#=============================================================================== data_global #=============================================================================== _audit_creation_date 06-05-2007 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Louis Ricard' _publ_contact_author_address ;Laboratoire DCPH Ecole Polytechnique Route de Saclay F91128 Palaiseau France ; _publ_contact_author_email louis.ricard@polytechnique.fr _publ_contact_author_phone 330169334572 _publ_contact_author_fax 330169333990 _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Inorganic Chemistry. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, X-Ray and Electronic structures of a Bis-(3,4)dimethylphosphole-Xanthene Nickel Dibromide Complex and its Use in the Regioselective Catalyzed Dimerization of Ethylene into 1-Butene. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name ; Guilhem Mora, Steven Van Zuthphen, Christian Klemps, Xavier-Frederic Le goff, Yves Jean Pascal Le Floch ; _publ_author_address ;Laboratoire Heteroelements et Coordination, CNRS UMR 7653, DCPH Ecole Polytechnique, F-91128 Palaiseau Cedex France ; #=============================================================================== # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. #============================================================================= data_gm233 #compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H28 Br2 Ni O P2' _chemical_formula_weight 648.96 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5190(10) _cell_length_b 18.0280(10) _cell_length_c 13.7460(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.8900(10) _cell_angle_gamma 90.00 _cell_volume 2603.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 7342 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'Block' _exptl_crystal_colour 'Dark Red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 3.956 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.4261 _exptl_absorpt_correction_T_max 0.6931 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24900 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 30.03 _reflns_number_total 7590 _reflns_number_gt 5621 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0301P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7590 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0635 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Ni1 Ni -0.02564(2) 0.077925(14) 0.288714(14) 0.01760(6) Uani 1 1 d . . . Br1 Br 0.121787(17) 0.083983(11) 0.418122(12) 0.02277(6) Uani 1 1 d . . . Br2 Br -0.169049(17) 0.085012(12) 0.154554(12) 0.02376(6) Uani 1 1 d . . . P1 P 0.11128(4) 0.02552(3) 0.19515(3) 0.01860(11) Uani 1 1 d . . . P2 P -0.18921(4) 0.08812(3) 0.38184(3) 0.01881(11) Uani 1 1 d . . . O1 O -0.08163(11) -0.05430(7) 0.31248(8) 0.0183(3) Uani 1 1 d . . . C1 C 0.28041(16) 0.02324(11) 0.22180(12) 0.0226(4) Uani 1 1 d . . . H1 H 0.3205 0.0055 0.2808 0.027 Uiso 1 1 calc R . . C2 C 0.34163(16) 0.05031(12) 0.14615(13) 0.0231(4) Uani 1 1 d . . . C3 C 0.25612(18) 0.07065(11) 0.06108(13) 0.0224(4) Uani 1 1 d . . . C4 C 0.13289(17) 0.05765(11) 0.07398(12) 0.0205(4) Uani 1 1 d . . . H4 H 0.0662 0.0645 0.0256 0.025 Uiso 1 1 calc R . . C5 C 0.30674(19) 0.10333(13) -0.02970(14) 0.0332(5) Uani 1 1 d . . . H5A H 0.2361 0.1126 -0.0773 0.050 Uiso 1 1 calc R . . H5B H 0.3668 0.0685 -0.0573 0.050 Uiso 1 1 calc R . . H5C H 0.3504 0.1501 -0.0137 0.050 Uiso 1 1 calc R . . C6 C 0.48225(18) 0.06244(14) 0.14574(15) 0.0379(6) Uani 1 1 d . . . H6A H 0.5233 0.0407 0.2046 0.057 Uiso 1 1 calc R . . H6B H 0.5000 0.1158 0.1443 0.057 Uiso 1 1 calc R . . H6C H 0.5155 0.0389 0.0880 0.057 Uiso 1 1 calc R . . C7 C 0.05823(16) -0.07066(10) 0.18388(12) 0.0183(4) Uani 1 1 d . . . C8 C 0.10853(17) -0.11689(12) 0.11395(12) 0.0220(4) Uani 1 1 d . . . H8 H 0.1749 -0.0992 0.0757 0.026 Uiso 1 1 calc R . . C9 C 0.06273(17) -0.18800(12) 0.09990(13) 0.0250(4) Uani 1 1 d . . . H9 H 0.0970 -0.2187 0.0516 0.030 Uiso 1 1 calc R . . C10 C -0.03331(17) -0.21486(11) 0.15618(13) 0.0245(4) Uani 1 1 d . . . H10 H -0.0648 -0.2637 0.1452 0.029 Uiso 1 1 calc R . . C11 C -0.08429(16) -0.17143(11) 0.22848(12) 0.0201(4) Uani 1 1 d . . . C12 C -0.03637(16) -0.10014(11) 0.24062(12) 0.0185(4) Uani 1 1 d . . . C13 C -0.18464(17) -0.19912(11) 0.29594(12) 0.0216(4) Uani 1 1 d . . . C14 C -0.26428(17) -0.13328(11) 0.32639(12) 0.0202(4) Uani 1 1 d . . . C15 C -0.39025(18) -0.13838(12) 0.35155(13) 0.0262(4) Uani 1 1 d . . . H15 H -0.4328 -0.1847 0.3449 0.031 Uiso 1 1 calc R . . C16 C -0.45578(19) -0.07776(12) 0.38607(14) 0.0283(5) Uani 1 1 d . . . H16 H -0.5419 -0.0830 0.4028 0.034 Uiso 1 1 calc R . . C17 C -0.39581(17) -0.00991(12) 0.39614(12) 0.0240(4) Uani 1 1 d . . . H17 H -0.4405 0.0313 0.4208 0.029 Uiso 1 1 calc R . . C18 C -0.26969(16) -0.00137(11) 0.37030(11) 0.0186(4) Uani 1 1 d . . . C19 C -0.20709(16) -0.06349(11) 0.33597(11) 0.0182(4) Uani 1 1 d . . . C20 C -0.26815(19) -0.26016(12) 0.24750(14) 0.0317(5) Uani 1 1 d . . . H20A H -0.3289 -0.2782 0.2938 0.047 Uiso 1 1 calc R . . H20B H -0.2141 -0.3013 0.2279 0.047 Uiso 1 1 calc R . . H20C H -0.3147 -0.2399 0.1899 0.047 Uiso 1 1 calc R . . C21 C -0.11539(19) -0.23244(12) 0.38772(13) 0.0295(5) Uani 1 1 d . . . H21A H -0.0602 -0.1947 0.4190 0.044 Uiso 1 1 calc R . . H21B H -0.0638 -0.2749 0.3690 0.044 Uiso 1 1 calc R . . H21C H -0.1783 -0.2489 0.4333 0.044 Uiso 1 1 