13 C14 1.3838(14) . ? C14 C15 1.3926(13) . ? C15 C16 1.3922(12) . ? C17 C18 1.3979(11) . ? C17 C22 1.4014(13) . ? C18 C19 1.3922(12) . ? C19 C20 1.3860(16) . ? C20 C21 1.3903(16) . ? C21 C22 1.3908(13) . ? C23 C24 1.3954(12) . ? C23 C28 1.3957(13) . ? C24 C25 1.3953(12) . ? C25 C26 1.3837(16) . ? C26 C27 1.3887(16) . ? C27 C28 1.3929(13) . ? C29 C30 1.5047(11) . ? C30 C35 1.3953(12) . ? C30 C31 1.4017(10) . ? C31 C32 1.3897(12) . ? C32 C33 1.3933(12) . ? C33 C34 1.3918(12) . ? C34 C35 1.3894(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P2 87.992(18) . . yes N1 Ni1 P1 86.535(18) . . yes P2 Ni1 P1 164.876(10) . . yes N1 Ni1 I1 177.22(2) . . yes P2 Ni1 I1 91.888(7) . . yes P1 Ni1 I1 94.251(7) . . yes C11 P1 C5 106.20(4) . . ? C11 P1 C2 106.07(4) . . ? C5 P1 C2 108.83(4) . . ? C11 P1 Ni1 117.94(3) . . ? C5 P1 Ni1 117.00(3) . . ? C2 P1 Ni1 99.86(2) . . ? C17 P2 C23 105.57(4) . . ? C17 P2 C4 108.80(4) . . ? C23 P2 C4 104.83(4) . . ? C17 P2 Ni1 114.56(3) . . ? C23 P2 Ni1 124.28(3) . . ? C4 P2 Ni1 97.24(2) . . ? C33 O1 C36 117.59(7) . . ? C1 N1 C3 108.04(6) . . ? C1 N1 C29 108.40(6) . . ? C3 N1 C29 107.11(6) . . ? C1 N1 Ni1 105.90(5) . . ? C3 N1 Ni1 114.06(5) . . ? C29 N1 Ni1 113.10(5) . . ? N1 C1 C2 112.75(7) . . ? C1 C2 P1 108.76(5) . . ? N1 C3 C4 111.76(6) . . ? C3 C4 P2 105.61(5) . . ? C6 C5 C10 119.23(8) . . ? C6 C5 P1 123.15(7) . . ? C10 C5 P1 117.51(6) . . ? C5 C6 C7 119.85(9) . . ? C8 C7 C6 120.47(8) . . ? C9 C8 C7 119.78(8) . . ? C8 C9 C10 120.01(9) . . ? C9 C10 C5 120.57(8) . . ? C12 C11 C16 119.74(7) . . ? C12 C11 P1 121.48(6) . . ? C16 C11 P1 118.70(6) . . ? C13 C12 C11 119.77(8) . . ? C14 C13 C12 120.43(8) . . ? C13 C14 C15 120.10(8) . . ? C16 C15 C14 119.86(8) . . ? C15 C16 C11 120.09(8) . . ? C18 C17 C22 119.54(8) . . ? C18 C17 P2 121.86(7) . . ? C22 C17 P2 118.59(6) . . ? C19 C18 C17 119.77(9) . . ? C20 C19 C18 120.45(9) . . ? C19 C20 C21 120.12(9) . . ? C20 C21 C22 119.94(10) . . ? C21 C22 C17 120.14(9) . . ? C24 C23 C28 119.41(8) . . ? C24 C23 P2 121.07(7) . . ? C28 C23 P2 119.50(7) . . ? C25 C24 C23 120.22(9) . . ? C26 C25 C24 120.17(9) . . ? C25 C26 C27 119.81(9) . . ? C26 C27 C28 120.48(10) . . ? C27 C28 C23 119.90(9) . . ? C30 C29 N1 114.27(6) . . ? C35 C30 C31 117.79(8) . . ? C35 C30 C29 120.01(7) . . ? C31 C30 C29 122.18(7) . . ? C32 C31 C30 120.91(8) . . ? C31 C32 C33 120.15(7) . . ? O1 C33 C34 124.22(8) . . ? O1 C33 C32 116.00(7) . . ? C34 C33 C32 119.78(8) . . ? C35 C34 C33 119.44(8) . . ? C34 C35 C30 121.84(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 47.94 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.642 _refine_diff_density_min -1.927 _refine_diff_density_rms 0.126 #===END data_dqc15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H37 Co I2 N O P2' _chemical_formula_sum 'C36 H37 Co I2 N O P2' _chemical_formula_weight 874.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.2880(4) _cell_length_b 13.5281(5) _cell_length_c 27.2546(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3424.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9561 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 40.69 _exptl_crystal_description Needle _exptl_crystal_colour Green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 2.427 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5944 _exptl_absorpt_correction_T_max 0.7482 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KAPPA APEX II' _diffrn_measurement_method '\w scans; 17 settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 211299 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 