data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd1a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 N2, P F6' _chemical_formula_sum 'C23 H29 F6 N2 P' _chemical_formula_weight 478.45 _chemical_absolute_configuration ad 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' 'P' 'P' 0.1023 0.0942 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 11.0984(2) _cell_length_b 14.5283(2) _cell_length_c 14.7057(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2371.16(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4357 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.176 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9492 _exptl_absorpt_correction_T_max 0.9657 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5429 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5429 _reflns_number_gt 4357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.0917P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.047(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(11) _refine_ls_number_reflns 5429 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1101 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _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 C1 C 0.6874(2) 0.41628(16) 0.04775(15) 0.0308(5) Uani 1 1 d . . . H1 H 0.6429 0.3639 0.0670 0.037 Uiso 1 1 calc R . . C2 C 0.6998(2) 0.57748(16) 0.00539(16) 0.0316(5) Uani 1 1 d . . . C3 C 0.8262(2) 0.57097(17) 0.04943(17) 0.0355(6) Uani 1 1 d . . . C4 C 0.8723(2) 0.48612(17) -0.00123(16) 0.0337(5) Uani 1 1 d . . . H4 H 0.9608 0.4768 0.0080 0.040 Uiso 1 1 calc R . . C5 C 0.7243(2) 0.56202(18) -0.09661(16) 0.0367(6) Uani 1 1 d . . . H5A H 0.7351 0.6216 -0.1284 0.044 Uiso 1 1 calc R . . H5B H 0.6568 0.5283 -0.1253 0.044 Uiso 1 1 calc R . . C6 C 0.8418(2) 0.5043(2) -0.10075(17) 0.0411(6) Uani 1 1 d . . . H6A H 0.8285 0.4459 -0.1339 0.049 Uiso 1 1 calc R . . H6B H 0.9071 0.5391 -0.1310 0.049 Uiso 1 1 calc R . . C7 C 0.6316(3) 0.66622(18) 0.0235(2) 0.0481(7) Uani 1 1 d . . . H7A H 0.5510 0.6622 -0.0034 0.072 Uiso 1 1 calc R . . H7B H 0.6753 0.7180 -0.0036 0.072 Uiso 1 1 calc R . . H7C H 0.6244 0.6757 0.0893 0.072 Uiso 1 1 calc R . . C8 C 0.8263(3) 0.5612(2) 0.15344(17) 0.0465(7) Uani 1 1 d . . . H8A H 0.7784 0.5073 0.1708 0.070 Uiso 1 1 calc R . . H8B H 0.7912 0.6166 0.1808 0.070 Uiso 1 1 calc R . . H8C H 0.9092 0.5535 0.1750 0.070 Uiso 1 1 calc R . . C9 C 0.9043(3) 0.65496(19) 0.0257(2) 0.0473(7) Uani 1 1 d . . . H9A H 0.9876 0.6436 0.0449 0.071 Uiso 1 1 calc R . . H9B H 0.8731 0.7094 0.0573 0.071 Uiso 1 1 calc R . . H9C H 0.9021 0.6655 -0.0401 0.071 Uiso 1 1 calc R . . C10 C 0.5034(2) 0.50169(19) 0.07036(17) 0.0387(6) Uani 1 1 d . . . H10A H 0.4929 0.5582 0.1072 0.046 Uiso 1 1 calc R . . H10B H 0.4854 0.4484 0.1100 0.046 Uiso 1 1 calc R . . C11 C 0.4134(2) 0.50324(17) -0.00640(18) 0.0374(6) Uani 1 1 d . . . C12 C 0.4212(3) 0.44235(19) -0.0787(2) 0.0478(7) Uani 1 1 d . . . H12 H 0.4874 0.4010 -0.0822 0.057 Uiso 1 1 calc R . . C13 C 0.3345(3) 0.4410(2) -0.1457(2) 0.0568(8) Uani 1 1 d . . . H13 H 0.3410 0.3990 -0.1950 0.068 Uiso 1 1 calc R . . C14 C 0.2375(3) 0.5010(2) -0.1410(2) 0.0570(8) Uani 1 1 d . . . H14 H 0.1772 0.5000 -0.1869 0.068 Uiso 1 1 calc R . . C15 C 0.2289(3) 0.5616(2) -0.0701(2) 0.0532(8) Uani 1 1 d . . . H15 H 0.1624 0.6027 -0.0670 0.064 Uiso 1 1 calc R . . C16 C 0.3161(2) 0.56379(19) -0.0026(2) 0.0450(7) Uani 1 1 d . . . H16 H 0.3095 0.6064 0.0462 0.054 Uiso 1 1 calc R . . C17 C 0.8601(2) 0.31409(17) 0.03363(17) 0.0331(5) Uani 1 1 d . . . H17A H 0.8903 0.2974 -0.0275 0.040 Uiso 1 1 calc R . . H17B H 0.7997 0.2674 0.0519 0.040 Uiso 1 1 calc R . . C18 C 0.9633(2) 0.31313(16) 0.10035(15) 0.0315(5) Uani 1 1 d . . . C19 C 0.9407(2) 0.3095(2) 0.19327(17) 0.0426(6) Uani 1 1 d . . . H19 H 0.8600 0.3068 0.2148 0.051 Uiso 1 1 calc R . . C20 C 1.0350(3) 0.3098(2) 0.25440(19) 0.0555(8) Uani 1 1 d . . . H20 H 1.0191 0.3079 0.3178 0.067 Uiso 1 1 calc R . . C21 C 1.1524(3) 0.3128(2) 0.2238(2) 0.0563(8) Uani 1 1 d . . . H21 H 1.2173 0.3115 0.2659 0.068 Uiso 1 1 calc R . . C22 C 1.1752(3) 0.3175(2) 0.1319(2) 0.0536(8) Uani 1 1 d . . . H22 H 1.2559 0.3208 0.1106 0.064 Uiso 1 1 calc R . . C23 C 1.0810(2) 0.3175(2) 0.07059(18) 0.0419(6) Uani 1 1 d . . . H23 H 1.0974 0.3206 0.0073 0.050 Uiso 1 1 calc R . . P1 P 0.54733(5) 0.25263(4) 0.23766(4) 0.03167(16) Uani 1 1 d . . . N1 N 0.63038(17) 0.49586(14) 0.04088(13) 0.0320(4) Uani 1 1 d . . . N2 N 0.80166(17) 0.40583(13) 0.02954(13) 0.0293(4) Uani 1 1 d . . . F1 F 0.62565(14) 0.34552(10) 0.23434(10) 0.0467(4) Uani 1 1 d . . . F2 F 0.63633(17) 0.20859(13) 0.16482(12) 0.0619(5) Uani 1 1 d . . . F3 F 0.6284(2) 0.21602(13) 0.31891(12) 0.0714(6) Uani 1 1 d . . . F4 F 0.4698(2) 0.16159(12) 0.24040(12) 0.0703(6) Uani 1 1 d . . . F5 F 0.45995(18) 0.30090(13) 0.30864(11) 0.0610(5) Uani 1 1 d . . . F6 F 0.46811(15) 0.29087(11) 0.15517(10) 0.0496(4) 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 C1 0.0304(12) 0.0321(13) 0.0298(12) 0.0033(10) 0.0004(9) -0.0002(10) C2 0.0360(13) 0.0266(12) 0.0320(12) 0.0043(10) 0.0056(10) 0.0018(10) C3 0.0406(14) 0.0300(13) 0.0359(13) 0.0024(10) 0.0019(11) -0.0037(11) C4 0.0304(12) 0.0344(13) 0.0365(13) 0.0044(11) 0.0019(10) -0.0016(11) C5 0.0419(14) 0.0383(13) 0.0300(12) 0.0063(11) 0.0019(11) 0.0015(11) C6 0.0475(15) 0.0426(14) 0.0332(13) 0.0056(12) 0.0105(11) 0.0094(13) C7 0.0510(17) 0.0344(14) 0.0588(17) 0.0040(13) 0.0161(14) 0.0076(13) C8 0.0627(18) 0.0434(15) 0.0335(13) -0.0010(12) -0.0037(13) -0.0077(14) C9 0.0481(16) 0.0391(15) 0.0548(16) 0.0082(13) 0.0017(14) -0.0117(12) C10 0.0312(12) 0.0423(14) 0.0426(14) 0.0065(12) 0.0098(10) 0.0041(11) C11 0.0303(12) 0.0314(12) 0.0506(15) 0.0068(12) 0.0001(11) 0.0005(11) C12 0.0397(15) 0.0337(14) 0.0700(19) -0.0047(14) -0.0032(14) 0.0006(11) C13 0.0500(18) 0.0452(17) 0.075(2) -0.0106(16) -0.0092(16) -0.0081(14) C14 0.0420(15) 0.0553(18) 0.074(2) 0.0043(17) -0.0170(15) -0.0046(15) C15 0.0376(15) 0.0476(16) 0.074(2) 0.0087(16) -0.0042(15) 0.0048(13) C16 0.0381(14) 0.0390(14) 0.0580(17) 0.0032(13) -0.0001(13) 0.0058(12) C17 0.0315(12) 0.0301(12) 0.0377(13) -0.0025(10) -0.0052(10) 0.0043(10) C18 0.0304(12) 0.0282(11) 0.0360(12) -0.0041(10) -0.0046(10) 0.0049(10) C19 0.0334(14) 0.0555(16) 0.0388(13) 0.0065(13) 0.0020(11) 0.0068(13) C20 0.0532(17) 0.076(2) 0.0375(14) 0.0009(14) -0.0091(14) 0.0168(16) C21 0.0451(17) 0.0640(19) 0.0597(19) -0.0144(16) -0.0236(14) 0.0142(14) C22 0.0296(13) 0.0649(19) 0.0662(19) -0.0127(16) -0.0030(13) 0.0111(14) C23 0.0349(14) 0.0494(16) 0.0415(13) -0.0099(12) 0.0030(11) 0.0060(12) P1 0.0330(3) 0.0346(3) 0.0274(3) -0.0003(3) 0.0006(3) -0.0018(3) N1 0.0276(9) 0.0321(11) 0.0362(11) 0.0039(9) 0.0067(8) 0.0019(9) N2 0.0278(10) 0.0288(10) 0.0313(10) 0.0017(8) -0.0014(8) 0.0033(8) F1 0.0486(9) 0.0541(9) 0.0375(8) -0.0026(7) -0.0035(7) -0.0201(7) F2 0.0639(11) 0.0665(11) 0.0552(10) -0.0144(9) 0.0153(9) 0.0198(9) F3 0.0930(15) 0.0701(13) 0.0511(10) 0.0116(9) -0.0306(10) 0.0159(11) F4 0.1046(15) 0.0513(10) 0.0549(10) -0.0006(8) 0.0052(11) -0.0397(10) F5 0.0594(11) 0.0690(11) 0.0547(9) -0.0139(9) 0.0260(9) -0.0009(10) F6 0.0433(9) 0.0565(9) 0.0491(9) 0.0034(7) -0.0210(8) -0.0041(8) _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 C1 N2 1.305(3) . ? C1 N1 1.322(3) . ? C1 H1 0.9500 . ? C2 N1 1.507(3) . ? C2 C7 1.519(3) . ? C2 C5 1.541(3) . ? C2 C3 1.549(4) . ? C3 C4 1.528(3) . ? C3 C8 1.536(3) . ? C3 C9 1.537(3) . ? C4 N2 1.477(3) . ? C4 C6 1.525(3) . ? C4 H4 1.0000 . ? C5 C6 1.551(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.477(3) . ? C10 C11 1.507(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.386(4) . ? C11 C16 1.394(4) . ? C12 C13 1.378(4) . ? C12 H12 0.9500 . ? C13 C14 1.387(4) . ? C13 H13 0.9500 . ? C14 C15 1.368(5) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.483(3) . ? C17 C18 1.508(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.379(4) . ? C18 C19 1.390(3) . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.377(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? P1 F4 1.5784(17) . ? P1 F3 1.5876(17) . ? P1 F5 1.5880(17) . ? P1 F2 1.5913(17) . ? P1 F6 1.5979(16) . ? P1 F1 1.6059(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 N2 C1 N1 123.5(2) . . ? N2 C1 H1 118.3 . . ? N1 C1 H1 118.3 . . ? N1 C2 C7 110.65(19) . . ? N1 C2 C5 108.2(2) . . ? C7 C2 C5 112.5(2) . . ? N1 C2 C3 105.68(18) . . ? C7 C2 C3 115.5(2) . . ? C5 C2 C3 103.75(19) . . ? C4 C3 C8 114.3(2) . . ? C4 C3 C9 109.9(2) . . ? C8 C3 C9 107.4(2) . . ? C4 C3 C2 98.6(2) . . ? C8 C3 C2 115.0(2) . . ? C9 C3 C2 111.6(2) . . ? N2 C4 C6 108.2(2) . . ? N2 C4 C3 108.06(19) . . ? C6 C4 C3 104.7(2) . . ? N2 C4 H4 111.8 . . ? C6 C4 H4 111.8 . . ? C3 C4 H4 111.8 . . ? C2 C5 C6 105.4(2) . . ? C2 C5 H5A 110.7 . . ? C6 C5 H5A 110.7 . . ? C2 C5 H5B 110.7 . . ? C6 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C4 C6 C5 104.06(19) . . ? C4 C6 H6A 110.9 . . ? C5 C6 H6A 110.9 . . ? C4 C6 H6B 110.9 . . ? C5 C6 H6B 110.9 . . ? H6A C6 H6B 109.0 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 114.4(2) . . ? N1 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N1 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C16 118.8(2) . . ? C12 C11 C10 121.6(2) . . ? C16 C11 C10 119.5(2) . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 119.8(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.7(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 119.8(3) . . ? C15 C16 H16 120.1 . . ? C11 C16 H16 120.1 . . ? N2 C17 C18 111.50(19) . . ? N2 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N2 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C23 C18 C19 119.0(2) . . ? C23 C18 C17 120.8(2) . . ? C19 C18 C17 120.2(2) . . ? C20 C19 C18 120.2(3) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 120.3(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C22 C21 C20 119.7(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 120.7(3) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? F4 P1 F3 90.51(11) . . ? F4 P1 F5 91.17(10) . . ? F3 P1 F5 89.97(11) . . ? F4 P1 F2 91.06(11) . . ? F3 P1 F2 91.15(10) . . ? F5 P1 F2 177.50(11) . . ? F4 P1 F6 90.62(10) . . ? F3 P1 F6 178.75(11) . . ? F5 P1 F6 90.54(10) . . ? F2 P1 F6 88.30(10) . . ? F4 P1 F1 179.62(11) . . ? F3 P1 F1 89.87(10) . . ? F5 P1 F1 88.82(9) . . ? F2 P1 F1 88.94(10) . . ? F6 P1 F1 89.00(9) . . ? C1 N1 C10 119.0(2) . . ? C1 N1 C2 118.03(19) . . ? C10 N1 C2 123.0(2) . . ? C1 N2 C4 119.2(2) . . ? C1 N2 C17 121.4(2) . . ? C4 N2 C17 119.36(19) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.208 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.043 #===END data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd1b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H27 N4, P F6' _chemical_formula_sum 'C21 H27 F6 N4 P' _chemical_formula_weight 480.44 _chemical_absolute_configuration ad 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' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.57300(10) _cell_length_b 11.8530(2) _cell_length_c 18.6130(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.7240(10) _cell_angle_gamma 90.00 _cell_volume 2291.87(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7560 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.184 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9468 _exptl_absorpt_correction_T_max 0.9554 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9445 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.54 _reflns_number_total 9445 _reflns_number_gt 7560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+2.3595P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.059(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.15(15) _refine_ls_number_reflns 9445 _refine_ls_number_parameters 621 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.000 _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 C1 C 0.8048(4) 0.6662(4) 0.0968(2) 0.0347(9) Uani 1 1 d . . . C2 C 0.7563(4) 0.7841(4) 0.0706(2) 0.0349(9) Uani 1 1 d . . . C3 C 0.6714(4) 0.7616(5) -0.0053(2) 0.0421(10) Uani 1 1 d . . . H3A H 0.7223 0.7698 -0.0445 0.051 Uiso 1 1 calc R . . H3B H 0.5981 0.8148 -0.0147 0.051 Uiso 1 1 calc R . . C4 C 0.6229(4) 0.6383(4) -0.0017(2) 0.0423(10) Uani 1 1 d . . . H4A H 0.5276 0.6352 -0.0117 0.051 Uiso 1 1 calc R . . H4B H 0.6558 0.5897 -0.0374 0.051 Uiso 1 1 calc R . . C5 C 0.6779(4) 0.6015(4) 0.0773(2) 0.0351(9) Uani 1 1 d . . . H5 H 0.6908 0.5180 0.0815 0.042 Uiso 1 1 calc R . . C6 C 0.9007(4) 0.6191(5) 0.0516(3) 0.0484(12) Uani 1 1 d . . . H6A H 0.9850 0.6545 0.0677 0.073 Uiso 1 1 calc R . . H6B H 0.8697 0.6356 -0.0002 0.073 Uiso 1 1 calc R . . H6C H 0.9085 0.5373 0.0587 0.073 Uiso 1 1 calc R . . C7 C 0.8675(4) 0.6600(5) 0.1774(2) 0.0461(12) Uani 1 1 d . . . H7A H 0.8084 0.6908 0.2073 0.069 Uiso 1 1 calc R . . H7B H 0.9473 0.7041 0.1857 0.069 Uiso 1 1 calc R . . H7C H 0.8870 0.5812 0.1911 0.069 Uiso 1 1 calc R . . C8 C 0.8624(5) 0.8708(5) 0.0679(3) 0.0497(12) Uani 1 1 d . . . H8A H 0.8241 0.9403 0.0450 0.075 Uiso 1 1 calc R . . H8B H 0.9237 0.8405 0.0394 0.075 Uiso 1 1 calc R . . H8C H 0.9074 0.8873 0.1178 0.075 Uiso 1 1 calc R . . C9 C 0.6617(4) 0.9405(4) 0.1467(3) 0.0369(10) Uani 1 1 d . . . H9A H 0.5725 0.9576 0.1523 0.044 Uiso 1 1 calc R . . H9B H 0.6847 0.9929 0.1097 0.044 Uiso 1 1 calc R . . C10 C 0.7507(4) 0.9600(4) 0.2184(2) 0.0351(10) Uani 1 1 d . . . C11 C 0.8431(5) 1.0444(4) 0.2289(3) 0.0453(12) Uani 1 1 d . . . H11 H 0.8550 1.0911 0.1892 0.054 Uiso 1 1 calc R . . C12 C 0.9177(5) 1.0599(5) 0.2972(3) 0.0526(13) Uani 1 1 d . . . H12 H 0.9809 1.1178 0.3054 0.063 Uiso 1 1 calc R . . C13 C 0.8987(5) 0.9900(5) 0.3535(3) 0.0448(11) Uani 1 1 d . . . H13 H 0.9494 0.9977 0.4011 0.054 Uiso 1 1 calc R . . C14 C 0.8045(4) 0.9087(5) 0.3388(3) 0.0448(11) Uani 1 1 d . . . H14 H 0.7913 0.8606 0.3776 0.054 Uiso 1 1 calc R . . C15 C 0.5012(4) 0.5638(4) 0.1505(2) 0.0319(9) Uani 1 1 d . . . H15A H 0.4549 0.5199 0.1084 0.038 Uiso 1 1 calc R . . H15B H 0.4367 0.6060 0.1722 0.038 Uiso 1 1 calc R . . C16 C 0.5738(4) 0.4841(4) 0.2068(2) 0.0325(9) Uani 1 1 d . . . C17 C 0.5825(5) 0.3701(4) 0.1922(3) 0.0479(12) Uani 1 1 d . . . H17 H 0.5408 0.3393 0.1468 0.057 Uiso 1 1 calc R . . C18 C 0.6537(7) 0.3017(5) 0.2458(3) 0.0661(17) Uani 1 1 d . . . H18 H 0.6599 0.2228 0.2382 0.079 Uiso 1 1 calc R . . C19 C 0.7143(6) 0.3501(6) 0.3092(3) 0.0661(18) Uani 1 1 d . . . H19 H 0.7657 0.3054 0.3458 0.079 Uiso 1 1 calc R . . C20 C 0.7009(6) 0.4637(6) 0.3202(3) 0.0594(16) Uani 1 1 d . . . H20 H 0.7441 0.4960 0.3647 0.071 Uiso 1 1 calc R . . C21 C 0.5907(4) 0.7503(4) 0.14249(19) 0.0280(8) Uani 1 1 d . . . H21 H 0.5332 0.7756 0.1727 0.034 Uiso 1 1 calc R . . C101 C 0.7597(4) 0.2128(4) 0.5491(2) 0.0370(9) Uani 1 1 d . . . C102 C 0.8033(4) 0.1061(4) 0.5948(2) 0.0348(9) Uani 1 1 d . . . C103 C 0.8977(4) 0.1524(4) 0.6608(2) 0.0419(10) Uani 1 1 d . . . H10A H 0.8967 0.1050 0.7045 0.050 Uiso 1 1 calc R . . H10B H 0.9863 0.1540 0.6507 0.050 Uiso 1 1 calc R . . C104 C 0.8510(4) 0.2717(5) 0.6727(3) 0.0472(12) Uani 1 1 d . . . H10C H 0.9190 0.3277 0.6692 0.057 Uiso 1 1 calc R . . H10D H 0.8265 0.2784 0.7213 0.057 Uiso 1 1 calc R . . C105 C 0.7329(4) 0.2903(4) 0.6112(2) 0.0414(10) Uani 1 1 d . . . H105 H 0.7238 0.3710 0.5956 0.050 Uiso 1 1 calc R . . C106 C 0.8715(4) 0.2634(5) 0.5168(3) 0.0471(12) Uani 1 1 d . . . H10E H 0.8881 0.2157 0.4766 0.071 Uiso 1 1 calc R . . H10F H 0.9490 0.2669 0.5549 0.071 Uiso 1 1 calc R . . H10G H 0.8483 0.3396 0.4985 0.071 Uiso 1 1 calc R . . C107 C 0.6450(4) 0.1969(5) 0.4872(2) 0.0465(12) Uani 1 1 d . . . H10H H 0.6185 0.2702 0.4651 0.070 Uiso 1 1 calc R . . H10I H 0.5735 0.1634 0.5065 0.070 Uiso 1 1 calc R . . H10J H 0.6692 0.1467 0.4501 0.070 Uiso 1 1 calc R . . C108 C 0.8555(5) 0.0123(5) 0.5549(3) 0.0490(12) Uani 1 1 d . . . H10K H 0.8856 -0.0490 0.5891 0.074 Uiso 1 1 calc R . . H10L H 0.9275 0.0405 0.5335 0.074 Uiso 1 1 calc R . . H10M H 0.7876 -0.0158 0.5159 0.074 Uiso 1 1 calc R . . C109 C 0.6697(4) -0.0535(4) 0.6429(2) 0.0353(9) Uani 1 1 d . . . H10N H 0.6947 -0.1030 0.6050 0.042 Uiso 1 1 calc