calc R . . C22 C -0.30708(17) 0.15909(11) 0.36239(13) 0.0238(4) Uani 1 1 d . . . H22 H -0.3517 0.1688 0.3019 0.029 Uiso 1 1 calc R . . C23 C -0.32350(16) 0.19661(11) 0.44534(13) 0.0231(4) Uani 1 1 d . . . C24 C -0.24700(17) 0.16640(11) 0.53089(12) 0.0221(4) Uani 1 1 d . . . C25 C -0.17431(17) 0.10849(11) 0.50985(12) 0.0204(4) Uani 1 1 d . . . H25 H -0.1220 0.0818 0.5561 0.024 Uiso 1 1 calc R . . C26 C -0.25166(18) 0.20193(12) 0.62996(13) 0.0287(5) Uani 1 1 d . . . H26A H -0.2004 0.1728 0.6776 0.043 Uiso 1 1 calc R . . H26B H -0.3400 0.2037 0.6493 0.043 Uiso 1 1 calc R . . H26C H -0.2176 0.2525 0.6274 0.043 Uiso 1 1 calc R . . C27 C -0.4067(2) 0.26310(13) 0.45446(15) 0.0350(5) Uani 1 1 d . . . H27A H -0.4374 0.2795 0.3895 0.052 Uiso 1 1 calc R . . H27B H -0.3578 0.3031 0.4869 0.052 Uiso 1 1 calc R . . H27C H -0.4794 0.2503 0.4930 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01839(12) 0.01614(14) 0.01826(12) -0.00036(9) 0.00076(9) -0.00015(9) Br1 0.02518(10) 0.02271(12) 0.02002(9) -0.00016(7) -0.00290(7) 0.00012(8) Br2 0.02119(10) 0.02896(13) 0.02090(9) 0.00080(8) -0.00117(7) 0.00211(8) P1 0.0178(2) 0.0186(3) 0.0193(2) -0.00009(19) 0.00010(17) -0.0006(2) P2 0.0208(2) 0.0157(3) 0.0200(2) -0.00110(19) 0.00130(18) 0.0013(2) O1 0.0184(6) 0.0159(7) 0.0208(6) -0.0044(5) 0.0027(5) -0.0009(5) C1 0.0194(9) 0.0250(12) 0.0232(9) -0.0019(8) -0.0019(7) 0.0017(8) C2 0.0184(9) 0.0240(12) 0.0270(9) -0.0037(8) 0.0006(7) 0.0007(8) C3 0.0241(10) 0.0180(11) 0.0254(9) -0.0040(8) 0.0042(8) 0.0002(8) C4 0.0229(9) 0.0176(11) 0.0208(9) 0.0007(8) -0.0028(7) -0.0008(8) C5 0.0296(11) 0.0399(15) 0.0306(10) 0.0073(10) 0.0065(9) -0.0021(10) C6 0.0208(10) 0.0544(17) 0.0384(12) 0.0001(11) 0.0002(9) -0.0030(10) C7 0.0192(9) 0.0179(11) 0.0178(8) 0.0007(7) -0.0007(7) 0.0009(7) C8 0.0211(9) 0.0235(12) 0.0214(9) 0.0001(8) 0.0016(7) 0.0022(8) C9 0.0277(10) 0.0226(12) 0.0248(9) -0.0047(8) 0.0032(8) 0.0067(9) C10 0.0292(10) 0.0157(11) 0.0283(9) -0.0033(8) -0.0024(8) 0.0010(8) C11 0.0207(9) 0.0169(11) 0.0223(9) -0.0009(8) -0.0018(7) 0.0003(8) C12 0.0195(9) 0.0177(10) 0.0180(8) -0.0002(7) -0.0010(7) 0.0016(7) C13 0.0234(9) 0.0149(10) 0.0264(9) -0.0008(8) 0.0006(7) -0.0021(8) C14 0.0249(9) 0.0156(11) 0.0200(8) 0.0011(7) -0.0008(7) -0.0015(8) C15 0.0272(10) 0.0206(12) 0.0310(10) -0.0029(9) 0.0030(8) -0.0068(9) C16 0.0228(10) 0.0283(13) 0.0343(11) -0.0003(9) 0.0069(8) -0.0028(9) C17 0.0236(10) 0.0244(12) 0.0245(9) -0.0023(8) 0.0054(7) 0.0011(8) C18 0.0222(9) 0.0158(10) 0.0179(8) 0.0013(7) 0.0012(7) -0.0007(8) C19 0.0182(9) 0.0208(11) 0.0157(8) 0.0011(7) 0.0003(7) -0.0007(8) C20 0.0325(11) 0.0233(13) 0.0394(11) -0.0062(9) 0.0043(9) -0.0064(9) C21 0.0364(11) 0.0219(12) 0.0301(10) 0.0054(9) 0.0017(9) 0.0015(9) C22 0.0227(9) 0.0195(11) 0.0292(9) 0.0016(8) 0.0006(8) 0.0027(8) C23 0.0198(9) 0.0187(11) 0.0309(10) -0.0009(8) 0.0037(8) 0.0006(8) C24 0.0217(9) 0.0187(11) 0.0261(9) -0.0026(8) 0.0043(7) -0.0059(8) C25 0.0215(9) 0.0184(11) 0.0212(8) -0.0010(8) 0.0005(7) -0.0028(8) C26 0.0273(10) 0.0274(13) 0.0315(10) -0.0086(9) 0.0045(8) -0.0019(9) C27 0.0336(12) 0.0287(14) 0.0430(12) -0.0017(10) 0.0046(9) 0.0118(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 P1 2.1926(5) . ? Ni1 P2 2.2035(5) . ? Ni1 Br1 2.3028(3) . ? Ni1 Br2 2.3265(3) . ? P1 C4 1.7888(18) . ? P1 C1 1.7988(17) . ? P1 C7 1.8257(19) . ? P2 C22 1.7923(19) . ? P2 C25 1.7966(17) . ? P2 C18 1.8251(19) . ? O1 C19 1.384(2) . ? O1 C12 1.390(2) . ? C1 C2 1.342(3) . ? C2 C3 1.485(2) . ? C2 C6 1.496(2) . ? C3 C4 1.338(2) . ? C3 C5 1.502(3) . ? C7 C8 1.396(3) . ? C7 C12 1.400(3) . ? C8 C9 1.380(3) . ? C9 C10 1.390(3) . ? C10 C11 1.394(3) . ? C11 C12 1.388(3) . ? C11 C13 1.524(2) . ? C13 C14 1.524(3) . ? C13 C20 1.539(3) . ? C13 C21 1.546(2) . ? C14 C15 1.389(3) . ? C14 C19 1.398(3) . ? C15 C16 1.388(3) . ? C16 C17 1.380(3) . ? C17 C18 1.399(2) . ? C18 C19 1.393(2) . ? C22 C23 1.344(3) . ? C23 C27 1.493(3) . ? C23 C24 1.494(2) . ? C24 C25 1.334(3) . ? C24 C26 1.508(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Ni1 P2 158.74(2) . . ? P1 Ni1 Br1 92.113(15) . . ? P2 Ni1 Br1 93.581(15) . . ? P1 Ni1 Br2 88.714(15) . . ? P2 Ni1 Br2 87.810(15) . . ? Br1 Ni1 Br2 173.837(14) . . ? C4 P1 C1 91.50(8) . . ? C4 P1 C7 106.33(8) . . ? C1 P1 C7 106.89(9) . . ? C4 P1 Ni1 121.65(6) . . ? C1 P1 Ni1 124.23(6) . . ? C7 P1 Ni1 104.60(6) . . ? C22 P2 C25 91.47(9) . . ? C22 P2 C18 107.68(9) . . ? C25 P2 C18 106.44(8) . . ? C22 P2 Ni1 121.83(6) . . ? C25 P2 Ni1 123.63(6) . . ? C18 P2 Ni1 104.37(6) . . ? C19 O1 C12 117.35(13) . . ? C2 C1 P1 110.00(13) . . ? C1 C2 C3 113.87(16) . . ? C1 C2 C6 124.70(17) . . ? C3 C2 C6 121.38(17) . . ? C4 C3 C2 113.88(16) . . ? C4 C3 C5 124.43(17) . . ? C2 C3 C5 121.69(17) . . ? C3 C4 P1 110.46(13) . . ? C8 C7 C12 117.50(17) . . ? C8 C7 P1 120.03(15) . . ? C12 C7 P1 122.42(14) . . ? C9 C8 C7 120.61(18) . . ? C8 C9 C10 120.28(18) . . ? C9 C10 C11 121.18(18) . . ? C12 C11 C10 117.11(17) . . ? C12 C11 C13 119.26(16) . . ? C10 C11 C13 123.59(17) . . ? C11 C12 O1 120.04(16) . . ? C11 C12 C7 123.29(17) . . ? O1 C12 C7 116.67(16) . . ? C14 C13 C11 108.63(16) . . ? C14 C13 C20 111.49(15) . . ? C11 C13 C20 111.65(15) . . ? C14 C13 C21 108.75(14) . . ? C11 C13 C21 108.15(15) . . ? C20 C13 C21 108.08(16) . . ? C15 C14 C19 116.58(18) . . ? C15 C14 C13 124.15(17) . . ? C19 C14 C13 119.15(16) . . ? C16 C15 C14 121.95(19) . . ? C17 C16 C15 