41.83 _reflns_number_total 23667 _reflns_number_gt 21941 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.7-0' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(4) _refine_ls_number_reflns 23667 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0381 _refine_ls_wR_factor_gt 0.0376 _refine_ls_goodness_of_fit_ref 1.548 _refine_ls_restrained_S_all 1.548 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.191666(15) 0.784492(10) 0.181645(5) 0.01008(2) Uani 1 1 d . . . I1 I 0.281623(9) 0.769529(5) 0.270773(3) 0.01692(2) Uani 1 1 d . . . I2 I 0.050091(8) 0.635655(5) 0.151177(3) 0.01485(1) Uani 1 1 d . . . P1 P 0.05022(3) 0.928994(19) 0.185184(10) 0.01037(4) Uani 1 1 d . . . P2 P 0.39543(3) 0.80056(2) 0.130974(10) 0.01037(5) Uani 1 1 d . . . O1 O 0.39740(12) 1.14016(8) -0.07789(3) 0.0260(2) Uani 1 1 d . . . N1 N 0.35377(10) 1.02523(7) 0.14963(4) 0.01176(15) Uani 1 1 d . . . C1 C 0.31602(12) 1.02533(8) 0.20201(4) 0.01234(18) Uani 1 1 d . . . H1A H 0.3643 1.0820 0.2180 0.015 Uiso 1 1 calc R . . H1B H 0.3538 0.9641 0.2172 0.015 Uiso 1 1 calc R . . C2 C 0.15373(12) 1.03188(8) 0.21215(4) 0.01351(18) Uani 1 1 d . . . H2A H 0.1168 1.0950 0.1988 0.016 Uiso 1 1 calc R . . H2B H 0.1380 1.0326 0.2481 0.016 Uiso 1 1 calc R . . C3 C 0.50456(12) 0.99473(8) 0.14274(4) 0.01347(18) Uani 1 1 d . . . H3A H 0.5665 1.0360 0.1641 0.016 Uiso 1 1 calc R . . H3B H 0.5325 1.0080 0.1083 0.016 Uiso 1 1 calc R . . C4 C 0.53409(11) 0.88522(8) 0.15419(4) 0.01331(18) Uani 1 1 d . . . H4A H 0.5417 0.8770 0.1902 0.016 Uiso 1 1 calc R . . H4B H 0.6280 0.8666 0.1397 0.016 Uiso 1 1 calc R . . C5 C -0.03567(12) 0.97454(8) 0.12922(4) 0.01286(18) Uani 1 1 d . . . C6 C -0.07581(13) 1.07335(9) 0.12244(5) 0.0172(2) Uani 1 1 d . . . H6 H -0.0556 1.1208 0.1472 0.021 Uiso 1 1 calc R . . C7 C -0.14527(14) 1.10238(10) 0.07951(5) 0.0210(2) Uani 1 1 d . . . H7 H -0.1726 1.1695 0.0752 0.025 Uiso 1 1 calc R . . C8 C -0.17470(14) 1.03378(11) 0.04310(5) 0.0231(3) Uani 1 1 d . . . H8 H -0.2206 1.0540 0.0136 0.028 Uiso 1 1 calc R . . C9 C -0.13705(14) 0.93556(11) 0.04981(5) 0.0204(2) Uani 1 1 d . . . H9 H -0.1572 0.8885 0.0249 0.025 Uiso 1 1 calc R . . C10 C -0.06982(12) 0.90562(9) 0.09295(4) 0.0152(2) Uani 1 1 d . . . H10 H -0.0470 0.8378 0.0977 0.018 Uiso 1 1 calc R . . C11 C -0.10327(11) 0.91450(8) 0.22637(4) 0.01178(17) Uani 1 1 d . . . C12 C -0.18629(13) 0.99563(8) 0.24038(5) 0.0165(2) Uani 1 1 d . . . H12 H -0.1624 1.0597 0.2286 0.020 Uiso 1 1 calc R . . C13 C -0.30401(13) 0.98338(9) 0.27146(5) 0.0188(2) Uani 1 1 d . . . H13 H -0.3593 1.0391 0.2813 0.023 Uiso 1 1 calc R . . C14 C -0.34030(13) 0.88959(9) 0.28806(4) 0.0178(2) Uani 1 1 d . . . H14 H -0.4203 0.8809 0.3094 0.021 Uiso 1 1 calc R . . C15 C -0.25954(13) 0.80869(9) 0.27350(5) 0.0195(2) Uani 1 1 d . . . H15 H -0.2855 0.7445 0.2845 0.023 Uiso 1 1 calc R . . C16 C -0.14071(14) 0.82050(9) 0.24294(4) 0.0169(2) Uani 1 1 d . . . H16 H -0.0853 0.7647 0.2334 0.020 Uiso 1 1 calc R . . C17 C 0.37141(12) 0.82900(8) 0.06646(4) 0.01172(17) Uani 1 1 d . . . C18 C 0.48506(12) 0.86471(9) 0.03774(4) 0.01582(19) Uani 1 1 d . . . H18 H 0.5759 0.8776 0.0524 0.019 Uiso 1 1 calc R . . C19 C 0.46547(14) 0.88127(9) -0.01201(4) 0.0188(2) Uani 1 1 d . . . H19 H 0.5431 0.9053 -0.0313 0.023 Uiso 1 1 calc R . . C20 C 0.33223(14) 0.86280(10) -0.03380(4) 0.0188(2) Uani 1 1 d . . . H20 H 0.3189 0.8744 -0.0679 0.023 Uiso 1 1 calc R . . C21 C 0.21950(14) 0.82750(9) -0.00558(4) 0.0179(2) Uani 1 1 d . . . H21 H 0.1286 0.8152 -0.0204 0.022 Uiso 1 1 calc R . . C22 C 0.23846(12) 0.80996(9) 0.04431(4) 