R . . H10O H 0.5784 -0.0687 0.6448 0.042 Uiso 1 1 calc R . . C110 C 0.7530(4) -0.0811(4) 0.7171(2) 0.0345(9) Uani 1 1 d . . . C111 C 0.8434(5) -0.1664(4) 0.7249(3) 0.0473(12) Uani 1 1 d . . . H111 H 0.8549 -0.2108 0.6842 0.057 Uiso 1 1 calc R . . C112 C 0.9169(5) -0.1858(5) 0.7935(3) 0.0513(13) Uani 1 1 d . . . H112 H 0.9801 -0.2438 0.8002 0.062 Uiso 1 1 calc R . . C113 C 0.8983(4) -0.1218(4) 0.8513(3) 0.0405(10) Uani 1 1 d . . . H113 H 0.9467 -0.1348 0.8989 0.049 Uiso 1 1 calc R . . C114 C 0.8055(4) -0.0358(4) 0.8385(2) 0.0398(10) Uani 1 1 d . . . H114 H 0.7931 0.0099 0.8785 0.048 Uiso 1 1 calc R . . C115 C 0.5189(4) 0.3265(4) 0.6515(2) 0.0382(10) Uani 1 1 d . . . H11A H 0.4510 0.2839 0.6699 0.046 Uiso 1 1 calc R . . H11B H 0.4785 0.3657 0.6060 0.046 Uiso 1 1 calc R . . C116 C 0.5772(4) 0.4127(4) 0.7080(2) 0.0396(11) Uani 1 1 d . . . C117 C 0.5764(6) 0.5245(5) 0.6916(3) 0.0570(14) Uani 1 1 d . . . H117 H 0.5361 0.5503 0.6446 0.068 Uiso 1 1 calc R . . C118 C 0.6347(7) 0.6007(6) 0.7441(4) 0.0748(19) Uani 1 1 d . . . H118 H 0.6336 0.6792 0.7339 0.090 Uiso 1 1 calc R . . C119 C 0.6929(7) 0.5608(6) 0.8098(4) 0.072(2) Uani 1 1 d . . . H119 H 0.7354 0.6110 0.8462 0.087 Uiso 1 1 calc R . . C120 C 0.6901(6) 0.4445(6) 0.8238(3) 0.0606(16) Uani 1 1 d . . . H120 H 0.7312 0.4171 0.8703 0.073 Uiso 1 1 calc R . . C121 C 0.6023(4) 0.1396(4) 0.6419(2) 0.0298(8) Uani 1 1 d . . . H121 H 0.5310 0.1123 0.6612 0.036 Uiso 1 1 calc R . . N1 N 0.5896(3) 0.6438(3) 0.12492(17) 0.0280(7) Uani 1 1 d . . . N2 N 0.6675(3) 0.8241(3) 0.12042(18) 0.0306(7) Uani 1 1 d . . . N3 N 0.6284(4) 0.5317(4) 0.2700(2) 0.0436(10) Uani 1 1 d . . . N4 N 0.7305(3) 0.8938(4) 0.2730(2) 0.0405(9) Uani 1 1 d . . . N5 N 0.6841(3) 0.0660(3) 0.62254(18) 0.0319(8) Uani 1 1 d . . . N6 N 0.6164(3) 0.2482(3) 0.63539(18) 0.0326(7) Uani 1 1 d . . . N7 N 0.7338(3) -0.0151(4) 0.7729(2) 0.0377(9) Uani 1 1 d . . . N8 N 0.6313(4) 0.3710(4) 0.7738(2) 0.0474(10) Uani 1 1 d . . . P3 P 0.76409(11) 0.24699(11) 0.02551(7) 0.0414(3) Uani 1 1 d . . . F1 F 0.7247(4) 0.1520(5) -0.0305(3) 0.133(2) Uani 1 1 d . . . F2 F 0.8506(3) 0.3135(5) -0.0184(3) 0.1105(19) Uani 1 1 d . . . F3 F 0.6414(3) 0.3201(3) -0.0088(2) 0.0760(12) Uani 1 1 d . . . F4 F 0.6801(3) 0.1904(3) 0.07983(18) 0.0679(9) Uani 1 1 d . . . F5 F 0.8864(3) 0.1746(3) 0.06165(18) 0.0587(8) Uani 1 1 d . . . F6 F 0.8025(3) 0.3405(3) 0.0905(2) 0.0832(13) Uani 1 1 d . . . P4 P 0.75583(11) 0.64245(10) 0.52173(7) 0.0411(3) Uani 1 1 d D . . F7 F 0.8505(3) 0.5688(4) 0.4866(3) 0.0617(16) Uani 0.716(7) 1 d PDU A 1 F8 F 0.8701(3) 0.7257(3) 0.5551(2) 0.0746(11) Uani 1 1 d DU A 1 F9 F 0.6625(4) 0.6996(4) 0.5688(2) 0.0519(13) Uani 0.716(7) 1 d PDU A 1 F10 F 0.6450(3) 0.5538(4) 0.4933(3) 0.1009(16) Uani 1 1 d U A 1 F11 F 0.8041(5) 0.5725(5) 0.5954(2) 0.0700(16) Uani 0.716(7) 1 d PDU A 1 F12 F 0.6972(6) 0.7082(6) 0.4535(3) 0.101(2) Uani 0.716(7) 1 d PDU A 1 F7A F 0.8065(9) 0.6533(9) 0.4447(3) 0.077(4) Uani 0.284(7) 1 d PDU A 2 F9A F 0.7081(9) 0.6371(10) 0.5955(4) 0.126(7) Uani 0.284(7) 1 d PDU A 2 F11A F 0.8416(9) 0.5370(4) 0.5406(6) 0.093(5) Uani 0.284(7) 1 d PDU A 2 F12A F 0.6682(7) 0.7508(7) 0.4986(6) 0.108(6) Uani 0.284(7) 1 d PDU 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 C1 0.0296(18) 0.035(2) 0.039(2) -0.0020(17) 0.0043(16) 0.0020(16) C2 0.0277(18) 0.036(2) 0.043(2) 0.0026(18) 0.0126(17) 0.0018(17) C3 0.040(2) 0.060(3) 0.0270(18) 0.003(2) 0.0075(17) 0.006(2) C4 0.039(2) 0.058(3) 0.030(2) -0.007(2) 0.0089(17) -0.003(2) C5 0.0310(19) 0.037(2) 0.040(2) -0.0016(18) 0.0127(17) 0.0014(16) C6 0.037(2) 0.051(3) 0.059(3) 0.002(2) 0.015(2) 0.003(2) C7 0.0295(19) 0.058(3) 0.046(2) 0.006(2) -0.0053(18) 0.003(2) C8 0.043(2) 0.047(3) 0.062(3) 0.003(2) 0.018(2) -0.007(2) C9 0.038(2) 0.027(2) 0.044(2) 0.0031(18) 0.0030(19) -0.0013(18) C10 0.036(2) 0.028(2) 0.041(2) -0.0039(19) 0.0067(19) 0.0011(17) C11 0.056(3) 0.035(3) 0.044(2) 0.004(2) 0.007(2) -0.014(2) C12 0.053(3) 0.040(3) 0.059(3) -0.004(2) -0.003(2) -0.017(2) C13 0.040(2) 0.053(3) 0.040(2) -0.007(2) 0.004(2) -0.004(2) C14 0.044(2) 0.054(3) 0.037(2) 0.000(2) 0.007(2) -0.004(2) C15 0.0306(19) 0.032(2) 0.033(2) 0.0009(17) 0.0058(16) -0.0017(16) C16 0.038(2) 0.031(2) 0.030(2) 0.0003(17) 0.0127(18) 0.0025(18) C17 0.069(3) 0.033(3) 0.042(2) 0.003(2) 0.012(2) 0.004(2) C18 0.096(5) 0.045(3) 0.060(3) 0.012(3) 0.020(3) 0.029(3) C19 0.083(4) 0.073(4) 0.044(3) 0.021(3) 0.015(3) 0.033(3) C20 0.063(3) 0.084(5) 0.032(2) 0.003(3) 0.009(2) 0.022(3) C21 0.0273(17) 0.032(2) 0.0235(17) 0.0012(17) 0.0018(14) 0.0025(17) C101 0.0305(19) 0.044(3) 0.036(2) 0.0049(18) 0.0061(17) -0.0017(17) C102 0.0291(18) 0.037(2) 0.040(2) -0.0008(18) 0.0110(17) 0.0026(17) C103 0.0294(18) 0.055(3) 0.039(2) 0.002(2) 0.0016(17) -0.0049(19) C104 0.039(2) 0.055(3) 0.049(3) -0.013(2) 0.011(2) -0.014(2) C105 0.045(2) 0.035(2) 0.049(2) 0.0043(19) 0.021(2) -0.0008(19) C106 0.038(2) 0.052(3) 0.056(3) 0.013(2) 0.021(2) -0.001(2) C107 0.036(2) 0.071(4) 0.031(2) 0.012(2) 0.0030(17) 0.003(2) C108 0.051(3) 0.045(3) 0.055(3) -0.010(2) 0.020(2) 0.006(2) C109 0.039(2) 0.033(2) 0.033(2) 0.0002(18) 0.0040(18) -0.0012(18) C110 0.036(2) 0.028(2) 0.040(2) 0.0006(18) 0.0080(19) -0.0010(18) C111 0.052(3) 0.040(3) 0.047(3) -0.006(2) 0.003(2) 0.015(2) C112 0.058(3) 0.046(3) 0.048(3) 0.000(2) 0.005(2) 0.021(2) C113 0.038(2) 0.044(3) 0.041(2) 0.011(2) 0.0088(19) 0.0059(19) C114 0.038(2) 0.048(3) 0.037(2) -0.001(2) 0.0145(19) 0.005(2) C115 0.041(2) 0.041(3) 0.035(2) 0.0002(19) 0.0118(18) 0.0063(19) C116 0.042(2) 0.044(3) 0.037(2) -0.001(2) 0.020(2) 0.000(2) C117 0.076(4) 0.046(3) 0.056(3) 0.011(3) 0.029(3) -0.003(3) C118 0.116(5) 0.046(4) 0.072(4) -0.007(3) 0.043(4) -0.017(4) C119 0.106(5) 0.061(4) 0.061(3) -0.023(3) 0.043(4) -0.034(4) C120 0.078(4) 0.075(4) 0.034(3) -0.007(3) 0.023(3) -0.016(3) C121 0.0288(17) 0.035(2) 0.0252(18) -0.0005(17) 0.0048(15) 0.0014(17) N1 0.0270(14) 0.0303(18) 0.0275(15) -0.0026(14) 0.0072(12) -0.0014(14) N2 0.0305(16) 0.0297(19) 0.0325(17) 0.0034(14) 0.0083(14) 0.0004(14) N3 0.050(2) 0.052(3) 0.0292(18) -0.0014(17) 0.0073(17) 0.0116(19) N4 0.0388(19) 0.048(2) 0.0352(19) 0.0022(18) 0.0078(16) -0.0087(17) N5 0.0327(17) 0.031(2) 0.0314(17) -0.0008(14) 0.0056(14) 0.0010(15) N6 0.0317(16) 0.0322(19) 0.0359(17) -0.0010(15) 0.0112(14) 0.0003(15) N7 0.0385(19) 0.040(2) 0.0355(19) -0.0010(16) 0.0091(16) 0.0063(17) N8 0.056(2) 0.048(3) 0.040(2) 0.0019(19) 0.0121(19) -0.009(2) P3 0.0314(5) 0.0397(7) 0.0529(7) 0.0061(6) 0.0072(5) 0.0008(5) F1 0.087(3) 0.164(5) 0.127(3) -0.114(4) -0.040(3) 0.037(3) F2 0.053(2) 0.154(5) 0.134(4) 0.090(3) 0.044(2) 0.018(2) F3 0.0324(14) 0.093(3) 0.103(3) 0.055(2) 0.0126(16) 0.0119(16) F4 0.0648(19) 0.071(2) 0.071(2) 0.0164(18) 0.0205(16) 0.0064(18) F5 0.0453(15) 0.0513(19) 0.075(2) 0.0022(16) 0.0003(14) 0.0141(14) F6 0.0574(19) 0.053(2) 0.136(3) -0.038(2) 0.009(2) -0.0015(16) P4 0.0330(5) 0.0413(7) 0.0471(6) -0.0101(5) 0.0026(5) 0.0041(5) F7 0.037(2) 0.075(3) 0.074(3) -0.035(3) 0.011(2) 0.008(2) F8 0.0645(19) 0.066(2) 0.101(3) -0.033(2) 0.0351(19) -0.0299(17) F9 0.042(2) 0.051(3) 0.066(3) -0.026(2) 0.0175(19) -0.0050(19) F10 0.0460(18) 0.109(3) 0.147(4) -0.081(3) 0.018(2) -0.018(2) F11 0.063(3) 0.093(4) 0.051(3) 0.019(3) 0.004(2) 0.005(3) F12 0.095(4) 0.130(5) 0.078(3) 0.072(4) 0.016(3) 0.030(4) F7A 0.086(7) 0.091(8) 0.064(6) -0.038(6) 0.040(6) -0.019(6) F9A 0.135(10) 0.150(11) 0.106(9) 0.011(8) 0.059(8) -0.015(9) F11A 0.101(8) 0.070(8) 0.108(9) 0.013(7) 0.014(7) 0.026(6) F12A 0.095(8) 0.089(8) 0.126(10) -0.019(7) -0.015(7) 0.047(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 C1 C7 1.526(6) . ? C1 C5 1.528(5) . ? C1 C2 1.536(6) . ? C1 C6 1.537(6) . ? C2 N2 1.514(5) . ? C2 C8 1.529(6) . ? C2 C3 1.549(6) . ? C3 C4 1.554(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.541(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N1 1.490(5) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N2 1.468(6) . ? C9 C10 1.500(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N4 1.333(6) . ? C10 C11 1.386(6) . ? C11 C12 1.379(7) . ? C11 H11 0.9500 . ? C12 C13 1.380(7) . ? C12 H12 0.9500 . ? C13 C14 1.376(7) . ? C13 H13 0.9500 . ? C14 N4 1.337(6) . ? C14 H14 0.9500 . ? C15 N1 1.472(5) . ? C15 C16 1.509(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N3 1.336(6) . ? C16 C17 1.385(7) . ? C17 C18 1.392(7) . ? C17 H17 0.9500 . ? C18 C19 1.361(9) . ? C18 H18 0.9500 . ? C19 C20 1.373(9) . ? C19 H19 0.9500 . ? C20 N3 1.357(7) . ? C20 H20 0.9500 . ? C21 N1 1.303(6) . ? C21 N2 1.310(5) . ? C21 H21 0.9500 . ? C101 C107 1.521(6) . ? C101 C106 1.542(6) . ? C101 C105 1.543(6) . ? C101 C102 1.546(6) . ? C102 C108 1.498(6) . ? C102 N5 1.525(5) . ? C102 C103 1.533(6) . ? C103 C104 1.528(7) . ? C103 H10A 0.9900 . ? C103 H10B 0.9900 . ? C104 C105 1.545(6) . ? C104 H10C 0.9900 . ? C104 H10D 0.9900 . ? C105 N6 1.474(5) . ? C105 H105 1.0000 . ? C106 H10E 0.9800 . ? C106 H10F 0.9800 . ? C106 H10G 0.9800 . ? C107 H10H 0.9800 . ? C107 H10I 0.9800 . ? C107 H10J 0.9800 . ? C108 H10K 0.9800 . ? C108 H10L 0.9800 . ? C108 H10M 0.9800 . ? C109 N5 1.481(6) . ? C109 C110 1.529(6) . ? C109 H10N 0.9900 . ? C109 H10O 0.9900 . ? C110 N7 1.346(6) . ? C110 C111 1.380(6) . ? C111 C112 1.385(7) . ? C111 H111 0.9500 . ? C112 C113 1.360(7) . ? C112 H112 0.9500 . ? C113 C114 1.403(6) . ? C113 H113 0.9500 . ? C114 N7 1.335(6) . ? C114 H114 0.9500 . ? C115 N6 1.459(6) . ? C115 C116 1.513(7) . ? C115 H11A 0.9900 . ? C115 H11B 0.9900 . ? C116 N8 1.346(6) . ? C116 C117 1.359(8) . ? C117 C118 1.387(9) . ? C117 H117 0.9500 . ? C118 C119 1.348(10) . ? C118 H118 0.9500 . ? C119 C120 1.405(9) . ? C119 H119 0.9500 . ? C120 N8 1.341(7) . ? C120 H120 0.9500 . ? C121 N6 1.304(6) . ? C121 N5 1.325(5) . ? C121 H121 0.9500 . ? P3 F1 1.539(4) . ? P3 F2 1.551(3) . ? P3 F3 1.592(3) . ? P3 F5 1.593(3) . ? P3 F4 1.611(3) . ? P3 F6 1.636(4) . ? P4 F12 1.520(4) . ? P4 F11A 1.546(4) . ? P4 F9A 1.550(5) . ? P4 F7 1.561(3) . ? P4 F9 1.588(3) . ? P4 F10 1.590(4) . ? P4 F8 1.594(3) . ? P4 F12A 1.595(5) . ? P4 F11 1.603(4) . ? P4 F7A 1.626(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 C7 C1 C5 114.3(4) . . ? C7 C1 C2 114.4(4) . . ? C5 C1 C2 98.9(3) . . ? C7 C1 C6 108.1(4) . . ? C5 C1 C6 109.1(3) . . ? C2 C1 C6 111.8(4) . . ? N2 C2 C8 110.5(4) . . ? N2 C2 C1 107.4(3) . . ? C8 C2 C1 114.8(3) . . ? N2 C2 C3 107.0(3) . . ? C8 C2 C3 113.0(4) . . ? C1 C2 C3 103.6(4) . . ? C2 C3 C4 105.3(4) . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3B 110.7 . . ? C4 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C5 C4 C3 103.7(4) . . ? C5 C4 H4A 111.0 . . ? C3 C4 H4A 111.0 . . ? C5 C4 H4B 111.0 . . ? C3 C4 H4B 111.0 . . ? H4A C4 H4B 109.0 . . ? N1 C5 C1 108.0(3) . . ? N1 C5 C4 107.8(3) . . ? C1 C5 C4 104.1(3) . . ? N1 C5 H5 112.2 . . ? C1 C5 H5 112.2 . . ? C4 C5 H5 112.2 . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C2 C8 H8A 109.5 . . ? C2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N2 C9 C10 112.5(4) . . ? N2 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N2 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? N4 C10 C11 121.7(4) . . ? N4 C10 C9 115.1(4) . . ? C11 C10 C9 123.0(4) . . ? C12 C11 C10 119.6(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C13 118.8(5) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 118.2(5) . . ? C14 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? N4 C14 C13 123.6(5) . . ? N4 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? N1 C15 C16 110.9(3) . . ? N1 C15 H15A 109.5 . . ? C16 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N3 C16 C17 123.4(4) . . ? N3 C16 C15 115.4(4) . . ? C17 C16 C15 121.2(4) . . ? C16 C17 C18 118.4(5) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? C19 C18 C17 118.6(6) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 119.9(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? N3 C20 C19 122.7(6) . . ? N3 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N1 C21 N2 123.0(4) . . ? N1 C21 H21 118.5 . . ? N2 C21 H21 118.5 . . ? C107 C101 C106 108.3(3) . . ? C107 C101 C105 114.2(4) . . ? C106 C101 C105 108.8(4) . . ? C107 C101 C102 115.4(4) . . ? C106 C101 C102 111.1(3) . . ? C105 C101 C102 98.7(3) . . ? C108 C102 N5 109.9(4) . . ? C108 C102 C103 114.7(4) . . ? N5 C102 C103 107.2(3) . . ? C108 C102 C101 115.7(4) . . ? N5 C102 C101 105.1(3) . . ? C103 C102 C101 103.4(4) . . ? C104 C103 C102 105.5(4) . . ? C104 C103 H10A 110.6 . . ? C102 C103 H10A 110.6 . . ? C104 C103 H10B 110.6 . . ? C102 C103 H10B 110.6 . . ? H10A C103 H10B 108.8 . . ? C103 C104 C105 105.3(4) . . ? C103 C104 H10C 110.7 . . ? C105 C104 H10C 110.7 . . ? C103 C104 H10D 110.7 . . ? C105 C104 H10D 110.7 . . ? H10C C104 H10D 108.8 . . ? N6 C105 C101 108.0(4) . . ? N6 C105 C104 109.4(4) . . ? C101 C105 C104 103.5(3) . . ? N6 C105 H105 111.9 . . ? C101 C105 H105 111.9 . . ? C104 C105 H105 111.9 . . ? C101 C106 H10E 109.5 . . ? C101 C106 H10F 109.5 . . ? H10E C106 H10F 109.5 . . ? C101 C106 H10G 109.5 . . ? H10E C106 H10G 109.5 . . ? H10F C106 H10G 109.5 . . ? C101 C107 H10H 109.5 . . ? C101 C107 H10I 109.5 . . ? H10H C107 H10I 109.5 . . ? C101 C107 H10J 109.5 . . ? H10H C107 H10J 109.5 . . ? H10I C107 H10J 109.5 . . ? C102 C108 H10K 109.5 . . ? C102 C108 H10L 109.5 . . ? H10K C108 H10L 109.5 . . ? C102 C108 H10M 109.5 . . ? H10K C108 H10M 109.5 . . ? H10L C108 H10M 109.5 . . ? N5 C109 C110 111.5(4) . . ? N5 C109 H10N 109.3 . . ? C110 C109 H10N 109.3 . . ? N5 C109 H10O 109.3 . . ? C110 C109 H10O 109.3 . . ? H10N C109 H10O 108.0 . . ? N7 C110 C111 123.1(4) . . ? N7 C110 C109 115.3(4) . . ? C111 C110 C109 121.6(4) . . ? C110 C111 C112 118.6(5) . . ? C110 C111 H111 120.7 . . ? C112 C111 H111 120.7 . . ? C113 C112 C111 119.8(5) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C112 C113 C114 118.1(4) . . ? C112 C113 H113 120.9 . . ? C114 C113 H113 120.9 . . ? N7 C114 C113 123.3(4) . . ? N7 C114 H114 118.4 . . ? C113 C114 H114 118.4 . . ? N6 C115 C116 111.1(4) . . ? N6 C115 H11A 109.4 . . ? C116 C115 H11A 109.4 . . ? N6 C115 H11B 109.4 . . ? C116 C115 H11B 109.4 . . ? H11A C115 H11B 108.0 . . ? N8 C116 C117 123.1(5) . . ? N8 C116 C115 115.7(4) . . ? C117 C116 C115 121.2(5) . . ? C116 C117 C118 119.6(6) . . ? C116 C117 H117 120.2 . . ? C118 C117 H117 120.2 . . ? C119 C118 C117 118.6(6) . . ? C119 C118 H118 120.7 . . ? C117 C118 H118 120.7 . . ? C118 C119 C120 119.4(6) . . ? C118 C119 H119 120.3 . . ? C120 C119 H119 120.3 . . ? N8 C120 C119 122.1(6) . . ? N8 C120 H120 118.9 . . ? C119 C120 H120 118.9 . . ? N6 C121 N5 122.2(4) . . ? N6 C121 H121 118.9 . . ? N5 C121 H121 118.9 . . ? C21 N1 C15 121.3(3) . . ? C21 N1 C5 119.9(3) . . ? C15 N1 C5 118.8(3) . . ? C21 N2 C9 117.2(4) . . ? C21 N2 C2 118.3(4) . . ? C9 N2 C2 124.6(3) . . ? C16 N3 C20 116.9(5) . . ? C10 N4 C14 118.2(4) . . ? C121 N5 C109 117.2(4) . . ? C121 N5 C102 120.6(4) . . ? C109 N5 C102 121.0(3) . . ? C121 N6 C115 120.8(4) . . ? C121 N6 C105 118.6(4) . . ? C115 N6 C105 120.6(4) . . ? C114 N7 C110 117.2(4) . . ? C120 N8 C116 117.2(5) . . ? F1 P3 F2 97.3(3) . . ? F1 P3 F3 91.7(2) . . ? F2 P3 F3 91.7(2) . . ? F1 P3 F5 89.3(2) . . ? F2 P3 F5 89.1(2) . . ? F3 P3 F5 178.7(2) . . ? F1 P3 F4 90.5(3) . . ? F2 P3 F4 172.2(3) . . ? F3 P3 F4 88.57(18) . . ? F5 P3 F4 90.55(18) . . ? F1 P3 F6 175.0(3) . . ? F2 P3 F6 87.4(3) . . ? F3 P3 F6 89.9(2) . . ? F5 P3 F6 89.01(19) . . ? F4 P3 F6 84.7(2) . . ? F12 P4 F11A 137.3(5) . . ? F12 P4 F9A 127.7(5) . . ? F11A P4 F9A 92.3(3) . . ? F12 P4 F7 97.5(3) . . ? F11A P4 F7 41.2(4) . . ? F9A P4 F7 133.5(5) . . ? F12 P4 F9 92.5(3) . . ? F11A P4 F9 128.2(4) . . ? F9A P4 F9 36.0(4) . . ? F7 P4 F9 169.3(3) . . ? F12 P4 F10 84.2(4) . . ? F11A P4 F10 84.6(4) . . ? F9A P4 F10 85.8(4) . . ? F7 P4 F10 88.9(2) . . ? F9 P4 F10 88.3(2) . . ? F12 P4 F8 99.8(3) . . ? F11A P4 F8 92.4(3) . . ? F9A P4 F8 91.6(3) . . ? F7 P4 F8 90.6(2) . . ? F9 P4 F8 91.4(2) . . ? F10 P4 F8 175.9(3) . . ? F12 P4 F12A 40.2(4) . . ? F11A P4 F12A 177.5(4) . . ? F9A P4 F12A 90.2(3) . . ? F7 P4 F12A 136.3(4) . . ? F9 P4 F12A 54.3(4) . . ? F10 P4 F12A 95.0(4) . . ? F8 P4 F12A 