119.98(19) . . ? C16 C17 C18 120.43(19) . . ? C19 C18 C17 117.90(17) . . ? C19 C18 P2 120.99(14) . . ? C17 C18 P2 121.11(15) . . ? O1 C19 C18 117.08(16) . . ? O1 C19 C14 119.77(17) . . ? C18 C19 C14 123.15(17) . . ? C23 C22 P2 110.50(13) . . ? C22 C23 C27 125.18(17) . . ? C22 C23 C24 113.40(17) . . ? C27 C23 C24 121.41(16) . . ? C25 C24 C23 113.98(16) . . ? C25 C24 C26 124.96(16) . . ? C23 C24 C26 121.03(17) . . ? C24 C25 P2 110.46(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.415 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.080 #END*** data_ckl-108a #compound % _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H37 Br2 Cl Ni O P2' _chemical_formula_weight 885.65 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' 'Br' 'Br' -0.2901 2.4595 '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' '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.504(1) _cell_length_b 10.503(1) _cell_length_c 19.600(1) _cell_angle_alpha 84.716(1) _cell_angle_beta 89.498(1) _cell_angle_gamma 74.856(1) _cell_volume 1880.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 4143 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Green' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.831 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6297 _exptl_absorpt_correction_T_max 0.8952 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17225 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 26.02 _reflns_number_total 7367 _reflns_number_gt 4859 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0351P)^2^+0.0000P] 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_number_reflns 7367 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 1.27585(4) 0.42546(3) 0.304281(19) 0.03467(12) Uani 1 1 d . . . Br2 Br 1.22363(4) 0.28699(4) 0.11230(2) 0.03802(13) Uani 1 1 d . . . Ni1 Ni 1.14402(5) 0.36361(4) 0.21812(2) 0.02450(13) Uani 1 1 d . . . P1 P 1.05200(10) 0.19910(8) 0.27591(5) 0.0247(2) Uani 1 1 d . . . P2 P 0.94958(10) 0.54688(8) 0.18948(5) 0.0239(2) Uani 1 1 d . . . O1 O 0.8621(3) 0.43461(19) 0.31387(11) 0.0236(6) Uani 1 1 d . . . C1 C 0.9065(4) 0.3526(3) 0.37378(17) 0.0225(8) Uani 1 1 d . . . C2 C 0.9982(4) 0.2291(3) 0.36394(18) 0.0253(8) Uani 1 1 d . . . C3 C 1.0464(4) 0.1442(3) 0.42224(18) 0.0277(9) Uani 1 1 d . . . H3 H 1.1099 0.0589 0.4182 0.033 Uiso 1 1 calc R . . C4 C 1.0023(4) 0.1831(3) 0.48635(19) 0.0314(9) Uani 1 1 d . . . H4 H 1.0359 0.1240 0.5260 0.038 Uiso 1 1 calc R . . C5 C 0.9093(4) 0.3076(3) 0.49356(18) 0.0279(9) Uani 1 1 d . . . H5 H 0.8806 0.3327 0.5380 0.033 Uiso 1 1 calc R . . C6 C 0.8580(4) 0.3957(3) 0.43639(17) 0.0229(8) Uani 1 1 d . . . C7 C 0.7483(4) 0.5309(3) 0.43686(17) 0.0259(9) Uani 1 1 d . . . C8 C 0.7899(4) 0.6221(3) 0.37971(18) 0.0242(8) Uani 1 1 d . . . C9 C 0.7691(4) 0.7593(3) 0.37983(18) 0.0273(9) Uani 1 1 d . . . H9 H 0.7344 0.8011 0.4199 0.033 Uiso 1 1 calc R . . C10 C 0.7982(4) 0.8341(3) 0.32265(19) 0.0302(9) Uani 1 1 d . . . H10 H 0.7806 0.9272 0.3237 0.036 Uiso 1 1 calc R . . C11 C 0.8525(4) 0.7771(3) 0.26370(18) 0.0267(9) Uani 1 1 d . . . H11 H 0.8733 0.8302 0.2250 0.032 Uiso 1 1 calc R . . C12 C 0.8764(4) 0.6401(3) 0.26177(18) 0.0253(9) Uani 1 1 d . . . C13 C 0.8428(4) 0.5695(3) 0.31979(18) 0.0228(8) Uani 1 1 d . . . C14 C 0.5972(4) 0.5134(3) 0.41822(19) 0.0286(9) Uani 1 1 d . . . H14A H 0.5240 0.5986 0.4182 0.043 Uiso 1 1 calc R . . H14B H 0.5714 0.4489 0.4520 0.043 Uiso 1 1 calc R . . H14C H 0.6005 0.4816 0.3726 0.043 Uiso 1 1 calc R . . C15 C 0.7421(4) 0.5856(3) 0.50645(18) 0.0331(9) Uani 1 1 d . . . H15A H 0.8392 0.5923 0.5192 0.050 Uiso 1 1 calc R . . H15B H 0.7098 0.5261 0.5409 0.050 Uiso 1 1 calc R . . H15C H 0.6733 0.6736 0.5040 0.050 Uiso 1 1 calc R . . C16 C 1.1825(4) 0.0369(3) 0.28291(18) 0.0266(9) Uani 1 1 d . . . C17 C 1.1401(4) -0.0755(3) 0.30950(18) 0.0295(9) Uani 1 1 d . . . H17 H 1.0434 -0.0669 0.3251 0.035 Uiso 1 1 calc R . . C18 C 1.2391(5) -0.1997(3) 0.31316(19) 0.0355(10) Uani 1 1 d . . . H18 H 1.2112 -0.2758 0.3322 0.043 Uiso 1 1 calc R . . C19 C 1.3781(5) -0.2114(4) 0.2888(2) 0.0403(11) Uani 1 1 d . . . H19 H 1.4453 -0.2964 0.2909 0.048 Uiso 1 1 calc R . . C20 C 1.4214(4) -0.1022(4) 0.2616(2) 0.0412(11) Uani 1 1 d . . . H20 H 1.5174 -0.1119 0.2450 0.049 Uiso 1 1 calc R . . C21 C 1.3228(4) 0.0226(3) 0.25885(19) 0.0325(9) Uani 1 1 d . . . H21 H 1.3521 0.0983 0.2403 0.039 Uiso 1 1 calc R . . C22 C 0.8953(4) 0.1663(3) 0.23512(17) 0.0238(8) Uani 1 1 d . . . C23 C 0.7521(4) 0.2149(3) 0.2571(2) 0.0317(9) Uani 1 1 d . . . H23 H 0.7340 0.2638 0.2961 0.038 Uiso 1 1 calc R . . C24 C 0.6373(4) 0.1918(3) 0.2220(2) 0.0361(10) Uani 1 1 d . . . H24 H 0.5404 0.2259 0.2368 0.043 Uiso 1 1 calc R . . C25 C 0.6612(4) 0.1200(4) 0.1657(2) 0.0372(10) Uani 1 1 d . . . H25 H 0.5817 0.1031 0.1424 0.045 Uiso 1 1 calc R . . C26 C 0.8024(4) 0.0726(3) 0.14330(19) 0.0324(9) Uani 1 1 d . . . H26 H 0.8198 0.0232 0.1044 0.039 Uiso 1 1 calc R . . C27 C 0.9178(4) 0.0968(3) 0.17737(18) 0.0292(9) Uani 1 1 d . . . H27 H 1.0139 0.0656 0.1611 0.035 Uiso 1 1 calc R . . C28 C 1.0107(4) 0.6661(3) 0.13174(17) 0.0240(8) Uani 1 1 d . . . C29 C 1.1275(4) 0.7102(3) 0.15414(19) 0.0302(9) Uani 1 1 d . . . H29 H 1.1710 0.6772 0.1979 0.036 Uiso 1 1 calc R . . C30 C 1.1800(4) 0.8008(3) 0.1135(2) 0.0341(10) Uani 1 1 d . . . H30 H 1.2582 0.8313 0.1297 0.041 Uiso 1 1 calc R . . C31 C 1.1190(4) 0.8475(3) 0.0492(2) 0.0345(10) Uani 1 1 d . . . H31 