0.01477(19) Uani 1 1 d . . . H22 H 0.1609 0.7850 0.0634 0.018 Uiso 1 1 calc R . . C23 C 0.48311(11) 0.67967(8) 0.12918(4) 0.01186(18) Uani 1 1 d . . . C24 C 0.59671(13) 0.65486(9) 0.16026(4) 0.0161(2) Uani 1 1 d . . . H24 H 0.6353 0.7028 0.1820 0.019 Uiso 1 1 calc R . . C25 C 0.65373(13) 0.55909(9) 0.15930(5) 0.0183(2) Uani 1 1 d . . . H25 H 0.7306 0.5422 0.1807 0.022 Uiso 1 1 calc R . . C26 C 0.59903(14) 0.48880(9) 0.12737(5) 0.0184(2) Uani 1 1 d . . . H26 H 0.6395 0.4243 0.1265 0.022 Uiso 1 1 calc R . . C27 C 0.48537(14) 0.51278(9) 0.09678(5) 0.0187(2) Uani 1 1 d . . . H27 H 0.4471 0.4644 0.0751 0.022 Uiso 1 1 calc R . . C28 C 0.42701(13) 0.60751(8) 0.09765(4) 0.0156(2) Uani 1 1 d . . . H28 H 0.3485 0.6234 0.0767 0.019 Uiso 1 1 calc R . . C29 C 0.33603(13) 1.12594(8) 0.12923(4) 0.01447(19) Uani 1 1 d . . . H29A H 0.4070 1.1703 0.1450 0.017 Uiso 1 1 calc R . . H29B H 0.2387 1.1504 0.1378 0.017 Uiso 1 1 calc R . . C30 C 0.35488(12) 1.13190(8) 0.07446(4) 0.01401(18) Uani 1 1 d . . . C31 C 0.47310(13) 1.17898(9) 0.05362(5) 0.0180(2) Uani 1 1 d . . . H31 H 0.5423 1.2090 0.0745 0.022 Uiso 1 1 calc R . . C32 C 0.49301(15) 1.18334(10) 0.00285(5) 0.0206(2) Uani 1 1 d . . . H32 H 0.5756 1.2147 -0.0106 0.025 Uiso 1 1 calc R . . C33 C 0.39062(14) 1.14126(9) -0.02771(4) 0.0181(2) Uani 1 1 d . . . C34 C 0.26871(14) 1.09630(9) -0.00743(4) 0.0178(2) Uani 1 1 d . . . H34 H 0.1969 1.0694 -0.0283 0.021 Uiso 1 1 calc R . . C35 C 0.25232(13) 1.09091(9) 0.04291(4) 0.0160(2) Uani 1 1 d . . . H35 H 0.1701 1.0589 0.0563 0.019 Uiso 1 1 calc R . . C36 C 0.53456(19) 1.15868(11) -0.09986(6) 0.0324(3) Uani 1 1 d . . . H36A H 0.5666 1.2255 -0.0913 0.049 Uiso 1 1 calc R . . H36B H 0.5264 1.1528 -0.1356 0.049 Uiso 1 1 calc R . . H36C H 0.6046 1.1104 -0.0877 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.00994(6) 0.01101(6) 0.00928(6) -0.00018(4) 0.00027(4) -0.00038(4) I1 0.02277(4) 0.01629(3) 0.01169(3) 0.00258(2) -0.00493(3) -0.00557(3) I2 0.01604(3) 0.01508(3) 0.01343(3) -0.00111(2) -0.00165(2) -0.00370(3) P1 0.01035(11) 0.01090(10) 0.00987(11) 0.00018(8) 0.00134(10) -0.00068(9) P2 0.00950(11) 0.01283(11) 0.00879(11) -0.00004(8) -0.00012(9) 0.00047(9) O1 0.0363(5) 0.0286(5) 0.0130(4) 0.0021(4) 0.0037(4) -0.0058(4) N1 0.0119(4) 0.0127(4) 0.0107(4) 0.0009(3) 0.0010(3) -0.0001(3) C1 0.0128(5) 0.0131(4) 0.0111(4) -0.0009(3) 0.0008(3) -0.0021(3) C2 0.0138(5) 0.0132(4) 0.0135(5) -0.0025(3) 0.0017(4) -0.0017(3) C3 0.0115(4) 0.0141(4) 0.0148(5) 0.0009(3) 0.0008(3) -0.0014(3) C4 0.0106(4) 0.0155(4) 0.0138(4) -0.0010(3) -0.0017(4) -0.0002(3) C5 0.0105(4) 0.0161(4) 0.0120(4) 0.0025(3) 0.0022(3) 0.0008(4) C6 0.0151(5) 0.0160(5) 0.0205(5) 0.0040(4) 0.0008(4) 0.0005(4) C7 0.0169(5) 0.0210(5) 0.0251(6) 0.0095(5) -0.0009(5) 0.0024(4) C8 0.0158(5) 0.0356(7) 0.0181(6) 0.0099(5) -0.0031(4) 0.0014(5) C9 0.0165(5) 0.0305(6) 0.0143(5) 0.0002(5) -0.0024(4) 0.0009(5) C10 0.0127(5) 0.0189(5) 0.0139(5) -0.0002(4) 0.0004(4) 0.0014(4) C11 0.0113(4) 0.0134(4) 0.0106(4) -0.0003(3) 0.0013(3) -0.0007(3) C12 0.0157(5) 0.0127(4) 0.0211(5) -0.0018(4) 0.0052(4) -0.0008(4) C13 0.0149(5) 0.0187(5) 0.0227(5) -0.0065(4) 0.0048(5) -0.0007(4) C14 0.0148(5) 0.0238(6) 0.0147(5) -0.0041(4) 0.0048(4) -0.0042(4) C15 0.0215(6) 0.0184(5) 0.0188(5) 0.0033(4) 0.0073(4) -0.0032(4) C16 0.0193(5) 0.0147(5) 0.0169(5) 0.0020(4) 0.0073(4) 0.0015(4) C17 0.0117(4) 0.0134(4) 0.0101(4) -0.0002(3) 0.0003(3) 0.0020(3) C18 0.0128(5) 0.0220(5) 0.0126(4) 0.0006(4) 0.0017(3) 0.0010(4) C19 0.0200(6) 0.0238(6) 0.0127(5) 0.0020(4) 0.0049(4) 0.0005(4) C20 0.0252(6) 0.0211(5) 