# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Ekkehardt Hahn' 'Roland Frohlich' 'Tania Pape' 'Christian Radloff' _publ_contact_author_name 'Ekkehardt Hahn' _publ_contact_author_email Ekkehardt _publ_section_title ; Supramolecular structures from mono and dimetalated biscarbene ligands ; # Attachment 'cif-1a.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 728536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 I2 N4 O2' _chemical_formula_weight 506.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 6.8318(3) _cell_length_b 12.6696(6) _cell_length_c 20.2465(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1752.46(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 3.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6521 _exptl_absorpt_correction_T_max 0.9893 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.687126 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20161 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 31.98 _reflns_number_total 2909 _reflns_number_gt 2338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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^)+(0.0196P)^2^+1.2532P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2909 _refine_ls_number_parameters 93 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0489 _refine_ls_wR_factor_gt 0.0452 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 I1 I 0.998644(15) 0.768214(9) 0.140202(5) 0.02516(4) Uani 1 1 d . . . C1 C 0.2781(2) 0.52949(12) 0.12878(8) 0.0207(3) Uani 1 1 d . . . H1 H 0.3585 0.5390 0.1666 0.025 Uiso 1 1 calc R . . N1 N 0.31547(18) 0.56969(10) 0.06923(6) 0.0196(2) Uani 1 1 d . . . N2 N 0.11288(19) 0.47426(10) 0.12782(6) 0.0197(2) Uani 1 1 d . . . C2 C 0.1645(2) 0.54101(11) 0.02688(7) 0.0179(3) Uani 1 1 d . . . C3 C 0.0353(2) 0.47910(12) 0.06454(7) 0.0183(3) Uani 1 1 d . . . C4 C -0.1349(2) 0.43472(11) 0.03921(7) 0.0192(3) Uani 1 1 d . . . H4 H -0.2217 0.3923 0.0645 0.023 Uiso 1 1 calc R . . C5 C 0.4714(2) 0.64468(15) 0.05356(9) 0.0264(3) Uani 1 1 d . . . H5A H 0.4170 0.7162 0.0516 0.040 Uiso 1 1 calc R . . H5B H 0.5293 0.6265 0.0107 0.040 Uiso 1 1 calc R . . H5C H 0.5725 0.6416 0.0879 0.040 Uiso 1 1 calc R . . C6 C 0.0281(2) 0.41652(14) 0.18354(8) 0.0258(3) Uani 1 1 d . . . H6A H 0.0357 0.3405 0.1749 0.039 Uiso 1 1 calc R . . H6B H -0.1091 0.4372 0.1891 0.039 Uiso 1 1 calc R . . H6C H 0.1011 0.4332 0.2239 0.039 Uiso 1 1 calc R . . O1 O 0.6300(2) 0.61416(11) 0.21791(6) 0.0352(3) Uani 1 1 d . . . H1P H 0.7287 0.6428 0.2063 0.042 Uiso 1 1 d R . . H1O H 0.6000 0.6556 0.2457 0.042 Uiso 1 1 d 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 I1 0.02361(6) 0.02449(7) 0.02737(7) 0.00295(4) 0.00015(4) 0.00318(4) C1 0.0211(7) 0.0207(7) 0.0203(6) -0.0021(5) -0.0023(5) 0.0004(5) N1 0.0186(6) 0.0196(6) 0.0207(6) -0.0016(5) -0.0021(5) -0.0016(4) N2 0.0219(6) 0.0201(6) 0.0172(5) -0.0001(5) -0.0022(5) -0.0002(5) C2 0.0170(6) 0.0169(6) 0.0198(6) -0.0023(5) -0.0020(5) -0.0009(5) C3 0.0204(7) 0.0174(6) 0.0172(6) -0.0012(5) -0.0014(5) 0.0006(5) C4 0.0196(6) 0.0178(6) 0.0204(7) 0.0001(5) 0.0006(5) -0.0012(5) C5 0.0220(8) 0.0293(8) 0.0279(8) -0.0012(6) -0.0011(6) -0.0080(6) C6 0.0295(8) 0.0288(8) 0.0192(7) 0.0025(6) 0.0002(6) -0.0033(6) O1 0.0353(7) 0.0388(7) 0.0314(6) -0.0055(5) 0.0044(5) -0.0107(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.3283(19) . ? C1 N1 1.334(2) . ? N1 C2 1.3895(18) . ? N1 C5 1.4622(19) . ? N2 C3 1.3878(18) . ? N2 C6 1.464(2) . ? C2 C4 1.388(2) 5_565 ? C2 C3 1.406(2) . ? C3 C4 1.390(2) . ? C4 C2 1.388(2) 5_565 ? 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 110.52(13) . . ? C1 N1 C2 108.43(12) . . ? C1 N1 C5 125.70(13) . . ? C2 N1 C5 125.23(13) . . ? C1 N2 C3 108.35(13) . . ? C1 N2 C6 126.02(13) . . ? C3 N2 C6 125.62(13) . . ? C4 C2 N1 130.19(13) 5_565 . ? C4 C2 C3 123.71(13) 5_565 . ? N1 C2 C3 106.10(12) . . ? N2 C3 C4 129.97(14) . . ? N2 C3 C2 106.59(12) . . ? C4 C3 C2 123.44(13) . . ? C2 C4 C3 112.84(13) 5_565 . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 31.98 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.454 _refine_diff_density_min -0.656 _refine_diff_density_rms 0.083 # Attachment 'cif-1b.cif' data_sad2 _database_code_depnum_ccdc_archive 'CCDC 728537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 Br2 N4' _chemical_formula_weight 432.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.1257(7) _cell_length_b 14.067(2) _cell_length_c 12.8338(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.602(8) _cell_angle_gamma 90.00 _cell_volume 909.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 5.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5499 _exptl_absorpt_correction_T_max 0.8485 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports Maximum and minimum effective transmission: 1.000000 0.672886 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4364 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_av_sigmaI/netI 0.1978 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.71 _diffrn_reflns_theta_max 71.76 _reflns_number_total 1547 _reflns_number_gt 733 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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^)+(0.0554P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1547 _refine_ls_number_parameters 102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1505 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1418 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.843 _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 Br1 Br 0.0677(2) 0.23230(7) 0.75788(8) 0.0450(4) Uani 1 1 d . . . C1 C 0.0258(18) 0.6387(7) 0.8849(8) 0.036(3) Uani 1 1 d . . . H1 H -0.1067 0.6803 0.8488 0.043 Uiso 1 1 calc R . . C2 C 0.3826(17) 0.5854(7) 0.9954(7) 0.030(2) Uani 1 1 d . . . C3 C 0.2780(17) 0.5128(7) 0.9260(7) 0.031(2) Uani 1 1 d . . . C4 C 0.3889(17) 0.4224(7) 0.9275(7) 0.036(3) Uani 1 1 d . . . H4 H 0.3174 0.3722 0.8815 0.043 Uiso 1 1 calc R . . C5 C 0.2688(18) 0.7617(8) 1.0112(7) 0.054(3) Uani 1 1 d . . . H5A H 0.4367 0.7848 0.9925 0.064 Uiso 1 1 calc R . . H5B H 0.2926 0.7595 1.0895 0.064 Uiso 1 1 calc R . . C6 C 0.047(2) 0.8311(8) 0.9689(9) 0.064(3) Uani 1 1 d . . . H6A H 0.0316 0.8371 0.8919 0.096 Uiso 1 1 calc R . . H6B H 0.0883 0.8934 1.0021 0.096 Uiso 1 1 calc R . . H6C H -0.1203 0.8077 0.9854 0.096 Uiso 1 1 calc R . . C7 C -0.1119(18) 0.4990(7) 0.7675(8) 0.051(3) Uani 1 1 d . . . H7A H -0.2843 0.5321 0.7476 0.061 Uiso 1 1 calc R . . H7B H -0.1480 0.4330 0.7877 0.061 Uiso 1 1 calc R . . C8 C 0.025(2) 0.4969(7) 0.6735(8) 0.057(3) Uani 1 1 d . . . H8A H 0.0641 0.5621 0.6540 0.086 Uiso 1 1 calc R . . H8B H -0.0902 0.4662 0.6136 0.086 Uiso 1 1 calc R . . H8C H 0.1915 0.4611 0.6917 0.086 Uiso 1 1 calc R . . N1 N 0.2137(15) 0.6639(7) 0.9682(6) 0.039(2) Uani 1 1 d . . . N2 N 0.0506(14) 0.5480(6) 0.8600(6) 0.030(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0364(5) 0.0587(8) 0.0379(6) -0.0115(7) 0.0014(4) -0.0050(6) C1 0.030(5) 0.046(7) 0.034(7) 0.005(5) 0.010(5) -0.004(5) C2 0.029(5) 0.043(7) 0.019(6) 0.002(5) 0.005(5) -0.006(5) C3 0.027(5) 0.043(7) 0.023(6) 0.005(5) 0.006(5) 0.004(5) C4 0.026(5) 0.048(7) 0.032(7) -0.001(5) 0.002(5) -0.009(5) C5 0.045(7) 0.080(10) 0.035(6) 0.017(7) 0.007(5) 0.007(7) C6 0.059(8) 0.052(8) 0.078(10) 0.003(7) 0.003(7) 0.008(7) C7 0.041(7) 0.062(8) 0.044(9) -0.016(6) -0.008(6) 0.004(6) C8 0.063(8) 0.060(9) 0.039(8) -0.017(6) -0.013(6) -0.010(6) N1 0.027(5) 0.048(6) 0.038(6) -0.002(4) -0.002(4) 0.001(4) N2 0.026(4) 0.034(5) 0.030(5) -0.001(4) 0.001(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.326(10) . ? C1 N1 1.348(10) . ? C2 C4 1.391(11) 3_667 ? C2 C3 1.396(12) . ? C2 N1 1.408(11) . ? C3 C4 1.391(11) . ? C3 N2 1.400(10) . ? C4 C2 1.391(11) 3_667 ? C5 N1 1.490(13) . ? C5 C6 1.520(12) . ? C7 N2 1.488(10) . ? C7 C8 1.504(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 111.0(9) . . ? C4 C2 C3 124.8(9) 3_667 . ? C4 C2 N1 129.6(9) 3_667 . ? C3 C2 N1 105.6(8) . . ? C4 C3 C2 123.5(9) . . ? C4 C3 N2 128.6(9) . . ? C2 C3 N2 107.9(9) . . ? C2 C4 C3 111.7(9) 3_667 . ? N1 C5 C6 112.5(8) . . ? N2 C7 C8 111.9(8) . . ? C1 N1 C2 107.9(9) . . ? C1 N1 C5 126.6(9) . . ? C2 N1 C5 124.5(8) . . ? C1 N2 C3 107.5(8) . . ? C1 N2 C7 125.0(8) . . ? C3 N2 C7 126.9(8) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 71.76 _diffrn_measured_fraction_theta_full 0.865 _refine_diff_density_max 0.843 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.126 # Attachment 'cif-1c.cif' data_sad3 _database_code_depnum_ccdc_archive 'CCDC 728538' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H40 Br2 N4' _chemical_formula_weight 544.42 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 29.972(4) _cell_length_b 29.972(4) _cell_length_c 8.656(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6734(2) _cell_formula_units_Z 9 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2538 _exptl_absorpt_coefficient_mu 2.