H 1.1548 0.9105 0.0212 0.041 Uiso 1 1 calc R . . C32 C 1.0053(4) 0.8019(3) 0.02603(19) 0.0337(10) Uani 1 1 d . . . H32 H 0.9647 0.8324 -0.0185 0.040 Uiso 1 1 calc R . . C33 C 0.9506(4) 0.7127(3) 0.06689(18) 0.0287(9) Uani 1 1 d . . . H33 H 0.8718 0.6830 0.0508 0.034 Uiso 1 1 calc R . . C34 C 0.7922(4) 0.5162(3) 0.14932(18) 0.0258(9) Uani 1 1 d . . . C35 C 0.6521(4) 0.5630(4) 0.1738(2) 0.0375(10) Uani 1 1 d . . . H35 H 0.6368 0.6158 0.2114 0.045 Uiso 1 1 calc R . . C36 C 0.5359(4) 0.5335(4) 0.1440(2) 0.0423(11) Uani 1 1 d . . . H36 H 0.4413 0.5641 0.1621 0.051 Uiso 1 1 calc R . . C37 C 0.5541(5) 0.4605(4) 0.0885(2) 0.0398(10) Uani 1 1 d . . . H37 H 0.4731 0.4410 0.0678 0.048 Uiso 1 1 calc R . . C38 C 0.6930(4) 0.4159(4) 0.0632(2) 0.0397(10) Uani 1 1 d . . . H38 H 0.7070 0.3667 0.0242 0.048 Uiso 1 1 calc R . . C39 C 0.8110(4) 0.4419(3) 0.09362(19) 0.0329(9) Uani 1 1 d . . . H39 H 0.9059 0.4087 0.0763 0.039 Uiso 1 1 calc R . . C40 C 0.4211(14) 0.0228(14) 0.0073(9) 0.1191(15) Uani 0.50 1 d P A 1 H40A H 0.3670 -0.0170 -0.0239 0.143 Uiso 0.50 1 calc PR A 1 H40B H 0.3506 0.0705 0.0397 0.143 Uiso 0.50 1 calc PR A 1 Cl1 Cl 0.5608(8) -0.1120(9) 0.0564(5) 0.1191(15) Uani 0.50 1 d P . 1 Cl2 Cl 0.4908(8) 0.1263(9) -0.0364(5) 0.1191(15) Uani 0.50 1 d P . 1 C41 C 0.3861(13) -0.1251(13) 0.5534(5) 0.046(8) Uani 0.50 1 d P B 1 H41A H 0.4434 -0.1693 0.5942 0.069 Uiso 0.50 1 calc PR B 1 H41B H 0.3728 -0.1917 0.5240 0.069 Uiso 0.50 1 calc PR B 1 H41C H 0.2907 -0.0728 0.5672 0.069 Uiso 0.50 1 calc PR B 1 C42 C 0.4653(8) -0.0349(6) 0.5145(5) 0.046(3) Uani 0.50 1 d PG . 1 C43 C 0.5555(8) 0.0204(7) 0.5510(3) 0.044(6) Uani 0.50 1 d PG . 1 H43 H 0.5682 -0.0009 0.5991 0.052 Uiso 0.50 1 calc PR . 1 C44 C 0.6271(7) 0.1068(7) 0.5172(5) 0.053(3) Uani 0.50 1 d PG . 1 H44 H 0.6888 0.1446 0.5421 0.063 Uiso 0.50 1 calc PR . 1 C45 C 0.6085(9) 0.1380(6) 0.4468(5) 0.078(12) Uani 0.50 1 d PG . 1 H45 H 0.6575 0.1970 0.4236 0.093 Uiso 0.50 1 calc PR . 1 C46 C 0.5183(9) 0.0827(8) 0.4103(3) 0.054(3) Uani 0.50 1 d PG . 1 H46 H 0.5055 0.1040 0.3622 0.064 Uiso 0.50 1 calc PR . 1 C47 C 0.4466(7) -0.0037(7) 0.4441(4) 0.053(7) Uani 0.50 1 d PG . 1 H47 H 0.3849 -0.0415 0.4192 0.063 Uiso 0.50 1 calc PR . 1 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 Br1 0.0396(3) 0.0368(2) 0.0296(2) -0.00563(16) -0.00399(18) -0.01256(18) Br2 0.0348(3) 0.0508(2) 0.0288(2) -0.01202(18) 0.00514(18) -0.00911(19) Ni1 0.0237(3) 0.0252(2) 0.0249(3) -0.00255(18) 0.0024(2) -0.0070(2) P1 0.0242(6) 0.0226(5) 0.0275(6) -0.0034(4) 0.0033(4) -0.0063(4) P2 0.0253(6) 0.0238(5) 0.0220(5) -0.0015(4) 0.0030(4) -0.0058(4) O1 0.0308(15) 0.0207(12) 0.0194(13) -0.0012(9) 0.0014(11) -0.0069(10) C1 0.025(2) 0.0224(18) 0.022(2) 0.0015(14) -0.0003(16) -0.0115(16) C2 0.026(2) 0.0240(18) 0.028(2) -0.0017(15) 0.0002(17) -0.0100(16) C3 0.025(2) 0.0244(18) 0.033(2) 0.0000(16) -0.0002(18) -0.0060(16) C4 0.038(2) 0.031(2) 0.027(2) 0.0065(16) -0.0072(18) -0.0143(18) C5 0.028(2) 0.036(2) 0.022(2) -0.0018(16) 0.0035(17) -0.0128(17) C6 0.021(2) 0.0273(18) 0.023(2) -0.0013(15) 0.0038(16) -0.0104(15) C7 0.029(2) 0.0271(19) 0.022(2) -0.0033(15) 0.0069(17) -0.0077(16) C8 0.020(2) 0.0266(19) 0.025(2) -0.0039(15) 0.0013(16) -0.0055(16) C9 0.024(2) 0.031(2) 0.025(2) -0.0083(16) 0.0037(17) -0.0022(16) C10 0.031(2) 0.0229(18) 0.037(2) -0.0027(16) 0.0011(19) -0.0072(17) C11 0.024(2) 0.0259(19) 0.031(2) 0.0008(15) 0.0018(17) -0.0084(16) C12 0.022(2) 0.0229(18) 0.028(2) -0.0031(15) -0.0001(17) -0.0014(15) C13 0.022(2) 0.0200(17) 0.026(2) -0.0034(14) 0.0026(16) -0.0051(15) C14 0.024(2) 0.035(2) 0.028(2) -0.0050(16) 0.0040(17) -0.0075(17) C15 0.037(2) 0.038(2) 0.026(2) -0.0063(16) 0.0054(18) -0.0122(18) C16 0.026(2) 0.0269(19) 0.027(2) -0.0057(15) -0.0014(17) -0.0055(16) C17 0.030(2) 0.028(2) 0.030(2) -0.0053(16) 0.0004(18) -0.0052(17) C18 0.048(3) 0.026(2) 0.031(2) -0.0015(16) -0.001(2) -0.0081(19) C19 0.043(3) 0.035(2) 0.035(2) -0.0059(18) -0.003(2) 0.007(2) C20 0.027(2) 0.050(3) 0.039(3) -0.004(2) 0.003(2) 0.002(2) C21 0.028(2) 0.035(2) 0.033(2) -0.0044(17) -0.0026(19) -0.0058(18) C22 0.027(2) 0.0207(17) 0.024(2) -0.0010(14) 0.0016(17) -0.0068(15) C23 0.029(2) 0.0273(19) 0.040(2) -0.0079(16) 0.0039(19) -0.0068(17) C24 0.027(2) 0.029(2) 0.053(3) -0.0079(18) 0.004(2) -0.0085(17) C25 0.035(3) 0.041(2) 0.039(3) 0.0002(18) -0.008(2) -0.018(2) C26 0.039(3) 0.032(2) 0.028(2) -0.0026(16) -0.0035(19) -0.0105(18) C27 0.032(2) 0.0274(19) 0.028(2) 0.0002(16) 0.0031(18) -0.0091(17) C28 0.025(2) 0.0232(18) 0.023(2) -0.0022(15) 0.0036(17) -0.0049(16) C29 0.034(2) 0.0306(19) 0.025(2) 0.0016(16) -0.0002(18) -0.0085(18) C30 0.032(2) 0.0277(19) 0.045(3) -0.0037(18) 0.005(2) -0.0118(18) C31 0.042(3) 0.030(2) 0.033(3) 0.0031(17) 0.011(2) -0.0144(19) C32 0.047(3) 0.033(2) 0.019(2) 0.0023(16) 0.0023(19) -0.0100(19) C33 0.027(2) 0.032(2) 0.026(2) -0.0048(16) 0.0008(18) -0.0066(17) C34 0.025(2) 0.0254(18) 0.027(2) 0.0007(15) -0.0003(17) -0.0061(16) C35 0.031(3) 0.048(2) 0.033(2) -0.0065(18) 0.004(2) -0.010(2) C36 0.024(2) 0.060(3) 0.041(3) 0.003(2) 0.000(2) -0.010(2) C37 0.036(3) 0.041(2) 0.046(3) 0.0025(19) -0.011(2) -0.019(2) C38 0.038(3) 0.042(2) 0.041(3) -0.0118(19) -0.007(2) -0.011(2) C39 0.024(2) 0.035(2) 0.039(2) -0.0071(17) 0.0010(19) -0.0060(17) C40 0.084(4) 0.123(2) 0.156(5) -0.040(3) 0.009(3) -0.030(3) Cl1 0.084(4) 0.123(2) 0.156(5) -0.040(3) 0.009(3) -0.030(3) Cl2 0.084(4) 