88.1(3) . . ? F12 P4 F11 174.6(3) . . ? F11A P4 F11 46.1(4) . . ? F9A P4 F11 47.5(5) . . ? F7 P4 F11 86.7(3) . . ? F9 P4 F11 83.1(3) . . ? F10 P4 F11 92.3(3) . . ? F8 P4 F11 83.6(2) . . ? F12A P4 F11 136.4(4) . . ? F12 P4 F7A 51.2(4) . . ? F11A P4 F7A 89.3(3) . . ? F9A P4 F7A 177.8(4) . . ? F7 P4 F7A 48.1(4) . . ? F9 P4 F7A 142.5(4) . . ? F10 P4 F7A 95.9(3) . . ? F8 P4 F7A 86.8(3) . . ? F12A P4 F7A 88.2(3) . . ? F11 P4 F7A 133.7(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.589 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.062 #===END data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Cl N2 Rh' _chemical_formula_sum 'C31 H40 Cl N2 Rh' _chemical_formula_weight 579.01 _chemical_absolute_configuration ad 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 14.2752(3) _cell_length_b 17.6422(3) _cell_length_c 21.5550(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5428.54(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9476 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8063 _exptl_absorpt_correction_T_max 0.8645 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12403 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.47 _reflns_number_total 12403 _reflns_number_gt 9476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+28.0348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(6) _refine_ls_number_reflns 12403 _refine_ls_number_parameters 636 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0865 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _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 C1 C 0.9529(5) 0.5881(4) 0.8528(4) 0.0243(18) Uani 1 1 d . . . C2 C 0.9972(7) 0.5003(5) 0.7675(5) 0.045(3) Uani 1 1 d . . . H2 H 0.9945 0.4987 0.7211 0.055 Uiso 1 1 calc R . . C3 C 0.9328(6) 0.4455(5) 0.7967(5) 0.052(3) Uani 1 1 d . . . C4 C 0.9688(7) 0.4470(4) 0.8644(4) 0.0336(19) Uani 1 1 d . . . C5 C 1.0750(7) 0.4373(6) 0.8522(6) 0.062(3) Uani 1 1 d . . . H5A H 1.1119 0.4589 0.8868 0.074 Uiso 1 1 calc R . . H5B H 1.0910 0.3829 0.8480 0.074 Uiso 1 1 calc R . . C6 C 1.0954(6) 0.4787(6) 0.7930(5) 0.045(2) Uani 1 1 d . . . H6A H 1.1293 0.4456 0.7634 0.055 Uiso 1 1 calc R . . H6B H 1.1335 0.5245 0.8010 0.055 Uiso 1 1 calc R . . C7 C 0.9488(7) 0.3678(5) 0.7657(4) 0.056(2) Uani 1 1 d . . . H7A H 0.9340 0.3713 0.7214 0.084 Uiso 1 1 calc R . . H7B H 0.9081 0.3299 0.7852 0.084 Uiso 1 1 calc R . . H7C H 1.0144 0.3528 0.7709 0.084 Uiso 1 1 calc R . . C8 C 0.8327(5) 0.4648(4) 0.7887(4) 0.0410(19) Uani 1 1 d . . . H8A H 0.8200 0.5140 0.8081 0.062 Uiso 1 1 calc R . . H8B H 0.7939 0.4258 0.8083 0.062 Uiso 1 1 calc R . . H8C H 0.8179 0.4675 0.7444 0.062 Uiso 1 1 calc R . . C9 C 0.9374(7) 0.3879(4) 0.9072(4) 0.047(2) Uani 1 1 d . . . H9A H 0.9677 0.3951 0.9476 0.071 Uiso 1 1 calc R . . H9B H 0.9542 0.3381 0.8906 0.071 Uiso 1 1 calc R . . H9C H 0.8693 0.3910 0.9123 0.071 Uiso 1 1 calc R . . C10 C 0.9550(6) 0.6349(5) 0.7479(4) 0.031(2) Uani 1 1 d . . . H10A H 0.9377 0.6823 0.7697 0.037 Uiso 1 1 calc R . . H10B H 0.9013 0.6202 0.7214 0.037 Uiso 1 1 calc R . . C11 C 1.0400(6) 0.6507(5) 0.7061(4) 0.0271(19) Uani 1 1 d . . . C12 C 1.1244(6) 0.6667(5) 0.7329(5) 0.038(2) Uani 1 1 d . . . H12 H 1.1306 0.6663 0.7767 0.046 Uiso 1 1 calc R . . C13 C 1.2031(6) 0.6839(6) 0.6947(4) 0.035(2) Uani 1 1 d . . . H13 H 1.2628 0.6935 0.7126 0.042 Uiso 1 1 calc R . . C14 C 1.1905(6) 0.6865(6) 0.6301(4) 0.037(2) Uani 1 1 d . . . H14 H 1.2419 0.6988 0.6039 0.044 Uiso 1 1 calc R . . C15 C 1.1058(6) 0.6718(5) 0.6049(4) 0.041(2) Uani 1 1 d . . . H15 H 1.0984 0.6754 0.5612 0.049 Uiso 1 1 calc R . . C16 C 1.0269(7) 0.6509(5) 0.6420(4) 0.035(2) Uani 1 1 d . . . H16 H 0.9685 0.6378 0.6239 0.042 Uiso 1 1 calc R . . C17 C 0.9527(6) 0.5410(5) 0.9581(4) 0.033(2) Uani 1 1 d . . . H17A H 0.8991 0.5122 0.9753 0.039 Uiso 1 1 calc R . . H17B H 0.9398 0.5956 0.9646 0.039 Uiso 1 1 calc R . . C18 C 1.0417(7) 0.5196(5) 0.9945(4) 0.032(2) Uani 1 1 d . . . C19 C 1.1233(6) 0.5583(5) 0.9827(5) 0.039(2) Uani 1 1 d . . . H19 H 1.1250 0.5957 0.9511 0.047 Uiso 1 1 calc R . . C20 C 1.2041(7) 0.5426(6) 1.0173(6) 0.052(3) Uani 1 1 d . . . H20 H 1.2598 0.5707 1.0104 0.063 Uiso 1 1 calc R . . C21 C 1.2021(8) 0.4868(5) 1.0606(6) 0.050(3) Uani 1 1 d . . . H21 H 1.2580 0.4744 1.0823 0.060 Uiso 1 1 calc R . . C22 C 1.1204(8) 0.4474(6) 1.0739(5) 0.056(3) Uani 1 1 d . . . H22 H 1.1192 0.4105 1.1060 0.067 Uiso 1 1 calc R . . C23 C 1.0392(8) 0.4631(6) 1.0391(5) 0.043(3) Uani 1 1 d . . . H23 H 0.9833 0.4352 1.0461 0.052 Uiso 1 1 calc R . . C24 C 0.7804(5) 0.6460(5) 0.9075(3) 0.0217(17) Uani 1 1 d . . . H24 H 0.8085 0.5973 0.9106 0.026 Uiso 1 1 calc R . . C25 C 0.8721(5) 0.8141(4) 0.8868(4) 0.0258(17) Uani 1 1 d . . . H25 H 0.9334 0.8278 0.8738 0.031 Uiso 1 1 calc R . . C26 C 0.8611(6) 0.7859(4) 0.9445(4) 0.0261(19) Uani 1 1 d . . . H26 H 0.9161 0.7772 0.9683 0.031 Uiso 1 1 calc R . . C27 C 0.7679(6) 0.7670(5) 0.9744(4) 0.031(2) Uani 1 1 d . . . H27A H 0.7183 0.7986 0.9555 0.038 Uiso 1 1 calc R . . H27B H 0.7709 0.7796 1.0192 0.038 Uiso 1 1 calc R . . C28 C 0.7421(5) 0.6835(5) 0.9670(4) 0.0267(18) Uani 1 1 d . . . H28A H 0.6730 0.6789 0.9671 0.032 Uiso 1 1 calc R . . H28B H 0.7661 0.6553 1.0034 0.032 Uiso 1 1 calc R . . C29 C 0.7754(5) 0.6808(5) 0.8492(4) 0.0224(17) Uani 1 1 d . . . H29 H 0.8049 0.6559 0.8153 0.027 Uiso 1 1 calc R . . C30 C 0.7255(6) 0.7564(4) 0.8362(4) 0.0258(18) Uani 1 1 d . . . H30A H 0.6733 0.7626 0.8660 0.031 Uiso 1 1 calc R . . H30B H 0.6984 0.7550 0.7939 0.031 Uiso 1 1 calc R . . C31 C 0.7923(6) 0.8252(5) 0.8415(4) 0.030(2) Uani 1 1 d . . . H31A H 0.8187 0.8361 0.8000 0.036 Uiso 1 1 calc R . . H31B H 0.7555 0.8700 0.8545 0.036 Uiso 1 1 calc R . . C32 C 1.4483(5) 0.4119(4) 0.8537(4) 0.0228(18) Uani 1 1 d . . . C33 C 1.4977(8) 0.5422(8) 0.8805(6) 0.073(4) Uani 1 1 d . . . H33 H 1.4903 0.5782 0.9161 0.088 Uiso 1 1 calc R . . C34 C 1.4404(10) 0.5654(7) 0.8244(7) 0.077(4) Uani 1 1 d . . . C35 C 1.4785(9) 0.5119(7) 0.7771(6) 0.059(3) Uani 1 1 d . . . C36 C 1.5849(8) 0.5266(7) 0.7855(6) 0.064(3) Uani 1 1 d . . . H36A H 1.6217 0.4818 0.7725 0.077 Uiso 1 1 calc R . . H36B H 1.6050 0.5709 0.7607 0.077 Uiso 1 1 calc R . . C37 C 1.5980(9) 0.5419(8) 0.8542(6) 0.078(4) Uani 1 1 d . . . H37A H 1.6290 0.5914 0.8611 0.093 Uiso 1 1 calc R . . H37B H 1.6361 0.5015 0.8738 0.093 Uiso 1 1 calc R . . C38 C 1.3354(5) 0.5591(4) 0.8361(4) 0.0419(19) Uani 1 1 d . . . H38A H 1.3211 0.5090 0.8533 0.063 Uiso 1 1 calc R . . H38B H 1.3015 0.5658 0.7969 0.063 Uiso 1 1 calc R . . H38C H 1.3160 0.5984 0.8656 0.063 Uiso 1 1 calc R . . C39 C 1.4632(10) 0.6482(7) 0.8085(7) 0.096(4) Uani 1 1 d . . . H39A H 1.4680 0.6778 0.8469 0.145 Uiso 1 1 calc R . . H39B H 1.4134 0.6692 0.7824 0.145 Uiso 1 1 calc R . . H39C H 1.5229 0.6504 0.7861 0.145 Uiso 1 1 calc R . . C40 C 1.4488(10) 0.5278(6) 0.7107(5) 0.085(4) Uani 1 1 d . . . H40A H 1.4835 0.4945 0.6824 0.128 Uiso 1 1 calc R . . H40B H 1.4624 0.5808 0.7004 0.128 Uiso 1 1 calc R . . H40C H 1.3815 0.5184 0.7063 0.128 Uiso 1 1 calc R . . C41 C 1.4547(7) 0.4559(6) 0.9605(5) 0.044(3) Uani 1 1 d . . . H41A H 1.4400 0.4018 0.9679 0.053 Uiso 1 1 calc R . . H41B H 1.4011 0.4860 0.9761 0.053 Uiso 1 1 calc R . . C42 C 1.5389(7) 0.4759(6) 0.9979(5) 0.037(2) Uani 1 1 d . . . C43 C 1.6250(8) 0.4389(6) 0.9889(6) 0.059(4) Uani 1 1 d . . . H43 H 1.6298 0.3993 0.9592 0.071 Uiso 1 1 calc R . . C44 C 1.7015(8) 0.4595(6) 1.0226(7) 0.058(3) Uani 1 1 d . . . H44 H 1.7601 0.4359 1.0149 0.070 Uiso 1 1 calc R . . C45 C 1.6947(8) 0.5153(6) 1.0687(6) 0.057(3) Uani 1 1 d . . . H45 H 1.7470 0.5268 1.0943 0.069 Uiso 1 1 calc R . . C46 C 1.6128(8) 0.5527(6) 1.0762(5) 0.058(3) Uani 1 1 d . . . H46 H 1.6084 0.5940 1.1043 0.070 Uiso 1 1 calc R . . C47 C 1.5360(7) 0.5301(6) 1.0425(4) 0.040(2) Uani 1 1 d . . . H47 H 1.4776 0.5537 1.0510 0.047 Uiso 1 1 calc R . . C48 C 1.4435(6) 0.3695(5) 0.7455(4) 0.032(2) Uani 1 1 d . . . H48A H 1.3912 0.3838 0.7177 0.038 Uiso 1 1 calc R . . H48B H 1.4256 0.3220 0.7669 0.038 Uiso 1 1 calc R . . C49 C 1.5290(7) 0.3544(5) 0.7065(5) 0.031(2) Uani 1 1 d . . . C50 C 1.6166(6) 0.3363(5) 0.7325(4) 0.032(2) Uani 1 1 d . . . H50 H 1.6240 0.3366 0.7763 0.038 Uiso 1 1 calc R . . C51 C 1.6904(6) 0.3184(5) 0.6960(4) 0.033(2) Uani 1 1 d . . . H51 H 1.7483 0.3064 0.7153 0.040 Uiso 1 1 calc R . . C52 C 1.6855(6) 0.3168(6) 0.6329(4) 0.040(2) Uani 1 1 d . . . H52 H 1.7390 0.3052 0.6084 0.048 Uiso 1 1 calc R . . C53 C 1.5965(6) 0.3332(5) 0.6047(4) 0.036(2) Uani 1 1 d . . . H53 H 1.5887 0.3313 0.5609 0.044 Uiso 1 1 calc R . . C54 C 1.5233(7) 0.3518(6) 0.6430(4) 0.035(2) Uani 1 1 d . . . H54 H 1.4648 0.3637 0.6243 0.042 Uiso 1 1 calc R . . C55 C 1.2712(5) 0.3180(5) 0.8462(4) 0.0251(18) Uani 1 1 d . . . H55 H 1.3000 0.3442 0.8127 0.030 Uiso 1 1 calc R . . C56 C 1.2756(5) 0.3494(4) 0.9068(4) 0.0259(19) Uani 1 1 d . . . H56 H 1.3064 0.3968 0.9107 0.031 Uiso 1 1 calc R . . C57 C 1.2377(6) 0.3164(5) 0.9639(4) 0.033(2) Uani 1 1 d . . . H57A H 1.1687 0.3215 0.9637 0.040 Uiso 1 1 calc R . . H57B H 1.2621 0.3449 1.0000 0.040 Uiso 1 1 calc R . . C58 C 1.2640(6) 0.2314(5) 0.9709(4) 0.033(2) Uani 1 1 d . . . H58A H 1.2650 0.2183 1.0155 0.040 Uiso 1 1 calc R . . H58B H 1.2150 0.2002 0.9508 0.040 Uiso 1 1 calc R . . C59 C 1.3574(6) 0.2121(5) 0.9428(4) 0.032(2) Uani 1 1 d . . . H59 H 1.4123 0.2174 0.9674 0.039 Uiso 1 1 calc R . . C60 C 1.3659(5) 0.1866(4) 0.8815(4) 0.0267(17) Uani 1 1 d . . . H60 H 1.4272 0.1748 0.8673 0.032 Uiso 1 1 calc R . . C61 C 1.2873(6) 0.1761(5) 0.8361(4) 0.036(2) Uani 1 1 d . . . H61A H 1.2504 0.1308 0.8480 0.043 Uiso 1 1 calc R . . H61B H 1.3137 0.1670 0.7943 0.043 Uiso 1 1 calc R . . C62 C 1.2225(6) 0.2451(5) 0.8338(4) 0.032(2) Uani 1 1 d . . . H62A H 1.1928 0.2475 0.7923 0.038 Uiso 1 1 calc R . . H62B H 1.1720 0.2383 0.8648 0.038 Uiso 1 1 calc R . . N1 N 0.9701(5) 0.5765(4) 0.7931(3) 0.0316(17) Uani 1 1 d . . . N2 N 0.9585(4) 0.5262(4) 0.8904(4) 0.0280(15) Uani 1 1 d . . . N3 N 1.4618(5) 0.4677(4) 0.8944(4) 0.0372(19) Uani 1 1 d . . . N4 N 1.4559(5) 0.4305(4) 0.7931(3) 0.0251(15) Uani 1 1 d . . . Cl1 Cl 1.07268(13) 0.73054(11) 0.89369(11) 0.0328(5) Uani 1 1 d . . . Cl2 Cl 1.56735(13) 0.26886(11) 0.89434(12) 0.0345(5) Uani 1 1 d . . . Rh1 Rh 0.91263(3) 0.69362(3) 0.88442(3) 0.01967(14) Uani 1 1 d . . . Rh2 Rh 1.40846(3) 0.30581(3) 0.88289(3) 0.02027(15) 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 C1 0.016(3) 0.022(4) 0.036(5) -0.003(4) -0.003(3) 0.000(3) C2 0.070(6) 0.031(5) 0.036(5) 0.001(4) 0.007(5) 0.018(4) C3 0.030(4) 0.042(5) 0.083(8) -0.026(5) -0.004(5) 0.010(4) C4 0.054(5) 0.010(3) 0.038(5) 0.006(3) -0.010(4) 0.000(3) C5 0.056(6) 0.048(6) 0.081(8) -0.024(5) -0.026(6) 0.028(5) C6 0.032(4) 0.032(5) 0.072(7) -0.012(5) 0.013(5) 0.000(4) C7 0.076(6) 0.038(4) 0.053(6) -0.010(4) 0.004(5) -0.005(5) C8 0.031(4) 0.032(4) 0.061(6) -0.013(4) -0.011(4) -0.012(3) C9 0.081(6) 0.017(3) 0.043(4) 0.004(3) -0.003(4) -0.009(4) C10 0.034(4) 0.033(4) 0.027(5) 0.004(4) -0.007(4) 0.006(4) C11 0.034(4) 0.022(4) 0.025(5) -0.002(4) -0.001(4) 0.013(4) C12 0.039(5) 0.040(5) 0.036(6) -0.008(4) -0.010(4) 0.011(4) C13 0.029(4) 0.037(5) 0.039(5) -0.006(4) -0.007(4) 0.004(4) C14 0.048(5) 0.032(5) 0.032(5) -0.006(5) -0.006(4) 0.013(4) C15 0.048(5) 0.051(6) 0.023(5) 0.000(4) 0.011(4) 0.006(4) C16 0.043(5) 0.038(5) 0.023(5) -0.003(4) -0.003(4) 0.012(5) C17 0.027(4) 0.035(5) 0.036(5) 0.019(4) 0.000(4) 0.007(4) C18 0.044(5) 0.025(5) 0.026(5) 0.003(4) -0.008(4) 0.001(4) C19 0.029(5) 0.033(5) 0.056(6) 0.011(4) -0.006(5) 0.006(4) C20 0.038(5) 0.029(5) 0.090(9) -0.019(6) -0.020(6) 0.002(5) C21 0.058(6) 0.032(5) 0.061(7) -0.008(5) -0.036(5) 0.014(5) C22 0.086(8) 0.037(6) 0.045(6) 0.007(5) -0.037(6) 0.013(6) C23 0.061(6) 0.026(5) 0.044(6) -0.004(4) -0.017(5) 0.005(5) C24 0.016(3) 0.029(4) 0.020(4) -0.003(3) -0.002(3) 0.000(3) C25 0.027(3) 0.016(4) 0.035(5) -0.001(4) 0.000(4) 0.006(3) C26 0.035(4) 0.020(4) 0.023(5) -0.001(3) -0.002(3) -0.002(3) C27 0.034(4) 0.035(5) 0.025(5) -0.009(4) 0.001(4) -0.001(4) C28 0.026(4) 0.029(4) 0.025(4) 0.001(4) 0.003(3) 0.001(4) C29 0.016(3) 0.026(4) 0.026(4) -0.006(4) 0.004(3) -0.003(3) C30 0.029(4) 0.023(4) 0.026(4) 0.000(4) -0.006(4) 0.009(3) C31 0.032(4) 0.023(4) 0.034(5) 0.007(4) 0.004(4) 0.001(3) C32 0.021(3) 0.023(4) 0.025(4) -0.001(4) 0.004(3) 0.005(3) C33 0.078(8) 0.068(8) 0.074(8) 0.004(6) -0.001(7) -0.015(6) C34 0.074(8) 0.061(7) 0.095(11) 0.004(7) -0.009(8) 0.000(6) C35 0.068(7) 0.054(6) 0.056(7) 0.028(5) 0.021(5) 0.017(6) C36 0.062(7) 0.047(6) 0.083(9) 0.010(6) 0.016(7) -0.006(6) C37 0.063(7) 0.078(8) 0.092(10) 0.014(7) -0.005(7) -0.014(6) C38 0.035(4) 0.034(4) 0.057(6) 0.007(4) -0.001(4) 0.013(3) C39 0.103(10) 0.083(9) 0.104(11) 0.006(8) -0.009(9) -0.007(8) C40 0.126(11) 0.052(6) 0.077(8) -0.004(6) -0.008(8) -0.028(7) C41 0.043(5) 0.052(6) 0.037(6) -0.015(5) 0.013(5) -0.007(5) C42 0.037(5) 0.027(5) 0.046(7) -0.005(4) 0.006(4) -0.010(4) C43 0.042(6) 0.037(6) 0.097(10) -0.022(6) 0.019(6) -0.007(5) C44 0.040(6) 0.033(5) 0.102(10) -0.003(7) 0.006(7) -0.008(5) C45 0.062(7) 0.041(6) 0.069(8) 0.008(6) -0.016(6) -0.007(5) C46 0.071(7) 0.053(7) 0.051(7) -0.016(6) -0.013(6) 0.024(6) C47 0.047(5) 0.038(5) 0.035(6) -0.017(4) -0.007(4) 0.006(4) C48 0.027(4) 0.041(5) 0.028(5) 0.008(4) -0.001(3) -0.011(4) C49 0.034(4) 0.028(4) 0.032(5) 0.004(4) 0.002(4) -0.002(4) C50 0.044(5) 0.029(4) 0.022(4) -0.002(4) -0.003(4) -0.006(4) C51 0.033(4) 0.031(5) 0.035(5) 0.004(4) 0.001(4) -0.003(4) C52 0.031(4) 0.047(6) 0.041(6) 0.002(5) 0.013(4) 0.009(4) C53 0.033(4) 0.046(5) 0.030(5) 0.007(4) -0.009(4) 0.002(4) C54 0.030(4) 0.036(5) 0.039(6) 0.008(5) 0.002(4) 0.000(4) C55 0.019(3) 0.031(5) 0.026(4) 0.000(4) -0.001(3) -0.002(4) C56 0.020(3) 0.017(4) 0.040(5) -0.007(4) 0.006(3) 0.001(3) C57 0.036(4) 0.039(5) 0.024(4) -0.006(4) 0.008(4) 0.003(5) C58 0.043(5) 0.030(4) 0.026(5) -0.003(4) 0.006(4) -0.011(4) C59 0.031(4) 0.026(5) 0.039(6) 0.012(4) 0.002(4) -0.009(4) C60 0.037(4) 0.016(4) 0.027(4) 0.004(4) 0.005(4) 0.006(3) C61 0.050(5) 0.028(5) 0.029(5) -0.001(4) -0.010(4) -0.010(4) C62 0.023(4) 0.041(5) 0.031(5) 0.000(4) -0.004(4) -0.003(4) N1 0.043(4) 0.027(4) 0.025(4) -0.007(3) 0.003(3) 0.008(3) N2 0.028(3) 0.020(3) 0.036(4) 0.006(3) -0.003(3) 0.002(3) N3 0.045(4) 0.023(3) 0.044(5) -0.011(3) 0.017(4) -0.014(3) N4 0.025(3) 0.024(3) 0.027(4) 0.003(3) -0.004(3) 0.000(3) Cl1 0.0250(8) 0.0294(10) 0.0442(13) -0.0026(10) -0.0046(10) -0.0047(8) Cl2 0.0240(8) 0.0304(10) 0.0491(14) 0.0015(11) -0.0034(10) 0.0065(8) Rh1 0.0181(2) 0.0171(3) 0.0238(3) -0.0015(3) -0.0005(3) -0.0006(2) Rh2 0.0201(3) 0.0181(3) 0.0226(3) 0.0007(3) -0.0008(3) 0.0013(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 C1 N1 1.325(11) . ? C1 N2 1.363(11) . ? C1 Rh1 2.063(8) . ? C2 C3 1.476(14) . ? C2 N1 1.505(11) . ? C2 C6 1.553(13) . ? C2 H2 1.0000 . ? C3 C8 1.479(11) . ? C3 C7 1.541(12) . ? C3 C4 1.548(13) . ? C4 C9 1.463(11) . ? C4 N2 1.512(10) . ? C4 C5 1.548(14) . ? C5 C6 1.498(15) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.435(11) . ? C10 C11 1.537(12) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.364(12) . ? C11 C16 1.394(12) . ? C12 C13 1.425(12) . ? C12 H12 0.9500 . ? C13 C14 1.407(12) . ? C13 H13 0.9500 . ? C14 C15 1.351(13) . ? C14 H14 0.9500 . ? C15 C16 1.429(13) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.485(11) . ? C17 C18 1.541(12) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.374(13) . ? C18 C23 1.385(14) . ? C19 C20 1.400(14) . ? C19 H19 0.9500 . ? C20 C21 1.357(15) . ? C20 H20 0.9500 . ? C21 C22 1.388(16) . ? C21 H21 0.9500 . ? C22 C23 1.408(13) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.401(11) . ? C24 C28 1.544(11) . ? C24 Rh1 2.125(7) . ? C24 H24 0.9500 . ? C25 C26 1.350(11) . ? C25 C31 1.512(11) . ? C25 Rh1 2.204(7) . ? C25 H25 0.9500 . ? C26 C27 1.515(11) . ? C26 Rh1 2.206(8) . ? C26 H26 0.9500 . ? C27 C28 1.527(12) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.538(10) . ? C29 Rh1 2.113(7) . ? C29 H29 0.9500 . ? C30 C31 1.548(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N3 1.333(11) . ? C32 N4 1.351(11) . ? C32 Rh2 