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7358 _exptl_absorpt_correction_T_max 0.9227 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.715221 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16439 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.76 _reflns_number_total 2856 _reflns_number_gt 2081 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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^)+(0.0989P)^2^+83.0275P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2856 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.2082 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Br1 Br 0.05759(3) 0.42376(3) 0.09411(7) 0.0436(3) Uani 1 1 d . . . C1 C 0.9964(3) 0.4206(3) 0.7602(7) 0.0372(16) Uani 1 1 d . . . H1 H 0.9953 0.3975 0.8371 0.045 Uiso 1 1 calc R . . C2 C 0.9850(3) 0.4791(3) 0.6400(7) 0.0335(14) Uani 1 1 d . . . C3 C 1.0129(3) 0.4645(3) 0.5432(7) 0.0343(14) Uani 1 1 d . . . C4 C 1.0297(3) 0.4854(3) 0.3976(7) 0.0347(14) Uani 1 1 d . . . H4 H 1.0492 0.4764 0.3314 0.042 Uiso 1 1 calc R . . C5 C 1.0454(3) 0.4007(3) 0.5667(8) 0.0434(17) Uani 1 1 d . . . H5A H 1.0552 0.4101 0.4573 0.052 Uiso 1 1 calc R . . H5B H 1.0215 0.3630 0.5713 0.052 Uiso 1 1 calc R . . C6 C 1.0930(3) 0.4138(3) 0.6596(8) 0.051(2) Uani 1 1 d . . . H6A H 1.1083 0.3934 0.6201 0.061 Uiso 1 1 calc R . . H6B H 1.0829 0.4037 0.7685 0.061 Uiso 1 1 calc R . . C7 C 1.1333(4) 0.4702(4) 0.6541(11) 0.070(3) Uani 1 1 d . . . H7A H 1.1177 0.4907 0.6897 0.083 Uiso 1 1 calc R . . H7B H 1.1443 0.4800 0.5455 0.083 Uiso 1 1 calc R . . C8 C 1.1805(4) 0.4840(6) 0.7521(15) 0.109(5) Uani 1 1 d . . . H8A H 1.1703 0.4761 0.8606 0.164 Uiso 1 1 calc R . . H8B H 1.2053 0.5209 0.7413 0.164 Uiso 1 1 calc R . . H8C H 1.1963 0.4640 0.7176 0.164 Uiso 1 1 calc R . . C9 C 0.9442(3) 0.4495(3) 0.9065(7) 0.0426(17) Uani 1 1 d . . . H9A H 0.9529 0.4853 0.9294 0.051 Uiso 1 1 calc R . . H9B H 0.9531 0.4360 0.9987 0.051 Uiso 1 1 calc R . . C10 C 0.8869(3) 0.4173(3) 0.8777(9) 0.057(2) Uani 1 1 d . . . H10A H 0.8773 0.3808 0.8638 0.068 Uiso 1 1 calc R . . H10B H 0.8779 0.4291 0.7818 0.068 Uiso 1 1 calc R . . C11 C 0.8572(4) 0.4220(5) 1.0124(12) 0.081(3) Uani 1 1 d . . . H11A H 0.8685 0.4128 1.1088 0.097 Uiso 1 1 calc R . . H11B H 0.8656 0.4583 1.0215 0.097 Uiso 1 1 calc R . . C12 C 0.8001(5) 0.3883(7) 0.9960(19) 0.134(6) Uani 1 1 d . . . H12A H 0.7898 0.3910 0.8905 0.200 Uiso 1 1 calc R . . H12B H 0.7827 0.3993 1.0695 0.200 Uiso 1 1 calc R . . H12C H 0.7905 0.3524 1.0172 0.200 Uiso 1 1 calc R . . N1 N 1.0190(2) 0.4275(2) 0.6234(6) 0.0375(13) Uani 1 1 d . . . N2 N 0.9756(2) 0.4500(2) 0.7753(6) 0.0362(13) 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 Br1 0.0620(5) 0.0540(5) 0.0211(4) -0.0016(3) 0.0021(3) 0.0338(4) C1 0.055(4) 0.038(4) 0.016(3) 0.003(2) -0.003(3) 0.021(3) C2 0.047(4) 0.038(4) 0.015(3) 0.001(2) 0.002(2) 0.021(3) C3 0.045(4) 0.037(4) 0.022(3) -0.002(3) -0.003(3) 0.022(3) C4 0.042(4) 0.041(4) 0.019(3) -0.002(3) 0.000(3) 0.019(3) C5 0.064(5) 0.049(4) 0.029(3) -0.008(3) -0.004(3) 0.038(4) C6 0.071(5) 0.077(6) 0.027(3) 0.006(3) 0.005(3) 0.053(5) C7 0.060(6) 0.088(7) 0.060(6) -0.005(5) 0.003(4) 0.037(5) C8 0.069(7) 0.165(14) 0.085(8) -0.022(9) -0.014(6) 0.052(8) C9 0.062(5) 0.050(4) 0.019(3) 0.005(3) 0.011(3) 0.030(4) C10 0.063(5) 0.064(5) 0.045(4) 0.002(4) 0.019(4) 0.033(4) C11 0.090(8) 0.097(8) 0.060(6) 0.009(5) 0.033(5) 0.049(7) C12 0.085(9) 0.167(15) 0.126(13) 0.025(11) 0.046(9) 0.045(10) N1 0.053(3) 0.043(3) 0.021(3) 0.002(2) 0.005(2) 0.027(3) N2 0.053(4) 0.043(3) 0.014(2) 0.006(2) 0.004(2) 0.025(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 N2 1.312(9) . ? C1 N1 1.328(8) . ? C2 C4 1.379(9) 10_766 ? C2 C3 1.397(9) . ? C2 N2 1.403(8) . ? C3 C4 1.385(9) . ? C3 N1 1.398(8) . ? C4 C2 1.379(9) 10_766 ? C5 N1 1.467(9) . ? C5 C6 1.508(10) . ? C6 C7 1.510(13) . ? C7 C8 1.518(14) . ? C9 N2 1.471(8) . ? C9 C10 1.512(12) . ? C10 C11 1.515(11) . ? C11 C12 1.497(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 111.2(6) . . ? C4 C2 C3 124.8(6) 10_766 . ? C4 C2 N2 129.4(6) 10_766 . ? C3 C2 N2 105.8(6) . . ? C4 C3 C2 123.0(6) . . ? C4 C3 N1 130.4(6) . . ? C2 C3 N1 106.6(5) . . ? C2 C4 C3 112.2(6) 10_766 . ? N1 C5 C6 112.2(6) . . ? C5 C6 C7 113.5(7) . . ? C6 C7 C8 113.7(10) . . ? N2 C9 C10 113.4(6) . . ? C9 C10 C11 110.3(8) . . ? C12 C11 C10 113.0(10) . . ? C1 N1 C3 107.8(5) . . ? C1 N1 C5 126.0(6) . . ? C3 N1 C5 126.2(5) . . ? C1 N2 C2 108.6(5) . . ? C1 N2 C9 125.9(5) . . ? C2 N2 C9 125.4(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.921 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.136 # Attachment 'cif-2a.cif' data_sad4 _database_code_depnum_ccdc_archive 'CCDC 728539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H68 I4 N4 O2 P4 Pt2' _chemical_formula_weight 1958.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.137(3) _cell_length_b 18.015(2) _cell_length_c 17.714(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.985(2) _cell_angle_gamma 90.00 _cell_volume 7022.5(14) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3720 _exptl_absorpt_coefficient_mu 5.872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3453 _exptl_absorpt_correction_T_max 0.8916 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.568088 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45283 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 23.75 _reflns_number_total 10682 _reflns_number_gt 6806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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. Hydrogen atoms attached on the disordered H2O molecule were not calculated. ; _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^)+(0.0562P)^2^+104.7565P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10682 _refine_ls_number_parameters 765 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Pt1 Pt 0.23846(2) 0.97167(3) 0.63974(3) 0.02829(16) Uani 1 1 d . . . P1 P 0.34257(16) 0.9704(2) 0.6864(2) 0.0292(8) Uani 1 1 d . . . P2 P 0.24924(18) 0.9883(2) 0.5199(2) 0.0324(9) Uani 1 1 d . . . I1 I 0.22488(5) 0.95493(7) 0.78162(6) 0.0462(3) Uani 1 1 d . . . C1 C 0.1463(6) 0.9799(7) 0.5925(8) 0.027(3) Uani 1 1 d . . . N1 N 0.1146(5) 1.0432(6) 0.5831(6) 0.028(3) Uani 1 1 d . . . N2 N 0.1071(5) 0.9259(6) 0.5572(6) 0.028(3) Uani 1 1 d . . . C2 C 0.0535(6) 1.0319(8) 0.5417(8) 0.030(3) Uani 1 1 d . . . C3 C 0.0485(6) 0.9554(7) 0.5243(8) 0.027(3) Uani 1 1 d . . . C4 C 0.0048(7) 1.0783(9) 0.5172(8) 0.037(4) Uani 1 1 d . . . H4 H 0.0077 1.1301 0.5281 0.045 Uiso 1 1 calc R . . C5 C 0.1394(7) 1.1177(7) 0.6098(9) 0.040(4) Uani 1 1 d . . . H5A H 0.1776 1.1126 0.6531 0.060 Uiso 1 1 calc R . . H5B H 0.1101 1.1456 0.6286 0.060 Uiso 1 1 calc R . . H5C H 0.1469 1.1442 0.5655 0.060 Uiso 1 1 calc R . . C6 C 0.1218(7) 0.8466(7) 0.5523(10) 0.038(4) Uani 1 1 d . . . H6A H 0.1650 0.8384 0.5802 0.057 Uiso 1 1 calc R . . H6B H 0.1129 0.8322 0.4965 0.057 Uiso 1 1 calc R . . H6C H 0.0973 0.8165 0.5770 0.057 Uiso 1 1 calc R . . C7 C 0.3775(7) 1.0481(7) 0.7491(9) 0.032(3) Uani 1 1 d . . . C8 C 0.3822(9) 1.0447(10) 0.8295(10) 0.062(5) Uani 1 1 d . . . H8 H 0.3684 1.0023 0.8509 0.075 Uiso 1 1 calc R . . C9 C 0.4075(9) 1.1045(10) 0.8771(10) 0.059(5) Uani 1 1 d . . . H9 H 0.4096 1.1037 0.9315 0.071 Uiso 1 1 calc R . . C10 C 0.4293(8) 1.1635(9) 0.8486(11) 0.050(5) Uani 1 1 d . . . H10 H 0.4471 1.2032 0.8833 0.061 Uiso 1 1 calc R . . C11 C 0.4263(8) 1.1676(9) 0.7702(10) 0.047(4) Uani 1 1 d . . . H11 H 0.4429 1.2090 0.7507 0.056 Uiso 1 1 calc R . . C12 C 0.3987(7) 1.1101(8) 0.7200(10) 0.044(4) Uani 1 1 d . . . H12 H 0.3942 1.1133 0.6649 0.052 Uiso 1 1 calc R . . C13 C 0.3808(7) 0.8899(8) 0.7396(9) 0.038(4) Uani 1 1 d . . . C14 C 0.3515(7) 0.8284(8) 0.7526(8) 0.034(4) Uani 1 1 d . . . H14 H 0.3083 0.8278 0.7348 0.041 Uiso 1 1 calc R . . C15 C 0.3821(8) 0.7672(8) 0.7906(9) 0.043(4) Uani 1 1 d . . . H15 H 0.3602 0.7241 0.7962 0.051 Uiso 1 1 calc R . . C16 C 0.4449(8) 0.7681(9) 0.8208(9) 0.042(4) Uani 1 1 d . . . H16 H 0.4665 0.7264 0.8485 0.051 Uiso 1 1 calc R . . C17 C 0.4749(8) 0.8297(10) 0.8100(10) 0.053(5) Uani 1 1 d . . . H17 H 0.5180 0.8307 0.8302 0.064 Uiso 1 1 calc R . . C18 C 0.4444(7) 0.8915(9) 0.7700(9) 0.042(4) Uani 1 1 d . . . H18 H 0.4664 0.9342 0.7634 0.050 Uiso 1 1 calc R . . C19 C 0.3702(6) 0.9752(8) 0.6001(8) 0.032(3) Uani 1 1 d . . . H19A H 0.4111 0.9978 0.6156 0.038 Uiso 1 1 calc R . . H19B H 0.3732 0.9245 0.5800 0.038 Uiso 1 1 calc R . . C20 C 0.3267(6) 1.0214(9) 0.5356(9) 0.042(4) Uani 1 1 d . . . H20A H 0.3373 1.0171 0.4857 0.051 Uiso 1 1 calc R . . H20B H 0.3298 1.0743 0.5515 0.051 Uiso 1 1 calc R . . C21 C 0.2428(6) 0.9033(8) 0.4643(7) 0.029(3) Uani 1 1 d . . . C22 C 0.2626(7) 0.8368(9) 0.5016(9) 0.043(4) Uani 1 1 d . . . H22 H 0.2764 0.8350 0.5579 0.051 Uiso 1 1 calc R . . C23 C 0.2630(8) 0.7728(10) 0.4593(10) 0.054(5) Uani 1 1 d . . . H23 H 0.2786 0.7280 0.4863 0.065 Uiso 1 1 calc R . . C24 C 0.2408(9) 0.7737(12) 0.3780(12) 0.071(6) Uani 1 1 d . . . H24 H 0.2398 0.7295 0.3484 0.085 Uiso 1 1 calc R . . C25 C 0.2200(10) 0.8390(11) 0.3402(11) 0.064(6) Uani 1 1 d . . . H25 H 0.2050 0.8398 0.2839 0.077 Uiso 1 1 calc R . . C26 C 0.2201(9) 0.9043(10) 0.3818(9) 0.057(5) Uani 1 1 d . . . H26 H 0.2049 0.9490 0.3544 0.068 Uiso 1 1 calc R . . C27 C 0.1996(7) 1.0555(9) 0.4562(8) 0.036(4) Uani 1 1 d . . . C28 C 0.2190(8) 1.1266(9) 0.4484(10) 0.054(5) Uani 1 1 d . . . H28 H 0.2600 1.1408 0.4737 0.064 Uiso 1 1 calc R . . C29 C 0.1772(9) 1.1771(10) 0.4026(11) 0.059(5) Uani 1 1 d . . . H29 