0.0100(4) 0.0005(4) -0.0013(4) 0.0061(5) C21 0.0184(5) 0.0208(5) 0.0146(5) -0.0006(4) -0.0045(4) 0.0018(4) C22 0.0133(5) 0.0173(5) 0.0136(5) 0.0019(4) -0.0010(4) 0.0006(4) C23 0.0111(4) 0.0142(4) 0.0103(4) 0.0014(3) 0.0016(3) 0.0014(3) C24 0.0147(5) 0.0187(5) 0.0149(5) 0.0011(4) -0.0026(4) 0.0011(4) C25 0.0147(5) 0.0213(5) 0.0188(6) 0.0056(4) -0.0006(4) 0.0045(4) C26 0.0194(5) 0.0174(5) 0.0183(5) 0.0044(4) 0.0062(4) 0.0048(4) C27 0.0219(6) 0.0168(5) 0.0176(5) -0.0019(4) 0.0014(4) 0.0034(4) C28 0.0150(5) 0.0164(5) 0.0155(5) -0.0014(4) -0.0015(4) 0.0026(4) C29 0.0177(5) 0.0119(4) 0.0138(4) 0.0002(3) 0.0015(4) 0.0004(4) C30 0.0166(5) 0.0127(4) 0.0127(4) 0.0026(4) 0.0013(4) 0.0013(4) C31 0.0185(6) 0.0178(5) 0.0177(5) 0.0026(4) -0.0008(4) -0.0039(4) C32 0.0218(6) 0.0210(5) 0.0191(6) 0.0050(4) 0.0041(4) -0.0048(4) C33 0.0253(6) 0.0149(5) 0.0139(5) 0.0037(4) 0.0011(4) 0.0008(4) C34 0.0196(5) 0.0179(5) 0.0159(5) 0.0002(4) -0.0020(4) -0.0017(4) C35 0.0159(5) 0.0161(5) 0.0160(5) 0.0016(4) 0.0008(4) -0.0012(4) C36 0.0429(9) 0.0304(7) 0.0239(7) 0.0029(5) 0.0136(6) -0.0010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 P2 2.3529(3) . yes Co1 P1 2.3572(3) . yes Co1 I2 2.54416(17) . yes Co1 I1 2.57678(19) . yes P1 C11 1.8250(11) . ? P1 C5 1.8281(11) . ? P1 C2 1.8443(11) . ? P2 C17 1.8137(11) . ? P2 C23 1.8277(11) . ? P2 C4 1.8359(11) . ? O1 C33 1.3690(15) . ? O1 C36 1.4298(19) . ? N1 C1 1.4700(14) . ? N1 C3 1.4721(15) . ? N1 C29 1.4807(14) . ? C1 C2 1.5350(16) . ? C3 C4 1.5386(15) . ? C5 C10 1.3955(16) . ? C5 C6 1.4000(16) . ? C6 C7 1.3925(18) . ? C7 C8 1.386(2) . ? C8 C9 1.386(2) . ? C9 C10 1.3915(17) . ? C11 C16 1.3935(16) . ? C11 C12 1.3946(16) . ? C12 C13 1.3929(17) . ? C13 C14 1.3887(18) . ? C14 C15 1.3849(18) . ? C15 C16 1.3920(17) . ? C17 C18 1.4001(16) . ? C17 C22 1.3985(16) . ? C18 C19 1.3862(16) . ? C19 C20 1.3952(18) . ? C20 C21 1.3841(19) . ? C21 C22 1.3914(16) . ? C23 C24 1.3942(16) . ? C23 C28 1.4009(16) . ? C24 C25 1.3998(17) . ? C25 C26 1.3856(19) . ? C26 C27 1.3838(18) . ? C27 C28 1.3916(17) . ? C29 C30 1.5051(15) . ? C30 C31 1.3907(17) . ? C30 C35 1.3981(17) . ? C31 C32 1.3973(18) . ? C32 C33 1.3865(19) . ? C33 C34 1.3991(18) . ? C34 C35 1.3822(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Co1 P1 113.307(11) . . yes P2 Co1 I2 107.294(9) . . yes P1 Co1 I2 112.434(10) . . yes P2 Co1 I1 107.443(9) . . yes P1 Co1 I1 101.964(9) . . yes I2 Co1 I1 114.400(6) . . yes C11 P1 C5 102.03(5) . . ? C11 P1 C2 104.08(5) . . ? C5 P1 C2 107.79(5) . . ? C11 P1 Co1 111.80(4) . . ? C5 P1 Co1 119.25(4) . . ? C2 P1 Co1 110.59(4) . . ? C17 P2 C23 102.63(5) . . ? C17 P2 C4 106.74(5) . . ? C23 P2 C4 104.77(5) . . ? C17 P2 Co1 119.32(4) . . ? C23 P2 Co1 106.94(4) . . ? C4 P2 Co1 114.81(4) . . ? C33 O1 C36 117.22(12) . . ? C1 N1 C3 110.56(9) . . ? C1 N1 C29 109.71(8) . . ? C3 N1 C29 108.42(9) . . ? N1 C1 C2 114.15(9) . . ? C1 C2 P1 113.36(8) . . ? N1 C3 C4 114.43(9) . . ? C3 C4 P2 113.93(7) . . ? C10 C5 C6 118.93(11) . . ? C10 C5 P1 117.72(8) . . ? C6 C5 P1 123.25(9) . . ? C7 C6 C5 120.24(12) . . ? C8 C7 C6 120.28(12) . . ? C7 C8 C9 119.84(12) . . ? C8 C9 C10 120.25(12) . . ? C9 C10 C5 120.41(11) . . ? C16 C11 C12 119.44(10) . . ? C16 C11 P1 119.49(8) . . ? C12 C11 P1 121.05(8) . . ? C13 C12 C11 120.46(10) . . ? C14 C13 C12 119.82(11) . . ? C15 C14 C13 119.82(11) . . ? C14 C15 C16 120.68(11) . . ? C15 C16 C11 119.77(11) . . ? C18 C17 C22 119.20(10) . . ? C18 C17 P2 121.50(8) . . ? C22 C17 P2 119.22(8) . . ? C19 C18 C17 120.24(11) . . ? C18 C19 C20 120.25(11) . . ? C21 C20 C19 119.75(11) . . ? C20 