2.054(8) . ? C33 N3 1.443(14) . ? C33 C34 1.517(17) . ? C33 C37 1.539(16) . ? C33 H33 1.0000 . ? C34 C35 1.493(17) . ? C34 C38 1.524(15) . ? C34 C39 1.536(17) . ? C35 N4 1.511(13) . ? C35 C40 1.520(16) . ? C35 C36 1.551(16) . ? C36 C37 1.516(17) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N3 1.444(12) . ? C41 C42 1.490(14) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C47 1.357(13) . ? C42 C43 1.405(15) . ? C43 C44 1.362(16) . ? C43 H43 0.9500 . ? C44 C45 1.402(17) . ? C44 H44 0.9500 . ? C45 C46 1.351(15) . ? C45 H45 0.9500 . ? C46 C47 1.374(14) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 N4 1.498(11) . ? C48 C49 1.505(12) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.372(13) . ? C49 C50 1.408(12) . ? C50 C51 1.351(12) . ? C50 H50 0.9500 . ? C51 C52 1.363(13) . ? C51 H51 0.9500 . ? C52 C53 1.438(11) . ? C52 H52 0.9500 . ? C53 C54 1.372(13) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.421(11) . ? C55 C62 1.487(11) . ? C55 Rh2 2.125(7) . ? C55 H55 0.9500 . ? C56 C57 1.464(12) . ? C56 Rh2 2.110(8) . ? C56 H56 0.9500 . ? C57 C58 1.552(12) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.503(12) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.403(12) . ? C59 Rh2 2.221(8) . ? C59 H59 0.9500 . ? C60 C61 1.499(11) . ? C60 Rh2 2.190(8) . ? C60 H60 0.9500 . ? C61 C62 1.530(12) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? Cl1 Rh1 2.384(2) . ? Cl2 Rh2 2.3729(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 N1 C1 N2 116.3(7) . . ? N1 C1 Rh1 120.8(6) . . ? N2 C1 Rh1 122.9(6) . . ? C3 C2 N1 105.5(8) . . ? C3 C2 C6 104.5(8) . . ? N1 C2 C6 108.8(8) . . ? C3 C2 H2 112.5 . . ? N1 C2 H2 112.5 . . ? C6 C2 H2 112.5 . . ? C2 C3 C8 113.7(9) . . ? C2 C3 C7 107.8(8) . . ? C8 C3 C7 107.3(8) . . ? C2 C3 C4 100.6(8) . . ? C8 C3 C4 115.3(9) . . ? C7 C3 C4 112.0(8) . . ? C9 C4 N2 113.3(7) . . ? C9 C4 C5 109.1(8) . . ? N2 C4 C5 105.2(7) . . ? C9 C4 C3 118.7(8) . . ? N2 C4 C3 109.5(6) . . ? C5 C4 C3 99.4(8) . . ? C6 C5 C4 106.3(8) . . ? C6 C5 H5A 110.5 . . ? C4 C5 H5A 110.5 . . ? C6 C5 H5B 110.5 . . ? C4 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C5 C6 C2 104.2(8) . . ? C5 C6 H6A 110.9 . . ? C2 C6 H6A 110.9 . . ? C5 C6 H6B 110.9 . . ? C2 C6 H6B 110.9 . . ? H6A C6 H6B 108.9 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 114.2(7) . . ? N1 C10 H10A 108.7 . . ? C11 C10 H10A 108.7 . . ? N1 C10 H10B 108.7 . . ? C11 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C16 122.5(9) . . ? C12 C11 C10 119.2(8) . . ? C16 C11 C10 118.3(8) . . ? C11 C12 C13 119.8(9) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 118.5(8) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 120.4(9) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 122.1(9) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C11 C16 C15 116.7(9) . . ? C11 C16 H16 121.7 . . ? C15 C16 H16 121.7 . . ? N2 C17 C18 114.3(7) . . ? N2 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? N2 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C23 120.5(9) . . ? C19 C18 C17 118.9(8) . . ? C23 C18 C17 120.6(9) . . ? C18 C19 C20 120.1(9) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C21 C20 C19 119.5(10) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 121.5(9) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C23 118.9(9) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C18 C23 C22 119.3(10) . . ? C18 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C29 C24 C28 122.7(7) . . ? C29 C24 Rh1 70.2(4) . . ? C28 C24 Rh1 109.9(5) . . ? C29 C24 H24 118.6 . . ? C28 C24 H24 118.6 . . ? Rh1 C24 H24 89.9 . . ? C26 C25 C31 123.7(7) . . ? C26 C25 Rh1 72.3(5) . . ? C31 C25 Rh1 107.9(5) . . ? C26 C25 H25 118.2 . . ? C31 C25 H25 118.2 . . ? Rh1 C25 H25 89.8 . . ? C25 C26 C27 125.1(8) . . ? C25 C26 Rh1 72.1(5) . . ? C27 C26 Rh1 112.4(5) . . ? C25 C26 H26 117.4 . . ? C27 C26 H26 117.4 . . ? Rh1 C26 H26 85.5 . . ? C26 C27 C28 112.3(7) . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C27 C28 C24 114.5(7) . . ? C27 C28 H28A 108.6 . . ? C24 C28 H28A 108.6 . . ? C27 C28 H28B 108.6 . . ? C24 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C24 C29 C30 124.5(7) . . ? C24 C29 Rh1 71.2(5) . . ? C30 C29 Rh1 113.7(5) . . ? C24 C29 H29 117.8 . . ? C30 C29 H29 117.8 . . ? Rh1 C29 H29 85.1 . . ? C29 C30 C31 112.4(6) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? C25 C31 C30 114.3(7) . . ? C25 C31 H31A 108.7 . . ? C30 C31 H31A 108.7 . . ? C25 C31 H31B 108.7 . . ? C30 C31 H31B 108.7 . . ? H31A C31 H31B 107.6 . . ? N3 C32 N4 116.3(8) . . ? N3 C32 Rh2 120.8(6) . . ? N4 C32 Rh2 122.7(6) . . ? N3 C33 C34 102.6(10) . . ? N3 C33 C37 113.7(11) . . ? C34 C33 C37 102.1(11) . . ? N3 C33 H33 112.5 . . ? C34 C33 H33 112.5 . . ? C37 C33 H33 112.5 . . ? C35 C34 C33 100.2(11) . . ? C35 C34 C38 115.2(11) . . ? C33 C34 C38 112.3(11) . . ? C35 C34 C39 111.8(12) . . ? C33 C34 C39 108.6(11) . . ? C38 C34 C39 108.4(10) . . ? C34 C35 N4 111.5(9) . . ? C34 C35 C40 115.2(10) . . ? N4 C35 C40 109.4(10) . . ? C34 C35 C36 99.8(11) . . ? N4 C35 C36 110.0(9) . . ? C40 C35 C36 110.7(10) . . ? C37 C36 C35 105.4(10) . . ? C37 C36 H36A 110.7 . . ? C35 C36 H36A 110.7 . . ? C37 C36 H36B 110.7 . . ? C35 C36 H36B 110.7 . . ? H36A C36 H36B 108.8 . . ? C36 C37 C33 104.2(10) . . ? C36 C37 H37A 110.9 . . ? C33 C37 H37A 110.9 . . ? C36 C37 H37B 110.9 . . ? C33 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 C42 116.3(8) . . ? N3 C41 H41A 108.2 . . ? C42 C41 H41A 108.2 . . ? N3 C41 H41B 108.2 . . ? C42 C41 H41B 108.2 . . ? H41A C41 H41B 107.4 . . ? C47 C42 C43 116.9(10) . . ? C47 C42 C41 121.7(10) . . ? C43 C42 C41 121.4(9) . . ? C44 C43 C42 120.2(10) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.7(11) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.2(11) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C47 119.1(10) . . ? C45 C46 H46 120.5 . . ? C47 C46 H46 120.5 . . ? C42 C47 C46 123.7(10) . . ? C42 C47 H47 118.2 . . ? C46 C47 H47 118.2 . . ? N4 C48 C49 114.5(7) . . ? N4 C48 H48A 108.6 . . ? C49 C48 H48A 108.6 . . ? N4 C48 H48B 108.6 . . ? C49 C48 H48B 108.6 . . ? H48A C48 H48B 107.6 . . ? C54 C49 C50 116.3(9) . . ? C54 C49 C48 121.0(9) . . ? C50 C49 C48 122.5(8) . . ? C51 C50 C49 120.9(8) . . ? C51 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? C50 C51 C52 123.1(9) . . ? C50 C51 H51 118.4 . . ? C52 C51 H51 118.4 . . ? C51 C52 C53 117.6(8) . . ? C51 C52 H52 121.2 . . ? C53 C52 H52 121.2 . . ? C54 C53 C52 117.8(8) . . ? C54 C53 H53 121.1 . . ? C52 C53 H53 121.1 . . ? C49 C54 C53 124.3(9) . . ? C49 C54 H54 117.8 . . ? C53 C54 H54 117.8 . . ? C56 C55 C62 121.5(8) . . ? C56 C55 Rh2 69.9(5) . . ? C62 C55 Rh2 114.2(6) . . ? C56 C55 H55 119.2 . . ? C62 C55 H55 119.2 . . ? Rh2 C55 H55 86.1 . . ? C55 C56 C57 127.0(7) . . ? C55 C56 Rh2 70.9(4) . . ? C57 C56 Rh2 113.1(6) . . ? C55 C56 H56 116.5 . . ? C57 C56 H56 116.5 . . ? Rh2 C56 H56 85.8 . . ? C56 C57 C58 112.1(7) . . ? C56 C57 H57A 109.2 . . ? C58 C57 H57A 109.2 . . ? C56 C57 H57B 109.2 . . ? C58 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C59 C58 C57 113.2(7) . . ? C59 C58 H58A 108.9 . . ? C57 C58 H58A 108.9 . . ? C59 C58 H58B 108.9 . . ? C57 C58 H58B 108.9 . . ? H58A C58 H58B 107.7 . . ? C60 C59 C58 121.9(8) . . ? C60 C59 Rh2 70.3(5) . . ? C58 C59 Rh2 110.9(6) . . ? C60 C59 H59 119.1 . . ? C58 C59 H59 119.1 . . ? Rh2 C59 H59 88.9 . . ? C59 C60 C61 126.2(7) . . ? C59 C60 Rh2 72.7(5) . . ? C61 C60 Rh2 109.6(5) . . ? C59 C60 H60 116.9 . . ? C61 C60 H60 116.9 . . ? Rh2 C60 H60 87.6 . . ? C60 C61 C62 112.1(7) . . ? C60 C61 H61A 109.2 . . ? C62 C61 H61A 109.2 . . ? C60 C61 H61B 109.2 . . ? C62 C61 H61B 109.2 . . ? H61A C61 H61B 107.9 . . ? C55 C62 C61 113.6(7) . . ? C55 C62 H62A 108.9 . . ? C61 C62 H62A 108.9 . . ? C55 C62 H62B 108.9 . . ? C61 C62 H62B 108.9 . . ? H62A C62 H62B 107.7 . . ? C1 N1 C10 121.4(7) . . ? C1 N1 C2 122.9(8) . . ? C10 N1 C2 115.5(7) . . ? C1 N2 C17 116.1(7) . . ? C1 N2 C4 121.7(7) . . ? C17 N2 C4 122.2(7) . . ? C32 N3 C33 126.1(9) . . ? C32 N3 C41 122.2(8) . . ? C33 N3 C41 111.1(9) . . ? C32 N4 C48 118.5(7) . . ? C32 N4 C35 118.0(8) . . ? C48 N4 C35 123.5(8) . . ? C1 Rh1 C29 92.5(3) . . ? C1 Rh1 C24 88.2(3) . . ? C29 Rh1 C24 38.6(3) . . ? C1 Rh1 C25 161.9(4) . . ? C29 Rh1 C25 82.4(3) . . ? C24 Rh1 C25 98.2(3) . . ? C1 Rh1 C26 162.2(3) . . ? C29 Rh1 C26 88.9(3) . . ? C24 Rh1 C26 81.8(3) . . ? C25 Rh1 C26 35.6(3) . . ? C1 Rh1 Cl1 90.4(2) . . ? C29 Rh1 Cl1 161.4(2) . . ? C24 Rh1 Cl1 160.0(2) . . ? C25 Rh1 Cl1 89.2(2) . . ? C26 Rh1 Cl1 93.9(2) . . ? C32 Rh2 C56 89.5(3) . . ? C32 Rh2 C55 92.8(3) . . ? C56 Rh2 C55 39.2(3) . . ? C32 Rh2 C60 161.3(3) . . ? C56 Rh2 C60 96.0(3) . . ? C55 Rh2 C60 80.6(3) . . ? C32 Rh2 C59 161.2(3) . . ? C56 Rh2 C59 80.5(3) . . ? C55 Rh2 C59 89.4(3) . . ? C60 Rh2 C59 37.1(3) . . ? C32 Rh2 Cl2 91.0(2) . . ? C56 Rh2 Cl2 159.0(2) . . ? C55 Rh2 Cl2 161.5(2) . . ? C60 Rh2 Cl2 90.2(2) . . ? C59 Rh2 Cl2 92.8(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.550 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.118 #===END data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd5a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H40 Cl Ir N2' _chemical_formula_sum 'C31 H40 Cl Ir N2' _chemical_formula_weight 668.30 _chemical_absolute_configuration ad 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 17.6218(3) _cell_length_b 14.3216(3) _cell_length_c 21.4272(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5407.63(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10884 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 29.58 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 5.059 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3121 _exptl_absorpt_correction_T_max 0.6877 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14343 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 29.58 _reflns_number_total 14343 _reflns_number_gt 10884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0521P)^2^+32.8235P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 0.030(15) _refine_ls_number_reflns 14343 _refine_ls_number_parameters 635 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1096 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _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 C1 C 0.6655(5) 1.2003(6) 0.1047(5) 0.027(2) Uani 1 1 d . . . C2 C 0.8041(6) 1.2250(10) 0.1159(7) 0.054(4) Uani 1 1 d . . . C3 C 0.8102(8) 1.3333(8) 0.1004(6) 0.060(3) Uani 1 1 d . . . H3A H 0.7835 1.3707 0.1324 0.072 Uiso 1 1 calc R . . H3B H 0.8640 1.3530 0.0990 0.072 Uiso 1 1 calc R . . C4 C 0.7739(7) 1.3458(10) 0.0382(8) 0.066(4) Uani 1 1 d . . . H4A H 0.8098 1.3744 0.0082 0.079 Uiso 1 1 calc R . . H4B H 0.7283 1.3860 0.0414 0.079 Uiso 1 1 calc R . . C5 C 0.7519(6) 1.2443(8) 0.0174(6) 0.045(3) Uani 1 1 d . . . H5 H 0.7537 1.2371 -0.0290 0.054 Uiso 1 1 calc R . . C6 C 0.8072(7) 1.1810(8) 0.0494(6) 0.050(3) Uani 1 1 d . . . C7 C 0.8631(10) 1.1790(14) 0.1560(10) 0.098(6) Uani 1 1 d . . . H7A H 0.8566 1.1991 0.1994 0.147 Uiso 1 1 calc R . . H7B H 0.9137 1.1968 0.1413 0.147 Uiso 1 1 calc R . . H7C H 0.8574 1.1110 0.1534 0.147 Uiso 1 1 calc R . . C8 C 0.8866(7) 1.1980(9) 0.0174(8) 0.073(4) Uani 1 1 d . . . H8A H 0.8790 1.2154 -0.0264 0.110 Uiso 1 1 calc R . . H8B H 0.9169 1.1406 0.0196 0.110 Uiso 1 1 calc R . . H8C H 0.9133 1.2484 0.0391 0.110 Uiso 1 1 calc R . . C9 C 0.7930(7) 1.0837(8) 0.0462(7) 0.051(3) Uani 1 1 d . . . H9A H 0.7524 1.0674 0.0756 0.076 Uiso 1 1 calc R . . H9B H 0.8392 1.0494 0.0572 0.076 Uiso 1 1 calc R . . H9C H 0.7774 1.0670 0.0038 0.076 Uiso 1 1 calc R . . C10 C 0.7117(6) 1.2012(8) 0.2096(6) 0.040(3) Uani 1 1 d . . . H10A H 0.7423 1.1487 0.2261 0.048 Uiso 1 1 calc R . . H10B H 0.6577 1.1857 0.2168 0.048 Uiso 1 1 calc R . . C11 C 0.7304(6) 1.2873(8) 0.2471(5) 0.030(3) Uani 1 1 d . . . C12 C 0.7853(7) 1.2826(9) 0.2943(6) 0.043(3) Uani 1 1 d . . . H12 H 0.8118 1.2262 0.3026 0.052 Uiso 1 1 calc R . . C13 C 0.7998(7) 1.3643(11) 0.3292(6) 0.055(4) Uani 1 1 d . . . H13 H 0.8376 1.3622 0.3608 0.065 Uiso 1 1 calc R . . C14 C 0.7623(7) 1.4454(10) 0.3194(7) 0.053(4) Uani 1 1 d . . . H14 H 0.7721 1.4984 0.3448 0.063 Uiso 1 1 calc R . . C15 C 0.7080(6) 1.4499(8) 0.2706(6) 0.039(3) Uani 1 1 d . . . H15 H 0.6822 1.5068 0.2621 0.047 Uiso 1 1 calc R . . C16 C 0.6926(6) 1.3708(9) 0.2353(6) 0.042(3) Uani 1 1 d . . . H16 H 0.6560 1.3737 0.2028 0.050 Uiso 1 1 calc R . . C17 C 0.6200(6) 1.2029(8) -0.0030(5) 0.035(3) Uani 1 1 d . . . H17A H 0.5729 1.1829 0.0183 0.042 Uiso 1 1 calc R . . H17B H 0.6361 1.1513 -0.0307 0.042 Uiso 1 1 calc R . . C18 C 0.6025(6) 1.2881(8) -0.0428(5) 0.033(3) Uani 1 1 d . . . C19 C 0.5854(6) 1.3739(8) -0.0166(6) 0.037(3) Uani 1 1 d . . . H19 H 0.5869 1.3805 0.0275 0.044 Uiso 1 1 calc R . . C20 C 0.5666(7) 1.4497(8) -0.0524(6) 0.044(3) Uani 1 1 d . . . H20 H 0.5557 1.5080 -0.0333 0.053 Uiso 1 1 calc R . . C21 C 0.5636(7) 1.4403(8) -0.1181(6) 0.043(3) Uani 1 1 d . . . H21 H 0.5496 1.4921 -0.1432 0.051 Uiso 1 1 calc R . . C22 C 0.5810(7) 1.3559(9) -0.1456(6) 0.050(3) Uani 1 1 d . . . H22 H 0.5795 1.3492 -0.1897 0.059 Uiso 1 1 calc R . . C23 C 0.6006(6) 1.2814(8) -0.1080(6) 0.038(3) Uani 1 1 d . . . H23 H 0.6133 1.2235 -0.1270 0.046 Uiso 1 1 calc R . . C24 C 0.4667(5) 1.1099(7) 0.1943(5) 0.029(2) Uani 1 1 d . . . H24 H 0.4745 1.1645 0.2186 0.035 Uiso 1 1 calc R . . C25 C 0.4395(5) 1.1197(6) 0.1331(5) 0.0251(19) Uani 1 1 d . . . H25 H 0.4276 1.1809 0.1190 0.030 Uiso 1 1 calc R . . C26 C 0.4281(6) 1.0418(7) 0.0897(5) 0.030(2) Uani 1 1 d . . . H26A H 0.4175 1.0675 0.0477 0.036 Uiso 1 1 calc R . . H26B H 0.3829 1.0060 0.1030 0.036 Uiso 1 1 calc R . . C27 C 0.4963(5) 0.9739(7) 0.0848(5) 0.028(2) Uani 1 1 d . . . H27A H 0.4897 0.9221 0.1149 0.034 Uiso 1 1 calc R . . H27B H 0.4983 0.9468 0.0423 0.034 Uiso 1 1 calc R . . C28 C 0.5709(6) 1.0256(6) 0.0986(5) 0.026(2) Uani 1 1 d . . . H28 H 0.5957 1.0567 0.0652 0.032 Uiso 1 1 calc R . . C29 C 0.6039(5) 1.0292(6) 0.1579(5) 0.021(2) Uani 1 1 d . . . H29 H 0.6518 1.0590 0.1621 0.025 Uiso 1 1 calc R . . C30 C 0.5680(6) 0.9887(7) 0.2151(5) 0.029(2) Uani 1 1 d . . . H30A H 0.5967 1.0094 0.2523 0.035 Uiso 1 1 calc R . . H30B H 0.5711 0.9197 0.2131 0.035 Uiso 1 1 calc R . . C31 C 0.4840(6) 1.0176(7) 0.2227(5) 0.032(2) Uani 1 1 d . . . H31A H 0.4514 0.9696 0.2030 0.038 Uiso 1 1 calc R . . H31B H 0.4713 1.0197 0.2677 0.038 Uiso 1 1 calc R . . C32 C 0.8388(5) 0.6944(6) 0.1021(5) 0.0191(19) Uani 1 1 d . . . C33 C 0.6953(6) 0.6919(9) 0.1075(7) 0.051(3) Uani 1 1 d . . . C34 C 0.6887(5) 0.5893(6) 0.0852(5) 0.038(2) Uani 1 1 d . . . H34A H 0.6353 0.5678 0.0861 0.046 Uiso 1 1 calc R . . H34B H 0.7199 0.5472 0.1114 0.046 Uiso 1 1 calc R . . C35 C 0.7198(7) 0.5934(9) 0.0165(7) 0.058(3) Uani 1 1 d . . . H35A H 0.6794 0.5803 -0.0144 0.069 Uiso 1 1 calc R . . H35B H 0.7624 0.5494 0.0102 0.069 Uiso 1 1 calc R . . C36 C 0.7475(6) 0.6995(9) 0.0130(6) 0.049(3) Uani 1 1 d . . . H36 H 0.7470 0.7235 -0.0309 0.059 Uiso 1 1 calc R . . C37 C 0.6965(6) 0.7530(8) 0.0531(7) 0.055(3) Uani 1 1 d . . . C38 C 0.6354(6) 0.7126(10) 0.1569(6) 0.051(3) Uani 1 1 d . . . H38A H 0.6471 0.7722 0.1773 0.077 Uiso 1 1 calc R . . H38B H 0.6353 0.6626 0.1881 0.077 Uiso 1 1 calc R . . H38C H 0.5854 0.7165 0.1371 0.077 Uiso 1 1 calc R . . C39 C 0.6172(7) 0.7561(9) 0.0211(7) 0.064(4) Uani 1 1 d . . . H39A H 0.5882 0.7003 0.0325 0.096 Uiso 1 1 calc R . . H39B H 0.6238 0.7581 -0.0243 0.096 Uiso 1 1 calc R . . H39C H 0.5898 0.8119 0.0348 0.096 Uiso 1 1 calc R . . C40 C 0.7228(6) 0.8518(8) 0.0613(7) 0.051(3) Uani 1 1 d . . . H40A H 0.6952 0.8807 0.0961 0.077 Uiso 1 1 calc R . . H40B H 0.7130 0.8871 0.0230 0.077 Uiso 1 1 calc R . . H40C H 0.7773 0.8524 0.0703 0.077 Uiso 1 1 calc R . . C41 C 0.7883(7) 0.6940(8) 0.2074(5) 0.034(3) Uani 1 1 d . . . H41A H 0.8415 0.6755 0.2159 0.041 Uiso 1 1 calc R . . H41B H 0.7551 0.6431 0.2226 0.041 Uiso 1 1 calc R . . C42 C 0.7704(7) 0.7834(9) 0.2445(6) 0.037(3) Uani 1 1 d . . . C43 C 0.7185(7) 0.7817(10) 0.2932(6) 0.043(3) Uani 1 1 d . . . H43 H 0.6950 0.7241 0.3036 0.052 Uiso 1 1 calc R . . C44 C 