H 0.1894 1.2270 0.3993 0.071 Uiso 1 1 calc R . . C30 C 0.1190(9) 1.1567(10) 0.3621(10) 0.056(5) Uani 1 1 d . . . H30 H 0.0923 1.1914 0.3282 0.067 Uiso 1 1 calc R . . C31 C 0.0993(8) 1.0879(11) 0.3698(9) 0.053(5) Uani 1 1 d . . . H31 H 0.0581 1.0754 0.3440 0.063 Uiso 1 1 calc R . . C32 C 0.1392(7) 1.0337(10) 0.4160(9) 0.049(4) Uani 1 1 d . . . H32 H 0.1258 0.9844 0.4198 0.059 Uiso 1 1 calc R . . Pt41 Pt 0.23937(3) -0.03230(4) 0.10538(3) 0.03633(17) Uani 1 1 d . . . P41 P 0.34263(19) -0.0370(3) 0.1402(2) 0.0435(11) Uani 1 1 d . . . P42 P 0.2482(2) 0.0868(2) 0.0758(2) 0.0429(11) Uani 1 1 d . . . I41 I 0.22847(5) -0.17657(6) 0.12984(7) 0.0483(3) Uani 1 1 d . . . C41 C 0.1487(6) -0.0245(8) 0.0705(7) 0.025(3) Uani 1 1 d . . . N41 N 0.1118(5) -0.0399(6) -0.0052(6) 0.028(3) Uani 1 1 d . . . N42 N 0.1113(6) 0.0024(6) 0.1082(7) 0.035(3) Uani 1 1 d . . . C42 C 0.0516(7) -0.0224(8) -0.0132(8) 0.033(3) Uani 1 1 d . . . C43 C 0.0519(6) 0.0039(8) 0.0612(8) 0.028(3) Uani 1 1 d . . . C44 C -0.0010(6) -0.0277(8) -0.0785(8) 0.031(3) Uani 1 1 d . . . H44 H -0.0015 -0.0456 -0.1291 0.037 Uiso 1 1 calc R . . C45 C 0.1309(7) -0.0735(9) -0.0692(9) 0.043(4) Uani 1 1 d . . . H45A H 0.1751 -0.0804 -0.0511 0.064 Uiso 1 1 calc R . . H45B H 0.1196 -0.0407 -0.1156 0.064 Uiso 1 1 calc R . . H45C H 0.1109 -0.1216 -0.0835 0.064 Uiso 1 1 calc R . . C46 C 0.1307(7) 0.0234(9) 0.1933(8) 0.040(4) Uani 1 1 d . . . H46A H 0.1089 -0.0070 0.2215 0.059 Uiso 1 1 calc R . . H46B H 0.1216 0.0760 0.1984 0.059 Uiso 1 1 calc R . . H46C H 0.1745 0.0151 0.2163 0.059 Uiso 1 1 calc R . . C47 C 0.3757(7) -0.1046(9) 0.0885(9) 0.043(4) Uani 1 1 d . . . C48 C 0.3790(9) -0.0874(10) 0.0141(10) 0.062(5) Uani 1 1 d . . . H48 H 0.3646 -0.0410 -0.0099 0.075 Uiso 1 1 calc R . . C49 C 0.4034(11) -0.1384(11) -0.0248(11) 0.080(7) Uani 1 1 d . . . H49 H 0.4062 -0.1263 -0.0758 0.096 Uiso 1 1 calc R . . C50 C 0.4240(10) -0.2063(11) 0.0071(11) 0.067(6) Uani 1 1 d . . . H50 H 0.4427 -0.2397 -0.0198 0.080 Uiso 1 1 calc R . . C51 C 0.4166(8) -0.2261(10) 0.0830(10) 0.054(5) Uani 1 1 d . . . H51 H 0.4280 -0.2738 0.1055 0.064 Uiso 1 1 calc R . . C52 C 0.3924(8) -0.1737(10) 0.1217(10) 0.057(5) Uani 1 1 d . . . H52 H 0.3871 -0.1853 0.1715 0.068 Uiso 1 1 calc R . . C53 C 0.3824(8) -0.0548(10) 0.2442(9) 0.048(4) Uani 1 1 d . . . C54 C 0.4450(7) -0.0614(9) 0.2736(10) 0.042(4) Uani 1 1 d . . . H54 H 0.4694 -0.0578 0.2393 0.051 Uiso 1 1 calc R . . C55 C 0.4709(8) -0.0734(10) 0.3527(10) 0.056(5) Uani 1 1 d . . . H55 H 0.5140 -0.0756 0.3728 0.068 Uiso 1 1 calc R . . C56 C 0.4386(9) -0.0823(10) 0.4049(11) 0.060(5) Uani 1 1 d . . . H56 H 0.4586 -0.0898 0.4598 0.072 Uiso 1 1 calc R . . C57 C 0.3750(9) -0.0801(11) 0.3751(10) 0.059(5) Uani 1 1 d . . . H57 H 0.3507 -0.0875 0.4091 0.071 Uiso 1 1 calc R . . C58 C 0.3487(8) -0.0670(8) 0.2954(9) 0.044(4) Uani 1 1 d . . . H58 H 0.3057 -0.0664 0.2746 0.052 Uiso 1 1 calc R . . C59 C 0.3664(8) 0.0480(10) 0.1179(9) 0.057(5) Uani 1 1 d . . . H59A H 0.3769 0.0791 0.1663 0.069 Uiso 1 1 calc R . . H59B H 0.4040 0.0410 0.1032 0.069 Uiso 1 1 calc R . . C60 C 0.3194(9) 0.0914(10) 0.0493(11) 0.065(6) Uani 1 1 d . . . H60A H 0.3144 0.0675 -0.0026 0.077 Uiso 1 1 calc R . . H60B H 0.3324 0.1435 0.0471 0.077 Uiso 1 1 calc R . . C61 C 0.2593(7) 0.1502(8) 0.1580(10) 0.040(4) Uani 1 1 d . . . C62 C 0.2744(8) 0.1265(10) 0.2346(10) 0.055(5) Uani 1 1 d . . . H62 H 0.2752 0.0745 0.2442 0.066 Uiso 1 1 calc R . . C63 C 0.2882(9) 0.1728(11) 0.2979(11) 0.067(6) Uani 1 1 d . . . H63 H 0.2989 0.1537 0.3504 0.080 Uiso 1 1 calc R . . C64 C 0.2864(8) 0.2503(13) 0.2842(13) 0.070(6) Uani 1 1 d . . . H64 H 0.2951 0.2842 0.3275 0.085 Uiso 1 1 calc R . . C65 C 0.2717(8) 0.2763(10) 0.2065(15) 0.072(7) Uani 1 1 d . . . H65 H 0.2696 0.3283 0.1970 0.086 Uiso 1 1 calc R . . C66 C 0.2599(8) 0.2267(11) 0.1411(12) 0.065(6) Uani 1 1 d . . . H66 H 0.2528 0.2443 0.0885 0.079 Uiso 1 1 calc R . . C67 C 0.1868(9) 0.1220(9) -0.0054(10) 0.053(5) Uani 1 1 d . . . C68 C 0.1354(9) 0.1508(10) 0.0113(11) 0.059(5) Uani 1 1 d . . . H68 H 0.1369 0.1580 0.0650 0.071 Uiso 1 1 calc R . . C69 C 0.0824(10) 0.1688(12) -0.0495(14) 0.082(7) Uani 1 1 d . . . H69 H 0.0482 0.1887 -0.0377 0.098 Uiso 1 1 calc R . . C70 C 0.0811(12) 0.1569(11) -0.1277(13) 0.079(7) Uani 1 1 d . . . H70 H 0.0456 0.1684 -0.1702 0.095 Uiso 1 1 calc R . . C71 C 0.1314(13) 0.1283(11) -0.1432(12) 0.079(7) Uani 1 1 d . . . H71 H 0.1299 0.1195 -0.1966 0.094 Uiso 1 1 calc R . . C72 C 0.1831(11) 0.1125(10) -0.0838(10) 0.070(6) Uani 1 1 d . . . H72 H 0.2174 0.0944 -0.0967 0.084 Uiso 1 1 calc R . . I13 I 0.02033(7) 0.26555(7) 0.63969(8) 0.0707(4) Uani 1 1 d . . . I14 I 0.39315(5) 0.21744(6) 0.52483(6) 0.0476(3) Uani 1 1 d . . . O81 O 0.4799(12) 0.3595(18) 0.9179(16) 0.076(8) Uani 0.50 1 d P . . H81 H 0.5051 0.3299 0.9089 0.115 Uiso 0.50 1 calc PR . . C81 C 0.4419(18) 0.383(3) 0.850(2) 0.082(14) Uani 0.50 1 d P . . H81A H 0.4326 0.4354 0.8542 0.123 Uiso 0.50 1 calc PR . . H81B H 0.4043 0.3538 0.8368 0.123 Uiso 0.50 1 calc PR . . H81C H 0.4607 0.3766 0.8075 0.123 Uiso 0.50 1 calc PR . . O82 O 0.0431(11) 0.8204(13) 0.7199(14) 0.055(6) Uani 0.50 1 d P . . H82 H 0.0423 0.8441 0.7605 0.083 Uiso 0.50 1 calc PR . . C82 C 0.089(3) 0.775(3) 0.738(3) 0.12(2) Uani 0.50 1 d P . . H82A H 0.1239 0.7999 0.7752 0.182 Uiso 0.50 1 calc PR . . H82B H 0.0981 0.7608 0.6903 0.182 Uiso 0.50 1 calc PR . . H82C H 0.0782 0.7312 0.7638 0.182 Uiso 0.50 1 calc PR . . O1 O 0.0568(8) 0.9734(12) 0.7259(11) 0.041(5) Uani 0.50 1 d P . . O2 O 0.0386(9) 0.9151(11) 0.3042(12) 0.041(5) Uani 0.50 1 d P . . 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 Pt1 0.0253(3) 0.0312(3) 0.0273(3) 0.0000(3) 0.0066(2) 0.0009(3) P1 0.026(2) 0.031(2) 0.0283(19) -0.0016(17) 0.0064(16) 0.0010(18) P2 0.031(2) 0.037(2) 0.026(2) 0.0009(17) 0.0043(17) -0.0003(18) I1 0.0413(6) 0.0680(8) 0.0328(5) 0.0030(5) 0.0165(5) 0.0062(6) C1 0.026(8) 0.028(8) 0.031(8) -0.002(6) 0.017(6) 0.002(7) N1 0.035(7) 0.025(7) 0.027(6) -0.006(5) 0.014(5) -0.008(5) N2 0.033(7) 0.022(6) 0.028(6) 0.012(5) 0.007(5) 0.006(5) C2 0.029(8) 0.029(8) 0.028(7) -0.002(7) 0.005(6) -0.001(7) C3 0.024(8) 0.029(8) 0.031(8) -0.001(6) 0.010(6) 0.005(6) C4 0.037(9) 0.041(9) 0.033(8) -0.008(7) 0.009(7) 0.001(8) C5 0.030(9) 0.027(8) 0.051(10) -0.017(7) -0.005(7) -0.008(7) C6 0.028(8) 0.016(7) 0.061(11) -0.008(7) 0.001(8) 0.005(6) C7 0.035(9) 0.014(7) 0.044(9) -0.006(6) 0.009(7) 0.007(6) C8 0.087(15) 0.064(13) 0.041(10) 0.002(9) 0.026(10) -0.021(11) C9 0.077(14) 0.067(13) 0.034(10) -0.015(9) 0.017(9) -0.018(11) C10 0.049(11) 0.039(10) 0.063(12) -0.026(9) 0.018(9) -0.015(9) C11 0.055(11) 0.033(9) 0.060(11) -0.025(8) 0.031(9) -0.022(8) C12 0.041(10) 0.036(9) 0.061(11) 0.003(8) 0.027(9) 0.001(8) C13 0.037(10) 0.039(9) 0.038(9) 0.002(7) 0.012(7) 0.007(8) C14 0.036(9) 0.027(8) 0.037(8) -0.010(7) 0.008(7) -0.001(7) C15 0.062(12) 0.020(8) 0.046(10) -0.004(7) 0.017(9) -0.006(8) C16 0.051(11) 0.041(10) 0.029(9) 0.002(7) 0.004(8) 0.019(8) C17 0.038(10) 0.052(11) 0.059(11) 0.015(9) 0.000(9) 0.011(9) C18 0.024(9) 0.038(9) 0.058(10) -0.005(8) 0.004(8) -0.001(7) C19 0.035(8) 0.035(8) 0.024(7) 0.002(7) 0.006(6) -0.001(7) C20 0.028(8) 0.050(10) 0.047(10) -0.011(8) 0.008(7) -0.013(8) C21 0.026(8) 0.041(9) 0.017(7) 0.002(7) 0.004(6) -0.003(7) C22 0.043(10) 0.061(11) 0.027(8) -0.010(8) 0.013(7) -0.012(9) C23 0.059(12) 0.051(11) 0.050(11) -0.007(9) 0.014(9) 0.015(9) C24 0.080(15) 0.073(15) 0.061(13) -0.030(12) 0.023(11) -0.010(12) C25 0.097(16) 0.062(13) 0.037(10) -0.010(10) 0.026(10) -0.016(12) C26 0.083(14) 0.057(12) 0.033(9) -0.015(9) 0.020(9) -0.015(10) C27 0.029(9) 0.052(10) 0.029(8) 0.006(7) 0.011(7) 0.017(8) C28 0.054(12) 0.047(11) 0.062(12) 0.022(9) 0.020(10) 0.001(9) C29 0.058(13) 0.044(11) 0.074(13) 0.012(10) 0.018(11) 0.020(10) C30 0.063(13) 0.051(12) 0.044(10) 0.004(9) 0.000(9) 0.011(10) C31 0.039(10) 0.073(14) 0.034(9) -0.003(9) -0.005(8) 0.015(10) C32 0.049(11) 0.061(11) 0.034(9) 0.007(9) 0.007(8) 0.003(9) Pt41 0.0311(3) 0.0479(4) 0.0288(3) -0.0015(3) 0.0076(3) 0.0023(3) P41 0.038(2) 0.056(3) 0.036(2) 0.000(2) 0.0097(19) 0.002(2) P42 0.046(3) 0.047(3) 0.038(2) -0.003(2) 0.017(2) -0.006(2) I41 0.0530(7) 0.0432(6) 0.0488(7) 0.0016(5) 0.0158(5) -0.0006(5) C41 0.023(7) 0.034(8) 0.017(7) 0.002(6) 0.006(6) 0.008(7) N41 0.028(7) 0.035(7) 0.019(6) -0.008(5) 0.007(5) -0.001(6) N42 0.037(8) 0.033(7) 0.029(7) 0.001(6) -0.001(6) 0.006(6) C42 0.044(10) 0.031(8) 0.028(8) 0.003(7) 0.018(7) 0.008(7) C43 0.031(9) 0.032(8) 0.020(7) 0.001(6) 0.005(7) 0.006(7) C44 0.037(9) 0.039(8) 0.020(7) -0.008(7) 0.013(7) -0.005(8) C45 0.039(10) 0.060(11) 0.033(9) -0.013(8) 0.015(7) -0.002(8) C46 0.037(9) 0.054(10) 0.024(8) -0.003(7) 0.004(7) 0.011(8) C47 0.049(10) 0.055(11) 0.028(8) 0.003(8) 0.016(8) 0.001(8) C48 0.090(15) 0.056(12) 0.051(11) 0.017(10) 0.037(11) 0.016(11) C49 0.14(2) 0.063(13) 0.040(11) 0.018(10) 0.030(13) 0.033(14) C50 0.088(16) 0.075(14) 0.047(11) -0.001(10) 0.034(11) 0.008(12) C51 0.066(13) 0.050(11) 0.046(10) -0.006(9) 0.019(9) 0.005(9) C52 0.059(12) 0.065(12) 0.042(10) 0.002(10) 0.010(9) 0.003(10) C53 0.055(12) 0.056(11) 0.034(9) -0.009(8) 0.015(9) -0.001(9) C54 0.031(9) 0.047(10) 0.051(10) 0.002(8) 0.015(8) -0.003(8) C55 0.049(11) 