C21 C22 120.40(11) . . ? C21 C22 C17 120.15(11) . . ? C24 C23 C28 119.11(10) . . ? C24 C23 P2 122.43(9) . . ? C28 C23 P2 118.31(8) . . ? C23 C24 C25 119.85(11) . . ? C26 C25 C24 120.54(11) . . ? C27 C26 C25 119.83(11) . . ? C26 C27 C28 120.18(12) . . ? C27 C28 C23 120.48(11) . . ? N1 C29 C30 114.12(9) . . ? C31 C30 C35 117.92(10) . . ? C31 C30 C29 121.43(11) . . ? C35 C30 C29 120.64(10) . . ? C30 C31 C32 121.89(11) . . ? C33 C32 C31 119.14(11) . . ? O1 C33 C32 124.96(11) . . ? O1 C33 C34 115.29(11) . . ? C32 C33 C34 119.75(11) . . ? C35 C34 C33 120.28(11) . . ? C34 C35 C30 120.97(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 41.83 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.983 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.097 #===END data_dqc16 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H33 I N Ni P2, C4 H8 O, I' _chemical_formula_sum 'C38 H41 I2 N Ni O P2' _chemical_formula_weight 902.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7033(3) _cell_length_b 12.3287(4) _cell_length_c 15.5781(5) _cell_angle_alpha 86.4940(10) _cell_angle_beta 87.5220(10) _cell_angle_gamma 89.1920(10) _cell_volume 1858.24(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9601 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 36.36 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.299 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.7471 _exptl_absorpt_process_details 'SADABS v2008/1, Bruker-AXS, Madison, WI' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 15 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 81487 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 36.37 _reflns_number_total 17784 _reflns_number_gt 15405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.630' _computing_cell_refinement 'Bruker SAINT-Plus v7.66A' _computing_data_reduction 'Bruker SAINT-Plus v7.66A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker XP v5.1' _computing_publication_material 'Bruker XCIF 2008' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type 'Full matrix' _refine_ls_weighting_scheme Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary 'Direct methods' _atom_sites_solution_secondary 'Difference Fourier map' _atom_sites_solution_hydrogens 'Geometric positions' _refine_ls_hydrogen_treatment Riding _chemical_absolute_configuration ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17784 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0348 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 2.081 _refine_ls_restrained_S_all 2.081 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.505575(18) 0.248397(14) 0.284235(11) 0.01116(3) Uani 1 1 d . . . I1 I 0.368500(10) 0.236926(7) 0.153901(6) 0.01613(2) Uani 1 1 d . . . I2 I 0.748324(10) 0.757325(8) 0.420280(6) 0.01749(2) Uani 1 1 d . . . P1 P 0.48803(4) 0.42853(3) 0.28578(2) 0.01240(5) Uani 1 1 d . . . P2 P 0.53855(4) 0.06976(3) 0.29464(2) 0.01246(5) Uani 1 1 d . . . N1 N 0.61756(12) 0.25306(9) 0.38805(7) 0.01293(17) Uani 1 1 d . . . C1 C 0.57288(15) 0.34715(11) 0.44069(9) 0.0157(2) Uani 1 1 d . . . H1A H 0.6345 0.3520 0.4893 0.019 Uiso 1 1 calc R . . H1B H 0.4777 0.3354 0.4647 0.019 Uiso 1 1 calc R . . C2 C 0.57837(15) 0.45226(11) 0.38440(9) 0.0158(2) Uani 1 1 d . . . H2A H 0.6754 0.4725 0.3699 0.019 Uiso 1 1 calc R . . H2B H 0.5327 0.5120 0.4150 0.019 Uiso 1 1 calc R . . C3 C 0.59633(15) 0.15000(11) 0.44449(9) 0.0154(2) Uani 1 1 d . . . H3A H 0.4985 0.1450 0.4651 0.018 Uiso 1 1 calc R . . H3B H 0.6541 0.1511 0.4953 0.018 Uiso 1 1 calc R . . C4 C 0.63546(15) 0.05245(11) 0.39342(9) 