0.6999(7) 0.8589(11) 0.3267(7) 0.059(4) Uani 1 1 d . . . H44 H 0.6625 0.8559 0.3586 0.070 Uiso 1 1 calc R . . C45 C 0.7358(7) 0.9406(10) 0.3136(7) 0.054(4) Uani 1 1 d . . . H45 H 0.7247 0.9951 0.3372 0.064 Uiso 1 1 calc R . . C46 C 0.7887(7) 0.9442(9) 0.2658(8) 0.056(4) Uani 1 1 d . . . H46 H 0.8131 1.0017 0.2565 0.067 Uiso 1 1 calc R . . C47 C 0.8060(6) 0.8677(9) 0.2321(7) 0.048(3) Uani 1 1 d . . . H47 H 0.8428 0.8715 0.1998 0.058 Uiso 1 1 calc R . . C48 C 0.8877(6) 0.6926(7) -0.0060(5) 0.027(2) Uani 1 1 d . . . H48A H 0.9353 0.6782 0.0166 0.032 Uiso 1 1 calc R . . H48B H 0.8767 0.6394 -0.0341 0.032 Uiso 1 1 calc R . . C49 C 0.8992(5) 0.7775(7) -0.0440(6) 0.026(2) Uani 1 1 d . . . C50 C 0.9012(6) 0.7700(7) -0.1094(5) 0.027(2) Uani 1 1 d . . . H50 H 0.8912 0.7117 -0.1289 0.032 Uiso 1 1 calc R . . C51 C 0.9180(6) 0.8486(7) -0.1458(5) 0.035(2) Uani 1 1 d . . . H51 H 0.9188 0.8433 -0.1899 0.042 Uiso 1 1 calc R . . C52 C 0.9335(7) 0.9341(8) -0.1181(5) 0.037(3) Uani 1 1 d . . . H52 H 0.9449 0.9870 -0.1431 0.044 Uiso 1 1 calc R . . C53 C 0.9323(6) 0.9417(7) -0.0545(5) 0.032(2) Uani 1 1 d . . . H53 H 0.9432 1.0001 -0.0354 0.038 Uiso 1 1 calc R . . C54 C 0.9152(6) 0.8637(8) -0.0171(5) 0.032(2) Uani 1 1 d . . . H54 H 0.9145 0.8700 0.0271 0.038 Uiso 1 1 calc R . . C55 C 0.9329(5) 0.5216(6) 0.0976(4) 0.0208(19) Uani 1 1 d . . . H55 H 0.9084 0.5526 0.0640 0.025 Uiso 1 1 calc R . . C56 C 0.8998(5) 0.5249(7) 0.1575(5) 0.026(2) Uani 1 1 d . . . H56 H 0.8521 0.5552 0.1613 0.031 Uiso 1 1 calc R . . C57 C 0.9345(6) 0.4836(7) 0.2173(5) 0.031(2) Uani 1 1 d . . . H57A H 0.9055 0.5059 0.2539 0.037 Uiso 1 1 calc R . . H57B H 0.9305 0.4147 0.2159 0.037 Uiso 1 1 calc R . . C58 C 1.0179(6) 0.5114(8) 0.2246(5) 0.033(2) Uani 1 1 d . . . H58A H 1.0501 0.4631 0.2048 0.040 Uiso 1 1 calc R . . H58B H 1.0307 0.5132 0.2696 0.040 Uiso 1 1 calc R . . C59 C 1.0362(5) 0.6067(7) 0.1954(5) 0.028(2) Uani 1 1 d . . . H59 H 1.0279 0.6614 0.2195 0.033 Uiso 1 1 calc R . . C60 C 1.0640(5) 0.6161(6) 0.1357(6) 0.029(2) Uani 1 1 d . . . H60 H 1.0763 0.6773 0.1219 0.034 Uiso 1 1 calc R . . C61 C 1.0768(6) 0.5354(7) 0.0898(5) 0.033(2) Uani 1 1 d . . . H61A H 1.1215 0.4987 0.1034 0.039 Uiso 1 1 calc R . . H61B H 1.0880 0.5613 0.0480 0.039 Uiso 1 1 calc R . . C62 C 1.0069(5) 0.4700(7) 0.0853(5) 0.027(2) Uani 1 1 d . . . H62A H 1.0051 0.4418 0.0432 0.033 Uiso 1 1 calc R . . H62B H 1.0124 0.4188 0.1161 0.033 Uiso 1 1 calc R . . N1 N 0.7247(4) 1.2069(5) 0.1407(5) 0.0294(19) Uani 1 1 d . . . N2 N 0.6775(5) 1.2174(6) 0.0429(4) 0.030(2) Uani 1 1 d . . . N3 N 0.7786(5) 0.7027(6) 0.1416(5) 0.035(2) Uani 1 1 d . . . N4 N 0.8247(5) 0.7018(6) 0.0401(4) 0.0278(19) Uani 1 1 d . . . Cl1 Cl 0.52008(12) 1.31865(16) 0.14551(14) 0.0318(6) Uani 1 1 d . . . Cl2 Cl 0.98270(13) 0.81415(17) 0.14668(15) 0.0350(7) Uani 1 1 d . . . Ir1 Ir 0.558107(15) 1.16098(2) 0.13454(2) 0.01899(8) Uani 1 1 d . . . Ir2 Ir 0.945068(16) 0.65704(2) 0.13490(2) 0.02013(9) 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 C1 0.020(4) 0.019(4) 0.041(6) -0.005(4) 0.008(4) -0.005(4) C2 0.016(4) 0.067(8) 0.079(9) -0.030(7) -0.011(5) -0.002(5) C3 0.075(8) 0.058(8) 0.049(7) -0.015(6) 0.017(6) -0.035(7) C4 0.029(5) 0.053(8) 0.117(14) 0.017(8) 0.011(7) -0.005(6) C5 0.033(6) 0.062(8) 0.039(6) -0.005(6) 0.006(4) -0.012(5) C6 0.053(7) 0.041(6) 0.056(7) 0.002(5) 0.022(6) -0.003(5) C7 0.076(11) 0.118(15) 0.101(15) 0.012(13) -0.007(10) 0.002(11) C8 0.044(7) 0.057(8) 0.119(13) 0.015(9) 0.020(8) 0.012(6) C9 0.040(6) 0.044(6) 0.068(9) -0.016(7) 0.011(6) 0.013(5) C10 0.029(5) 0.038(6) 0.054(8) 0.008(6) -0.020(5) 0.007(5) C11 0.022(5) 0.030(6) 0.037(7) 0.003(5) -0.004(5) -0.004(4) C12 0.029(6) 0.056(8) 0.046(8) -0.019(6) 0.000(6) 0.003(6) C13 0.043(7) 0.078(10) 0.043(8) -0.019(8) -0.004(6) -0.006(7) C14 0.036(6) 0.056(8) 0.067(10) -0.038(7) 0.015(6) -0.012(6) C15 0.031(6) 0.033(6) 0.053(7) -0.021(6) 0.001(5) -0.005(5) C16 0.036(6) 0.042(7) 0.047(7) -0.008(6) -0.016(6) -0.002(5) C17 0.035(5) 0.042(6) 0.028(6) -0.010(5) 0.000(4) -0.020(5) C18 0.031(5) 0.041(6) 0.026(6) 0.010(5) 0.007(5) -0.001(5) C19 0.040(6) 0.039(6) 0.031(6) -0.005(5) 0.006(5) -0.015(5) C20 0.036(6) 0.042(6) 0.053(8) -0.021(6) 0.011(6) -0.003(5) C21 0.043(6) 0.039(6) 0.046(9) 0.000(5) 0.001(6) -0.013(5) C22 0.056(7) 0.060(8) 0.033(8) -0.001(6) 0.007(6) -0.005(6) C23 0.028(5) 0.038(6) 0.049(8) -0.013(5) 0.007(5) -0.008(5) C24 0.022(5) 0.030(5) 0.034(6) -0.004(5) 0.008(5) -0.005(4) C25 0.017(4) 0.033(4) 0.025(5) 0.002(5) 0.000(5) -0.002(3) C26 0.025(5) 0.041(5) 0.025(6) -0.002(5) -0.001(5) -0.002(4) C27 0.033(5) 0.022(5) 0.029(6) -0.001(4) -0.005(5) 0.000(4) C28 0.033(5) 0.012(4) 0.033(6) -0.001(4) 0.007(5) -0.004(4) C29 0.017(4) 0.020(4) 0.026(6) 0.001(4) -0.002(4) -0.004(3) C30 0.032(5) 0.023(4) 0.033(6) 0.002(4) -0.014(5) -0.004(4) C31 0.037(5) 0.031(5) 0.028(6) -0.002(5) 0.005(5) 0.001(5) C32 0.016(4) 0.018(4) 0.023(5) 0.002(4) 0.002(4) 0.001(3) C33 0.027(5) 0.050(7) 0.076(9) 0.020(7) 0.014(5) 0.008(5) C34 0.030(5) 0.024(4) 0.061(7) 0.002(5) -0.010(5) -0.007(4) C35 0.044(6) 0.053(7) 0.076(10) -0.010(7) -0.001(7) -0.009(6) C36 0.036(6) 0.056(7) 0.055(7) 0.018(6) -0.026(5) -0.012(5) C37 0.032(6) 0.046(7) 0.087(9) 0.006(7) -0.031(6) -0.003(5) C38 0.027(5) 0.087(9) 0.040(6) -0.009(6) 0.003(4) 0.006(5) C39 0.052(7) 0.064(8) 0.076(9) 0.007(8) -0.018(7) 0.010(6) C40 0.033(5) 0.028(5) 0.093(11) 0.015(6) -0.008(6) 0.000(5) C41 0.041(6) 0.029(5) 0.033(6) 0.005(5) 0.008(5) 0.013(5) C42 0.028(6) 0.052(7) 0.032(7) -0.002(6) 0.007(5) 0.007(5) C43 0.034(6) 0.063(8) 0.031(7) 0.006(6) 0.010(5) -0.015(6) C44 0.050(7) 0.078(10) 0.048(8) -0.032(8) 0.021(6) -0.018(7) C45 0.035(6) 0.064(9) 0.063(10) -0.031(7) -0.006(6) 0.007(6) C46 0.031(6) 0.039(7) 0.097(12) 0.003(8) 0.002(7) 0.001(5) C47 0.036(6) 0.032(6) 0.077(10) 0.014(7) 0.012(7) 0.010(5) C48 0.037(5) 0.024(4) 0.019(5) -0.002(4) 0.005(4) 0.001(4) C49 0.017(4) 0.024(5) 0.037(6) -0.009(4) 0.006(4) 0.009(4) C50 0.039(6) 0.025(4) 0.017(5) 0.007(4) 0.004(4) 0.004(4) C51 0.058(6) 0.026(5) 0.019(6) 0.002(4) 0.006(5) 0.000(5) C52 0.040(6) 0.037(5) 0.034(7) 0.006(5) -0.001(5) 0.000(5) C53 0.034(5) 0.023(4) 0.039(6) 0.001(4) 0.001(5) 0.006(4) C54 0.034(5) 0.046(6) 0.016(5) 0.001(5) 0.002(4) -0.005(5) C55 0.025(4) 0.019(4) 0.019(5) 0.001(4) 0.004(4) -0.003(4) C56 0.025(5) 0.020(4) 0.034(6) -0.007(4) 0.000(4) -0.004(4) C57 0.035(5) 0.034(5) 0.024(5) 0.004(4) -0.010(5) 0.004(5) C58 0.030(5) 0.051(7) 0.018(5) 0.005(5) 0.000(4) 0.013(5) C59 0.020(4) 0.043(6) 0.021(5) -0.003(5) 0.003(4) 0.009(4) C60 0.019(4) 0.031(4) 0.036(6) 0.003(5) -0.004(5) 0.003(4) C61 0.021(4) 0.042(6) 0.035(7) -0.007(5) 0.007(5) 0.006(4) C62 0.026(5) 0.029(5) 0.027(6) -0.003(5) -0.006(4) 0.007(4) N1 0.021(3) 0.026(4) 0.041(6) -0.001(5) -0.004(4) -0.002(3) N2 0.021(4) 0.042(5) 0.026(5) -0.004(4) 0.006(3) -0.016(4) N3 0.030(4) 0.039(5) 0.036(6) 0.010(5) 0.011(5) 0.009(4) N4 0.028(4) 0.028(4) 0.027(5) 0.005(3) -0.006(4) -0.003(3) Cl1 0.0276(10) 0.0232(10) 0.0447(18) -0.0034(12) 0.0029(11) 0.0055(9) Cl2 0.0299(11) 0.0273(12) 0.0477(19) -0.0071(13) -0.0006(12) -0.0068(9) Ir1 0.01636(15) 0.01841(15) 0.0222(2) -0.00145(18) 0.00103(17) 0.00091(14) Ir2 0.01742(15) 0.02092(16) 0.0220(2) -0.00142(18) -0.00045(17) -0.00088(14) _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 C1 N1 1.301(13) . ? C1 N2 1.364(14) . ? C1 Ir1 2.075(9) . ? C2 C7 1.50(2) . ? C2 N1 1.520(14) . ? C2 C6 1.560(18) . ? C2 C3 1.589(18) . ? C3 C4 1.489(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.570(18) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N2 1.471(13) . ? C5 C6 1.498(17) . ? C5 H5 1.0000 . ? C6 C9 1.418(15) . ? C6 C8 1.576(16) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 N1 1.496(16) . ? C10 C11 1.508(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.392(16) . ? C11 C12 1.401(16) . ? C12 C13 1.411(17) . ? C12 H12 0.9500 . ? C13 C14 1.354(19) . ? C13 H13 0.9500 . ? C14 C15 1.420(18) . ? C14 H14 0.9500 . ? C15 C16 1.389(16) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.426(13) . ? C17 C18 1.522(16) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.385(15) . ? C18 C23 1.400(17) . ? C19 C20 1.370(17) . ? C19 H19 0.9500 . ? C20 C21 1.415(18) . ? C20 H20 0.9500 . ? C21 C22 1.379(17) . ? C21 H21 0.9500 . ? C22 C23 1.382(17) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.403(15) . ? C24 C31 1.486(14) . ? C24 Ir1 2.184(10) . ? C24 H24 0.9500 . ? C25 C26 1.468(13) . ? C25 Ir1 2.173(8) . ? C25 H25 0.9500 . ? C26 C27 1.549(13) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.537(13) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.399(14) . ? C28 Ir1 2.098(9) . ? C28 H28 0.9500 . ? C29 C30 1.498(14) . ? C29 Ir1 2.113(9) . ? C29 H29 0.9500 . ? C30 C31 1.546(14) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N4 1.355(13) . ? C32 N3 1.362(12) . ? C32 Ir2 2.071(8) . ? C33 C37 1.456(17) . ? C33 C38 1.524(16) . ? C33 C34 1.550(16) . ? C33 N3 1.647(15) . ? C34 C35 1.572(17) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.598(17) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.461(18) . ? C36 N4 1.480(12) . ? C36 H36 1.0000 . ? C37 C40 1.501(15) . ? C37 C39 1.557(15) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 N3 1.425(15) . ? C41 C42 1.541(16) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C47 1.386(17) . ? C42 C43 1.388(16) . ? C43 C44 1.358(18) . ? C43 H43 0.9500 . ? C44 C45 1.36(2) . ? C44 H44 0.9500 . ? C45 C46 1.39(2) . ? C45 H45 0.9500 . ? C46 C47 1.347(19) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.477(14) . ? C48 N4 1.491(13) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C54 1.392(14) . ? C49 C50 1.405(15) . ? C50 C51 1.401(13) . ? C50 H50 0.9500 . ? C51 C52 1.388(14) . ? C51 H51 0.9500 . ? C52 C53 1.366(16) . ? C52 H52 0.9500 . ? C53 C54 1.409(14) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.411(13) . ? C55 C62 1.521(13) . ? C55 Ir2 2.108(8) . ? C55 H55 0.9500 . ? C56 C57 1.537(14) . ? C56 Ir2 2.110(10) . ? C56 H56 0.9500 . ? C57 C58 1.531(14) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.536(15) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.377(15) . ? C59 Ir2 2.186(10) . ? C59 H59 0.9500 . ? C60 C61 1.534(14) . ? C60 Ir2 2.177(9) . ? C60 H60 0.9500 . ? C61 C62 1.551(13) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? Cl1 Ir1 2.367(2) . ? Cl2 Ir2 2.359(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 C1 N2 116.0(9) . . ? N1 C1 Ir1 124.6(8) . . ? N2 C1 Ir1 119.4(7) . . ? C7 C2 N1 111.3(13) . . ? C7 C2 C6 108.7(12) . . ? N1 C2 C6 106.5(8) . . ? C7 C2 C3 120.1(12) . . ? N1 C2 C3 107.6(9) . . ? C6 C2 C3 101.6(11) . . ? C4 C3 C2 106.0(10) . . ? C4 C3 H3A 110.5 . . ? C2 C3 H3A 110.5 . . ? C4 C3 H3B 110.5 . . ? C2 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? C3 C4 C5 104.4(11) . . ? C3 C4 H4A 110.9 . . ? C5 C4 H4A 110.9 . . ? C3 C4 H4B 110.9 . . ? C5 C4 H4B 110.9 . . ? H4A C4 H4B 108.9 . . ? N2 C5 C6 104.6(9) . . ? N2 C5 C4 110.9(10) . . ? C6 C5 C4 105.6(10) . . ? N2 C5 H5 111.8 . . ? C6 C5 H5 111.8 . . ? C4 C5 H5 111.8 . . ? C9 C6 C5 117.3(11) . . ? C9 C6 C2 115.8(11) . . ? C5 C6 C2 98.6(9) . . ? C9 C6 C8 106.7(10) . . ? C5 C6 C8 106.6(9) . . ? C2 C6 C8 111.5(11) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C11 116.6(10) . . ? N1 C10 H10A 108.1 . . ? C11 C10 H10A 108.1 . . ? N1 C10 H10B 108.1 . . ? C11 C10 H10B 108.1 . . ? H10A C10 H10B 107.3 . . ? C16 C11 C12 120.2(11) . . ? C16 C11 C10 120.0(9) . . ? C12 C11 C10 119.7(10) . . ? C11 C12 C13 117.9(12) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C14 C13 C12 122.7(12) . . ? C14 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C13 C14 C15 118.9(12) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.7(12) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 120.5(11) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N2 C17 C18 114.4(9) . . ? N2 C17 H17A 108.7 . . ? C18 C17 H17A 108.7 . . ? N2 C17 H17B 108.7 . . ? C18 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? C19 C18 C23 117.5(11) . . ? C19 C18 C17 121.9(11) . . ? C23 C18 C17 120.6(11) . . ? C20 C19 C18 121.9(12) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C19 C20 C21 119.4(11) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 120.1(12) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 118.8(12) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C22 C23 C18 122.4(11) . . ? C22 C23 H23 118.8 . . ? C18 C23 H23 118.8 . . ? C25 C24 C31 122.8(9) . . ? C25 C24 Ir1 70.8(5) . . ? C31 C24 Ir1 112.8(7) . . ? C25 C24 H24 118.6 . . ? C31 C24 H24 118.6 . . ? Ir1 C24 H24 86.5 . . ? C24 C25 C26 124.3(9) . . ? C24 C25 Ir1 71.6(5) . . ? C26 C25 Ir1 110.3(7) . . ? C24 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? Ir1 C25 H25 88.1 . . ? C25 C26 C27 114.5(8) . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C28 C27 C26 110.3(8) . . ? C28 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? C28 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C29 C28 C27 123.3(9) . . ? C29 C28 Ir1 71.2(6) . . ? C27 C28 Ir1 115.1(6) . . ? C29 C28 H28 118.4 . . ? C27 C28 H28 118.4 . . ? Ir1 C28 H28 83.9 . . ? C28 C29 C30 123.6(8) . . ? C28 C29 Ir1 70.0(5) . . ? C30 C29 Ir1 112.2(6) . . ? C28 C29 H29 118.2 . . ? C30 C29 H29 118.2 . . ? Ir1 C29 H29 87.8 . . ? C29 C30 C31 112.8(8) . . ? C29 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? C29 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C24 C31 C30 113.0(9) . . ? C24 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C24 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? N4 C32 N3 117.4(8) . . ? N4 C32 Ir2 121.2(7) . . ? N3 C32 Ir2 121.0(7) . . ? C37 C33 C38 116.6(10) . . ? C37 C33 C34 108.9(11) . . ? C38 C33 C34 110.2(10) . . ? C37 C33 N3 106.6(8) . . ? C38 C33 N3 106.9(10) . . ? C34 C33 N3 107.0(8) . . ? C33 C34 C35 103.1(9) . . ? C33 C34 H34A 111.2 . . ? C35 C34 H34A 111.2 . . ? C33 C34 H34B 111.2 . . ? C35 C34 H34B 111.2 . . ? H34A C34 H34B 109.1 . . ? C34 C35 C36 100.8(10) . . ? C34 C35 H35A 111.6 . . ? C36 C35 H35A 111.6 . . ? C34 C35 H35B 111.6 . . ? C36 C35 H35B 111.6 . . ? H35A C35 H35B 109.4 . . ? C37 C36 N4 108.9(10) . . ? C37 C36 C35 106.4(10) . . ? N4 C36 C35 106.5(9) . . ? C37 C36 H36 111.6 . . ? N4 C36 H36 111.6 . . ? C35 C36 H36 111.6 . . ? C33 C37 C36 99.5(9) . . ? C33 C37 C40 118.5(12) . . ? C36 C37 C40 111.9(11) . . ? C33 C37 C39 111.0(10) . . ? C36 C37 C39 107.9(10) . . ? C40 C37 C39 107.6(9) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 C42 114.4(9) . . ? N3 C41 H41A 108.7 . . ? C42 C41 H41A 108.7 . . ? N3 C41 H41B 108.7 . . ? C42 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? C47 C42 C43 117.3(12) . . ? C47 C42 C41 122.1(10) . . ? C43 C42 C41 120.6(12) . . ? C44 C43 C42 122.8(12) . . ? C44 C43 H43 118.6 . . ? C42 C43 H43 118.6 . . ? C43 C44 C45 118.7(12) . . ? C43 C44 H44 120.7 . . ? C45 C44 H44 120.7 . . ? C44 C45 C46 119.8(13) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? C47 C46 C45 121.2(13) . . ? C47 C46 H46 119.4 . . ? C45 C46 H46 119.4 . . ? C46 C47 C42 120.2(12) . . ? C46 C47 H47 119.9 . . ? C42 C47 H47 119.9 . . ? C49 C48 N4 113.2(8) . . ? C49 C48 H48A 108.9 . . ? N4 C48 H48A 108.9 . . ? C49 C48 H48B 108.9 . . ? N4 C48 H48B 108.9 . . ? H48A C48 H48B 107.8 . . ? C54 C49 C50 118.4(10) . . ? C54 C49 C48 122.0(10) . . ? C50 C49 C48 119.4(9) . . ? C51 C50 C49 119.9(10) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 120.8(10) . . ? C52 C51 H51 119.6 . . ? C50 C51 H51 119.6 . . ? C53 C52 C51 119.6(10) . . ? C53 C52 H52 120.2 . . ? C51 C52 H52 120.2 . . ? C52 C53 C54 120.5(10) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C49 C54 C53 120.7(10) . . ? C49 C54 H54 119.6 . . ? C53 C54 H54 119.6 . . ? C56 C55 C62 121.8(9) . . ? C56 C55 Ir2 70.5(6) . . ? C62 C55 Ir2 115.2(6) . . ? C56 C55 H55 119.1 . . ? C62 C55 H55 119.1 . . ? Ir2 C55 H55 84.6 . . ? C55 C56 C57 125.5(9) . . ? C55 C56 Ir2 70.4(6) . . ? C57 C56 Ir2 112.7(6) . . ? C55 C56 H56 117.2 . . ? C57 C56 H56 117.2 . . ? Ir2 C56 H56 86.8 . . ? C58 C57 C56 111.5(9) . . ? C58 C57 H57A 109.3 . . ? C56 C57 H57A 109.3 . . ? C58 C57 H57B 109.3 . . ? C56 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 113.0(8) . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58B 109.0 . . ? C59 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C60 C59 C58 122.7(9) . . ? C60 C59 Ir2 71.3(6) . . ? C58 C59 Ir2 112.4(7) . . ? C60 C59 H59 118.6 . . ? C58 C59 H59 118.6 . . ? Ir2 C59 H59 86.5 . . ? C59 C60 C61 125.1(9) . . ? C59 C60 Ir2 72.0(6) . . ? C61 C60 Ir2 109.8(6) . . ? C59 C60 H60 117.5 . . ? C61 C60 H60 117.5 . . ? Ir2 C60 H60 88.2 . . ? C60 C61 C62 112.2(8) . . ? C60 C61 H61A 109.2 . . ? C62 C61 H61A 109.2 . . ? C60 C61 H61B 109.2 . . ? C62 C61 H61B 109.2 . . ? H61A C61 H61B 107.9 . . ? C55 C62 C61 112.1(8) . . ? C55 C62 H62A 109.2 . . ? C61 C62 H62A 109.2 . . ? C55 C62 H62B 109.2 . . ? C61 C62 H62B 109.2 . . ? H62A C62 H62B 107.9 . . ? C1 N1 C10 117.4(9) . . ? C1 N1 C2 122.9(10) . . ? C10 N1 C2 119.7(9) . . ? C1 N2 C17 122.1(8) . . ? C1 N2 C5 123.1(9) . . ? C17 N2 C5 114.5(9) . . ? C32 N3 C41 121.0(9) . . ? C32 N3 C33 114.2(9) . . ? C41 N3 C33 122.5(9) . . ? C32 N4 C36 123.4(9) . . ? C32 N4 C48 120.4(8) . . ? C36 N4 C48 115.0(9) . . ? C1 Ir1 C28 92.3(4) . . ? C1 Ir1 C29 88.1(4) . . ? C28 Ir1 C29 38.8(4) . . ? C1 Ir1 C25 161.2(4) . . ? C28 Ir1 C25 81.2(4) . . ? C29 Ir1 C25 97.4(3) . . ? C1 Ir1 C24 160.7(4) . . ? C28 Ir1 C24 89.1(4) . . ? C29 Ir1 C24 81.0(4) . . ? C25 Ir1 C24 37.6(4) . . ? C1 Ir1 Cl1 91.7(3) . . ? C28 Ir1 Cl1 161.5(3) . . ? C29 Ir1 Cl1 159.5(3) . . ? C25 Ir1 Cl1 89.3(2) . . ? C24 Ir1 Cl1 93.0(3) . . ? C32 Ir2 C55 91.0(4) . . ? C32 Ir2 C56 88.2(4) . . ? C55 Ir2 C56 39.1(4) . . ? C32 Ir2 C60 160.6(4) . . ? C55 Ir2 C60 81.5(4) . . ? C56 Ir2 C60 96.9(4) . . ? C32 Ir2 C59 162.0(4) . . ? C55 Ir2 C59 89.8(4) . . ? C56 Ir2 C59 81.1(4) . . ? C60 Ir2 C59 36.8(4) . . ? C32 Ir2 Cl2 92.5(2) . . ? C55 Ir2 Cl2 161.1(3) . . ? C56 Ir2 Cl2 159.5(3) . . ? C60 Ir2 Cl2 89.2(2) . . ? C59 Ir2 Cl2 92.6(3) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.283 _refine_diff_density_min -1.815 _refine_diff_density_rms 0.192 #===END data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd6b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H54 F6 N4 Ni O2 P' _chemical_formula_sum 'C37 H54 F6 N4 Ni O2 P' _chemical_formula_weight 790.52 _chemical_absolute_configuration ad 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' 'F' 'F' 0.0171 0.0103 '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' '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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 18.6743(10) _cell_length_b 11.3718(7) _cell_length_c 19.8153(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.746(3) _cell_angle_gamma 90.00 _cell_volume 3821.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7424 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 25.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.617 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8366 _exptl_absorpt_correction_T_max 0.9758 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12313 _diffrn_reflns_av_R_equivalents 0.1010 _diffrn_reflns_av_sigmaI/netI 0.1308 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.68 _reflns_number_total 12313 _reflns_number_gt 7424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1060P)^2^+16.9637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 0.03(3) _refine_ls_number_reflns 12313 _refine_ls_number_parameters 819 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1831 _refine_ls_R_factor_gt 0.1083 _refine_ls_wR_factor_ref 0.2781 _refine_ls_wR_factor_gt 0.2315 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.6373(7) 0.6112(12) 0.3916(6) 0.047(3) Uani 1 1 d . . . C2 C 0.6776(7) 0.4113(10) 0.3639(7) 0.050(3) Uani 1 1 d . . . C3 C 0.7601(7) 0.4733(11) 0.3875(7) 0.058(3) Uani 1 1 d . . . C4 C 0.7694(7) 0.5214(11) 0.4628(7) 0.057(3) Uani 1 1 d . . . H4 H 0.8244 0.5497 0.4928 0.068 Uiso 1 1 calc R . . C5 C 0.6881(8) 0.3468(12) 0.4363(7) 0.062(3) Uani 1 1 d . . . H5A H 0.6372 0.3423 0.4406 0.075 Uiso 1 1 calc R . . H5B H 0.7080 0.2659 0.4368 0.075 Uiso 1 1 calc R . . C6 C 0.7484(8) 0.4199(13) 0.5007(7) 0.070(4) Uani 1 1 d . . . H6A H 0.7249 0.4489 0.5340 0.084 Uiso 1 1 calc R . . H6B H 0.7957 0.3725 0.5302 0.084 Uiso 1 1 calc R . . C7 C 0.6535(9) 0.3343(13) 0.2965(7) 0.081(4) Uani 1 1 d . . . H7A H 0.6476 0.3823 0.2534 0.122 Uiso 1 1 calc R . . H7B H 0.6032 0.2961 0.2872 0.122 Uiso 1 1 calc R . . H7C H 0.6940 0.2743 0.3049 0.122 Uiso 1 1 calc R . . C8 C 0.8264(9) 0.3838(14) 0.4001(10) 0.089(5) Uani 1 1 d . . . H8A H 0.8250 0.3220 0.4340 0.134 Uiso 1 1 calc R . . H8B H 0.8775 0.4239 0.4219 0.134 Uiso 1 1 calc R . . H8C H 0.8190 0.3485 0.3525 0.134 Uiso 1 1 calc R . . C9 C 0.7642(9) 0.5646(12) 0.3350(8) 0.078(4) Uani 1 1 d . . . H9A H 0.7566 0.5274 0.2879 0.117 Uiso 1 1 calc R . . H9B H 0.8159 0.6030 0.3567 0.117 Uiso 1 1 calc R . . H9C H 0.7228 0.6233 0.3261 0.117 Uiso 1 1 calc R . . C10 C 0.5408(8) 0.5082(12) 0.2933(7) 0.062(4) Uani 1 1 d . . . H10A H 0.5288 0.4262 0.2752 0.075 Uiso 1 1 calc R . . H10B H 0.5022 0.5316 0.3131 0.075 Uiso 1 1 calc R . . C11 C 0.5313(7) 0.5853(11) 0.2305(6) 0.048(3) Uani 1 1 d . . . C12 C 0.5098(9) 0.5458(13) 0.1595(7) 0.073(4) Uani 1 1 d . . . H12 H 0.5006 0.4643 0.1488 0.088 Uiso 1 1 calc R . . C13 C 0.5012(9) 0.6237(13) 0.1029(7) 0.070(4) Uani 1 1 d . . . H13 H 0.4845 0.5965 0.0533 0.084 Uiso 1 1 calc R . . C14 C 0.5176(8) 0.7436(14) 0.1197(7) 0.064(3) Uani 1 1 d . . . H14 H 0.5146 0.7990 0.0827 0.077 Uiso 1 1 calc R . . C15 C 0.5383(7) 0.7775(12) 0.1929(6) 0.053(3) Uani 1 1 d . . . H15 H 0.5477 0.8586 0.2046 0.064 Uiso 1 1 calc R . . C16 C 0.7344(7) 0.7253(12) 0.4887(6) 0.054(3) Uani 1 1 d . . . H16A H 0.7854 0.7131 0.5321 0.065 Uiso 1 1 calc R . . H16B H 0.6950 0.7481 0.5077 0.065 Uiso 1 1 calc R . . C17 C 0.7429(7) 0.8232(11) 0.4422(7) 0.051(3) Uani 1 1 d . . . C18 C 0.8133(8) 0.8843(15) 0.4580(8) 0.072(4) Uani 1 1 d . . . H18 H 0.8601 0.8587 0.4982 0.086 Uiso 1 1 calc R . . C19 C 0.8166(9) 0.9808(13) 0.4169(9) 0.072(4) Uani 1 1 d . . . H19 H 0.8640 1.0238 0.4291 0.086 Uiso 1 1 calc R . . C20 C 0.7471(8) 1.0116(13) 0.3569(8) 0.062(4) Uani 1 1 d . . . H20 H 0.7463 1.0758 0.3259 0.075 Uiso 1 1 calc R . . C21 C 0.6794(7) 0.9486(12) 0.3425(7) 0.054(3) Uani 1 1 d . . . H21 H 0.6331 0.9711 0.3006 0.065 Uiso 1 1 calc R . . C22 C 0.5260(6) 0.7494(13) 0.4340(6) 0.048(3) Uani 1 1 d . . . H22 H 0.5380 0.6682 0.4431 0.058 Uiso 1 1 calc R . . C23 C 0.4739(7) 0.7799(10) 0.3618(7) 0.048(3) Uani 1 1 d . . . H23 H 0.4293 0.7318 0.3353 0.057 Uiso 1 1 calc R . . C24 C 0.4873(6) 0.8821(11) 0.3278(6) 0.049(3) Uani 1 1 d . . . H24A H 0.4368 0.8999 0.2850 0.058 Uiso 1 1 calc R . . H24B H 0.5249 0.8592 0.3068 0.058 Uiso 1 1 calc R . . C25 C 0.5172(8) 0.9988(12) 0.3683(7) 0.055(3) Uani 1 1 d . . . H25A H 0.5200 1.0578 0.3327 0.066 Uiso 1 1 calc R . . H25B H 0.5712 0.9877 0.4076 0.066 Uiso 1 1 calc R . . C26 C 0.4628(8) 1.0458(11) 0.4040(7) 0.063(4) Uani 1 1 d . . . H26 H 0.4458 1.1254 0.3972 0.075 Uiso 1 1 calc R . . C27 C 0.4373(8) 0.9641(14) 0.4494(7) 0.064(4) Uani 1 1 d . . . H27 H 0.3832 0.9511 0.4377 0.077 Uiso 1 1 calc R . . C28 C 0.5049(9) 0.9002(15) 0.5177(7) 0.074(4) Uani 1 1 d . . . H28A H 0.5337 0.9602 0.5556 0.089 Uiso 1 1 calc R . . H28B H 0.4800 0.8453 0.5402 0.089 Uiso 1 1 calc R . . C29 C 0.5653(8) 0.8309(13) 0.4990(6) 0.058(3) Uani 1 1 d . . . H29A H 0.5992 0.8870 0.4875 0.069 Uiso 1 1 calc R . . H29B H 0.5995 0.7845 0.5430 0.069 Uiso 1 1 calc R . . C30 C 0.8769(9) 0.7396(14) 0.1349(7) 0.066(4) Uani 1 1 d . . . C31 C 0.7553(9) 0.8569(16) 0.0819(8) 0.076(4) Uani 1 1 d . . . C32 C 0.7867(9) 0.9019(13) 0.1625(8) 0.075(4) Uani 1 1 d . . . C33 C 0.8652(9) 0.9406(14) 0.1782(9) 0.077(4) Uani 1 1 d . . . H33 H 0.8900 0.9842 0.2263 0.092 Uiso 1 1 calc R . . C34 C 0.7878(10) 0.9538(12) 0.0447(9) 0.091(6) Uani 1 1 d . . . H34A H 0.7461 1.0112 0.0166 0.110 Uiso 1 1 calc R . . H34B H 0.8078 0.9175 0.0105 0.110 Uiso 1 1 calc R . . C35 C 0.8571(10) 1.0156(17) 0.1122(10) 0.099(5) Uani 1 1 d . . . H35A H 0.9065 1.0155 0.1051 0.119 Uiso 1 1 calc R . . H35B H 0.8432 1.0976 0.1184 0.119 Uiso 1 1 calc R . . C36 C 0.6724(10) 0.8250(15) 0.0427(11) 0.101(5) Uani 1 1 d . . . H36A H 0.6622 0.7968 -0.0072 0.151 Uiso 1 1 calc R . . H36B H 0.6395 0.8941 0.0389 0.151 Uiso 1 1 calc R . . H36C H 0.6597 0.7628 0.0701 0.151 Uiso 1 1 calc R . . C37 C 0.7383(12) 1.0033(16) 0.1701(9) 0.112(6) Uani 1 1 d . . . H37A H 0.6843 0.9767 0.1577 0.168 Uiso 1 1 calc R . . H37B H 0.7373 1.0668 0.1363 0.168 Uiso 1 1 calc R . . H37C H 0.7618 1.0323 0.2214 0.168 Uiso 1 1 calc R . . C38 C 0.7765(10) 0.8053(14) 0.2145(9) 0.087(5) Uani 1 1 d . . . H38A H 0.7206 0.7850 0.1968 0.130 Uiso 1 1 calc R . . H38B H 0.7961 0.8357 0.2653 0.130 Uiso 1 1 calc R . . H38C H 0.8066 0.7351 0.2137 0.130 Uiso 1 1 calc R . . C39 C 0.7702(7) 0.6398(15) 0.0405(7) 0.069(4) Uani 1 1 d . . . H39A H 0.8039 0.6186 0.0148 0.083 Uiso 1 1 calc R . . H39B H 0.7173 0.6595 0.0017 0.083 Uiso 1 1 calc R . . C40 C 0.7625(8) 0.5358(14) 0.0809(7) 0.065(4) Uani 1 1 d . . . C41 C 0.6907(9) 0.4844(15) 0.0677(9) 0.080(4) Uani 1 1 d . . . H41 H 0.6432 0.5140 0.0301 0.096 Uiso 1 1 calc R . . C42 C 0.6896(7) 0.3901(15) 0.1101(8) 0.068(4) Uani 1 1 d . . . H42 H 0.6404 0.3578 0.1039 0.082 Uiso 1 1 calc R . . C43 C 0.7583(10) 0.3407(15) 0.1615(8) 0.074(4) Uani 1 1 d . . . H43 H 0.7573 0.2713 0.1878 0.089 Uiso 1 1 calc R . . C44 C 0.8289(8) 0.3961(12) 0.1733(7) 0.055(3) Uani 1 1 d . . . H44 H 0.8768 0.3639 0.2089 0.066 Uiso 1 1 calc R . . C45 C 0.9896(10) 0.8286(14) 0.2335(8) 0.078(4) Uani 1 1 d . . . H45A H 1.0059 0.9070 0.2566 0.094 Uiso 1 1 calc R . . H45B H 1.0262 0.8046 0.2115 0.094 Uiso 1 1 calc R . . C46 C 0.9919(8) 0.7370(14) 0.2934(7) 0.068(4) Uani 1 1 d . . . C47 C 1.0135(10) 0.7757(16) 0.3650(8) 0.086(5) Uani 1 1 d . . . H47 H 1.0241 0.8563 0.3776 0.104 Uiso 1 1 calc R . . C48 C 1.0191(9) 0.6909(17) 0.4189(8) 0.083(5) Uani 1 1 d . . . H48 H 1.0361 0.7127 0.4696 0.099 Uiso 1 1 calc R . . C49 C 1.0002(8) 0.5789(15) 0.3977(6) 0.065(4) Uani 1 1 d . . . H49 H 1.0032 0.5206 0.4331 0.078 Uiso 1 1 calc R . . C50 C 0.9760(7) 0.5489(13) 0.3233(6) 0.057(3) Uani 1 1 d . . . H50 H 0.9633 0.4692 0.3089 0.069 Uiso 1 1 calc R . . C51 C 0.9749(7) 0.6027(13) 0.0771(6) 0.057(3) Uani 1 1 d . . . H51A H 1.0026 0.6654 0.0628 0.068 Uiso 1 1 calc R . . H51B H 0.9325 0.6421 0.0862 0.068 Uiso 1 1 calc R . . C52 C 1.0298(8) 0.5603(18) 0.1477(8) 0.079(5) Uani 1 1 d . . . H52 H 1.0762 0.6047 0.1749 0.095 Uiso 1 1 calc R . . C53 C 1.0174(9) 0.4564(15) 0.1775(8) 0.068(4) Uani 1 1 d . . . H53 H 1.0307 0.4533 0.2293 0.082 Uiso 1 1 calc R . . C54 C 0.9837(7) 0.3478(11) 0.1313(7) 0.052(3) Uani 1 1 d . . . H54A H 0.9294 0.3657 0.0948 0.062 Uiso 1 1 calc R . . H54B H 0.9801 0.2851 0.1644 0.062 Uiso 1 1 calc R . . C55 C 1.0299(9) 0.2995(14) 0.0890(8) 0.073(4) Uani 1 1 d . . . H55A H 1.0789 0.2622 0.1252 0.088 Uiso 1 1 calc R . . H55B H 0.9980 0.2375 0.0545 0.088 Uiso 1 1 calc R . . C56 C 1.0519(10) 0.3912(15) 0.0448(10) 0.080(5) Uani 1 1 d . . . H56 H 1.1056 0.4068 0.0556 0.097 Uiso 1 1 calc R . . C57 C 0.9875(10) 0.4553(13) -0.0154(8) 0.073(4) Uani 1 1 d . . . H57 H 0.9799 0.4511 -0.0658 0.088 Uiso 1 1 calc R . . C58 C 0.9345(8) 0.5286(13) 0.0094(7) 0.058(3) Uani 1 1 d . . . H58A H 0.9021 0.5809 -0.0321 0.069 Uiso 1 1 calc R . . H58B H 0.8979 0.4747 0.0187 0.069 Uiso 1 1 calc R . . N1 N 0.6212(5) 0.5128(9) 0.3540(5) 0.048(2) Uani 1 1 d . . . N2 N 0.7106(6) 0.6181(10) 0.4490(5) 0.059(3) Uani 1 1 d . . . N3 N 0.5459(5) 0.7035(9) 0.2477(5) 0.049(3) Uani 1 1 d . . . N4 N 0.6741(5) 0.8581(9) 0.3831(5) 0.045(2) Uani 1 1 d . . . N5 N 0.8029(7) 0.7450(10) 0.0848(6) 0.059(3) Uani 1 1 d . . . N6 N 0.9103(8) 0.8335(10) 0.1769(7) 0.072(3) Uani 1 1 d . . . N7 N 0.8320(6) 0.4957(9) 0.1356(5) 0.047(2) Uani 1 1 d . . . N8 N 0.9698(6) 0.6294(9) 0.2704(5) 0.053(3) Uani 1 1 d . . . F1 F 0.5247(6) 0.0243(8) 0.0878(5) 0.090(3) Uani 1 1 d . . . F2 F 0.5037(10) 0.2084(12) 0.0547(6) 0.161(6) Uani 1 1 d . . . F3 F 0.6007(5) 0.1649(12) 0.1648(6) 0.136(5) Uani 1 1 d . . . F4 F 0.4195(5) 0.1165(13) 0.0890(6) 0.139(5) Uani 1 1 d . . . F5 F 0.5195(8) 0.0707(9) 0.1966(5) 0.124(4) Uani 1 1 d . . . F6 F 0.4919(5) 0.2531(8) 0.1611(5) 0.101(3) Uani 1 1 d . . . F7 F -0.0332(13) 0.632(2) 0.5523(7) 0.241(11) Uani 1 1 d . . . F8 F 0.0735(10) 0.611(2) 0.6445(10) 0.252(11) Uani 1 1 d . . . F9 F 0.0214(11) 0.7842(11) 0.5963(11) 0.190(7) Uani 1 1 d . . . F10 F 0.0315(9) 0.7173(19) 0.7105(7) 0.240(11) Uani 1 1 d . . . F11 F -0.0748(7) 0.7449(17) 0.6229(9) 0.206(9) Uani 1 1 d . . . F12 F -0.0280(11) 0.5692(11) 0.6624(11) 0.196(8) Uani 1 1 d . . . P1 P 0.5089(2) 0.1387(3) 0.12568(19) 0.0626(10) Uani 1 1 d . . . P2 P 0.0003(2) 0.6753(4) 0.63337(18) 0.0586(9) Uani 1 1 d . . . Ni1 Ni 0.57312(8) 0.74923(13) 0.35554(7) 0.0430(4) Uani 1 1 d . . . Ni2 Ni 0.93511(9) 0.59229(13) 0.15922(8) 0.0483(4) Uani 1 1 d . . . C59 C 0.1711(17) 0.936(2) 0.2600(17) 0.242(17) Uiso 1 1 d D . . H59A H 0.1420 0.8994 0.2864 0.290 Uiso 1 1 calc R . . H59B H 0.1780 0.8778 0.2259 0.290 Uiso 1 1 calc R . . C60 C 0.1321(13) 1.049(2) 0.2201(11) 0.150(9) Uiso 1 1 d D . . H60A H 0.1448 1.0625 0.1770 0.180 Uiso 1 1 calc R . . H60B H 0.0742 1.0431 0.2019 0.180 Uiso 1 1 calc R . . C61 C 0.1635(15) 1.1493(19) 0.2754(14) 0.177(11) Uiso 1 1 d D . . H61A H 0.1756 1.2189 0.2519 0.213 Uiso 1 1 calc R . . H61B H 0.1248 1.1721 0.2951 0.213 Uiso 1 1 calc R . . C62 C 0.2374(14) 1.100(2) 0.3360(13) 0.181(11) Uiso 1 1 d D . . H62A H 0.2836 1.1499 0.3431 0.217 Uiso 1 1 calc R . . H62B H 0.2321 1.0959 0.3836 0.217 Uiso 1 1 calc R . . O1 O 0.2452(13) 0.986(2) 0.3105(12) 0.219(9) Uiso 1 1 d D . . C63 C 0.3339(18) 0.199(2) 0.2152(16) 0.200(13) Uiso 1 1 d D . . H63A H 0.3091 0.1414 0.2360 0.240 Uiso 1 1 calc R . . H63B H 0.3712 0.1583 0.1995 0.240 Uiso 1 1 calc R . . C64 C 0.2728(14) 0.267(2) 0.1517(13) 0.164(9) Uiso 1 1 d D . . H64A H 0.2799 0.2535 0.1056 0.197 Uiso 1 1 calc R . . H64B H 0.2192 0.2408 0.1434 0.197 Uiso 1 1 calc R . . C65 C 0.2820(16) 0.392(2) 0.1704(15) 0.195(12) Uiso 1 1 d D . . H65A H 0.2803 0.4386 0.1275 0.235 Uiso 1 1 calc R . . H65B H 0.2386 0.4190 0.1830 0.235 Uiso 1 1 calc R . . C66 C 0.3566(15) 0.408(2) 0.2329(14) 0.164(10) Uiso 1 1 d D . . H66A H 0.3529 0.4691 0.2672 0.197 Uiso 1 1 calc R . . H66B H 0.3980 0.4315 0.2167 0.197 Uiso 1 1 calc R . . O2 O 0.3728(16) 0.293(3) 0.2681(13) 0.280(13) Uiso 1 1 d D . . C67 C 0.6900(16) 0.147(3) 0.5828(14) 0.178(11) Uiso 1 1 d D . . H67A H 0.6371 0.1408 0.5412 0.213 Uiso 1 1 calc R . . H67B H 0.7036 0.2311 0.5949 0.213 Uiso 1 1 calc R . . C68 C 0.6959(13) 0.079(2) 0.6489(12) 0.154(8) Uiso 1 1 d D . . H68A H 0.6790 0.1269 0.6813 0.185 Uiso 1 1 calc R . . H68B H 0.6626 0.0073 0.6336 0.185 Uiso 1 1 calc R . . C69 C 0.7800(16) 0.047(3) 0.6879(14) 0.218(14) Uiso 1 1 d D . . H69A H 0.8117 0.1150 0.7156 0.261 Uiso 1 1 calc R . . H69B H 0.7874 -0.0187 0.7230 0.261 Uiso 1 1 calc R . . C70 C 0.8017(15) 0.012(3) 0.6292(15) 0.169(10) Uiso 1 1 d D . . H70A H 0.7916 -0.0725 0.6177 0.202 Uiso 1 1 calc R . . H70B H 0.8579 0.0294 0.6421 0.202 Uiso 1 1 calc R . . O3 O 0.7499(19) 0.085(3) 0.5676(15) 0.307(15) Uiso 1 1 d D . . C71 C 0.7657(14) 0.181(2) 0.8559(13) 0.161(9) Uiso 1 1 d D . . H71A H 0.7708 0.0941 0.8537 0.193 Uiso 1 1 calc R . . H71B H 0.7819 0.2183 0.8195 0.193 Uiso 1 1 calc R . . C72 C 0.6836(13) 0.216(3) 0.8438(15) 0.196(12) Uiso 1 1 d D . . H72A H 0.6520 0.2359 0.7909 0.235 Uiso 1 1 calc R . . H72B H 0.6572 0.1508 0.8575 0.235 Uiso 1 1 calc R . . C73 C 0.6911(19) 0.321(3) 0.8919(19) 0.262(19) Uiso 1 1 d D . . H73A H 0.6998 0.3942 0.8692 0.314 Uiso 1 1 calc R . . H73B H 0.6442 0.3308 0.9026 0.314 Uiso 1 1 calc R . . C74 C 0.7612(19) 0.288(3) 0.9587(15) 0.225(15) Uiso 1 1 d D . . H74A H 0.7888 0.3585 0.9869 0.270 Uiso 1 1 calc R . . H74B H 0.7467 0.2368 0.9915 0.270 Uiso 1 1 calc R . . O4 O 0.8099(12) 0.225(2) 0.9299(12) 0.229(10) Uiso 1 1 d 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 C1 0.046(7) 0.053(8) 