0.062(12) 0.050(11) 0.004(9) 0.005(9) -0.023(10) C56 0.056(13) 0.067(13) 0.050(11) -0.008(10) 0.005(10) 0.007(10) C57 0.060(13) 0.078(14) 0.037(10) -0.011(9) 0.012(9) 0.003(11) C58 0.048(10) 0.036(9) 0.040(10) -0.001(8) 0.003(8) 0.004(8) C59 0.046(11) 0.092(15) 0.034(9) -0.015(9) 0.013(8) 0.037(10) C60 0.091(16) 0.051(11) 0.067(13) -0.008(10) 0.048(12) -0.021(11) C61 0.036(9) 0.024(8) 0.061(11) -0.015(8) 0.018(8) -0.010(7) C62 0.067(13) 0.054(11) 0.042(11) -0.007(9) 0.016(9) -0.010(10) C63 0.083(15) 0.064(14) 0.050(12) -0.007(11) 0.015(11) -0.010(12) C64 0.041(11) 0.100(18) 0.067(15) -0.033(13) 0.013(11) -0.022(12) C65 0.030(10) 0.040(11) 0.12(2) -0.016(13) -0.009(11) 0.009(8) C66 0.040(11) 0.076(14) 0.077(14) -0.030(12) 0.013(10) -0.015(10) C67 0.073(14) 0.031(9) 0.053(12) -0.005(8) 0.014(10) -0.013(9) C68 0.066(13) 0.048(11) 0.050(11) 0.013(9) -0.004(10) -0.021(10) C69 0.068(15) 0.066(14) 0.089(17) 0.010(13) -0.011(13) -0.029(12) C70 0.11(2) 0.045(12) 0.056(14) 0.007(10) -0.020(13) -0.012(13) C71 0.13(2) 0.040(12) 0.051(13) -0.003(10) 0.011(15) 0.003(13) C72 0.117(19) 0.053(12) 0.036(11) 0.000(9) 0.018(12) -0.004(12) I13 0.0893(10) 0.0492(8) 0.0670(9) -0.0097(7) 0.0144(8) 0.0093(7) I14 0.0536(7) 0.0429(6) 0.0413(6) 0.0092(5) 0.0074(5) -0.0058(5) O81 0.052(18) 0.10(2) 0.08(2) -0.001(17) 0.020(15) -0.013(16) C81 0.05(3) 0.14(4) 0.05(3) 0.00(3) 0.02(2) -0.01(3) O82 0.051(15) 0.042(15) 0.069(16) 0.029(13) 0.013(13) 0.002(12) C82 0.16(6) 0.13(5) 0.11(4) 0.04(4) 0.09(4) 0.03(5) O1 0.021(11) 0.061(14) 0.036(11) 0.013(11) 0.001(9) -0.001(10) O2 0.030(12) 0.048(13) 0.042(12) -0.016(10) 0.006(10) -0.024(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 Pt1 C1 2.042(13) . ? Pt1 P2 2.233(4) . ? Pt1 P1 2.293(4) . ? Pt1 I1 2.6446(11) . ? Pt1 Pt1 10.6571(16) 3_576 ? P1 C13 1.805(15) . ? P1 C7 1.814(14) . ? P1 C19 1.832(14) . ? P2 C21 1.802(14) . ? P2 C27 1.804(15) . ? P2 C20 1.826(14) . ? C1 N1 1.337(17) . ? C1 N2 1.344(17) . ? N1 C2 1.391(17) . ? N1 C5 1.479(16) . ? N2 C3 1.404(17) . ? N2 C6 1.479(16) . ? C2 C4 1.363(19) . ? C2 C3 1.410(19) . ? C3 C4 1.368(19) 3_576 ? C4 C3 1.368(19) 3_576 ? C7 C12 1.38(2) . ? C7 C8 1.39(2) . ? C8 C9 1.38(2) . ? C9 C10 1.34(2) . ? C10 C11 1.37(2) . ? C11 C12 1.39(2) . ? C13 C14 1.35(2) . ? C13 C18 1.40(2) . ? C14 C15 1.37(2) . ? C15 C16 1.38(2) . ? C16 C17 1.35(2) . ? C17 C18 1.39(2) . ? C19 C20 1.52(2) . ? C21 C22 1.38(2) . ? C21 C26 1.39(2) . ? C22 C23 1.38(2) . ? C23 C24 1.37(2) . ? C24 C25 1.37(3) . ? C25 C26 1.39(2) . ? C27 C28 1.38(2) . ? C27 C32 1.41(2) . ? C28 C29 1.39(2) . ? C29 C30 1.37(2) . ? C30 C31 1.34(2) . ? C31 C32 1.42(2) . ? Pt41 C41 2.000(13) . ? Pt41 P42 2.234(4) . ? Pt41 P41 2.277(4) . ? Pt41 I41 2.6595(13) . ? Pt41 Pt41 10.6041(17) 3 ? P41 C59 1.72(2) . ? P41 C53 1.814(17) . ? P41 C47 1.828(16) . ? P42 C67 1.796(19) . ? P42 C61 1.806(15) . ? P42 C60 1.849(18) . ? C41 N42 1.337(17) . ? C41 N41 1.377(16) . ? N41 C42 1.392(17) . ? N41 C45 1.469(17) . ? N42 C43 1.368(17) . ? N42 C46 1.484(17) . ? C42 C43 1.399(19) . ? C42 C44 1.399(19) . ? C43 C44 1.374(19) 3 ? C44 C43 1.374(19) 3 ? C47 C48 1.38(2) . ? C47 C52 1.38(2) . ? C48 C49 1.37(2) . ? C49 C50 1.37(3) . ? C50 C51 1.45(2) . ? C51 C52 1.38(2) . ? C53 C58 1.38(2) . ? C53 C54 1.39(2) . ? C54 C55 1.36(2) . ? C55 C56 1.37(2) . ? C56 C57 1.40(2) . ? C57 C58 1.37(2) . ? C59 C60 1.57(2) . ? C61 C62 1.36(2) . ? C61 C66 1.41(2) . ? C62 C63 1.35(2) . ? C63 C64 1.42(3) . ? C64 C65 1.39(3) . ? C65 C66 1.42(3) . ? C67 C72 1.38(2) . ? C67 C68 1.41(3) . ? C68 C69 1.40(3) . ? C69 C70 1.39(3) . ? C70 C71 1.37(3) . ? C71 C72 1.36(3) . ? O81 C81 1.32(4) . ? O82 C82 1.29(5) . ? 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 C1 Pt1 P2 90.5(4) . . ? C1 Pt1 P1 175.4(4) . . ? P2 Pt1 P1 86.04(14) . . ? C1 Pt1 I1 89.0(4) . . ? P2 Pt1 I1 178.76(11) . . ? P1 Pt1 I1 94.36(10) . . ? C1 Pt1 Pt1 3.6(4) . 3_576 ? P2 Pt1 Pt1 87.08(10) . 3_576 ? P1 Pt1 Pt1 172.03(10) . 3_576 ? I1 Pt1 Pt1 92.44(3) . 3_576 ? C13 P1 C7 104.3(7) . . ? C13 P1 C19 103.4(7) . . ? C7 P1 C19 105.7(7) . . ? C13 P1 Pt1 119.2(5) . . ? C7 P1 Pt1 115.6(5) . . ? C19 P1 Pt1 107.3(5) . . ? C21 P2 C27 107.4(7) . . ? C21 P2 C20 105.8(7) . . ? C27 P2 C20 106.3(7) . . ? C21 P2 Pt1 113.0(5) . . ? C27 P2 Pt1 116.6(5) . . ? C20 P2 Pt1 107.0(5) . . ? N1 C1 N2 107.1(11) . . ? N1 C1 Pt1 125.2(10) . . ? N2 C1 Pt1 127.4(10) . . ? C1 N1 C2 111.7(11) . . ? C1 N1 C5 126.1(12) . . ? C2 N1 C5 122.1(12) . . ? C1 N2 C3 110.2(11) . . ? C1 N2 C6 126.3(11) . . ? C3 N2 C6 123.4(11) . . ? C4 C2 N1 133.1(13) . . ? C4 C2 C3 121.8(13) . . ? N1 C2 C3 105.1(12) . . ? C4 C3 N2 130.6(13) 3_576 . ? C4 C3 C2 123.4(13) 3_576 . ? N2 C3 C2 105.9(11) . . ? C2 C4 C3 114.8(13) . 3_576 ? C12 C7 C8 119.5(14) . . ? C12 C7 P1 122.4(12) . . ? C8 C7 P1 118.1(12) . . ? C9 C8 C7 118.3(16) . . ? C10 C9 C8 121.7(16) . . ? C9 C10 C11 121.2(15) . . ? C10 C11 C12 118.5(15) . . ? C7 C12 C11 120.7(16) . . ? C14 C13 C18 118.2(14) . . ? C14 C13 P1 123.7(12) . . ? C18 C13 P1 118.1(12) . . ? C13 C14 C15 122.0(15) . . ? C14 C15 C16 120.3(15) . . ? C17 C16 C15 118.5(15) . . ? C16 C17 C18 121.8(16) . . ? C17 C18 C13 119.1(15) . . ? C20 C19 P1 109.5(10) . . ? C19 C20 P2 109.1(11) . . ? C22 C21 C26 118.4(14) . . ? C22 C21 P2 121.3(10) . . ? C26 C21 P2 120.2(12) . . ? C21 C22 C23 121.7(14) . . ? C24 C23 C22 119.8(18) . . ? C25 C24 C23 119.2(18) . . ? C24 C25 C26 121.8(17) . . ? C25 C26 C21 119.0(18) . . ? C28 C27 C32 120.6(15) . . ? C28 C27 P2 121.5(13) . . ? C32 C27 P2 117.9(13) . . ? C27 C28 C29 118.5(17) . . ? C30 C29 C28 121.7(18) . . ? C31 C30 C29 120.4(17) . . ? C30 C31 C32 121.0(17) . . ? C27 C32 C31 117.7(16) . . ? C41 Pt41 P42 91.3(4) . . ? C41 Pt41 P41 177.1(4) . . ? P42 Pt41 P41 86.29(17) . . ? C41 Pt41 I41 88.6(4) . . ? P42 Pt41 I41 175.82(11) . . ? P41 Pt41 I41 93.64(12) . . ? C41 Pt41 Pt41 3.4(4) . 3 ? P42 Pt41 Pt41 88.47(12) . 3 ? P41 Pt41 Pt41 173.72(11) . 3 ? I41 Pt41 Pt41 91.34(3) . 3 ? C59 P41 C53 107.0(8) . . ? C59 P41 C47 105.4(8) . . ? C53 P41 C47 103.4(8) . . ? C59 P41 Pt41 106.8(6) . . ? C53 P41 Pt41 116.3(6) . . ? C47 P41 Pt41 117.1(6) . . ? C67 P42 C61 107.6(8) . . ? C67 P42 C60 109.1(9) . . ? C61 P42 C60 105.0(8) . . ? C67 P42 Pt41 114.8(5) . . ? C61 P42 Pt41 114.8(6) . . ? C60 P42 Pt41 104.8(6) . . ? N42 C41 N41 104.8(11) . . ? N42 C41 Pt41 130.6(10) . . ? N41 C41 Pt41 124.3(9) . . ? C41 N41 C42 110.8(11) . . ? C41 N41 C45 126.1(12) . . ? C42 N41 C45 123.0(11) . . ? C41 N42 C43 112.8(11) . . ? C41 N42 C46 124.0(12) . . ? C43 N42 C46 123.1(12) . . ? N41 C42 C43 105.4(12) . . ? N41 C42 C44 131.1(12) . . ? C43 C42 C44 123.6(13) . . ? N42 C43 C44 129.7(13) . 3 ? N42 C43 C42 106.2(12) . . ? C44 C43 C42 124.1(13) 3 . ? C43 C44 C42 112.4(12) 3 . ? C48 C47 C52 121.3(16) . . ? C48 C47 P41 119.1(13) . . ? C52 C47 P41 119.5(12) . . ? C49 C48 C47 118.9(17) . . ? C50 C49 C48 122.4(18) . . ? C49 C50 C51 118.4(18) . . ? C52 C51 C50 118.3(17) . . ? C47 C52 C51 120.5(17) . . ? C58 C53 C54 118.3(15) . . ? C58 C53 P41 118.8(13) . . ? C54 C53 P41 122.7(13) . . ? C55 C54 C53 118.5(16) . . ? C54 C55 C56 123.9(18) . . ? C55 C56 C57 118.2(18) . . ? C58 C57 C56 118.1(18) . . ? C57 C58 C53 122.8(17) . . ? C60 C59 P41 115.4(13) . . ? C59 C60 P42 103.9(11) . . ? C62 C61 C66 120.1(16) . . ? C62 C61 P42 122.3(13) . . ? C66 C61 P42 117.1(14) . . ? C63 C62 C61 123.6(18) . . ? C62 C63 C64 118.7(19) . . ? C65 C64 C63 119.1(18) . . ? C64 C65 C66 121.4(19) . . ? C61 C66 C65 117.0(19) . . ? C72 C67 C68 117.7(19) . . ? C72 C67 P42 123.5(17) . . ? C68 C67 P42 118.1(14) . . ? C69 C68 C67 121(2) . . ? C70 C69 C68 118(2) . . ? C71 C70 C69 120(2) . . ? C72 C71 C70 121(2) . . ? C71 C72 C67 121(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.75 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 5.059 _refine_diff_density_min -2.105 _refine_diff_density_rms 0.203 # Attachment 'cif-2d.cif' data_sad5 _database_code_depnum_ccdc_archive 'CCDC 728540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H91 Cl13 N4 O P4 Pt2' _chemical_formula_weight 2087.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1317(5) _cell_length_b 23.3036(13) _cell_length_c 17.7567(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.896(4) _cell_angle_gamma 90.00 _cell_volume 4581.