0.0161(2) Uani 1 1 d . . . H4A H 0.6096 -0.0160 0.4264 0.019 Uiso 1 1 calc R . . H4B H 0.7360 0.0508 0.3795 0.019 Uiso 1 1 calc R . . C5 C 0.57525(14) 0.51584(11) 0.20304(9) 0.0142(2) Uani 1 1 d . . . C6 C 0.62733(17) 0.61476(12) 0.22736(10) 0.0192(2) Uani 1 1 d . . . H6 H 0.6144 0.6346 0.2852 0.023 Uiso 1 1 calc R . . C7 C 0.69788(18) 0.68373(13) 0.16698(11) 0.0222(3) Uani 1 1 d . . . H7 H 0.7342 0.7500 0.1838 0.027 Uiso 1 1 calc R . . C8 C 0.71517(17) 0.65537(13) 0.08177(10) 0.0211(3) Uani 1 1 d . . . H8 H 0.7626 0.7027 0.0405 0.025 Uiso 1 1 calc R . . C9 C 0.66302(18) 0.55788(13) 0.05725(10) 0.0221(3) Uani 1 1 d . . . H9 H 0.6745 0.5390 -0.0009 0.027 Uiso 1 1 calc R . . C10 C 0.59392(17) 0.48769(12) 0.11770(9) 0.0187(2) Uani 1 1 d . . . H10 H 0.5596 0.4208 0.1009 0.022 Uiso 1 1 calc R . . C11 C 0.31623(15) 0.48713(11) 0.29888(9) 0.0156(2) Uani 1 1 d . . . C12 C 0.25013(17) 0.49306(13) 0.38068(10) 0.0204(3) Uani 1 1 d . . . H12 H 0.2952 0.4661 0.4307 0.025 Uiso 1 1 calc R . . C13 C 0.11804(18) 0.53873(14) 0.38785(13) 0.0258(3) Uani 1 1 d . . . H13 H 0.0746 0.5449 0.4432 0.031 Uiso 1 1 calc R . . C14 C 0.04911(18) 0.57533(14) 0.31491(14) 0.0275(3) Uani 1 1 d . . . H14 H -0.0412 0.6056 0.3204 0.033 Uiso 1 1 calc R . . C15 C 0.11322(17) 0.56730(14) 0.23390(13) 0.0249(3) Uani 1 1 d . . . H15 H 0.0660 0.5914 0.1839 0.030 Uiso 1 1 calc R . . C16 C 0.24637(16) 0.52414(12) 0.22554(10) 0.0195(2) Uani 1 1 d . . . H16 H 0.2899 0.5198 0.1700 0.023 Uiso 1 1 calc R . . C17 C 0.63922(14) 0.01196(11) 0.20741(9) 0.0152(2) Uani 1 1 d . . . C18 C 0.78386(16) 0.00711(13) 0.20742(11) 0.0211(3) Uani 1 1 d . . . H18 H 0.8305 0.0278 0.2561 0.025 Uiso 1 1 calc R . . C19 C 0.85939(18) -0.02839(15) 0.13542(12) 0.0260(3) Uani 1 1 d . . . H19 H 0.9572 -0.0324 0.1356 0.031 Uiso 1 1 calc R . . C20 C 0.79139(19) -0.05763(14) 0.06382(11) 0.0252(3) Uani 1 1 d . . . H20 H 0.8430 -0.0805 0.0148 0.030 Uiso 1 1 calc R . . C21 C 0.64840(19) -0.05359(13) 0.06356(10) 0.0223(3) Uani 1 1 d . . . H21 H 0.6024 -0.0743 0.0146 0.027 Uiso 1 1 calc R . . C22 C 0.57202(16) -0.01921(12) 0.13500(9) 0.0179(2) Uani 1 1 d . . . H22 H 0.4741 -0.0169 0.1346 0.022 Uiso 1 1 calc R . . C23 C 0.38684(14) -0.01364(11) 0.31498(9) 0.0146(2) Uani 1 1 d . . . C24 C 0.39405(15) -0.12636(11) 0.30730(9) 0.0169(2) Uani 1 1 d . . . H24 H 0.4784 -0.1597 0.2893 0.020 Uiso 1 1 calc R . . C25 C 0.27706(17) -0.18930(13) 0.32619(10) 0.0202(3) Uani 1 1 d . . . H25 H 0.2815 -0.2655 0.3202 0.024 Uiso 1 1 calc R . . C26 C 0.15336(17) -0.14068(14) 0.35386(11) 0.0225(3) Uani 1 1 d . . . H26 H 0.0734 -0.1835 0.3657 0.027 Uiso 1 1 calc R . . C27 C 0.14755(17) -0.02951(15) 0.36403(13) 0.0267(3) Uani 1 1 d . . . H27 H 0.0641 0.0031 0.3845 0.032 Uiso 1 1 calc R . . C28 C 0.26358(16) 0.03469(13) 0.34438(12) 0.0223(3) Uani 1 1 d . . . H28 H 0.2589 0.1108 0.3509 0.027 Uiso 1 1 calc R . . C29 C 0.76447(14) 0.26410(11) 0.35948(9) 0.0137(2) Uani 1 1 d . . . C30 C 0.86712(16) 0.26133(14) 0.41992(10) 0.0206(3) Uani 1 1 d . . . H30 H 0.8428 0.2530 0.4797 0.025 Uiso 1 1 calc R . . C31 C 1.00464(17) 0.27071(15) 0.39245(12) 0.0244(3) Uani 1 1 d . . . H31 H 1.0744 0.2681 0.4335 0.029 Uiso 1 1 calc R . . C32 C 1.04082(16) 0.28390(14) 0.30519(12) 0.0226(3) Uani 1 1 d . . . H32 H 1.1351 0.2908 0.2868 0.027 Uiso 1 1 calc R . . C33 C 0.93964(16) 0.28696(14) 0.24508(10) 0.0209(3) Uani 1 1 d . . . H33 H 0.9646 0.2956 0.1854 0.025 Uiso 1 1 calc R . . C34 C 0.80081(15) 0.27731(12) 0.27201(9) 0.0170(2) Uani 1 1 d . . . H34 H 0.7314 0.2798 0.2307 0.020 Uiso 1 1 calc R . . O1 O 0.70240(16) 