0.042(6) 0.001(6) 0.019(5) -0.001(6) C2 0.064(8) 0.026(6) 0.066(7) 0.001(6) 0.034(6) 0.006(6) C3 0.053(8) 0.042(7) 0.083(9) 0.012(7) 0.033(7) 0.019(6) C4 0.053(7) 0.046(8) 0.068(8) 0.011(6) 0.023(6) 0.003(6) C5 0.061(8) 0.040(7) 0.077(9) 0.014(7) 0.020(7) 0.020(6) C6 0.067(9) 0.076(10) 0.063(8) 0.003(8) 0.023(7) 0.017(7) C7 0.100(11) 0.058(9) 0.068(9) -0.018(8) 0.018(8) 0.018(8) C8 0.082(10) 0.074(11) 0.124(13) -0.003(10) 0.054(9) 0.020(8) C9 0.100(11) 0.060(10) 0.105(10) 0.001(8) 0.073(9) -0.002(8) C10 0.087(10) 0.032(7) 0.066(8) -0.007(6) 0.031(7) -0.015(7) C11 0.060(7) 0.038(7) 0.050(6) -0.005(6) 0.026(5) -0.002(6) C12 0.091(10) 0.052(9) 0.064(8) 0.007(7) 0.020(7) -0.009(7) C13 0.084(10) 0.069(11) 0.055(7) -0.023(8) 0.027(7) -0.007(8) C14 0.080(9) 0.051(8) 0.066(8) 0.014(8) 0.035(6) 0.000(8) C15 0.053(7) 0.049(8) 0.050(7) -0.011(6) 0.014(5) 0.002(6) C16 0.047(6) 0.066(9) 0.043(6) 0.001(6) 0.012(5) -0.001(6) C17 0.042(7) 0.050(8) 0.065(7) 0.003(6) 0.026(6) 0.001(6) C18 0.056(8) 0.080(11) 0.068(8) 0.002(8) 0.014(6) -0.008(8) C19 0.074(10) 0.059(10) 0.092(10) -0.013(8) 0.045(9) -0.014(8) C20 0.067(9) 0.049(8) 0.081(9) 0.005(7) 0.043(8) -0.016(7) C21 0.052(8) 0.052(9) 0.057(7) 0.000(6) 0.021(6) -0.003(6) C22 0.060(7) 0.040(7) 0.055(6) 0.000(7) 0.034(5) -0.003(7) C23 0.036(6) 0.035(8) 0.083(8) -0.010(6) 0.037(6) -0.006(5) C24 0.036(6) 0.052(9) 0.052(6) 0.009(6) 0.011(5) 0.017(6) C25 0.076(9) 0.046(8) 0.054(7) 0.002(6) 0.038(6) 0.015(7) C26 0.094(10) 0.032(7) 0.084(9) 0.003(6) 0.058(8) 0.017(7) C27 0.049(7) 0.084(11) 0.076(8) 0.003(8) 0.043(6) 0.016(7) C28 0.099(10) 0.080(11) 0.074(9) 0.015(8) 0.066(8) 0.022(9) C29 0.066(8) 0.057(8) 0.052(7) 0.007(6) 0.027(6) -0.005(7) C30 0.101(11) 0.060(10) 0.056(7) 0.001(8) 0.051(7) 0.025(9) C31 0.069(10) 0.098(12) 0.070(9) -0.003(9) 0.038(7) 0.029(9) C32 0.087(11) 0.047(8) 0.082(10) 0.003(7) 0.026(8) 0.019(8) C33 0.083(11) 0.063(10) 0.083(10) 0.007(8) 0.035(8) -0.008(8) C34 0.109(13) 0.035(8) 0.084(10) 0.010(8) -0.006(9) 0.020(8) C35 0.099(13) 0.087(13) 0.129(14) 0.029(12) 0.067(11) 0.003(10) C36 0.097(13) 0.075(12) 0.136(14) -0.038(11) 0.055(11) -0.014(9) C37 0.172(18) 0.092(14) 0.095(11) 0.020(10) 0.078(12) 0.054(13) C38 0.126(13) 0.070(10) 0.104(11) -0.013(9) 0.087(11) -0.012(9) C39 0.047(7) 0.097(12) 0.057(7) 0.026(8) 0.015(6) 0.029(7) C40 0.061(9) 0.075(10) 0.055(7) -0.002(7) 0.022(6) -0.002(7) C41 0.059(9) 0.072(11) 0.100(11) 0.002(10) 0.025(8) 0.002(8) C42 0.034(7) 0.085(12) 0.088(10) -0.033(9) 0.027(7) -0.015(7) C43 0.099(12) 0.069(10) 0.064(8) -0.023(8) 0.044(8) -0.012(9) C44 0.067(9) 0.043(8) 0.060(7) -0.011(6) 0.031(6) -0.002(7) C45 0.102(12) 0.057(10) 0.078(10) -0.002(8) 0.041(9) -0.001(8) C46 0.087(9) 0.056(9) 0.059(7) -0.003(8) 0.030(6) -0.017(8) C47 0.118(13) 0.084(12) 0.072(9) -0.040(9) 0.055(9) -0.041(10) C48 0.085(11) 0.098(13) 0.054(8) 0.004(9) 0.018(7) -0.025(9) C49 0.062(8) 0.076(11) 0.046(7) -0.005(7) 0.013(6) 0.000(8) C50 0.053(8) 0.065(9) 0.045(6) 0.001(7) 0.011(5) 0.004(6) C51 0.070(8) 0.055(8) 0.070(7) -0.002(7) 0.052(7) 0.008(7) C52 0.043(8) 0.125(17) 0.073(9) -0.032(10) 0.028(7) 0.006(9) C53 0.081(10) 0.065(11) 0.074(9) -0.009(8) 0.048(8) 0.008(8) C54 0.059(8) 0.034(7) 0.067(7) -0.001(6) 0.031(6) 0.010(6) C55 0.064(9) 0.078(12) 0.087(9) -0.004(8) 0.040(7) 0.018(7) C56 0.083(10) 0.065(10) 0.123(12) 0.010(10) 0.073(10) 0.027(9) C57 0.103(12) 0.061(10) 0.079(9) -0.002(8) 0.060(9) 0.003(9) C58 0.066(8) 0.060(9) 0.057(7) 0.006(7) 0.036(6) 0.011(7) N1 0.051(6) 0.036(6) 0.052(6) 0.000(5) 0.017(5) 0.006(5) N2 0.051(6) 0.062(8) 0.057(6) 0.008(6) 0.015(5) 0.017(5) N3 0.055(6) 0.049(7) 0.043(5) -0.008(5) 0.020(4) 0.000(5) N4 0.046(6) 0.040(6) 0.044(5) -0.005(5) 0.016(4) 0.000(5) N5 0.081(8) 0.045(6) 0.067(6) 0.011(6) 0.047(6) 0.018(6) N6 0.124(11) 0.027(6) 0.084(8) 0.005(6) 0.062(8) 0.018(7) N7 0.052(6) 0.040(6) 0.054(5) -0.005(5) 0.026(5) 0.005(5) N8 0.068(7) 0.034(6) 0.050(5) -0.010(5) 0.020(5) -0.009(5) F1 0.122(7) 0.069(6) 0.082(5) -0.026(5) 0.045(5) -0.002(5) F2 0.279(16) 0.129(11) 0.119(8) 0.050(8) 0.128(10) 0.032(10) F3 0.065(6) 0.159(10) 0.166(9) -0.078(9) 0.030(6) 0.011(6) F4 0.061(5) 0.215(14) 0.125(7) -0.063(9) 0.023(5) -0.051(7) F5 0.234(12) 0.071(6) 0.081(5) 0.035(5) 0.080(7) 0.066(7) F6 0.097(6) 0.049(5) 0.144(7) -0.041(6) 0.036(5) 0.007(5) F7 0.36(2) 0.29(2) 0.118(9) -0.086(13) 0.146(13) -0.18(2) F8 0.207(15) 0.36(3) 0.256(17) 0.057(17) 0.163(15) 0.197(17) F9 0.256(17) 0.087(10) 0.32(2) -0.016(11) 0.216(17) -0.041(10) F10 0.199(14) 0.34(3) 0.105(8) -0.148(13) -0.010(8) 0.039(15) F11 0.131(9) 0.281(19) 0.258(15) 0.194(16) 0.133(10) 0.131(12) F12 0.31(2) 0.075(9) 0.31(2) 0.022(10) 0.247(18) -0.029(10) P1 0.070(2) 0.047(2) 0.0592(19) 0.0059(17) 0.0157(17) 0.0083(17) P2 0.056(2) 0.056(2) 0.0611(19) -0.0065(17) 0.0217(15) -0.0003(17) Ni1 0.0445(8) 0.0376(8) 0.0479(7) 0.0013(7) 0.0202(6) 0.0056(7) Ni2 0.0597(10) 0.0395(9) 0.0477(8) 0.0004(7) 0.0245(7) 0.0045(8) _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 C1 N1 1.308(15) . ? C1 N2 1.367(14) . ? C1 Ni1 1.922(13) . ? C2 C7 1.500(17) . ? C2 N1 1.518(15) . ? C2 C5 1.548(17) . ? C2 C3 1.576(17) . ? C3 C9 1.494(17) . ? C3 C4 1.529(18) . ? C3 C8 1.541(17) . ? C4 N2 1.497(15) . ? C4 C6 1.514(18) . ? C4 H4 1.0000 . ? C5 C6 1.545(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.471(17) . ? C10 N1 1.482(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.368(17) . ? C11 N3 1.386(16) . ? C12 C13 1.38(2) . ? C12 H12 0.9500 . ? C13 C14 1.41(2) . ? C13 H13 0.9500 . ? C14 C15 1.389(17) . ? C14 H14 0.9500 . ? C15 N3 1.335(15) . ? C15 H15 0.9500 . ? C16 N2 1.418(16) . ? C16 C17 1.497(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N4 1.386(15) . ? C17 C18 1.400(18) . ? C18 C19 1.38(2) . ? C18 H18 0.9500 . ? C19 C20 1.390(19) . ? C19 H19 0.9500 . ? C20 C21 1.374(17) . ? C20 H20 0.9500 . ? C21 N4 1.336(16) . ? C21 H21 0.9500 . ? C22 C23 1.396(16) . ? C22 C29 1.505(17) . ? C22 Ni1 2.083(10) . ? C22 H22 0.9500 . ? C23 C24 1.417(16) . ? C23 Ni1 1.939(10) . ? C23 H23 0.9500 . ? C24 C25 1.531(18) . ? C24 Ni1 2.102(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.557(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.502(18) . ? C26 H26 0.9500 . ? C27 C28 1.589(19) . ? C27 H27 0.9500 . ? C28 C29 1.542(18) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 N5 1.323(17) . ? C30 N6 1.336(19) . ? C30 Ni2 1.945(15) . ? C31 C36 1.46(2) . ? C31 N5 1.539(18) . ? C31 C32 1.54(2) . ? C31 C34 1.58(2) . ? C32 C33 1.43(2) . ? C32 C37 1.51(2) . ? C32 C38 1.57(2) . ? C33 N6 1.487(19) . ? C33 C35 1.52(2) . ? C33 H33 1.0000 . ? C34 C35 1.58(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 N5 1.458(19) . ? C39 C40 1.47(2) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 N7 1.373(16) . ? C40 C41 1.38(2) . ? C41 C42 1.37(2) . ? C41 H41 0.9500 . ? C42 C43 1.38(2) . ? C42 H42 0.9500 . ? C43 C44 1.39(2) . ? C43 H43 0.9500 . ? C44 N7 1.372(16) . ? C44 H44 0.9500 . ? C45 N6 1.436(19) . ? C45 C46 1.57(2) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 N8 1.310(17) . ? C46 C47 1.375(18) . ? C47 C48 1.41(2) . ? C47 H47 0.9500 . ? C48 C49 1.34(2) . ? C48 H48 0.9500 . ? C49 C50 1.391(17) . ? C49 H49 0.9500 . ? C50 N8 1.359(16) . ? C50 H50 0.9500 . ? C51 C52 1.428(19) . ? C51 C58 1.493(18) . ? C51 Ni2 2.055(11) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.38(2) . ? C52 Ni2 1.911(13) . ? C52 H52 0.9500 . ? C53 C54 1.509(19) . ? C53 Ni2 2.101(15) . ? C53 H53 0.9500 . ? C54 C55 1.534(17) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.52(2) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.48(2) . ? C56 H56 0.9500 . ? C57 C58 1.525(19) . ? C57 H57 0.9500 . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? N3 Ni1 2.045(9) . ? N4 Ni1 2.127(10) . ? N7 Ni2 2.093(10) . ? N8 Ni2 2.064(9) . ? F1 P1 1.590(9) . ? F2 P1 1.581(10) . ? F3 P1 1.585(10) . ? F4 P1 1.538(10) . ? F5 P1 1.543(9) . ? F6 P1 1.572(9) . ? F7 P2 1.539(12) . ? F8 P2 1.483(11) . ? F9 P2 1.571(13) . ? F10 P2 1.470(10) . ? F11 P2 1.546(12) . ? F12 P2 1.524(11) . ? C59 O1 1.44(4) . ? C59 C60 1.53(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.52(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.51(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 O1 1.426(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 O2 1.46(4) . ? C63 C64 1.51(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.459(18) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.44(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 O2 1.45(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 O3 1.46(5) . ? C67 C68 1.49(4) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.48(4) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 C70 1.44(4) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C70 O3 1.46(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 O4 1.441(17) . ? C71 C72 1.50(4) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.50(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.47(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 O4 1.45(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? 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 C1 N2 115.7(11) . . ? N1 C1 Ni1 121.9(8) . . ? N2 C1 Ni1 120.9(9) . . ? C7 C2 N1 113.3(10) . . ? C7 C2 C5 115.0(11) . . ? N1 C2 C5 107.0(9) . . ? C7 C2 C3 114.6(11) . . ? N1 C2 C3 103.7(9) . . ? C5 C2 C3 102.0(10) . . ? C9 C3 C4 114.3(11) . . ? C9 C3 C8 107.5(11) . . ? C4 C3 C8 108.8(11) . . ? C9 C3 C2 115.7(11) . . ? C4 C3 C2 98.5(9) . . ? C8 C3 C2 111.9(11) . . ? N2 C4 C6 109.1(10) . . ? N2 C4 C3 108.0(9) . . ? C6 C4 C3 105.3(10) . . ? N2 C4 H4 111.4 . . ? C6 C4 H4 111.4 . . ? C3 C4 H4 111.4 . . ? C6 C5 C2 106.0(11) . . ? C6 C5 H5A 110.5 . . ? C2 C5 H5A 110.5 . . ? C6 C5 H5B 110.5 . . ? C2 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? C4 C6 C5 104.6(10) . . ? C4 C6 H6A 110.8 . . ? C5 C6 H6A 110.8 . . ? C4 C6 H6B 110.8 . . ? C5 C6 H6B 110.8 . . ? H6A C6 H6B 108.9 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 N1 112.8(11) . . ? C11 C10 H10A 109.0 . . ? N1 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? N1 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C12 C11 N3 121.0(11) . . ? C12 C11 C10 123.7(12) . . ? N3 C11 C10 115.3(10) . . ? C11 C12 C13 120.5(14) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C14 119.3(12) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C15 C14 C13 117.0(12) . . ? C15 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? N3 C15 C14 124.3(12) . . ? N3 C15 H15 117.9 . . ? C14 C15 H15 117.9 . . ? N2 C16 C17 112.8(9) . . ? N2 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? N2 C16 H16B 109.0 . . ? C17 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N4 C17 C18 119.9(12) . . ? N4 C17 C16 115.6(10) . . ? C18 C17 C16 124.3(11) . . ? C19 C18 C17 122.1(13) . . ? C19 C18 H18 119.0 . . ? C17 C18 H18 119.0 . . ? C18 C19 C20 116.5(13) . . ? C18 C19 H19 121.7 . . ? C20 C19 H19 121.7 . . ? C21 C20 C19 119.7(13) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? N4 C21 C20 124.8(12) . . ? N4 C21 H21 117.6 . . ? C20 C21 H21 117.6 . . ? C23 C22 C29 127.3(13) . . ? C23 C22 Ni1 64.3(6) . . ? C29 C22 Ni1 115.6(8) . . ? C23 C22 H22 116.4 . . ? C29 C22 H22 116.4 . . ? Ni1 C22 H22 90.1 . . ? C22 C23 C24 120.3(11) . . ? C22 C23 Ni1 75.3(6) . . ? C24 C23 Ni1 75.8(6) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? Ni1 C23 H23 120.1 . . ? C23 C24 C25 124.1(10) . . ? C23 C24 Ni1 63.4(6) . . ? C25 C24 Ni1 114.5(8) . . ? C23 C24 H24A 106.3 . . ? C25 C24 H24A 106.3 . . ? Ni1 C24 H24A 136.0 . . ? C23 C24 H24B 106.3 . . ? C25 C24 H24B 106.3 . . ? Ni1 C24 H24B 47.3 . . ? H24A C24 H24B 106.4 . . ? C24 C25 C26 111.8(11) . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C25 119.3(11) . . ? C27 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C26 C27 C28 117.1(11) . . ? C26 C27 H27 121.4 . . ? C28 C27 H27 121.4 . . ? C29 C28 C27 115.4(9) . . ? C29 C28 H28A 108.4 . . ? C27 C28 H28A 108.4 . . ? C29 C28 H28B 108.4 . . ? C27 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C22 C29 C28 112.1(11) . . ? C22 C29 H29A 109.2 . . ? C28 C29 H29A 109.2 . . ? C22 C29 H29B 109.2 . . ? C28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N5 C30 N6 119.9(13) . . ? N5 C30 Ni2 121.7(12) . . ? N6 C30 Ni2 117.9(11) . . ? C36 C31 N5 106.4(14) . . ? C36 C31 C32 119.5(13) . . ? N5 C31 C32 105.9(11) . . ? C36 C31 C34 117.0(14) . . ? N5 C31 C34 105.4(10) . . ? C32 C31 C34 101.4(14) . . ? C33 C32 C37 110.1(14) . . ? C33 C32 C31 103.8(13) . . ? C37 C32 C31 112.0(12) . . ? C33 C32 C38 117.7(13) . . ? C37 C32 C38 103.1(13) . . ? C31 C32 C38 110.5(13) . . ? C32 C33 N6 106.2(12) . . ? C32 C33 C35 105.1(13) . . ? N6 C33 C35 107.4(13) . . ? C32 C33 H33 112.5 . . ? N6 C33 H33 112.5 . . ? C35 C33 H33 112.5 . . ? C31 C34 C35 104.6(12) . . ? C31 C34 H34A 110.8 . . ? C35 C34 H34A 110.8 . . ? C31 C34 H34B 110.8 . . ? C35 C34 H34B 110.8 . . ? H34A C34 H34B 108.9 . . ? C33 C35 C34 103.4(13) . . ? C33 C35 H35A 111.1 . . ? C34 C35 H35A 111.1 . . ? C33 C35 H35B 111.1 . . ? C34 C35 H35B 111.1 . . ? H35A C35 H35B 109.1 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 C40 116.4(10) . . ? N5 C39 H39A 108.2 . . ? C40 C39 H39A 108.2 . . ? N5 C39 H39B 108.2 . . ? C40 C39 H39B 108.2 . . ? H39A C39 H39B 107.3 . . ? N7 C40 C41 122.0(14) . . ? N7 C40 C39 115.0(12) . . ? C41 C40 C39 123.0(13) . . ? C42 C41 C40 118.5(14) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C41 C42 C43 121.7(13) . . ? C41 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C42 C43 C44 117.5(15) . . ? C42 C43 H43 121.2 . . ? C44 C43 H43 121.2 . . ? N7 C44 C43 122.4(13) . . ? N7 C44 H44 118.8 . . ? C43 C44 H44 118.8 . . ? N6 C45 C46 108.0(12) . . ? N6 C45 H45A 110.1 . . ? C46 C45 H45A 110.1 . . ? N6 C45 H45B 110.1 . . ? C46 C45 H45B 110.1 . . ? H45A C45 H45B 108.4 . . ? N8 C46 C47 124.8(13) . . ? N8 C46 C45 117.0(11) . . ? C47 C46 C45 118.2(14) . . ? C46 C47 C48 117.4(15) . . ? C46 C47 H47 121.3 . . ? C48 C47 H47 121.3 . . ? C49 C48 C47 119.0(14) . . ? C49 C48 H48 120.5 . . ? C47 C48 H48 120.5 . . ? C48 C49 C50 119.4(14) . . ? C48 C49 H49 120.3 . . ? C50 C49 H49 120.3 . . ? N8 C50 C49 122.5(13) . . ? N8 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? C52 C51 C58 125.1(14) . . ? C52 C51 Ni2 63.6(7) . . ? C58 C51 Ni2 117.7(9) . . ? C52 C51 H51A 106.0 . . ? C58 C51 H51A 106.0 . . ? Ni2 C51 H51A 132.4 . . ? C52 C51 H51B 106.0 . . ? C58 C51 H51B 106.0 . . ? Ni2 C51 H51B 45.6 . . ? H51A C51 H51B 106.3 . . ? C53 C52 C51 121.8(15) . . ? C53 C52 Ni2 77.4(9) . . ? C51 C52 Ni2 74.4(7) . . ? C53 C52 H52 119.1 . . ? C51 C52 H52 119.1 . . ? Ni2 C52 H52 120.0 . . ? C52 C53 C54 122.8(12) . . ? C52 C53 Ni2 62.6(8) . . ? C54 C53 Ni2 114.1(10) . . ? C52 C53 H53 118.6 . . ? C54 C53 H53 118.6 . . ? Ni2 C53 H53 93.2 . . ? C53 C54 C55 115.9(12) . . ? C53 C54 H54A 108.3 . . ? C55 C54 H54A 108.3 . . ? C53 C54 H54B 108.3 . . ? C55 C54 H54B 108.3 . . ? H54A C54 H54B 107.4 . . ? C56 C55 C54 114.7(12) . . ? C56 C55 H55A 108.6 . . ? C54 C55 H55A 108.6 . . ? C56 C55 H55B 108.6 . . ? C54 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C57 C56 C55 118.4(13) . . ? C57 C56 H56 120.8 . . ? C55 C56 H56 120.8 . . ? C56 C57 C58 115.3(11) . . ? C56 C57 H57 122.4 . . ? C58 C57 H57 122.4 . . ? C51 C58 C57 116.4(11) . . ? C51 C58 H58A 108.2 . . ? C57 C58 H58A 108.2 . . ? C51 C58 H58B 108.2 . . ? C57 C58 H58B 108.2 . . ? H58A C58 H58B 107.3 . . ? C1 N1 C10 113.9(10) . . ? C1 N1 C2 126.6(10) . . ? C10 N1 C2 119.4(10) . . ? C1 N2 C16 118.9(10) . . ? C1 N2 C4 120.9(11) . . ? C16 N2 C4 119.6(10) . . ? C15 N3 C11 117.9(9) . . ? C15 N3 Ni1 125.9(8) . . ? C11 N3 Ni1 116.2(8) . . ? C21 N4 C17 116.9(10) . . ? C21 N4 Ni1 125.1(8) . . ? C17 N4 Ni1 117.3(8) . . ? C30 N5 C39 117.2(12) . . ? C30 N5 C31 118.1(12) . . ? C39 N5 C31 124.5(11) . . ? C30 N6 C45 121.0(12) . . ? C30 N6 C33 123.1(13) . . ? C45 N6 C33 115.1(13) . . ? C44 N7 C40 117.6(11) . . ? C44 N7 Ni2 123.7(8) . . ? C40 N7 Ni2 118.6(9) . . ? C46 N8 C50 116.7(10) . . ? C46 N8 Ni2 118.3(9) . . ? C50 N8 