0.123(2) 0.156(5) -0.040(3) 0.009(3) -0.030(3) C41 0.057(18) 0.043(9) 0.030(11) 0.002(7) 0.024(10) -0.003(10) C42 0.031(6) 0.031(5) 0.074(8) -0.012(5) 0.028(5) -0.002(4) C43 0.033(13) 0.036(7) 0.053(13) 0.006(7) 0.006(10) 0.003(8) C44 0.041(6) 0.051(5) 0.060(7) -0.008(5) -0.021(5) 0.002(5) C45 0.056(19) 0.043(12) 0.14(3) -0.024(12) 0.001(15) -0.022(11) C46 0.057(7) 0.053(6) 0.046(7) 0.000(5) -0.001(6) -0.007(5) C47 0.042(15) 0.067(10) 0.050(12) -0.045(8) -0.019(10) -0.002(9) _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 Br1 Ni1 2.3468(6) . ? Br2 Ni1 2.3418(5) . ? Ni1 P2 2.3229(9) . ? Ni1 P1 2.3334(11) . ? P1 C16 1.820(3) . ? P1 C22 1.821(4) . ? P1 C2 1.827(4) . ? P2 C34 1.811(4) . ? P2 C28 1.815(4) . ? P2 C12 1.825(3) . ? O1 C1 1.389(4) . ? O1 C13 1.396(4) . ? C1 C6 1.381(4) . ? C1 C2 1.390(4) . ? C2 C3 1.385(5) . ? C3 C4 1.385(5) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C7 1.527(4) . ? C7 C15 1.523(5) . ? C7 C8 1.524(5) . ? C7 C14 1.545(5) . ? C8 C13 1.379(5) . ? C8 C9 1.402(5) . ? C9 C10 1.377(5) . ? C9 H9 0.9500 . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 C12 1.401(4) . ? C11 H11 0.9500 . ? C12 C13 1.381(5) . ? 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 C21 1.386(5) . ? C16 C17 1.399(5) . ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C18 C19 1.379(6) . ? C18 H18 0.9500 . ? C19 C20 1.378(6) . ? C19 H19 0.9500 . ? C20 C21 1.395(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C27 1.388(5) . ? C22 C23 1.402(5) . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.377(5) . ? C24 H24 0.9500 . ? C25 C26 1.387(5) . ? C25 H25 0.9500 . ? C26 C27 1.379(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.391(5) . ? C28 C29 1.397(5) . ? C29 C30 1.375(5) . ? C29 H29 0.9500 . ? C30 C31 1.384(5) . ? C30 H30 0.9500 . ? C31 C32 1.387(5) . ? C31 H31 0.9500 . ? C32 C33 1.378(5) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.383(5) . ? C34 C35 1.391(5) . ? C35 C36 1.371(6) . ? C35 H35 0.9500 . ? C36 C37 1.372(5) . ? C36 H36 0.9500 . ? C37 C38 1.384(6) . ? C37 H37 0.9500 . ? C38 C39 1.375(5) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 Cl2 1.60(2) . ? C40 Cl1 1.866(18) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? Cl1 Cl2 0.684(9) 2_655 ? Cl1 C40 1.527(19) 2_655 ? Cl2 Cl1 0.684(9) 2_655 ? Cl2 C40 1.624(17) 2_655 ? C41 C42 1.508(10) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C42 1.211(11) 2_656 ? C42 C43 1.291(18) 2_656 ? C42 C47 1.331(18) 2_656 ? C42 C43 1.3900 . ? C42 C47 1.3900 . ? C42 C44 1.473(16) 2_656 ? C42 C46 1.509(17) 2_656 ? C42 C45 1.573(11) 2_656 ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ni1 P1 108.00(4) . . ? P2 Ni1 Br2 103.93(3) . . ? P1 Ni1 Br2 106.02(3) . . ? P2 Ni1 Br1 105.58(3) . . ? P1 Ni1 Br1 102.88(3) . . ? Br2 Ni1 Br1 129.20(3) . . ? C16 P1 C22 102.31(16) . . ? C16 P1 C2 104.86(16) . . ? C22 P1 C2 105.69(16) . . ? C16 P1 Ni1 112.94(13) . . ? C22 P1 Ni1 115.46(11) . . ? C2 P1 Ni1 114.33(11) . . ? C34 P2 C28 107.10(16) . . ? C34 P2 C12 104.71(16) . . ? C28 P2 C12 103.73(15) . . ? C34 P2 Ni1 116.65(11) . . ? C28 P2 Ni1 109.53(11) . . ? C12 P2 Ni1 114.12(11) . . ? C1 O1 C13 115.0(2) . . ? C6 C1 O1 120.1(3) . . ? C6 C1 C2 125.3(3) . . ? O1 C1 C2 114.5(3) . . ? C3 C2 C1 116.7(3) . . ? C3 C2 P1 126.5(3) . . ? C1 C2 P1 116.7(2) . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C1 C6 C5 116.1(3) . . ? C1 C6 C7 118.0(3) . . ? C5 C6 C7 125.8(3) . . ? C15 C7 C8 112.5(3) . . ? C15 C7 C6 112.2(3) . . ? C8 C7 C6 107.2(3) . . ? C15 C7 C14 109.7(3) . . ? C8 C7 C14 107.7(3) . . ? C6 C7 C14 107.4(3) . . ? C13 C8 C9 115.6(3) . . ? C13 C8 C7 118.3(3) . . ? C9 C8 C7 125.9(3) . . ? C10 C9 C8 120.9(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 121.6(3) . . ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 . . ? C10 C11 C12 119.2(3) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C13 C12 C11 117.1(3) . . ? C13 C12 P2 117.3(2) . . ? C11 C12 P2 125.6(3) . . ? C8 C13 C12 125.5(3) . . ? C8 C13 O1 119.8(3) . . ? C12 C13 O1 114.7(3) . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C7 C15 H15A 109.5 . . ? C7 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C7 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 119.3(3) . . ? C21 C16 P1 120.3(3) . . ? C17 C16 P1 120.4(3) . . ? C18 C17 C16 120.2(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 119.4(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 121.3(3) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C16 C21 C20 120.5(4) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C27 C22 C23 118.5(4) . . ? C27 C22 P1 118.5(3) . . ? C23 C22 P1 122.8(3) . . ? C24 C23 C22 120.0(3) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.4(4) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C22 120.9(3) . . ? C26 C27 H27 119.5 . . ? C22 C27 H27 119.5 . . ? C33 C28 C29 119.0(3) . . ? C33 C28 P2 123.9(3) . . ? C29 C28 P2 117.1(3) . . ? C30 C29 C28 120.7(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.1(4) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C30 C31 C32 119.5(4) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C28 120.0(4) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C39 C34 C35 118.6(4) . . ? C39 C34 P2 119.5(3) . . ? C35 C34 P2 121.8(3) . . ? C36 C35 C34 120.4(4) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 121.1(4) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C36 C37 C38 118.6(4) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? C39 C38 C37 120.9(4) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C34 120.3(3) . . ? C38 C39 H39 119.8 . . ? C34 C39 H39 119.8 . . ? Cl2 C40 Cl1 112.7(8) . . ? Cl2 C40 H40A 109.1 . . ? Cl1 C40 H40A 109.1 . . ? Cl2 C40 H40B 109.1 . . ? Cl1 C40 H40B 109.1 . . ? H40A C40 H40B 107.8 . . ? Cl2 Cl1 C40 83(2) 2_655 2_655 ? Cl2 Cl1 C40 59.1(16) 2_655 . ? C40 Cl1 C40 50.7(9) 2_655 . ? Cl1 Cl2 C40 71.7(18) 2_655 . ? Cl1 Cl2 C40 99.7(17) 2_655 2_655 ? C40 Cl2 C40 54.9(9) . 