0.33728(13) 0.96125(10) 0.0319(3) Uani 1 1 d . . . C41 C 0.8011(3) 0.2945(2) 1.02043(15) 0.0434(6) Uani 1 1 d . . . H41A H 0.7544 0.2567 1.0713 0.052 Uiso 1 1 calc R . . H41B H 0.8583 0.3533 1.0400 0.052 Uiso 1 1 calc R . . C42 C 0.8900(2) 0.21440(18) 0.96948(14) 0.0321(4) Uani 1 1 d . . . H42A H 0.9203 0.1518 1.0072 0.038 Uiso 1 1 calc R . . H42B H 0.9722 0.2505 0.9415 0.038 Uiso 1 1 calc R . . C43 C 0.7917(2) 0.17855(16) 0.90241(13) 0.0289(3) Uani 1 1 d . . . H43A H 0.8306 0.1946 0.8433 0.035 Uiso 1 1 calc R . . H43B H 0.7731 0.0998 0.9106 0.035 Uiso 1 1 calc R . . C44 C 0.6607(2) 0.24536(17) 0.91890(15) 0.0318(4) Uani 1 1 d . . . H44A H 0.6181 0.2682 0.8640 0.038 Uiso 1 1 calc R . . H44B H 0.5929 0.2024 0.9556 0.038 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01317(7) 0.00893(6) 0.01145(7) -0.00114(5) -0.00064(5) 0.00032(5) I1 0.01918(4) 0.01439(4) 0.01521(4) -0.00148(3) -0.00466(3) 0.00015(3) I2 0.01676(4) 0.01720(4) 0.01872(4) -0.00270(3) -0.00149(3) 0.00212(3) P1 0.01565(14) 0.00964(13) 0.01190(13) -0.00127(10) 0.00019(10) 0.00067(10) P2 0.01373(13) 0.00950(12) 0.01414(13) -0.00118(10) 0.00025(10) 0.00022(10) N1 0.0161(5) 0.0108(4) 0.0118(4) -0.0005(3) 0.0004(3) -0.0003(3) C1 0.0227(6) 0.0131(5) 0.0115(5) -0.0020(4) 0.0004(4) 0.0003(4) C2 0.0224(6) 0.0120(5) 0.0133(5) -0.0017(4) -0.0013(4) -0.0009(4) C3 0.0210(6) 0.0124(5) 0.0124(5) 0.0014(4) -0.0001(4) -0.0010(4) C4 0.0194(6) 0.0121(5) 0.0167(5) 0.0007(4) -0.0023(4) 0.0005(4) C5 0.0172(5) 0.0112(5) 0.0139(5) -0.0005(4) 0.0000(4) 0.0006(4) C6 0.0289(7) 0.0122(5) 0.0166(6) -0.0010(4) -0.0008(5) -0.0039(5) C7 0.0307(8) 0.0156(6) 0.0204(6) 0.0010(5) -0.0026(5) -0.0076(5) C8 0.0256(7) 0.0179(6) 0.0192(6) 0.0028(5) 0.0016(5) -0.0038(5) C9 0.0301(8) 0.0197(6) 0.0162(6) -0.0012(5) 0.0047(5) -0.0044(5) C10 0.0250(7) 0.0158(6) 0.0152(5) -0.0021(4) 0.0030(5) -0.0040(5) C11 0.0171(5) 0.0121(5) 0.0174(5) -0.0018(4) 0.0021(4) 0.0003(4) C12 0.0231(7) 0.0167(6) 0.0212(6) -0.0032(5) 0.0059(5) -0.0013(5) C13 0.0237(7) 0.0199(7) 0.0333(8) -0.0066(6) 0.0127(6) -0.0017(5) C14 0.0194(7) 0.0167(6) 0.0461(10) -0.0045(6) 0.0073(6) 0.0019(5) C15 0.0193(6) 0.0188(6) 0.0361(9) 0.0004(6) -0.0017(6) 0.0046(5) C16 0.0197(6) 0.0165(6) 0.0220(6) -0.0002(5) -0.0003(5) 0.0037(4) C17 0.0166(5) 0.0112(5) 0.0176(5) -0.0009(4) 0.0029(4) 0.0004(4) C18 0.0166(6) 0.0212(6) 0.0255(7) -0.0033(5) 0.0028(5) 0.0010(5) C19 0.0212(7) 0.0250(7) 0.0309(8) -0.0019(6) 0.0081(6) 0.0035(5) C20 0.0322(8) 0.0183(6) 0.0237(7) -0.0010(5) 0.0109(6) 0.0051(6) C21 0.0311(8) 0.0176(6) 0.0180(6) -0.0023(5) 0.0035(5) 0.0031(5) C22 0.0217(6) 0.0157(6) 0.0163(6) -0.0020(4) 0.0016(5) 0.0016(4) C23 0.0149(5) 0.0123(5) 0.0165(5) -0.0007(4) 0.0007(4) -0.0011(4) C24 0.0201(6) 0.0126(5) 0.0179(6) -0.0018(4) 0.0005(4) -0.0024(4) C25 0.0253(7) 0.0166(6) 0.0187(6) 0.0000(5) -0.0013(5) -0.0073(5) C26 0.0197(6) 0.0254(7) 0.0219(6) 0.0035(5) -0.0012(5) -0.0077(5) C27 0.0168(6) 0.0258(7) 0.0360(9) 0.0047(6) 0.0056(6) -0.0003(5) C28 0.0181(6) 0.0163(6) 0.0317(8) 0.0012(5) 0.0056(5) 0.0012(5) C29 0.0151(5) 0.0123(5) 0.0139(5) -0.0001(4) -0.0012(4) -0.0012(4) C30 0.0203(6) 0.0245(7) 0.0173(6) 0.0013(5) -0.0063(5) -0.0028(5) C31 0.0198(7) 0.0275(8) 0.0262(7) 0.0028(6) -0.0088(5) -0.0028(5) C32 0.0149(6) 0.0230(7) 0.0297(8) -0.0002(6) -0.0018(5) -0.0018(5) C33 0.0169(6) 0.0254(7) 0.0203(6) -0.0011(5) 0.0017(5) -0.0020(5) C34 0.0159(5) 0.0211(6) 0.0138(5) -0.0003(4) -0.0010(4) -0.0010(4) O1 0.0362(7) 0.0319(7) 0.0289(6) -0.0093(5) -0.0102(5) 0.0110(5) C41 0.0489(13) 0.0525(14) 0.0314(10) -0.0162(10) -0.0175(9) 