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2076 _exptl_absorpt_coefficient_mu 10.109 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2783 _exptl_absorpt_correction_T_max 0.6879 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports Maximum and minimum effective transmission: 1.000000 0.464263 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25947 _diffrn_reflns_av_R_equivalents 0.1092 _diffrn_reflns_av_sigmaI/netI 0.1830 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 72.51 _reflns_number_total 8531 _reflns_number_gt 4259 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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. One of the CHCl3 and the H2O-molecule is disorderd. The occupanciy factor is 0.5 therfore the hydrogen atoms on the water molecule were not clculated. Both of the molecules were constrained with one FVAR(Uij). ; _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^)+(0.0841P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8531 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _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 Pt1 Pt 0.26409(5) 0.16226(2) 0.88471(3) 0.03082(16) Uani 1 1 d . . . P1 P 0.1010(3) 0.21783(13) 0.85887(18) 0.0311(7) Uani 1 1 d . . . P2 P 0.3633(3) 0.23247(14) 0.82357(19) 0.0328(8) Uani 1 1 d . . . Cl1 Cl 0.4403(2) 0.10452(13) 0.90987(18) 0.0369(8) Uani 1 1 d . . . C1 C 0.1681(9) 0.0984(4) 0.9300(7) 0.027(3) Uani 1 1 d . . . N1 N 0.0958(8) 0.0618(4) 0.8900(5) 0.029(2) Uani 1 1 d . . . N2 N 0.1623(8) 0.0878(4) 1.0044(6) 0.028(2) Uani 1 1 d . . . C2 C 0.0380(10) 0.0248(5) 0.9371(8) 0.031(3) Uani 1 1 d . . . C3 C -0.0443(11) -0.0176(5) 0.9223(7) 0.030(3) Uani 1 1 d . . . H3 H -0.0729 -0.0293 0.8724 0.036 Uiso 1 1 calc R . . C4 C -0.0831(10) -0.0423(5) 0.9865(7) 0.032(3) Uani 1 1 d . . . C5 C 0.0784(11) 0.0578(5) 0.8074(7) 0.033(3) Uani 1 1 d . . . H5A H 0.0894 0.0963 0.7855 0.040 Uiso 1 1 calc R . . H5B H -0.0055 0.0454 0.7916 0.040 Uiso 1 1 calc R . . C6 C 0.1656(11) 0.0159(5) 0.7758(7) 0.038(3) Uani 1 1 d . . . H6A H 0.2496 0.0257 0.7953 0.045 Uiso 1 1 calc R . . H6B H 0.1485 -0.0236 0.7922 0.045 Uiso 1 1 calc R . . C7 C 0.1514(12) 0.0192(6) 0.6901(7) 0.044(4) Uani 1 1 d . . . H7A H 0.0663 0.0115 0.6708 0.053 Uiso 1 1 calc R . . H7B H 0.1726 0.0581 0.6738 0.053 Uiso 1 1 calc R . . C8 C 0.2327(15) -0.0245(7) 0.6579(8) 0.079(6) Uani 1 1 d . . . H8A H 0.2748 -0.0469 0.6993 0.118 Uiso 1 1 calc R . . H8B H 0.2920 -0.0047 0.6301 0.118 Uiso 1 1 calc R . . H8C H 0.1839 -0.0503 0.6235 0.118 Uiso 1 1 calc R . . C9 C 0.2387(11) 0.1117(5) 1.0683(7) 0.038(3) Uani 1 1 d . . . H9A H 0.1889 0.1221 1.1094 0.046 Uiso 1 1 calc R . . H9B H 0.2793 0.1468 1.0524 0.046 Uiso 1 1 calc R . . C10 C 0.3363(11) 0.0655(6) 1.0978(8) 0.047(4) Uani 1 1 d . . . H10A H 0.2953 0.0314 1.1166 0.056 Uiso 1 1 calc R . . H10B H 0.3815 0.0531 1.0555 0.056 Uiso 1 1 calc R . . C11 C 0.4239(15) 0.0899(7) 1.1613(10) 0.076(5) Uani 1 1 d . . . H11A H 0.4673 0.1229 1.1417 0.091 Uiso 1 1 calc R . . H11B H 0.3779 0.1041 1.2024 0.091 Uiso 1 1 calc R . . C12 C 0.5140(16) 0.0460(8) 1.1928(11) 0.109(8) Uani 1 1 d . . . H12A H 0.4746 0.0188 1.2244 0.163 Uiso 1 1 calc R . . H12B H 0.5805 0.0652 1.2234 0.163 Uiso 1 1 calc R . . H12C H 0.5458 0.0253 1.1510 0.163 Uiso 1 1 calc R . . C13 C -0.0444(11) 0.1840(5) 0.8379(8) 0.034(3) Uani 1 1 d . . . C14 C -0.0999(13) 0.1853(6) 0.7650(9) 0.050(4) Uani 1 1 d . . . H14 H -0.0621 0.2049 0.7268 0.059 Uiso 1 1 calc R . . C15 C -0.1003(11) 0.1581(6) 0.8941(7) 0.040(3) Uani 1 1 d . . . H15 H -0.0658 0.1606 0.9452 0.048 Uiso 1 1 calc R . . C16 C -0.2082(12) 0.1280(7) 0.8761(9) 0.057(4) Uani 1 1 d . . . H16 H -0.2427 0.1068 0.9142 0.068 Uiso 1 1 calc R . . C17 C -0.2648(13) 0.1289(6) 0.8032(11) 0.063(5) Uani 1 1 d . . . H17 H -0.3397 0.1096 0.7922 0.075 Uiso 1 1 calc R . . C18 C -0.2141(15) 0.1575(7) 0.7458(10) 0.069(5) Uani 1 1 d . . . H18 H -0.2533 0.1586 0.6957 0.082 Uiso 1 1 calc R . . C19 C 0.0852(11) 0.2678(5) 0.9335(8) 0.039(3) Uani 1 1 d . . . C20 C 0.0034(13) 0.3140(7) 0.9199(10) 0.073(6) Uani 1 1 d . . . H20 H -0.0466 0.3178 0.8735 0.088 Uiso 1 1 calc R . . C21 C 0.0002(15) 0.3547(7) 0.9802(14) 0.103(8) Uani 1 1 d . . . H21 H -0.0512 0.3872 0.9723 0.124 Uiso 1 1 calc R . . C22 C 0.0663(15) 0.3491(8) 1.0467(10) 0.074(6) Uani 1 1 d . . . H22 H 0.0579 0.3755 1.0866 0.088 Uiso 1 1 calc R . . C23 C 0.1439(16) 0.3059(7) 1.0561(10) 0.067(5) Uani 1 1 d . . . H23 H 0.1938 0.3028 1.1026 0.080 Uiso 1 1 calc R . . C24 C 0.1546(13) 0.2665(6) 1.0024(7) 0.046(4) Uani 1 1 d . . . H24 H 0.2120 0.2365 1.0120 0.055 Uiso 1 1 calc R . . C25 C 0.1260(11) 0.2601(6) 0.7755(7) 0.045(4) Uani 1 1 d . . . H25A H 0.1258 0.2353 0.7303 0.054 Uiso 1 1 calc R . . H25B H 0.0627 0.2898 0.7657 0.054 Uiso 1 1 calc R . . C26 C 0.2536(11) 0.2885(5) 0.7954(8) 0.047(4) Uani 1 1 d . . . H26A H 0.2502 0.3164 0.8372 0.057 Uiso 1 1 calc R . . H26B H 0.2779 0.3093 0.7507 0.057 Uiso 1 1 calc R . . C27 C 0.4886(11) 0.2710(5) 0.8712(7) 0.035(3) Uani 1 1 d . . . C28 C 0.4980(13) 0.3296(6) 0.8686(8) 0.052(4) Uani 1 1 d . . . H28 H 0.4353 0.3506 0.8407 0.063 Uiso 1 1 calc R . . C29 C 0.5931(16) 0.3589(7) 0.9041(10) 0.067(5) Uani 1 1 d . . . H29 H 0.5969 0.3995 0.9009 0.080 Uiso 1 1 calc R . . C30 C 0.6849(14) 0.3280(8) 0.9455(10) 0.071(6) Uani 1 1 d . . . H30 H 0.7513 0.3478 0.9715 0.085 Uiso 1 1 calc R . . C31 C 0.6799(15) 0.2695(9) 0.9487(10) 0.089(6) Uani 1 1 d . . . H31 H 0.7431 0.2485 0.9763 0.107 Uiso 1 1 calc R . . C32 C 0.5825(12) 0.2413(7) 0.9115(9) 0.058(4) Uani 1 1 d . . . H32 H 0.5795 0.2006 0.9134 0.070 Uiso 1 1 calc R . . C33 C 0.4135(11) 0.2057(6) 0.7353(7) 0.039(3) Uani 1 1 d . . . C34 C 0.4702(12) 0.2427(6) 0.6900(8) 0.050(4) Uani 1 1 d . . . H34 H 0.4855 0.2812 0.7060 0.060 Uiso 1 1 calc R . . C35 C 0.5044(16) 0.2248(8) 0.6224(10) 0.083(6) Uani 1 1 d . . . H35 H 0.5430 0.2507 0.5913 0.100 Uiso 1 1 calc R . . C36 C 0.4835(15) 0.1712(9) 0.6004(9) 0.080(6) Uani 1 1 d . . . H36 H 0.5052 0.1589 0.5526 0.096 Uiso 1 1 calc R . . C37 C 0.4281(13) 0.1313(7) 0.6482(8) 0.056(4) Uani 1 1 d . . . H37 H 0.4158 0.0926 0.6326 0.068 Uiso 1 1 calc R . . C38 C 0.3938(12) 0.1489(5) 0.7147(8) 0.042(4) Uani 1 1 d . . . H38 H 0.3570 0.1231 0.7468 0.051 Uiso 1 1 calc R . . Cl2 Cl 0.9263(4) 0.29806(18) 0.6027(2) 0.0718(13) Uani 1 1 d . . . Cl3 Cl 0.7683(4) 0.32331(18) 0.7187(3) 0.0767(13) Uani 1 1 d . . . Cl4 Cl 0.7518(5) 0.3893(2) 0.5806(3) 0.0939(16) Uani 1 1 d . . . C41 C 0.8528(15) 0.3523(6) 0.6493(8) 0.059(4) Uani 1 1 d . . . H41 H 0.9139 0.3799 0.6735 0.070 Uiso 1 1 calc R . . Cl11 Cl 0.2941(7) 0.4317(3) 0.9607(5) 0.0654(13) Uiso 0.50 1 d P . . Cl12 Cl 0.3784(7) 0.5047(3) 0.8531(5) 0.0654(13) Uiso 0.50 1 d P . . Cl13 Cl 0.1849(7) 0.5424(4) 0.9183(5) 0.0654(13) Uiso 0.50 1 d P . . C42 C 0.253(3) 0.4796(13) 0.8965(17) 0.0654(13) Uiso 0.50 1 d P . . H42 H 0.1978 0.4601 0.8565 0.079 Uiso 0.50 1 calc PR . . Cl10 Cl 0.0884(3) 0.41192(12) 0.75254(16) 0.0341(7) Uani 1 1 d . . . O11 O 0.1165(18) 0.5049(9) 0.9577(11) 0.0654(13) Uiso 0.50 1 d P . . 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 Pt1 0.0242(2) 0.0293(3) 0.0396(3) 0.0066(3) 0.0066(2) -0.0007(3) P1 0.0261(17) 0.0295(18) 0.0381(19) 0.0031(15) 0.0048(15) 0.0002(13) P2 0.0268(17) 0.0305(19) 0.042(2) 0.0049(16) 0.0082(16) -0.0027(13) Cl1 0.0218(15) 0.0353(18) 0.055(2) 0.0173(15) 0.0096(15) 0.0069(12) C1 0.011(5) 0.015(6) 0.057(8) 0.002(6) 0.007(6) -0.004(4) N1 0.027(6) 0.033(6) 0.028(5) 0.001(5) 0.006(5) -0.003(4) N2 0.024(5) 0.026(6) 0.034(6) 0.003(5) 0.004(5) 0.002(4) C2 0.020(6) 0.018(6) 0.054(8) 0.007(6) 0.004(6) 0.003(5) C3 0.042(8) 0.019(6) 0.029(7) -0.003(5) 0.001(6) 0.006(5) C4 0.020(6) 0.028(7) 0.048(8) 0.000(6) 0.005(6) -0.002(5) C5 0.035(7) 0.032(7) 0.035(7) 0.006(6) 0.009(6) 0.001(5) C6 0.037(8) 0.041(8) 0.035(7) 0.004(6) 0.008(6) 0.002(6) C7 0.056(9) 0.040(8) 0.039(8) -0.001(7) 0.014(7) 0.007(7) C8 0.108(15) 0.083(13) 0.054(10) -0.003(9) 0.049(11) 0.019(11) C9 0.035(8) 0.029(7) 0.048(8) 0.008(6) -0.009(7) -0.013(6) C10 0.028(8) 0.062(10) 0.051(9) -0.011(8) 0.000(7) -0.002(7) C11 0.075(13) 0.061(12) 0.089(14) -0.024(11) -0.003(11) 0.007(10) C12 0.079(16) 0.115(18) 0.125(18) 0.025(15) -0.027(14) 0.041(13) C13 0.031(7) 0.030(7) 0.043(8) -0.006(6) 0.008(7) 0.007(5) C14 0.046(9) 0.047(9) 0.057(10) 0.013(8) 0.011(8) 0.011(7) C15 0.028(7) 0.052(9) 0.040(7) -0.004(7) 0.007(6) -0.004(6) C16 0.034(9) 0.069(11) 0.067(11) 0.003(9) 0.001(9) -0.013(7) C17 0.031(9) 0.050(10) 0.106(15) -0.025(10) 0.004(10) 0.000(7) C18 0.061(11) 0.067(12) 0.076(12) -0.010(10) 0.004(10) -0.004(10) C19 0.028(7) 0.033(8) 0.055(9) 0.005(7) 0.000(7) -0.010(6) C20 0.038(10) 0.093(14) 0.087(13) -0.032(11) -0.008(9) 0.025(9) C21 0.041(11) 0.063(13) 0.21(3) -0.072(15) 0.018(14) 0.008(8) C22 0.051(11) 0.101(17) 0.069(12) -0.059(12) 0.005(10) -0.024(10) C23 0.063(12) 0.078(14) 0.059(11) 0.001(10) 0.003(10) -0.006(10) C24 0.057(10) 0.046(9) 0.033(8) -0.004(7) 0.001(7) 0.005(7) C25 0.044(8) 0.039(8) 0.051(9) 0.023(7) 0.004(7) 0.013(6) C26 0.037(8) 0.041(9) 0.066(10) 0.030(8) 0.016(8) 0.006(6) C27 0.032(7) 0.038(8) 0.041(8) -0.005(6) 0.023(7) -0.007(6) C28 0.049(9) 0.053(10) 0.054(9) 0.011(8) 0.003(8) -0.023(8) C29 0.068(12) 0.049(10) 0.088(13) -0.008(9) 0.032(11) -0.025(9) C30 0.045(10) 0.076(14) 0.095(14) -0.042(12) 0.021(10) -0.034(9) C31 0.049(11) 0.110(17) 0.104(16) -0.046(14) -0.006(11) 0.010(11) C32 0.039(9) 0.044(9) 0.094(13) -0.020(9) 0.019(9) -0.010(7) C33 0.041(8) 0.034(8) 0.042(8) -0.003(6) 0.005(7) -0.001(6) C34 0.058(9) 0.047(9) 0.049(9) -0.001(7) 0.021(8) -0.024(7) C35 0.097(15) 0.097(16) 0.061(12) -0.018(11) 0.033(11) -0.052(12) C36 0.065(12) 0.135(18) 0.046(10) -0.017(12) 0.033(9) 0.003(12) C37 0.054(10) 0.064(11) 0.050(9) -0.019(8) -0.003(8) 0.005(8) C38 0.050(9) 0.036(9) 0.041(8) 0.005(6) 0.010(7) 0.006(6) Cl2 0.095(3) 0.069(3) 0.049(2) -0.009(2) -0.005(2) 0.026(2) Cl3 0.069(3) 0.073(3) 0.090(3) 0.001(2) 0.013(3) -0.003(2) Cl4 0.111(4) 0.088(4) 0.077(3) -0.006(3) -0.018(3) 0.034(3) C41 0.076(12) 0.054(11) 0.044(9) 0.005(7) -0.003(8) 0.023(8) Cl10 0.0449(19) 0.0257(16) 0.0296(16) 0.0018(13) -0.0060(14) 0.0057(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.045(10) . ? Pt1 