Ni2 125.0(8) . . ? F4 P1 F5 92.7(8) . . ? F4 P1 F6 88.0(6) . . ? F5 P1 F6 88.9(5) . . ? F4 P1 F2 90.7(8) . . ? F5 P1 F2 176.5(8) . . ? F6 P1 F2 91.9(7) . . ? F4 P1 F3 178.2(7) . . ? F5 P1 F3 87.0(7) . . ? F6 P1 F3 90.2(5) . . ? F2 P1 F3 89.6(8) . . ? F4 P1 F1 91.3(6) . . ? F5 P1 F1 92.4(5) . . ? F6 P1 F1 178.6(6) . . ? F2 P1 F1 86.8(6) . . ? F3 P1 F1 90.5(5) . . ? F10 P2 F8 93.8(10) . . ? F10 P2 F12 85.1(11) . . ? F8 P2 F12 90.0(11) . . ? F10 P2 F7 179.3(13) . . ? F8 P2 F7 86.9(12) . . ? F12 P2 F7 95.1(10) . . ? F10 P2 F11 85.1(10) . . ? F8 P2 F11 178.5(13) . . ? F12 P2 F11 91.0(9) . . ? F7 P2 F11 94.2(12) . . ? F10 P2 F9 99.4(12) . . ? F8 P2 F9 93.5(10) . . ? F12 P2 F9 174.2(11) . . ? F7 P2 F9 80.4(9) . . ? F11 P2 F9 85.7(8) . . ? C1 Ni1 C23 125.9(5) . . ? C1 Ni1 N3 91.4(4) . . ? C23 Ni1 N3 106.6(4) . . ? C1 Ni1 C22 96.6(5) . . ? C23 Ni1 C22 40.4(5) . . ? N3 Ni1 C22 141.5(4) . . ? C1 Ni1 C24 166.6(5) . . ? C23 Ni1 C24 40.8(5) . . ? N3 Ni1 C24 94.6(4) . . ? C22 Ni1 C24 71.3(5) . . ? C1 Ni1 N4 91.9(5) . . ? C23 Ni1 N4 130.3(4) . . ? N3 Ni1 N4 102.8(4) . . ? C22 Ni1 N4 114.4(4) . . ? C24 Ni1 N4 98.4(4) . . ? C52 Ni2 C30 125.7(8) . . ? C52 Ni2 C51 42.0(6) . . ? C30 Ni2 C51 96.0(5) . . ? C52 Ni2 N8 105.9(5) . . ? C30 Ni2 N8 88.9(5) . . ? C51 Ni2 N8 141.1(5) . . ? C52 Ni2 N7 133.2(6) . . ? C30 Ni2 N7 91.7(6) . . ? C51 Ni2 N7 117.2(5) . . ? N8 Ni2 N7 101.2(4) . . ? C52 Ni2 C53 40.0(6) . . ? C30 Ni2 C53 165.7(6) . . ? C51 Ni2 C53 72.4(6) . . ? N8 Ni2 C53 94.9(5) . . ? N7 Ni2 C53 101.0(5) . . ? O1 C59 C60 97.9(15) . . ? O1 C59 H59A 112.2 . . ? C60 C59 H59A 112.2 . . ? O1 C59 H59B 112.2 . . ? C60 C59 H59B 112.2 . . ? H59A C59 H59B 109.8 . . ? C61 C60 C59 107.7(15) . . ? C61 C60 H60A 110.2 . . ? C59 C60 H60A 110.2 . . ? C61 C60 H60B 110.2 . . ? C59 C60 H60B 110.2 . . ? H60A C60 H60B 108.5 . . ? C62 C61 C60 104.2(15) . . ? C62 C61 H61A 110.9 . . ? C60 C61 H61A 110.9 . . ? C62 C61 H61B 110.9 . . ? C60 C61 H61B 110.9 . . ? H61A C61 H61B 108.9 . . ? O1 C62 C61 104.5(15) . . ? O1 C62 H62A 110.9 . . ? C61 C62 H62A 110.9 . . ? O1 C62 H62B 110.9 . . ? C61 C62 H62B 110.9 . . ? H62A C62 H62B 108.9 . . ? C62 O1 C59 113.3(18) . . ? O2 C63 C64 101.7(16) . . ? O2 C63 H63A 111.4 . . ? C64 C63 H63A 111.4 . . ? O2 C63 H63B 111.4 . . ? C64 C63 H63B 111.4 . . ? H63A C63 H63B 109.3 . . ? C65 C64 C63 108.6(16) . . ? C65 C64 H64A 110.0 . . ? C63 C64 H64A 110.0 . . ? C65 C64 H64B 110.0 . . ? C63 C64 H64B 110.0 . . ? H64A C64 H64B 108.4 . . ? C66 C65 C64 108.2(18) . . ? C66 C65 H65A 110.1 . . ? C64 C65 H65A 110.1 . . ? C66 C65 H65B 110.1 . . ? C64 C65 H65B 110.1 . . ? H65A C65 H65B 108.4 . . ? C65 C66 O2 103.1(18) . . ? C65 C66 H66A 111.1 . . ? O2 C66 H66A 111.1 . . ? C65 C66 H66B 111.1 . . ? O2 C66 H66B 111.1 . . ? H66A C66 H66B 109.1 . . ? C63 O2 C66 111.9(17) . . ? O3 C67 C68 98.5(16) . . ? O3 C67 H67A 112.1 . . ? C68 C67 H67A 112.1 . . ? O3 C67 H67B 112.1 . . ? C68 C67 H67B 112.1 . . ? H67A C67 H67B 109.7 . . ? C69 C68 C67 105.1(17) . . ? C69 C68 H68A 110.7 . . ? C67 C68 H68A 110.7 . . ? C69 C68 H68B 110.7 . . ? C67 C68 H68B 110.7 . . ? H68A C68 H68B 108.8 . . ? C70 C69 C68 104.0(18) . . ? C70 C69 H69A 111.0 . . ? C68 C69 H69A 111.0 . . ? C70 C69 H69B 111.0 . . ? C68 C69 H69B 111.0 . . ? H69A C69 H69B 109.0 . . ? C69 C70 O3 102.1(18) . . ? C69 C70 H70A 111.3 . . ? O3 C70 H70A 111.3 . . ? C69 C70 H70B 111.3 . . ? O3 C70 H70B 111.3 . . ? H70A C70 H70B 109.2 . . ? C70 O3 C67 113.5(17) . . ? O4 C71 C72 100.3(15) . . ? O4 C71 H71A 111.7 . . ? C72 C71 H71A 111.7 . . ? O4 C71 H71B 111.7 . . ? C72 C71 H71B 111.7 . . ? H71A C71 H71B 109.5 . . ? C73 C72 C71 107.2(18) . . ? C73 C72 H72A 110.3 . . ? C71 C72 H72A 110.3 . . ? C73 C72 H72B 110.3 . . ? C71 C72 H72B 110.3 . . ? H72A C72 H72B 108.5 . . ? C74 C73 C72 100.3(19) . . ? C74 C73 H73A 111.7 . . ? C72 C73 H73A 111.7 . . ? C74 C73 H73B 111.7 . . ? C72 C73 H73B 111.7 . . ? H73A C73 H73B 109.5 . . ? O4 C74 C73 104.0(19) . . ? O4 C74 H74A 111.0 . . ? C73 C74 H74A 111.0 . . ? O4 C74 H74B 111.0 . . ? C73 C74 H74B 111.0 . . ? H74A C74 H74B 109.0 . . ? C71 O4 C74 112.8(17) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.535 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.093 #===END data_global _publ_requested_journal '' _publ_contact_author ; B. Kariuki, School of Chemistry, Cardiff University, Main Building Park Place Cardiff CF10 3AT ; _publ_contact_author_email 'kariukib@cardiff.ac.uk' _publ_section_title ; <> ; _publ_section_references ; SHELX97 [Includes SHELXS97, SHELXL97, CIFTAB] - Programs for Crystal Structure Analysis (Release 97-2). G. M. Sheldrick, Institüt für Anorganische Chemie der Universität, Tammanstrasse 4, D-3400 Göttingen, Germany, 1998. DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; data_cmpd7b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 Cl N4 Ni, P F6' _chemical_formula_sum 'C21 H26 Cl F6 N4 Ni P' _chemical_formula_weight 573.59 _chemical_absolute_configuration ab 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 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 8.0670(4) _cell_length_b 14.0748(7) _cell_length_c 20.5513(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2333.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2556 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 23.23 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.080 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8129 _exptl_absorpt_correction_T_max 0.9480 _exptl_absorpt_process_details 'Denzo/Scalepack' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius Kappa CCD' _diffrn_measurement_method 'CCD scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3328 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 23.23 _reflns_number_total 3328 _reflns_number_gt 2556 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'cOLLECT,Nonius BV, 1997-2001' _computing_cell_refinement 'DENZO/SCALEPACK' _computing_data_reduction 'DENZO/SCALEPACK' _computing_structure_solution SHELXs-97 _computing_structure_refinement SHELXL-97 _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 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+5.6115P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 -0.03(3) _refine_ls_number_reflns 3328 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1231 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _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 C1 C 0.2749(11) 1.0112(6) 1.0137(4) 0.036(2) Uani 1 1 d . . . H1 H 0.1836 0.9831 1.0356 0.043 Uiso 1 1 calc R . . C2 C 0.3123(12) 1.1038(6) 1.0267(4) 0.037(2) Uani 1 1 d . . . H2 H 0.2448 1.1393 1.0558 0.044 Uiso 1 1 calc R . . C3 C 0.4472(11) 1.1458(6) 0.9979(4) 0.034(2) Uani 1 1 d . . . H3 H 0.4769 1.2097 1.0073 0.041 Uiso 1 1 calc R . . C4 C 0.5401(10) 1.0903(5) 0.9538(4) 0.029(2) Uani 1 1 d . . . H4 H 0.6341 1.1164 0.9324 0.035 Uiso 1 1 calc R . . C5 C 0.4932(10) 0.9981(5) 0.9420(3) 0.0258(19) Uani 1 1 d . . . C6 C 0.5856(10) 0.9367(5) 0.8952(3) 0.026(2) Uani 1 1 d . . . H6A H 0.6736 0.9749 0.8741 0.031 Uiso 1 1 calc R . . H6B H 0.6400 0.8845 0.9194 0.031 Uiso 1 1 calc R . . C7 C 0.3453(10) 0.8511(5) 0.8660(4) 0.029(2) Uani 1 1 d . . . C8 C 0.5170(11) 0.9073(5) 0.7723(3) 0.030(2) Uani 1 1 d . . . C9 C 0.3917(13) 0.9812(6) 0.7449(4) 0.046(3) Uani 1 1 d . . . H9A H 0.3721 1.0321 0.7772 0.056 Uiso 1 1 calc R . . H9B H 0.4365 1.0105 0.7047 0.056 Uiso 1 1 calc R . . C10 C 0.2298(12) 0.9296(6) 0.7299(4) 0.046(3) Uani 1 1 d . . . H10A H 0.1363 0.9573 0.7548 0.055 Uiso 1 1 calc R . . H10B H 0.2037 0.9323 0.6829 0.055 Uiso 1 1 calc R . . C11 C 0.2650(10) 0.8290(6) 0.7514(3) 0.035(2) Uani 1 1 d . . . H11 H 0.1977 0.7824 0.7259 0.042 Uiso 1 1 calc R . . C12 C 0.4523(10) 0.8129(6) 0.7406(4) 0.033(2) Uani 1 1 d . . . C13 C 0.6950(13) 0.9267(7) 0.7619(4) 0.054(3) Uani 1 1 d . . . H13A H 0.7613 0.8823 0.7879 0.081 Uiso 1 1 calc R . . H13B H 0.7201 0.9920 0.7751 0.081 Uiso 1 1 calc R . . H13C H 0.7218 0.9185 0.7157 0.081 Uiso 1 1 calc R . . C14 C 0.4895(11) 0.8138(7) 0.6663(3) 0.044(2) Uani 1 1 d . . . H14A H 0.4165 0.7684 0.6442 0.066 Uiso 1 1 calc R . . H14B H 0.6053 0.7958 0.6589 0.066 Uiso 1 1 calc R . . H14C H 0.4700 0.8777 0.6489 0.066 Uiso 1 1 calc R . . C15 C 0.5206(12) 0.7232(6) 0.7691(4) 0.045(3) Uani 1 1 d . . . H15A H 0.4575 0.6687 0.7527 0.067 Uiso 1 1 calc R . . H15B H 0.5117 0.7256 0.8167 0.067 Uiso 1 1 calc R . . H15C H 0.6373 0.7164 0.7567 0.067 Uiso 1 1 calc R . . C16 C 0.0920(11) 0.7652(6) 0.8469(4) 0.037(2) Uani 1 1 d . . . H16A H 0.0212 0.7445 0.8103 0.045 Uiso 1 1 calc R . . H16B H 0.0247 0.8058 0.8761 0.045 Uiso 1 1 calc R . . C17 C 0.1540(9) 0.6804(6) 0.8835(4) 0.033(2) Uani 1 1 d . . . C18 C 0.1115(12) 0.5873(7) 0.8687(4) 0.037(2) Uani 1 1 d . . . H18 H 0.0317 0.5751 0.8357 0.045 Uiso 1 1 calc R . . C19 C 0.1831(13) 0.5125(6) 0.9012(4) 0.043(2) Uani 1 1 d . . . H19 H 0.1540 0.4487 0.8912 0.051 Uiso 1 1 calc R . . C20 C 0.2978(11) 0.5328(6) 0.9482(4) 0.036(2) Uani 1 1 d . . . H20 H 0.3527 0.4828 0.9706 0.043 Uiso 1 1 calc R . . C21 C 0.3331(10) 0.6257(6) 0.9631(4) 0.033(2) Uani 1 1 d . . . H21 H 0.4103 0.6383 0.9969 0.039 Uiso 1 1 calc R . . Cl1 Cl 0.2510(3) 0.79752(15) 1.05805(9) 0.0389(6) Uani 1 1 d . . . F1 F 0.0524(6) 1.1336(4) 0.7838(2) 0.0542(15) Uani 1 1 d . . . F2 F 0.2083(7) 1.1256(4) 0.8740(2) 0.0669(17) Uani 1 1 d . . . F3 F 0.0030(7) 1.0214(3) 0.8618(2) 0.0555(14) Uani 1 1 d . . . F4 F -0.0204(6) 1.1346(3) 0.9369(2) 0.0540(15) Uani 1 1 d . . . F5 F -0.1762(6) 1.1394(4) 0.8455(2) 0.0587(15) Uani 1 1 d . . . F6 F 0.0253(8) 1.2461(3) 0.8599(3) 0.0625(17) Uani 1 1 d . . . P1 P 0.0179(3) 1.13421(17) 0.86060(11) 0.0360(6) Uani 1 1 d . . . Ni1 Ni 0.30836(13) 0.82795(7) 0.95455(5) 0.0307(3) Uani 1 1 d . . . N1 N 0.3604(8) 0.9581(5) 0.9715(3) 0.0322(18) Uani 1 1 d . . . N2 N 0.4787(9) 0.8958(4) 0.8447(3) 0.0314(17) Uani 1 1 d . . . N3 N 0.2335(8) 0.8191(5) 0.8222(3) 0.0289(16) Uani 1 1 d . . . N4 N 0.2638(8) 0.6996(4) 0.9321(3) 0.0301(16) 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 C1 0.040(6) 0.044(6) 0.025(4) 0.000(4) -0.005(4) -0.003(5) C2 0.050(6) 0.038(5) 0.023(4) -0.008(4) -0.004(5) 0.004(5) C3 0.046(6) 0.030(6) 0.027(5) -0.002(4) -0.010(4) 0.003(5) C4 0.028(5) 0.038(5) 0.022(4) 0.001(4) 0.004(4) 0.008(4) C5 0.034(5) 0.024(5) 0.019(4) -0.001(4) -0.004(4) 0.001(4) C6 0.029(5) 0.027(5) 0.021(4) 0.003(4) -0.003(4) -0.005(4) C7 0.036(6) 0.025(5) 0.025(4) -0.005(4) -0.001(4) 0.000(4) C8 0.042(6) 0.030(5) 0.017(4) 0.000(4) 0.007(5) -0.010(5) C9 0.086(8) 0.023(5) 0.031(5) -0.004(4) 0.005(5) 0.007(5) C10 0.057(7) 0.049(6) 0.030(5) 0.000(4) -0.006(5) 0.004(5) C11 0.046(6) 0.033(5) 0.025(4) -0.005(4) 0.002(4) -0.001(5) C12 0.043(6) 0.025(5) 0.032(4) -0.007(4) -0.002(4) 0.003(5) C13 0.052(7) 0.086(8) 0.024(5) -0.008(5) 0.014(5) -0.026(6) C14 0.047(6) 0.049(6) 0.036(5) -0.013(5) -0.001(4) 0.008(5) C15 0.047(7) 0.038(6) 0.048(6) 0.000(5) -0.005(5) 0.015(5) C16 0.029(5) 0.052(6) 0.032(5) -0.011(5) 0.001(4) -0.007(5) C17 0.030(5) 0.032(5) 0.036(5) 0.011(4) 0.008(4) 0.002(5) C18 0.038(6) 0.044(6) 0.030(5) 0.002(5) 0.007(5) -0.011(5) C19 0.058(7) 0.039(6) 0.032(5) -0.004(5) 0.023(5) 0.003(6) C20 0.037(5) 0.036(5) 0.035(5) 0.004(4) 0.010(5) 0.000(4) C21 0.029(5) 0.041(5) 0.028(5) 0.003(4) 0.009(4) -0.005(4) Cl1 0.0458(14) 0.0438(13) 0.0272(10) 0.0025(9) 0.0017(10) -0.0026(10) F1 0.058(4) 0.074(4) 0.030(3) 0.003(3) 0.000(3) 0.014(3) F2 0.033(3) 0.114(5) 0.053(3) 0.019(3) -0.007(3) 0.006(3) F3 0.068(4) 0.042(3) 0.057(3) -0.001(3) -0.007(3) 0.005(3) F4 0.063(4) 0.063(3) 0.036(3) -0.001(2) 0.003(3) 0.004(3) F5 0.036(3) 0.076(4) 0.064(3) 0.014(3) -0.002(3) 0.005(3) F6 0.090(5) 0.043(3) 0.055(3) -0.003(3) -0.002(4) -0.007(3) P1 0.0353(15) 0.0389(14) 0.0336(13) 0.0019(11) 0.0010(12) 0.0034(11) Ni1 0.0340(6) 0.0348(6) 0.0235(5) 0.0010(5) 0.0007(5) -0.0031(5) N1 0.035(5) 0.039(4) 0.023(4) 0.000(3) 0.002(3) 0.003(4) N2 0.035(4) 0.030(4) 0.029(4) 0.001(3) 0.007(4) -0.006(4) N3 0.032(4) 0.027(4) 0.028(3) 0.004(3) -0.002(3) -0.007(4) N4 0.027(4) 0.032(4) 0.032(4) 0.009(3) 0.006(3) 0.003(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 C1 N1 1.336(10) . ? C1 C2 1.364(11) . ? C1 H1 0.9500 . ? C2 C3 1.373(11) . ? C2 H2 0.9500 . ? C3 C4 1.413(11) . ? C3 H3 0.9500 . ? C4 C5 1.373(10) . ? C4 H4 0.9500 . ? C5 N1 1.354(9) . ? C5 C6 1.493(10) . ? C6 N2 1.467(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.320(10) . ? C7 N3 1.351(9) . ? C7 Ni1 1.874(7) . ? C8 C13 1.477(13) . ? C8 N2 1.528(9) . ? C8 C9 1.556(12) . ? C8 C12 1.570(11) . ? C9 C10 1.526(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.511(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N3 1.484(8) . ? C11 C12 1.544(11) . ? C11 H11 1.0000 . ? C12 C15 1.497(11) . ? C12 C14 1.557(10) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 N3 1.461(10) . ? C16 C17 1.496(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N4 1.362(9) . ? C17 C18 1.389(11) . ? C18 C19 1.374(12) . ? C18 H18 0.9500 . ? C19 C20 1.369(11) . ? C19 H19 0.9500 . ? C20 C21 1.372(10) . ? C20 H20 0.9500 . ? C21 N4 1.341(9) . ? C21 H21 0.9500 . ? Cl1 Ni1 2.219(2) . ? F1 P1 1.602(5) . ? F2 P1 1.566(6) . ? F3 P1 1.593(5) . ? F4 P1 1.598(5) . ? F5 P1 1.597(6) . ? F6 P1 1.576(5) . ? Ni1 N4 1.899(6) . ? Ni1 N1 1.911(7) . ? 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 C1 C2 123.2(8) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 120.1(8) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 117.3(8) . . ? C2 C3 H3 121.3 . . ? C4 C3 H3 121.3 . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N1 C5 C4 122.2(7) . . ? N1 C5 C6 116.3(7) . . ? C4 C5 C6 121.5(7) . . ? N2 C6 C5 112.9(7) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 N3 118.9(7) . . ? N2 C7 Ni1 122.3(6) . . ? N3 C7 Ni1 118.8(6) . . ? C13 C8 N2 111.0(7) . . ? C13 C8 C9 117.1(7) . . ? N2 C8 C9 107.0(7) . . ? C13 C8 C12 114.8(7) . . ? N2 C8 C12 104.3(6) . . ? C9 C8 C12 101.5(6) . . ? C10 C9 C8 108.1(7) . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9A 110.1 . . ? C10 C9 H9B 110.1 . . ? C8 C9 H9B 110.1 . . ? H9A C9 H9B 108.4 . . ? C11 C10 C9 103.1(7) . . ? C11 C10 H10A 111.2 . . ? C9 C10 H10A 111.2 . . ? C11 C10 H10B 111.2 . . ? C9 C10 H10B 111.2 . . ? H10A C10 H10B 109.1 . . ? N3 C11 C10 110.1(6) . . ? N3 C11 C12 107.2(6) . . ? C10 C11 C12 106.3(7) . . ? N3 C11 H11 111.1 . . ? C10 C11 H11 111.1 . . ? C12 C11 H11 111.1 . . ? C15 C12 C11 115.3(7) . . ? C15 C12 C14 108.7(7) . . ? C11 C12 C14 109.2(6) . . ? C15 C12 C8 115.4(6) . . ? C11 C12 C8 98.1(6) . . ? C14 C12 C8 109.6(7) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N3 C16 C17 109.1(7) . . ? N3 C16 H16A 109.9 . . ? C17 C16 H16A 109.9 . . ? N3 C16 H16B 109.9 . . ? C17 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? N4 C17 C18 120.5(8) . . ? N4 C17 C16 115.3(7) . . ? C18 C17 C16 124.1(8) . . ? C19 C18 C17 120.9(9) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 117.8(8) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C19 C20 C21 119.8(8) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? N4 C21 C20 123.1(8) . . ? N4 C21 H21 118.4 . . ? C20 C21 H21 118.4 . . ? F2 P1 F6 92.4(4) . . ? F2 P1 F3 89.7(3) . . ? F6 P1 F3 177.8(4) . . ? F2 P1 F5 177.9(4) . . ? F6 P1 F5 89.4(3) . . ? F3 P1 F5 88.6(3) . . ? F2 P1 F4 91.0(3) . . ? F6 P1 F4 90.7(3) . . ? F3 P1 F4 88.5(3) . . ? F5 P1 F4 90.0(3) . . ? F2 P1 F1 90.2(3) . . ? F6 P1 F1 89.4(3) . . ? F3 P1 F1 91.3(3) . . ? F5 P1 F1 88.8(3) . . ? F4 P1 F1 178.8(3) . . ? C7 Ni1 N4 87.7(3) . . ? C7 Ni1 N1 88.6(3) . . ? N4 Ni1 N1 176.1(3) . . ? C7 Ni1 Cl1 176.9(3) . . ? N4 Ni1 Cl1 90.59(19) . . ? N1 Ni1 Cl1 93.2(2) . . ? C1 N1 C5 117.8(7) . . ? C1 N1 Ni1 122.8(6) . . ? C5 N1 Ni1 119.4(5) . . ? C7 N2 C6 115.6(6) . . ? C7 N2 C8 122.5(7) . . ? C6 N2 C8 121.8(6) . . ? C7 N3 C16 117.6(6) . . ? C7 N3 C11 120.4(6) . . ? C16 N3 C11 121.6(6) . . ? C21 N4 C17 117.8(7) . . ? C21 N4 Ni1 122.9(6) . . ? C17 N4 Ni1 119.3(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.23 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.327 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.082