0.0213(11) C42 0.0259(8) 0.0347(10) 0.0348(9) 0.0051(7) -0.0042(7) 0.0043(7) C43 0.0332(9) 0.0258(8) 0.0275(8) -0.0026(6) -0.0011(7) 0.0053(6) C44 0.0270(8) 0.0313(9) 0.0377(10) -0.0069(7) -0.0039(7) 0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9911(12) . yes Ni1 P2 2.2181(4) . yes Ni1 P1 2.2264(4) . yes Ni1 I1 2.4870(2) . yes P1 C11 1.8158(14) . ? P1 C5 1.8160(14) . ? P1 C2 1.8421(14) . ? P2 C17 1.8145(14) . ? P2 C23 1.8131(14) . ? P2 C4 1.8378(15) . ? N1 C29 1.4805(17) . ? N1 C1 1.5091(17) . ? N1 C3 1.5117(17) . ? C1 C2 1.5198(19) . ? C3 C4 1.517(2) . ? C5 C10 1.398(2) . ? C5 C6 1.4059(19) . ? C6 C7 1.393(2) . ? C7 C8 1.396(2) . ? C8 C9 1.392(2) . ? C9 C10 1.395(2) . ? C11 C16 1.403(2) . ? C11 C12 1.407(2) . ? C12 C13 1.395(2) . ? C13 C14 1.392(3) . ? C14 C15 1.391(3) . ? C15 C16 1.394(2) . ? C17 C18 1.404(2) . ? C17 C22 1.403(2) . ? C18 C19 1.402(2) . ? C19 C20 1.389(3) . ? C20 C21 1.388(3) . ? C21 C22 1.395(2) . ? C23 C28 1.400(2) . ? C23 C24 1.4026(19) . ? C24 C25 1.395(2) . ? C25 C26 1.397(2) . ? C26 C27 1.389(3) . ? C27 C28 1.398(2) . ? C29 C34 1.3929(19) . ? C29 C30 1.3986(19) . ? C30 C31 1.388(2) . ? C31 C32 1.390(2) . ? C32 C33 1.384(2) . ? C33 C34 1.398(2) . ? O1 C44 1.418(2) . ? O1 C41 1.431(2) . ? C41 C42 1.537(3) . ? C42 C43 1.534(3) . ? C43 C44 1.526(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P2 86.60(3) . . yes N1 Ni1 P1 87.10(3) . . yes P2 Ni1 P1 173.670(16) . . yes N1 Ni1 I1 178.26(3) . . yes P2 Ni1 I1 91.743(11) . . yes P1 Ni1 I1 94.559(11) . . yes C11 P1 C5 105.04(6) . . ? C11 P1 C2 106.78(7) . . ? C5 P1 C2 104.21(6) . . ? C11 P1 Ni1 117.47(5) . . ? C5 P1 Ni1 120.90(5) . . ? C2 P1 Ni1 100.72(5) . . ? C17 P2 C23 107.04(6) . . ? C17 P2 C4 108.76(7) . . ? C23 P2 C4 105.18(7) . . ? C17 P2 Ni1 116.44(5) . . ? C23 P2 Ni1 117.02(5) . . ? C4 P2 Ni1 101.44(5) . . ? C29 N1 C1 110.12(10) . . ? C29 N1 C3 110.50(10) . . ? C1 N1 C3 107.46(10) . . ? C29 N1 Ni1 108.41(8) . . ? C1 N1 Ni1 110.76(8) . . ? C3 N1 Ni1 109.60(8) . . ? N1 C1 C2 109.75(11) . . ? C1 C2 P1 107.22(9) . . ? N1 C3 C4 109.51(11) . . ? C3 C4 P2 105.34(9) . . ? C10 C5 C6 119.50(13) . . ? C10 C5 P1 122.74(11) . . ? C6 C5 P1 117.75(11) . . ? C7 C6 C5 120.20(14) . . ? C8 C7 C6 119.92(14) . . ? C9 C8 C7 120.09(14) . . ? C8 C9 C10 120.26(14) . . ? C9 C10 C5 120.01(14) . . ? C16 C11 C12 119.36(14) . . ? C16 C11 P1 119.15(11) . . ? C12 C11 P1 121.46(12) . . ? C13 C12 C11 119.61(16) . . ? C12 C13 C14 120.80(16) . . ? C15 C14 C13 119.60(15) . . ? C14 C15 C16 120.42(17) . . ? C15 C16 C11 120.18(15) . . ? C18 C17 C22 119.29(13) . . ? C18 C17 P2 121.24(12) . . ? C22 C17 P2 119.21(11) . . ? C19 C18 C17 119.90(16) . . ? C20 C19 C18 120.10(16) . . ? C21 C20 C19 120.30(15) . . ? C20 C21 C22 120.18(16) . . ? C21 C22 C17 120.23(14) . . ? C28 C23 C24 119.87(13) . . ? C28 C23 P2 119.12(11) . . ? C24 C23 P2 120.87(11) . . ? C25 C24 C23 119.81(14) . . ? C26 C25 C24 120.25(14) . . ? C27 C26 C25 119.85(14) . . ? C26 C27 C28 120.46(16) . . ? C27 C28 C23 119.71(15) . . ? C34 C29 C30 119.77(13) . . ? C34 C29 N1 119.92(12) . . ? C30 C29 N1 120.31(12) . . ? C31 C30 C29 119.87(15) . . ? C30 C31 C32 120.33(14) . . ? C33 C32 C31 120.05(14) . . ? C32 C33 C34 120.10(15) . . ? C29 C34 C33 119.87(13) . . ? C44 O1 C41 104.15(17) . . ? O1 C41 C42 104.94(17) . . ? C41 C42 C43 102.97(16) . . ? C44 C43 C42 103.96(16) . . ? O1 C44 C43 105.87(16) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 36.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.974 _refine_diff_density_min -0.909 _refine_diff_density_rms 0.134 #===END