2_655 ? C42 C42 C43 67.4(10) 2_656 2_656 ? C42 C42 C47 66.1(9) 2_656 2_656 ? C43 C42 C47 133.4(9) 2_656 2_656 ? C42 C42 C43 59.0(7) 2_656 . ? C43 C42 C43 126.4(7) 2_656 . ? C47 C42 C43 7.9(6) 2_656 . ? C42 C42 C47 61.1(7) 2_656 . ? C43 C42 C47 7.3(6) 2_656 . ? C47 C42 C47 127.2(6) 2_656 . ? C43 C42 C47 120.0 . . ? C42 C42 C44 127.2(16) 2_656 2_656 ? C43 C42 C44 60.0(8) 2_656 2_656 ? C47 C42 C44 164.9(12) 2_656 2_656 ? C43 C42 C44 172.9(11) . 2_656 ? C47 C42 C44 66.6(11) . 2_656 ? C42 C42 C41 176.7(13) 2_656 . ? C43 C42 C41 115.1(7) 2_656 . ? C47 C42 C41 111.2(8) 2_656 . ? C43 C42 C41 118.4(8) . . ? C47 C42 C41 121.6(8) . . ? C44 C42 C41 55.2(6) 2_656 . ? C42 C42 C46 124.2(16) 2_656 2_656 ? C43 C42 C46 166.5(10) 2_656 2_656 ? C47 C42 C46 58.2(8) 2_656 2_656 ? C43 C42 C46 65.6(10) . 2_656 ? C47 C42 C46 173.8(9) . 2_656 ? C44 C42 C46 107.7(7) 2_656 2_656 ? C41 C42 C46 53.0(6) . 2_656 ? C42 C42 C45 173.6(14) 2_656 2_656 ? C43 C42 C45 114.1(11) 2_656 2_656 ? C47 C42 C45 111.7(11) 2_656 2_656 ? C43 C42 C45 119.2(12) . 2_656 ? C47 C42 C45 120.8(12) . 2_656 ? C44 C42 C45 54.2(4) 2_656 2_656 ? C41 C42 C45 4.3(5) . 2_656 ? C46 C42 C45 53.6(5) 2_656 2_656 ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C42 120.0 . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.902 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.090 #END*** data_gm334 #compound 6 #Louis Ricard, Apr 22 2007 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H26 Br2 Ni P2' _chemical_formula_sum 'C24 H26 Br2 Ni P2' _chemical_formula_weight 594.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' .3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'C2221 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 10.3650(10) _cell_length_b 14.1210(10) _cell_length_c 32.7530(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4793.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 3511 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description 'block' _exptl_crystal_colour 'dark red ' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 4.286 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.6273 _exptl_absorpt_correction_T_max 0.6273 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13180 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 30.03 _reflns_number_total 6833 _reflns_number_gt 5863 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Phenyl rings of the disordered part of the molecule were refined as rigid groups. Refinement of the disorder ratio led to a value close to 1/2 and was fixed to this value in the final refinement cycles. The Flack parameter was refined using TWIN BASF instructions. ; _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^)+(0.0186P)^2^+0.0000P] 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 0.00032(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 0.226(6) _refine_ls_number_reflns 6833 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0597 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Br1 Br 0.79109(3) 0.48872(2) 0.090709(7) 0.03316(7) Uani 1 1 d . A . Br2 Br 0.99658(3) 0.24650(2) 0.158337(8) 0.03342(7) Uani 1 1 d . A . Ni1 Ni 0.90070(3) 0.37530(3) 0.127129(9) 0.02698(8) Uani 1 1 d . . . P1 P 0.76238(6) 0.38998(5) 0.178590(18) 0.02349(14) Uani 1 1 d . A . C1 C 0.6923(2) 0.50299(18) 0.19051(7) 0.0260(5) Uani 1 1 d . . . H1 H 0.6416 0.5395 0.1722 0.031 Uiso 1 1 calc R A . C2 C 0.7212(3) 0.52858(18) 0.22867(7) 0.0270(5) Uani 1 1 d . A . C3 C 0.7981(3) 0.45617(17) 0.25136(8) 0.0275(5) Uani 1 1 d . . . C4 C 0.8239(2) 0.37816(19) 0.22986(7) 0.0258(5) Uani 1 1 d . A . H4 H 0.8682 0.3243 0.2401 0.031 Uiso 1 1 calc R . . C5 C 0.6827(3) 0.61911(19) 0.24917(9) 0.0381(6) Uani 1 1 d . . . H5A H 0.6419 0.6612 0.2292 0.057 Uiso 1 1 calc R A . H5B H 0.7595 0.6500 0.2605 0.057 Uiso 1 1 calc R . . H5C H 0.6217 0.6054 0.2712 0.057 Uiso 1 1 calc R . . C6 C 0.8447(3) 0.4761(2) 0.29405(7) 0.0435(8) Uani 1 1 d . A . H6A H 0.8833 0.4186 0.3056 0.065 Uiso 1 1 calc R . . H6B H 0.7718 0.4960 0.3111 0.065 Uiso 1 1 calc R . . H6C H 0.9094 0.5267 0.2933 0.065 Uiso 1 1 calc R . . C7 C 0.6258(3) 0.30983(18) 0.17265(7) 0.0273(6) Uani 1 1 d . . . C8 C 0.6317(3) 0.2352(2) 0.14529(9) 0.0426(8) Uani 1 1 d . A . H8 H 0.7081 0.2244 0.1300 0.051 Uiso 1 1 calc R . . C9 C 0.5252(3) 0.1759(2) 0.14022(9) 0.0487(9) Uani 1 1 d . . . H9 H 0.5305 0.1238 0.1219 0.058 Uiso 1 1 calc R A . C10 C 0.4145(3) 0.1916(2) 0.16109(9) 0.0435(8) Uani 1 1 d . A . H10 H 0.3416 0.1520 0.1568 0.052 Uiso 1 1 calc R . . C11 C 0.4084(3) 0.2656(3) 0.18868(10) 0.0503(9) Uani 1 1 d . . . H11 H 0.3315 0.2759 0.2038 0.060 Uiso 1 1 calc R A . C12 C 0.5129(3) 0.3244(2) 0.19433(9) 0.0439(8) Uani 1 1 d . A . H12 H 0.5074 0.3753 0.2132 0.053 Uiso 1 1 calc R . . P2 P 1.06140(14) 0.38665(12) 0.08315(4) 0.0214(3) Uani 0.50 1 d P A 1 C13 C 1.0928(6) 