P1 2.239(3) . ? Pt1 P2 2.307(3) . ? Pt1 Cl1 2.383(3) . ? P1 C19 1.787(14) . ? P1 C13 1.804(13) . ? P1 C25 1.823(12) . ? P2 C27 1.796(13) . ? P2 C26 1.823(12) . ? P2 C33 1.827(13) . ? C1 N1 1.327(13) . ? C1 N2 1.352(14) . ? N1 C2 1.402(13) . ? N1 C5 1.463(14) . ? N2 C4 1.398(13) 3_557 ? N2 C9 1.457(14) . ? C2 C3 1.355(15) . ? C2 C4 1.455(17) 3_557 ? C3 C4 1.387(15) . ? C4 N2 1.398(13) 3_557 ? C4 C2 1.455(17) 3_557 ? C5 C6 1.524(14) . ? C6 C7 1.515(15) . ? C7 C8 1.513(16) . ? C9 C10 1.580(17) . ? C10 C11 1.523(19) . ? C11 C12 1.50(2) . ? C13 C15 1.368(16) . ? C13 C14 1.376(17) . ? C14 C18 1.437(19) . ? C15 C16 1.401(17) . ? C16 C17 1.38(2) . ? C17 C18 1.39(2) . ? C19 C24 1.377(18) . ? C19 C20 1.414(18) . ? C20 C21 1.43(2) . ? C21 C22 1.33(3) . ? C22 C23 1.33(2) . ? C23 C24 1.338(19) . ? C25 C26 1.574(17) . ? C27 C28 1.371(16) . ? C27 C32 1.389(19) . ? C28 C29 1.359(19) . ? C29 C30 1.40(2) . ? C30 C31 1.37(2) . ? C31 C32 1.38(2) . ? C33 C34 1.376(16) . ? C33 C38 1.384(17) . ? C34 C35 1.361(18) . ? C35 C36 1.32(2) . ? C36 C37 1.44(2) . ? C37 C38 1.343(17) . ? Cl2 C41 1.758(14) . ? Cl3 C41 1.759(15) . ? Cl4 C41 1.793(14) . ? Cl11 C42 1.63(3) . ? Cl12 C42 1.76(3) . ? Cl13 C42 1.71(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 93.2(3) . . ? C1 Pt1 P2 175.0(4) . . ? P1 Pt1 P2 84.89(11) . . ? C1 Pt1 Cl1 88.2(3) . . ? P1 Pt1 Cl1 178.51(11) . . ? P2 Pt1 Cl1 93.67(11) . . ? C19 P1 C13 106.5(6) . . ? C19 P1 C25 106.5(6) . . ? C13 P1 C25 106.1(6) . . ? C19 P1 Pt1 111.3(5) . . ? C13 P1 Pt1 118.7(4) . . ? C25 P1 Pt1 106.9(4) . . ? C27 P2 C26 103.7(6) . . ? C27 P2 C33 106.5(6) . . ? C26 P2 C33 105.3(6) . . ? C27 P2 Pt1 121.3(4) . . ? C26 P2 Pt1 107.3(4) . . ? C33 P2 Pt1 111.4(4) . . ? N1 C1 N2 108.6(9) . . ? N1 C1 Pt1 124.7(9) . . ? N2 C1 Pt1 126.6(8) . . ? C1 N1 C2 111.4(10) . . ? C1 N1 C5 126.0(10) . . ? C2 N1 C5 122.5(10) . . ? C1 N2 C4 110.1(10) . 3_557 ? C1 N2 C9 127.5(10) . . ? C4 N2 C9 121.6(10) 3_557 . ? C3 C2 N1 132.4(13) . . ? C3 C2 C4 123.2(11) . 3_557 ? N1 C2 C4 104.4(10) . 3_557 ? C2 C3 C4 113.9(11) . . ? C3 C4 N2 131.5(12) . 3_557 ? C3 C4 C2 122.9(11) . 3_557 ? N2 C4 C2 105.5(10) 3_557 3_557 ? N1 C5 C6 112.7(10) . . ? C7 C6 C5 109.5(10) . . ? C8 C7 C6 110.0(11) . . ? N2 C9 C10 109.0(10) . . ? C11 C10 C9 110.9(11) . . ? C12 C11 C10 111.9(14) . . ? C15 C13 C14 120.1(13) . . ? C15 C13 P1 120.5(11) . . ? C14 C13 P1 119.4(10) . . ? C13 C14 C18 120.9(14) . . ? C13 C15 C16 119.9(13) . . ? C17 C16 C15 120.2(14) . . ? C16 C17 C18 121.2(15) . . ? C17 C18 C14 117.3(16) . . ? C24 C19 C20 117.5(14) . . ? C24 C19 P1 123.7(11) . . ? C20 C19 P1 118.6(12) . . ? C19 C20 C21 116.2(16) . . ? C22 C21 C20 122.8(17) . . ? C23 C22 C21 118.7(16) . . ? C22 C23 C24 122.4(17) . . ? C23 C24 C19 122.3(15) . . ? C26 C25 P1 104.8(9) . . ? C25 C26 P2 108.9(8) . . ? C28 C27 C32 117.3(13) . . ? C28 C27 P2 122.7(11) . . ? C32 C27 P2 120.0(10) . . ? C29 C28 C27 122.9(16) . . ? C28 C29 C30 118.6(15) . . ? C31 C30 C29 120.4(16) . . ? C30 C31 C32 119.3(18) . . ? C31 C32 C27 121.5(15) . . ? C34 C33 C38 121.0(12) . . ? C34 C33 P2 119.1(10) . . ? C38 C33 P2 119.9(10) . . ? C35 C34 C33 120.6(14) . . ? C36 C35 C34 119.6(15) . . ? C35 C36 C37 120.6(15) . . ? C38 C37 C36 120.0(15) . . ? C37 C38 C33 118.2(13) . . ? Cl2 C41 Cl3 111.2(8) . . ? Cl2 C41 Cl4 108.4(8) . . ? Cl3 C41 Cl4 108.5(9) . . ? Cl11 C42 Cl13 121.8(18) . . ? Cl11 C42 Cl12 110.9(18) . . ? Cl13 C42 Cl12 101.8(16) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 72.51 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.809 _refine_diff_density_min -2.160 _refine_diff_density_rms 0.196 # Attachment 'cif-3c.cif' data_han4494 _database_code_depnum_ccdc_archive 'CCDC 728541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H67 Br3 N4 O P2 Pt' _chemical_formula_weight 1248.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 42.4557(6) _cell_length_b 11.1735(5) _cell_length_c 28.2309(7) _cell_angle_alpha 90.00 _cell_angle_beta 123.574(1) _cell_angle_gamma 90.00 _cell_volume 11158.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10459 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4976 _exptl_absorpt_coefficient_mu 4.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3826 _exptl_absorpt_correction_T_max 0.8704 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40673 _diffrn_reflns_av_R_equivalents 0.081 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9983 _reflns_number_gt 5318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Free Br-ions splitted over two positions, phenyl groups refined with geometrical (AFIX 66) restraints, also SADI and ISOR was used. ; _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^)+(0.1379P)^2^+29.1831P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9983 _refine_ls_number_parameters 531 _refine_ls_number_restraints 376 _refine_ls_R_factor_all 0.1446 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2579 _refine_ls_wR_factor_gt 0.2194 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.047 _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 Pt Pt 0.387285(13) 0.43421(5) 0.26783(2) 0.0825(3) Uani 1 1 d . . . Br Br 0.37257(5) 0.50716(19) 0.33647(7) 0.1150(6) Uani 1 1 d . . . P1 P 0.44849(9) 0.3842(4) 0.33738(15) 0.0887(11) Uani 1 1 d . . . P2 P 0.40317(8) 0.3743(4) 0.20832(14) 0.0867(11) Uani 1 1 d . . . C1 C 0.3312(3) 0.4513(13) 0.2042(5) 0.075(3) Uani 1 1 d U . . N2 N 0.3071(3) 0.3542(10) 0.1908(4) 0.078(3) Uani 1 1 d . . . C3 C 0.2717(3) 0.3845(13) 0.1430(5) 0.077(3) Uani 1 1 d U . . C4 C 0.2387(3) 0.3197(13) 0.1128(5) 0.077(3) Uani 1 1 d U . . H4 H 0.2365 0.2406 0.1220 0.092 Uiso 1 1 calc R . . C5 C 0.2096(4) 0.3802(15) 0.0686(6) 0.086(4) Uani 1 1 d U . . N6 N 0.1714(3) 0.3435(11) 0.0277(5) 0.084(3) Uani 1 1 d . . . C7 C 0.1543(4) 0.4318(16) -0.0091(7) 0.095(4) Uani 1 1 d U . . H7 H 0.1291 0.4286 -0.0405 0.114 Uiso 1 1 calc R . . N8 N 0.1766(3) 0.5250(12) 0.0034(5) 0.089(3) Uani 1 1 d . . . C9 C 0.2120(3) 0.4969(14) 0.0516(5) 0.081(3) Uani 1 1 d U . . C10 C 0.2445(3) 0.5638(13) 0.0804(6) 0.085(4) Uani 1 1 d U . . H10 H 0.2465 0.6420 0.0700 0.102 Uiso 1 1 calc R . . C11 C 0.2742(3) 0.5031(13) 0.1267(6) 0.079(3) Uani 1 1 d U . . N12 N 0.3128(3) 0.5382(11) 0.1666(5) 0.087(3) Uani 1 1 d . . . C13 C 0.3143(3) 0.2442(12) 0.2210(5) 0.080(4) Uani 1 1 d DU . . H13A H 0.3417 0.2307 0.2443 0.096 Uiso 1 1 calc R . . H13B H 0.3029 0.1788 0.1933 0.096 Uiso 1 1 calc R . . C14 C 0.2997(4) 0.2386(13) 0.2587(5) 0.099(4) Uani 1 1 d DU . . H14A H 0.3107 0.3048 0.2860 0.119 Uiso 1 1 calc R . . H14B H 0.2723 0.2502 0.2353 0.119 Uiso 1 1 calc R . . C15 C 0.3081(5) 0.1243(14) 0.2907(7) 0.120(5) Uani 1 1 d DU . . H15A H 0.2997 0.0573 0.2640 0.144 Uiso 1 1 calc R . . H15B H 0.3355 0.1171 0.3176 0.144 Uiso 1 1 calc R . . C16 C 0.2899(6) 0.1146(18) 0.3223(9) 0.156(7) Uani 1 1 d DU . . H16A H 0.2975 0.1817 0.3483 0.234 Uiso 1 1 calc R . . H16B H 0.2974 0.0404 0.3437 0.234 Uiso 1 1 calc R . . H16C H 0.2626 0.1156 0.2958 0.234 Uiso 1 1 calc R . . C17 C 0.1554(4) 0.2299(14) 0.0296(6) 0.099(4) Uani 1 1 d DU . . H17A H 0.1719 0.1647 0.0328 0.119 Uiso 1 1 calc R . . H17B H 0.1307 0.2190 -0.0061 0.119 Uiso 1 1 calc R . . C18 C 0.1507(5) 0.2226(18) 0.0779(7) 0.143(7) Uani 1 1 d DU . . H18A H 0.1455 0.1389 0.0818 0.172 Uiso 1 1 calc R . . H18B H 0.1748 0.2441 0.1126 0.172 Uiso 1 1 calc R . . C19 C 0.1207(5) 0.2974(16) 0.0749(8) 0.149(7) Uani 1 1 d DU . . H19A H 0.1250 0.3011 0.1128 0.178 Uiso 1 1 calc R . . H19B H 0.1226 0.3790 0.0640 0.178 Uiso 1 1 calc R . . C20 C 0.0825(5) 0.251(2) 0.0342(11) 0.215(11) Uani 1 1 d DU . . H20A H 0.0649 0.3177 0.0174 0.322 Uiso 1 1 calc R . . H20B H 0.0750 0.1989 0.0538 0.322 Uiso 1 1 calc R . . H20C H 0.0823 0.2068 0.0045 0.322 Uiso 1 1 calc R . . C21 C 0.1673(4) 0.6340(15) -0.0268(7) 0.107(5) Uani 1 1 d DU . . H21A H 0.1474 0.6171 -0.0665 0.128 Uiso 1 1 calc R . . H21B H 0.1896 0.6602 -0.0261 0.128 Uiso 1 1 calc R . . C22 C 0.1545(8) 0.7362(18) -0.0081(13) 0.224(12) Uani 1 1 d DU . . H22A H 0.1444 0.7973 -0.0380 0.269 Uiso 1 1 calc R . . H22B H 0.1769 0.7707 0.0258 0.269 Uiso 1 1 calc R . . C23 C 0.1258(7) 0.714(2) 0.0053(12) 0.220(12) Uani 1 1 d DU . . H23A H 0.1008 0.7059 -0.0301 0.264 Uiso 1 1 calc R . . H23B H 0.1317 0.6393 0.0267 0.264 Uiso 1 1 calc R . . C24 C 0.1252(8) 0.814(3) 0.0390(12) 0.235(13) Uani 1 1 d DU . . H24A H 0.1461 0.8048 0.0784 0.352 Uiso 1 1 calc R . . H24B H 0.1015 0.8126 0.0366 0.352 Uiso 1 1 calc R . . H24C H 0.1277 0.8890 0.0243 0.352 Uiso 1 1 calc R . . C25 C 0.3280(4) 0.6533(13) 0.1669(7) 0.099(5) Uani 1 1 d DU . . H25A H 0.3130 0.6858 0.1282 0.119 Uiso 1 1 calc R . . H25B H 0.3538 0.6417 0.1766 0.119 Uiso 1 1 calc R . . C26 C 0.3291(7) 0.7440(17) 0.2062(9) 0.199(11) Uani 1 1 d DU . . H26A H 0.3420 0.7090 0.2443 0.239 Uiso 1 1 calc R . . H26B H 0.3031 0.7620 0.1942 0.239 Uiso 1 1 calc R . . C27 C 0.3483(8) 0.8587(17) 0.2098(10) 0.221(12) Uani 1 1 d DU . . H27A H 0.3563 0.8552 0.1833 0.265 Uiso 1 1 calc R . . H27B H 0.3300 0.9242 0.1976 0.265 Uiso 1 1 calc R . . C28 C 0.3812(10) 0.886(4) 0.2667(14) 0.37(3) Uani 1 1 d DU . . H28A H 0.3950 0.9523 0.2645 0.549 Uiso 1 1 calc R . . H28B H 0.3975 0.8161 0.2818 0.549 Uiso 1 1 calc R . . H28C H 0.3729 0.9068 0.2914 0.549 Uiso 1 1 calc R . . C29 C 0.4728(3) 0.3542(15) 0.3013(5) 0.094(4) Uani 1 1 d U . . H29A H 0.4792 0.4293 0.2905 0.113 Uiso 1 1 calc R . . H29B H 0.4961 0.3089 0.3261 0.113 Uiso 1 1 calc R . . C30 C 0.4446(3) 0.2802(13) 0.2478(5) 0.088(4) Uani 1 1 d U . . H30A H 0.4384 0.2046 0.2584 0.106 Uiso 1 1 calc R . . H30B H 0.4552 0.2628 0.2253 0.106 Uiso 1 1 calc R . . C31 C 0.4776(3) 0.4963(12) 0.3901(4) 0.096(4) Uani 1 1 d GU . . C32 C 0.4670(3) 0.6150(14) 0.3748(5) 0.141(7) Uani 1 1 d GU . . H32 H 0.4456 0.6336 0.3388 0.169 Uiso 1 1 calc R . . C33 C 0.4882(4) 0.7062(10) 0.4129(7) 0.172(9) Uani 1 1 d GU . . H33 H 0.4811 0.7864 0.4025 0.207 Uiso 1 1 calc R . . C34 C 0.5199(4) 0.6787(12) 0.4662(6) 0.147(7) Uani 1 1 d GU . . H34 H 0.5343 0.7403 0.4919 0.176 Uiso 1 1 calc R . . C35 C 0.5305(3) 0.5599(14) 0.4815(4) 0.128(6) Uani 1 1 d GU . . H35 H 0.5519 0.5413 0.5176 0.154 Uiso 1 1 calc R . . C36 C 0.5093(3) 0.4687(10) 0.4435(5) 0.120(6) Uani 1 1 d GU . . H36 H 0.5164 0.3885 0.4539 0.144 Uiso 1 1 calc R . . C41 C 0.4510(3) 0.2500(9) 0.3752(4) 0.096(4) Uani 1 1 d GU . . C42 C 0.4822(3) 0.1753(12) 0.3975(5) 0.119(5) Uani 1 1 d GU . . H42 H 0.5025 0.1965 0.3944 0.143 Uiso 1 1 calc R . . C43 C 0.4836(3) 0.0692(11) 0.4243(5) 0.166(9) Uani 1 1 d GU . . H43 H 0.5047 0.0187 0.4393 0.200 Uiso 1 1 calc R . . C44 C 0.4537(4) 0.0378(9) 0.4288(5) 0.144(7) Uani 1 1 d GU . . H44 H 0.4546 -0.0339 0.4469 0.172 Uiso 1 1 calc R . . C45 C 0.4224(3) 0.1126(12) 0.4066(5) 0.121(5) Uani 1 1 d GU . . H45 H 0.4022 0.0913 0.4096 0.145 Uiso 1 1 calc R . . C46 C 0.4210(3) 0.2186(10) 0.3798(4) 0.106(5) Uani 1 1 d GU . . H46 H 0.3999 0.2692 0.3647 0.127 Uiso 1 1 calc R . . C51 C 0.4199(3) 0.4909(11) 0.1832(5) 0.099(4) Uani 1 1 d GU . . C52 C 0.4269(3) 0.4679(11) 0.1414(5) 0.121(5) Uani 1 1 d GU . . H52 H 0.4218 0.3918 0.1245 0.145 Uiso 1 1 calc R . . C53 C 0.4415(3) 0.5575(15) 0.1246(5) 0.134(7) Uani 1 1 d GU . . H53 H 0.4462 0.5419 0.0963 0.161 Uiso 1 1 calc R . . C54 C 0.4491(4) 0.6700(13) 0.1497(7) 0.184(10) Uani 1 1 d GU . . H54 H 0.4589 0.7306 0.1383 0.221 Uiso 1 1 calc R . . C55 C 0.4421(4) 0.6930(11) 0.1915(7) 0.186(10) Uani 1 1 d GU . . H55 H 0.4473 0.7691 0.2084 0.223 Uiso 1 1 calc R . . C56 C 0.4276(3) 0.6035(13) 0.2083(5) 0.145(7) Uani 1 1 d GU . . H56 H 0.4229 0.6190 0.2365 0.174 Uiso 1 1 calc R . . C61 C 0.3654(2) 0.3023(10) 0.1468(3) 0.094(4) Uani 1 1 d GU . . C62 C 0.3393(3) 0.3699(8) 0.0999(4) 0.100(4) Uani 1 1 d GU . . H62 H 0.3439 0.4515 0.0979 0.120 Uiso 1 1 calc R . . C63 C 0.3063(2) 0.3170(11) 0.0559(3) 0.112(5) Uani 1 1 d GU . . H63 H 0.2886 0.3627 0.0242 0.134 Uiso 1 1 calc R . . C64 C 0.2994(2) 0.1964(11) 0.0588(4) 0.101(4) Uani 1 1 d GU . . H64 H 0.2771 0.1606 0.0291 0.122 Uiso 1 1 calc R . . C65 C 0.3256(3) 0.1288(8) 0.1057(4) 0.121(5) Uani 1 1 d GU . . H65 H 0.3210 0.0473 0.1077 0.145 Uiso 1 1 calc R . . C66 C 0.3586(2) 0.1818(10) 0.1498(3) 0.093(4) Uani 1 1 d GU . . H66 H 0.3763 0.1361 0.1815 0.111 Uiso 1 1 calc R . . O100 O 0.2394(4) 0.0398(13) 0.1366(6) 0.158(5) Uani 1 1 d . . . H100 H 0.2445 -0.0024 0.1175 0.237 Uiso 1 1 calc R . . C101 C 0.2234(7) -0.031(2) 0.1587(11) 0.181(9) Uani 1 1 d U . . H10A H 0.2359 -0.1086 0.1698 0.272 Uiso 1 1 calc R . . H10B H 0.1967 -0.0427 0.1300 0.272 Uiso 1 1 calc R . . H10C H 0.2264 0.0077 0.1916 0.272 Uiso 1 1 calc R . . Br1A Br 0.24879(6) -0.0954(2) 0.04907(10) 0.1026(9) Uani 0.748(4) 1 d PU A 1 Br1B Br 0.2004(2) -0.0432(7) 0.0022(4) 0.121(3) Uani 0.252(4) 1 d PU A 2 Br2A Br 0.0631(2) 0.3543(17) -0.1186(4) 0.110(3) Uani 0.58(3) 1 d PU B 1 Br2B Br 0.0563(3) 0.416(2) -0.1290(5) 0.125(3) Uani 0.42(3) 1 d PU B 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 Pt 0.0470(3) 0.1376(6) 0.0676(3) -0.0035(3) 0.0347(2) -0.0021(3) Br 0.0881(10) 0.1771(17) 0.1048(12) -0.0235(12) 0.0691(10) -0.0096(11) P1 0.0487(17) 0.153(3) 0.0599(19) -0.009(2) 0.0270(16) -0.0009(19) P2 0.0451(16) 0.156(3) 0.0564(18) -0.001(2) 0.0266(15) 0.0072(19) C1 0.049(6) 0.131(10) 0.069(7) 0.003(7) 0.047(6) 0.000(7) N2 0.060(6) 0.115(9) 0.071(7) 0.005(6) 0.044(6) 0.005(6) C3 0.047(6) 0.112(9) 0.074(8) -0.011(7) 0.035(6) -0.013(6) C4 0.065(7) 0.109(9) 0.070(7) 0.012(7) 0.046(6) 0.011(7) C5 0.059(7) 0.132(10) 0.075(8) -0.028(8) 0.043(7) -0.021(7) N6 0.060(6) 0.107(9) 0.081(8) -0.020(7) 0.037(6) -0.012(6) C7 0.063(8) 0.131(12) 0.088(9) -0.007(9) 0.040(7) -0.005(8) N8 0.062(7) 0.108(9) 0.075(7) 0.006(7) 0.024(6) 0.011(6) C9 0.062(7) 0.117(10) 0.069(7) -0.006(7) 0.040(6) 0.001(7) C10 0.048(6) 0.112(9) 0.091(9) -0.005(7) 0.036(6) -0.008(6) C11 0.056(7) 0.098(9) 0.090(9) -0.002(7) 0.046(7) -0.002(6) N12 0.045(5) 0.123(10) 0.085(8) 0.002(7) 0.030(6) -0.004(6) C13 0.063(7) 0.111(10) 0.081(8) -0.001(7) 0.049(6) 0.008(6) C14 0.086(9) 0.142(12) 0.078(8) -0.006(8) 0.050(7) -0.014(8) C15 0.114(11) 0.158(12) 0.114(11) 0.008(10) 0.079(10) -0.016(10) C16 0.179(15) 0.172(14) 0.149(14) 0.037(11) 0.111(12) -0.005(12) C17 0.081(8) 0.123(11) 0.087(9) -0.014(8) 0.043(7) -0.021(8) C18 0.120(12) 0.188(15) 0.149(14) 0.007(12) 0.092(11) -0.003(11) C19 0.129(12) 0.162(14) 0.174(15) 0.005(12) 0.095(12) -0.009(11) C20 0.173(17) 0.227(19) 0.223(19) 0.009(15) 0.096(14) 0.015(14) C21 0.076(8) 0.140(12) 0.103(10) -0.019(10) 0.049(8) 0.009(8) C22 0.198(18) 0.25(2) 0.27(2) 0.024(16) 0.161(16) 0.020(15) C23 0.205(18) 0.25(2) 0.24(2) 0.032(16) 0.147(15) 0.042(15) C24 0.21(2) 0.221(19) 0.23(2) -0.036(16) 0.096(15) -0.003(15) C25 0.062(7) 0.110(10) 0.119(11) -0.003(8) 0.046(7) -0.025(7) C26 0.234(19) 0.163(16) 0.186(17) 0.040(13) 0.107(14) -0.044(13) C27 0.25(2) 0.176(17) 0.203(19) 0.024(14) 0.102(15) -0.012(15) C28 0.36(3) 0.35(3) 0.36(3) 0.001(19) 0.18(2) -0.015(18) C29 0.056(7) 0.156(12) 0.072(8) -0.007(8) 0.035(6) 0.010(7) C30 0.055(6) 0.121(10) 0.070(8) -0.010(7) 0.023(6) 0.004(7) C31 0.059(7) 0.157(12) 0.082(9) -0.008(9) 0.046(7) -0.017(8) C32 0.115(12) 0.157(13) 0.150(14) -0.037(12) 0.073(11) -0.017(11) C33 0.144(14) 0.168(15) 0.200(17) -0.037(13) 0.091(13) 0.011(12) C34 0.124(12) 0.213(16) 0.135(13) -0.045(12) 0.092(11) -0.030(12) C35 0.123(12) 0.178(15) 0.110(11) -0.032(11) 0.081(10) -0.050(11) C36 0.106(11) 0.187(14) 0.075(9) -0.023(9) 0.054(8) -0.042(10) C41 0.073(8) 0.140(11) 0.064(7) 0.001(8) 0.031(7) -0.003(8) C42 0.108(11) 0.132(12) 0.092(10) 0.004(9) 0.039(9) 0.009(9) C43 0.152(15) 0.167(16) 0.145(15) 0.012(12) 0.060(12) 0.002(12) C44 0.152(14) 0.159(14) 0.113(12) 0.024(10) 0.069(11) 0.018(12) C45 0.106(11) 0.126(11) 0.097(10) 0.007(9) 0.034(9) -0.005(10) C46 0.087(9) 0.132(12) 0.090(9) -0.008(9) 0.043(8) -0.016(8) C51 0.061(7) 0.162(12) 0.093(9) 0.019(9) 0.055(7) 0.008(8) C52 0.086(9) 0.179(13) 0.115(11) 0.033(10) 0.066(9) 0.026(9) C53 0.112(11) 0.189(15) 0.140(13) 0.038(11) 0.094(11) 0.027(10) C54 0.156(15) 0.209(18) 0.218(18) 0.031(14) 0.122(14) -0.017(13) C55 0.173(16) 0.213(18) 0.203(17) 0.019(14) 0.123(14) -0.029(13) C56 0.091(10) 0.168(14) 0.185(16) 0.025(12) 0.082(11) -0.023(10) C61 0.062(7) 0.148(11) 0.082(9) -0.002(8) 0.046(7) 0.013(8) C62 0.065(8) 0.155(11) 0.079(9) -0.001(9) 0.040(7) 0.007(8) C63 0.070(8) 0.164(13) 0.094(10) 0.008(10) 0.041(8) 0.021(9) C64 0.059(7) 0.162(12) 0.078(9) -0.010(9) 0.035(7) 0.000(8) C65 0.084(9) 0.173(13) 0.112(11) -0.013(10) 0.058(9) 0.006(10) C66 0.054(7) 0.157(12) 0.059(7) -0.013(8) 0.026(6) -0.004(7) O100 0.168(13) 0.170(12) 0.169(13) -0.019(10) 0.115(11) -0.060(10) C101 0.165(16) 0.196(17) 0.177(17) -0.008(14) 0.091(13) -0.018(13) Br1A 0.0884(14) 0.1152(17) 0.1075(17) 0.0017(12) 0.0563(13) -0.0091(11) Br1B 0.112(5) 0.124(5) 0.130(6) -0.007(4) 0.069(4) -0.008(4) Br2A 0.058(2) 0.150(7) 0.110(3) -0.035(4) 0.039(2) -0.021(3) Br2B 0.074(3) 0.142(8) 0.115(4) -0.020(5) 0.026(3) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C1 2.051(12) . ? Pt P2 2.231(3) . ? Pt P1 2.297(3) . ? Pt Br 2.4795(16) . ? P1 C41 1.810(10) . ? P1 C31 1.810(10) . ? P1 C29 1.837(12) . ? P2 C61 1.775(8) . ? P2 C30 1.809(13) . ? P2 C51 1.807(10) . ? C1 N12 1.329(16) . ? C1 N2 1.392(16) . ? N2 C3 1.395(15) . ? N2 C13 1.429(15) . ? C3 C4 1.378(16) . ? C3 C11 1.427(19) . ? C4 C5 1.354(18) . ? C5 C9 1.41(2) . ? C5 N6 1.436(15) . ? N6 C7 1.321(17) . ? N6 C17 1.456(17) . ? C7 N8 1.319(17) . ? N8 C9 1.394(16) . ? N8 C21 1.411(19) . ? C9 C10 1.373(17) . ? C10 C11 1.390(18) . ? C11 N12 1.436(15) . ? N12 C25 1.437(16) . ? C13 C14 1.502(10) . ? C14 C15 1.489(10) . ? C15 C16 1.474(15) . ? C17 C18 1.485(10) . ? C18 C19 1.484(10) . ? C19 C20 1.470(15) . ? C21 C22 1.480(11) . ? C22 C23 1.484(11) . ? C23 C24 1.473(16) . ? C25 C26 1.484(11) . ? C26 C27 1.490(11) . ? C27 C28 1.463(16) . ? C29 C30 1.548(17) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C61 C62 1.3900 . ? C61 C66 1.3900 . ? C62 C63 1.3900 . ? C63 C64 1.3900 . ? C64 C65 1.3900 . ? C65 C66 1.3900 . ? O100 C101 1.40(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 C1 Pt P2 93.3(3) . . ? C1 Pt P1 171.3(4) . . ? P2 Pt P1 84.29(12) . . ? C1 Pt Br 88.9(3) . . ? P2 Pt Br 177.08(10) . . ? P1 Pt Br 93.83(10) . . ? C41 P1 C31 107.3(6) . . ? C41 P1 C29 108.0(7) . . ? C31 P1 C29 104.3(6) . . ? C41 P1 Pt 112.0(4) . . ? C31 P1 Pt 118.0(5) . . ? C29 P1 Pt 106.7(4) . . ? C61 P2 C30 112.5(6) . . ? C61 P2 C51 