0.4945(4) 0.05634(16) 0.0242(11) Uani 0.50 1 d P A 1 H13 H 1.0334 0.5266 0.0391 0.029 Uiso 0.50 1 calc PR A 1 C14 C 1.2143(8) 0.5231(6) 0.0645(2) 0.0279(16) Uani 0.50 1 d P A 1 C15 C 1.2863(6) 0.4590(4) 0.09157(16) 0.0263(11) Uani 0.50 1 d P A 1 C16 C 1.2209(6) 0.3799(5) 0.1024(2) 0.0267(15) Uani 0.50 1 d P A 1 H16 H 1.2551 0.3289 0.1180 0.032 Uiso 0.50 1 calc PR A 1 C17 C 1.2728(8) 0.6143(5) 0.0472(2) 0.0433(17) Uani 0.50 1 d P A 1 H17A H 1.2082 0.6473 0.0306 0.065 Uiso 0.50 1 calc PR A 1 H17B H 1.3478 0.5987 0.0303 0.065 Uiso 0.50 1 calc PR A 1 H17C H 1.2998 0.6554 0.0698 0.065 Uiso 0.50 1 calc PR A 1 C18 C 1.4234(7) 0.4819(6) 0.1039(2) 0.047(2) Uani 0.50 1 d P A 1 H18A H 1.4653 0.4247 0.1144 0.070 Uiso 0.50 1 calc PR A 1 H18B H 1.4227 0.5307 0.1252 0.070 Uiso 0.50 1 calc PR A 1 H18C H 1.4711 0.5052 0.0801 0.070 Uiso 0.50 1 calc PR A 1 C19 C 1.0488(4) 0.2963(3) 0.04307(10) 0.0232(11) Uani 0.50 1 d PG A 1 C20 C 0.9674(4) 0.3128(3) 0.01010(13) 0.0432(14) Uani 0.50 1 d PG A 1 H20 H 0.9154 0.3682 0.0094 0.052 Uiso 0.50 1 calc PR A 1 C21 C 0.9621(4) 0.2483(4) -0.02191(11) 0.0432(14) Uani 0.50 1 d PG A 1 H21 H 0.9065 0.2596 -0.0444 0.052 Uiso 0.50 1 calc PR A 1 C22 C 1.0383(5) 0.1673(3) -0.02094(11) 0.0512(19) Uani 0.50 1 d PG A 1 H22 H 1.0347 0.1232 -0.0428 0.061 Uiso 0.50 1 calc PR A 1 C23 C 1.1197(5) 0.1508(3) 0.01202(14) 0.0391(17) Uani 0.50 1 d PG A 1 H23 H 1.1717 0.0955 0.0127 0.047 Uiso 0.50 1 calc PR A 1 C24 C 1.1249(4) 0.2153(3) 0.04403(11) 0.0312(15) Uani 0.50 1 d PG A 1 H24 H 1.1806 0.2041 0.0666 0.037 Uiso 0.50 1 calc PR A 1 P2A P 1.02900(15) 0.34764(12) 0.07333(5) 0.0245(3) Uani 0.50 1 d P A 2 C13A C 0.9654(6) 0.3555(5) 0.02233(14) 0.0305(14) Uani 0.50 1 d P A 2 H13A H 0.9186 0.4084 0.0123 0.037 Uiso 0.50 1 calc PR A 2 C14A C 0.9911(7) 0.2799(5) 0.0006(2) 0.0318(14) Uani 0.50 1 d P A 2 C15A C 1.0722(6) 0.2092(5) 0.02376(18) 0.0306(13) Uani 0.50 1 d P A 2 C16A C 1.0990(6) 0.2331(4) 0.06135(17) 0.0267(12) Uani 0.50 1 d P A 2 H16A H 1.1482 0.1958 0.0798 0.032 Uiso 0.50 1 calc PR A 2 C17A C 0.9538(7) 0.2619(5) -0.04186(17) 0.0470(14) Uani 0.50 1 d P A 2 H17D H 0.8989 0.3137 -0.0516 0.070 Uiso 0.50 1 calc PR A 2 H17E H 0.9061 0.2021 -0.0435 0.070 Uiso 0.50 1 calc PR A 2 H17F H 1.0313 0.2579 -0.0589 0.070 Uiso 0.50 1 calc PR A 2 C18A C 1.1078(8) 0.1178(6) 0.0035(2) 0.0470(14) Uani 0.50 1 d P A 2 H18D H 1.1684 0.0829 0.0208 0.070 Uiso 0.50 1 calc PR A 2 H18E H 1.1485 0.1310 -0.0229 0.070 Uiso 0.50 1 calc PR A 2 H18F H 1.0300 0.0796 -0.0008 0.070 Uiso 0.50 1 calc PR A 2 C19A C 1.1630(4) 0.4292(3) 0.07774(13) 0.0310(13) Uani 0.50 1 d PG A 2 C20A C 1.2637(5) 0.4055(3) 0.10385(16) 0.038(2) Uani 0.50 1 d PG A 2 H20A H 1.2608 0.3479 0.1188 0.045 Uiso 0.50 1 calc PR A 2 C21A C 1.3686(4) 0.4660(4) 0.10803(17) 0.057(3) Uani 0.50 1 d PG A 2 H21A H 1.4374 0.4498 0.1259 0.068 Uiso 0.50 1 calc PR A 2 C22A C 1.3728(4) 0.5503(4) 0.08612(18) 0.062(2) Uani 0.50 1 d PG A 2 H22A H 1.4445 0.5916 0.0890 0.075 Uiso 0.50 1 calc PR A 2 C23A C 1.2721(6) 0.5740(3) 0.06001(18) 0.058(2) Uani 0.50 1 d PG A 2 H23A H 1.2750 0.6315 0.0450 0.069 Uiso 0.50 1 calc PR A 2 C24A C 1.1672(5) 0.5134(4) 0.05582(15) 0.042(2) Uani 0.50 1 d PG A 2 H24A H 1.0984 0.5297 0.0380 0.051 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.04239(17) 0.03226(15) 0.02483(13) 0.00363(11) -0.00157(12) 0.00707(13) Br2 0.03951(16) 0.03044(14) 0.03031(14) 0.00400(10) 0.00436(12) 0.00822(13) Ni1 0.02562(16) 0.03500(19) 0.02032(15) 0.00558(13) 0.00176(13) 0.00325(14) P1 0.0284(4) 0.0218(3) 0.0203(3) -0.0003(2) 0.0009(2) -0.0006(3) C1 0.0283(14) 0.0270(14) 0.0227(11) 0.0017(10) -0.0002(10) 0.0014(11) C2 0.0294(14) 0.0246(14) 0.0271(13) -0.0005(10) 0.0051(11) 0.0015(11) C3 0.0326(14) 0.0295(13) 0.0205(11) 0.0004(10) -0.0010(12) -0.0006(11) C4 0.0289(14) 0.0236(13) 0.0249(12) 0.0019(10) 0.0011(10) 0.0006(11) C5 0.0527(18) 0.0328(15) 0.0289(13) -0.0076(13) -0.0032(14) 0.0117(13) C6 0.059(2) 0.049(2) 0.0228(14) -0.0057(13) -0.0058(13) 0.0085(16) C7 0.0320(16) 0.0253(14) 0.0248(13) 0.0018(10) 0.0027(11) -0.0035(11) C8 0.0368(16) 0.0367(19) 0.0541(18) -0.0196(14) 0.0125(14) -0.0094(14) C9 0.051(2) 0.041(2) 0.054(2) -0.0185(15) 0.0045(16) -0.0146(16) C10 0.0419(18) 0.0410(18) 0.0476(18) 0.0014(14) -0.0001(15) -0.0204(15) C11 0.0367(18) 0.060(2) 0.0544(19) -0.0131(17) 0.0170(16) -0.0169(17) C12 0.0466(19) 0.0456(19) 0.0396(16) -0.0154(13) 0.0161(15) -0.0163(16) P2 0.0240(7) 0.0226(8) 0.0175(7) 0.0001(6) -0.0022(5) -0.0014(6) C13 0.028(3) 0.026(3) 0.019(2) -0.003(2) -0.001(2) -0.004(3) C14 0.035(4) 0.028(3) 0.021(3) -0.006(2) 0.001(3) -0.005(3) C15 0.025(3) 0.034(3) 0.020(3) -0.008(2) -0.003(3) -0.003(3) C16 0.027(4) 0.031(3) 0.022(3) -0.006(2) -0.006(3) -0.001(3) C17 0.044(4) 0.035(4) 0.051(4) 0.006(3) 0.005(3) -0.015(3) C18 0.035(5) 0.054(5) 0.051(5) -0.005(4) 0.002(4) -0.011(4) C19 0.023(3) 0.027(3) 0.020(2) 0.003(2) 0.0073(19) -0.005(2) C20 0.056(3) 0.050(4) 0.023(3) -0.012(2) -0.016(2) 0.000(3) C21 0.056(3) 0.050(4) 0.023(3) -0.012(2) -0.016(2) 0.000(3) C22 0.067(5) 0.054(5) 0.032(3) -0.020(3) 0.007(3) -0.016(4) C23 0.041(4) 0.041(5) 0.035(4) -0.014(3) -0.003(3) -0.004(3) C24 0.026(4) 0.037(4) 0.030(4) -0.006(3) 0.003(3) 0.003(3) P2A 0.0280(9) 0.0275(8) 0.0181(7) 0.0039(6) 0.0010(6) 0.0015(6) C13A 0.037(3) 0.042(4) 0.013(3) 0.006(2) 0.000(2) -0.004(3) C14A 0.039(3) 0.032(3) 0.025(3) 0.004(2) -0.002(3) -0.010(3) C15A 0.029(3) 0.034(3) 0.028(3) 0.000(3) 0.003(3) -0.001(3) C16A 0.023(3) 0.031(3) 0.026(3) 0.005(2) 0.004(2) 0.000(2) C17A 0.062(3) 0.053(3) 0.026(2) -0.008(2) -0.015(2) 0.007(3) C18A 0.062(3) 0.053(3) 0.026(2) -0.008(2) -0.015(2) 0.007(3) C19A 0.038(3) 0.032(3) 0.023(3) -0.011(2) 0.002(2) -0.014(3) C20A 0.029(5) 0.055(7) 0.029(4) -0.008(4) -0.003(3) -0.003(4) C21A 0.041(6) 0.082(8) 0.048(4) -0.013(4) 0.015(5) -0.007(5) C22A 0.046(5) 0.065(5) 0.077(5) -0.032(4) 0.020(4) -0.027(4) C23A 0.066(6) 0.034(5) 0.073(7) -0.010(4) 0.012(5) -0.020(5) C24A 0.052(7) 0.039(5) 0.036(5) 0.005(4) -0.006(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Ni1 2.2976(4) . ? Br2 Ni1 2.3109(4) . ? Ni1 P2 2.2080(14) . ? Ni1 P1 2.2225(7) . ? Ni1 P2A 2.2417(15) . ? P1 C1 1.796(3) . ? P1 C4 1.804(2) . ? P1 C7 1.822(3) . ? C1 C2 1.335(3) . ? C1 H1 0.9500 . ? C2 C3 1.494(3) . ? C2 C5 1.498(3) . ? C3 C4 1.334(3) . ? C3 C6 1.506(4) . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C12 1.385(4) . ? C7 C8 1.385(4) . ? C8 C9 1.396(4) . ? C8 H8 0.9500 . ? C9 C10 1.354(4) . ? C9 H9 0.9500 . ? C10 C11 1.383(4) . ? C10 H10 0.9500 . ? C11 C12 1.378(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? P2 C16 1.773(7) . ? P2 C13 1.788(6) . ? P2 C19 1.835(3) . ? C13 C14 1.349(9) . ? C13 H13 0.9500 . ? C14 C15 1.471(9) . ? C14 C17 1.532(9) . ? C15 C16 1.354(8) . ? C15 C18 1.512(8) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C20 H20 0.9500 . ? C21 C22 1.3900 . ? C21 H21 0.9500 . ? C22 C23 1.3900 . ? C22 H22 0.9500 . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? P2A C13A 1.799(5) . ? P2A C19A 1.810(4) . ? P2A C16A 1.815(6) . ? C13A C14A 1.309(8) . ? C13A H13A 0.9500 . ? C14A C17A 1.467(9) . ? C14A C15A 1.509(9) . ? C15A C16A 1.307(7) . ? C15A C18A 1.498(9) . ? C16A H16A 0.9500 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A C20A 1.3900 . ? C19A C24A 1.3900 . ? C20A C21A 1.3900 . ? C20A H20A 0.9500 . ? C21A C22A 1.3900 . ? C21A H21A 0.9500 . ? C22A C23A 1.3900 . ? C22A H22A 0.9500 . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A H24A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Ni1 P1 167.07(5) . . ? P2 Ni1 P2A 18.63(4) . . ? P1 Ni1 P2A 174.26(5) . . ? P2 Ni1 Br1 89.06(4) . . ? P1 Ni1 Br1 90.56(2) . . ? P2A Ni1 Br1 90.38(4) . . ? P2 Ni1 Br2 91.22(4) . . ? P1 Ni1 Br2 90.88(2) . . ? P2A Ni1 Br2 87.45(4) . . ? Br1 Ni1 Br2 172.28(2) . . ? C1 P1 C4 91.31(12) . . ? C1 P1 C7 105.12(12) . . ? C4 P1 C7 108.44(11) . . ? C1 P1 Ni1 120.57(8) . . ? C4 P1 Ni1 117.99(9) . . ? C7 P1 Ni1 111.23(8) . . ? C2 C1 P1 110.69(19) . . ? C2 C1 H1 124.7 . . ? P1 C1 H1 124.7 . . ? C1 C2 C3 113.6(2) . . ? C1 C2 C5 126.2(2) . . ? C3 C2 C5 120.2(2) . . ? C4 C3 C2 114.2(2) . . ? C4 C3 C6 125.4(3) . . ? C2 C3 C6 120.3(2) . . ? C3 C4 P1 110.1(2) . . ? C3 C4 H4 124.9 . . ? P1 C4 H4 124.9 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C7 C8 118.8(3) . . ? C12 C7 P1 120.6(2) . . ? C8 C7 P1 120.5(2) . . ? C7 C8 C9 120.0(3) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.8(3) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 119.5(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.4(3) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C16 P2 C13 92.9(3) . . ? C16 P2 C19 106.5(3) . . ? C13 P2 C19 104.7(2) . . ? C16 P2 Ni1 117.8(3) . . ? C13 P2 Ni1 121.30(19) . . ? C19 P2 Ni1 111.26(15) . . ? C14 C13 P2 109.1(6) . . ? C14 C13 H13 125.4 . . ? P2 C13 H13 125.4 . . ? C13 C14 C15 114.1(7) . . ? C13 C14 C17 123.3(8) . . ? C15 C14 C17 122.6(6) . . ? C16 C15 C14 114.3(6) . . ? C16 C15 C18 125.2(6) . . ? C14 C15 C18 120.4(7) . . ? C15 C16 P2 109.2(5) . . ? C15 C16 H16 125.4 . . ? P2 C16 H16 125.4 . . ? C20 C19 C24 120.0 . . ? C20 C19 P2 118.9(2) . . ? C24 C19 P2 121.0(2) . . ? C21 C20 C19 120.0 . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 120.0 . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.0 . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C13A P2A C19A 108.4(3) . . ? C13A P2A C16A 90.0(3) . . ? C19A P2A C16A 106.1(3) . . ? C13A P2A Ni1 120.1(2) . . ? C19A P2A Ni1 106.35(16) . . ? C16A P2A Ni1 124.20(18) . . ? C14A C13A P2A 112.3(6) . . ? C14A C13A H13A 123.9 . . ? P2A C13A H13A 123.9 . . ? C13A C14A C17A 127.0(7) . . ? C13A C14A C15A 112.4(6) . . ? C17A C14A C15A 120.6(6) . . ? C16A C15A C18A 126.0(6) . . ? C16A C15A C14A 114.9(6) . . ? C18A C15A C14A 119.0(6) . . ? C15A C16A P2A 110.4(5) . . ? C15A C16A H16A 124.8 . . ? P2A C16A H16A 124.8 . . ? C14A C17A H17D 109.5 . . ? C14A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C14A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C15A C18A H18D 109.5 . . ? C15A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C15A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C20A C19A C24A 120.0 . . ? C20A C19A P2A 118.2(3) . . ? C24A C19A P2A 121.8(3) . . ? C21A C20A C19A 120.0 . . ? C21A C20A H20A 120.0 . . ? C19A C20A H20A 120.0 . . ? C22A C21A C20A 120.0 . . ? C22A C21A H21A 120.0 . . ? C20A C21A H21A 120.0 . . ? C21A C22A C23A 120.0 . . ? C21A C22A H22A 120.0 . . ? C23A C22A H22A 120.0 . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C19A 120.0 . . ? C23A C24A H24A 120.0 . . ? C19A C24A H24A 120.0 . . ? _diffrn_measured_fraction_theta_max .989 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full .989 _refine_diff_density_max .386 _refine_diff_density_min -.455 _refine_diff_density_rms .066 #END***