106.3(5) . . ? C30 P2 C51 101.5(6) . . ? C61 P2 Pt 112.8(3) . . ? C30 P2 Pt 107.9(5) . . ? C51 P2 Pt 115.3(5) . . ? N12 C1 N2 109.4(10) . . ? N12 C1 Pt 130.8(9) . . ? N2 C1 Pt 119.3(10) . . ? C1 N2 C3 108.1(11) . . ? C1 N2 C13 128.6(11) . . ? C3 N2 C13 123.1(11) . . ? C4 C3 N2 130.9(13) . . ? C4 C3 C11 121.4(12) . . ? N2 C3 C11 107.8(11) . . ? C5 C4 C3 113.9(13) . . ? C4 C5 C9 125.1(12) . . ? C4 C5 N6 130.3(15) . . ? C9 C5 N6 104.6(13) . . ? C7 N6 C5 107.8(12) . . ? C7 N6 C17 127.9(12) . . ? C5 N6 C17 124.2(13) . . ? N8 C7 N6 112.1(13) . . ? C7 N8 C9 108.2(13) . . ? C7 N8 C21 126.8(13) . . ? C9 N8 C21 125.0(13) . . ? C10 C9 N8 130.1(15) . . ? C10 C9 C5 122.6(13) . . ? N8 C9 C5 107.3(12) . . ? C9 C10 C11 112.6(13) . . ? C10 C11 C3 124.5(12) . . ? C10 C11 N12 130.6(13) . . ? C3 C11 N12 104.8(11) . . ? C1 N12 C25 125.9(11) . . ? C1 N12 C11 109.8(11) . . ? C25 N12 C11 124.2(12) . . ? N2 C13 C14 115.0(10) . . ? C15 C14 C13 114.3(10) . . ? C16 C15 C14 113.6(12) . . ? N6 C17 C18 112.7(12) . . ? C19 C18 C17 117.6(12) . . ? C20 C19 C18 112.8(13) . . ? N8 C21 C22 119.2(16) . . ? C21 C22 C23 118.4(14) . . ? C24 C23 C22 110.5(15) . . ? N12 C25 C26 116.4(13) . . ? C25 C26 C27 115.4(14) . . ? C28 C27 C26 114.0(16) . . ? C30 C29 P1 105.7(9) . . ? C29 C30 P2 104.7(9) . . ? C32 C31 C36 120.0 . . ? C32 C31 P1 116.7(8) . . ? C36 C31 P1 123.3(8) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C35 C36 C31 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 119.6(7) . . ? C46 C41 P1 120.4(7) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 P2 121.0(8) . . ? C56 C51 P2 119.0(8) . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C55 C54 C53 120.0 . . ? C54 C55 C56 120.0 . . ? C55 C56 C51 120.0 . . ? C62 C61 C66 120.0 . . ? C62 C61 P2 120.0(7) . . ? C66 C61 P2 119.1(7) . . ? C63 C62 C61 120.0 . . ? C62 C63 C64 120.0 . . ? C65 C64 C63 120.0 . . ? C66 C65 C64 120.0 . . ? C65 C66 C61 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pt P1 C41 -34(2) . . . . ? P2 Pt P1 C41 -108.4(4) . . . . ? Br Pt P1 C41 73.9(4) . . . . ? C1 Pt P1 C31 -159(2) . . . . ? P2 Pt P1 C31 126.4(4) . . . . ? Br Pt P1 C31 -51.3(4) . . . . ? C1 Pt P1 C29 84(2) . . . . ? P2 Pt P1 C29 9.6(6) . . . . ? Br Pt P1 C29 -168.1(6) . . . . ? C1 Pt P2 C61 -27.1(6) . . . . ? P1 Pt P2 C61 144.5(5) . . . . ? Br Pt P2 C61 -165(2) . . . . ? C1 Pt P2 C30 -152.0(7) . . . . ? P1 Pt P2 C30 19.6(5) . . . . ? Br Pt P2 C30 70(2) . . . . ? C1 Pt P2 C51 95.4(6) . . . . ? P1 Pt P2 C51 -93.1(4) . . . . ? Br Pt P2 C51 -43(2) . . . . ? P2 Pt C1 N12 -80.0(12) . . . . ? P1 Pt C1 N12 -153.6(15) . . . . ? Br Pt C1 N12 98.1(12) . . . . ? P2 Pt C1 N2 91.0(8) . . . . ? P1 Pt C1 N2 17(3) . . . . ? Br Pt C1 N2 -91.0(8) . . . . ? N12 C1 N2 C3 -1.4(13) . . . . ? Pt C1 N2 C3 -174.1(7) . . . . ? N12 C1 N2 C13 -176.8(10) . . . . ? Pt C1 N2 C13 10.5(15) . . . . ? C1 N2 C3 C4 179.1(12) . . . . ? C13 N2 C3 C4 -5(2) . . . . ? C1 N2 C3 C11 0.1(13) . . . . ? C13 N2 C3 C11 175.8(10) . . . . ? N2 C3 C4 C5 179.3(12) . . . . ? C11 C3 C4 C5 -1.8(17) . . . . ? C3 C4 C5 C9 2.9(18) . . . . ? C3 C4 C5 N6 179.7(12) . . . . ? C4 C5 N6 C7 -176.7(13) . . . . ? C9 C5 N6 C7 0.6(14) . . . . ? C4 C5 N6 C17 5(2) . . . . ? C9 C5 N6 C17 -177.2(11) . . . . ? C5 N6 C7 N8 -1.4(16) . . . . ? C17 N6 C7 N8 176.4(12) . . . . ? N6 C7 N8 C9 1.6(17) . . . . ? N6 C7 N8 C21 -179.7(12) . . . . ? C7 N8 C9 C10 179.4(14) . . . . ? C21 N8 C9 C10 1(2) . . . . ? C7 N8 C9 C5 -1.2(15) . . . . ? C21 N8 C9 C5 -179.9(12) . . . . ? C4 C5 C9 C10 -3(2) . . . . ? N6 C5 C9 C10 179.8(12) . . . . ? C4 C5 C9 N8 177.8(12) . . . . ? N6 C5 C9 N8 0.3(13) . . . . ? N8 C9 C10 C11 -179.7(12) . . . . ? C5 C9 C10 C11 1.0(18) . . . . ? C9 C10 C11 C3 0.1(19) . . . . ? C9 C10 C11 N12 178.0(13) . . . . ? C4 C3 C11 C10 0(2) . . . . ? N2 C3 C11 C10 179.5(12) . . . . ? C4 C3 C11 N12 -178.0(11) . . . . ? N2 C3 C11 N12 1.1(13) . . . . ? N2 C1 N12 C25 178.9(12) . . . . ? Pt C1 N12 C25 -9(2) . . . . ? N2 C1 N12 C11 2.1(14) . . . . ? Pt C1 N12 C11 173.8(9) . . . . ? C10 C11 N12 C1 179.8(13) . . . . ? C3 C11 N12 C1 -2.0(14) . . . . ? C10 C11 N12 C25 3(2) . . . . ? C3 C11 N12 C25 -178.8(12) . . . . ? C1 N2 C13 C14 98.5(14) . . . . ? C3 N2 C13 C14 -76.3(15) . . . . ? N2 C13 C14 C15 -178.9(12) . . . . ? C13 C14 C15 C16 -173.3(15) . . . . ? C7 N6 C17 C18 -108.4(16) . . . . ? C5 N6 C17 C18 69.0(16) . . . . ? N6 C17 C18 C19 70.9(19) . . . . ? C17 C18 C19 C20 74(2) . . . . ? C7 N8 C21 C22 95(2) . . . . ? C9 N8 C21 C22 -86(2) . . . . ? N8 C21 C22 C23 -46(3) . . . . ? C21 C22 C23 C24 163(3) . . . . ? C1 N12 C25 C26 -80.5(19) . . . . ? C11 N12 C25 C26 95.8(19) . . . . ? N12 C25 C26 C27 174.5(17) . . . . ? C25 C26 C27 C28 -119(3) . . . . ? C41 P1 C29 C30 78.1(11) . . . . ? C31 P1 C29 C30 -168.0(10) . . . . ? Pt P1 C29 C30 -42.5(11) . . . . ? P1 C29 C30 P2 58.5(11) . . . . ? C61 P2 C30 C29 -175.9(8) . . . . ? C51 P2 C30 C29 70.8(10) . . . . ? Pt P2 C30 C29 -50.9(10) . . . . ? C41 P1 C31 C32 -150.8(6) . . . . ? C29 P1 C31 C32 94.8(8) . . . . ? Pt P1 C31 C32 -23.2(6) . . . . ? C41 P1 C31 C36 30.0(8) . . . . ? C29 P1 C31 C36 -84.4(8) . . . . ? Pt P1 C31 C36 157.6(5) . . . . ? C36 C31 C32 C33 0.0 . . . . ? P1 C31 C32 C33 -179.2(7) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C31 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? P1 C31 C36 C35 179.2(7) . . . . ? C31 P1 C41 C42 -79.7(7) . . . . ? C29 P1 C41 C42 32.2(8) . . . . ? Pt P1 C41 C42 149.4(5) . . . . ? C31 P1 C41 C46 103.3(7) . . . . ? C29 P1 C41 C46 -144.8(7) . . . . ? Pt P1 C41 C46 -27.6(7) . . . . ? C46 C41 C42 C43 0.0 . . . . ? P1 C41 C42 C43 -177.0(8) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? P1 C41 C46 C45 177.0(8) . . . . ? C61 P2 C51 C52 -47.2(7) . . . . ? C30 P2 C51 C52 70.6(7) . . . . ? Pt P2 C51 C52 -173.1(5) . . . . ? C61 P2 C51 C56 135.7(7) . . . . ? C30 P2 C51 C56 -106.4(7) . . . . ? Pt P2 C51 C56 9.9(7) . . . . ? C56 C51 C52 C53 0.0 . . . . ? P2 C51 C52 C53 -177.0(8) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? P2 C51 C56 C55 177.1(8) . . . . ? C30 P2 C61 C62 -151.6(6) . . . . ? C51 P2 C61 C62 -41.2(6) . . . . ? Pt P2 C61 C62 86.1(5) . . . . ? C30 P2 C61 C66 39.6(8) . . . . ? C51 P2 C61 C66 149.9(6) . . . . ? Pt P2 C61 C66 -82.7(5) . . . . ? C66 C61 C62 C63 0.0 . . . . ? P2 C61 C62 C63 -168.7(6) . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C65 0.0 . . . . ? C63 C64 C65 C66 0.0 . . . . ? C64 C65 C66 C61 0.0 . . . . ? C62 C61 C66 C65 0.0 . . . . ? P2 C61 C66 C65 168.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.362 _refine_diff_density_min -2.232 _refine_diff_density_rms 0.137 # Attachment 'cif-4.cif' data_sad6 _database_code_depnum_ccdc_archive 'CCDC 716395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H56 Br2 N4 Ni2' _chemical_formula_weight 882.14 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.3023(14) _cell_length_b 23.345(2) _cell_length_c 23.2655(19) _cell_angle_alpha 90.00 _cell_angle_beta 96.0980(10) _cell_angle_gamma 90.00 _cell_volume 9344.4(13) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent sticks' _exptl_crystal_colour 'intense red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3648 _exptl_absorpt_coefficient_mu 2.545 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7499 _exptl_absorpt_correction_T_max 0.8833 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.768428 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55925 _diffrn_reflns_av_R_equivalents 0.1490 _diffrn_reflns_av_sigmaI/netI 0.1421 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 24.18 _reflns_number_total 14800 _reflns_number_gt 6801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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. Hydrogen atoms attached at the disordered Carbon (19c) in the Butyl-group were not calculated. The disordered Toluene molecules were restrained with Dfix or Afix command. ; _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^)+(0.1704P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14800 _refine_ls_number_parameters 826 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.1906 _refine_ls_R_factor_gt 0.0859 _refine_ls_wR_factor_ref 0.3137 _refine_ls_wR_factor_gt 0.2493 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 Br1A Br 0.49948(8) 1.01650(6) 0.25274(6) 0.0483(4) Uani 1 1 d . . . Br2A Br -0.05967(8) 0.94961(7) 0.34499(7) 0.0562(4) Uani 1 1 d . . . Ni1A Ni 0.51666(10) 0.91865(8) 0.24166(7) 0.0441(5) Uani 1 1 d . . . Ni2A Ni -0.05028(10) 0.85250(8) 0.32892(8) 0.0498(5) Uani 1 1 d . . . N4A N 0.0772(6) 0.8684(5) 0.2591(4) 0.040(3) Uani 1 1 d . . . N1A N 0.3508(6) 0.8998(4) 0.2169(4) 0.038(3) Uani 1 1 d . . . N2A N 0.3899(6) 0.8867(5) 0.3082(5) 0.042(3) Uani 1 1 d . . . N3A N 0.1181(7) 0.8518(5) 0.3486(5) 0.046(3) Uani 1 1 d . . . C1A C 0.4151(7) 0.9003(5) 0.2565(6) 0.041(3) Uani 1 1 d . . . C2A C 0.2847(7) 0.8870(5) 0.2437(5) 0.035(3) Uani 1 1 d . . . C3A C 0.2074(7) 0.8852(5) 0.2214(5) 0.038(3) Uani 1 1 d . . . H3D H 0.1899 0.8924 0.1820 0.045 Uiso 1 1 calc R . . C4A C 0.1568(7) 0.8714(5) 0.2636(6) 0.040(3) Uani 1 1 d . . . C5A C 0.1832(8) 0.8620(5) 0.3215(6) 0.040(3) Uani 1 1 d . . . C6A C 0.2619(7) 0.8650(6) 0.3448(6) 0.045(4) Uani 1 1 d . . . H6D H 0.2794 0.8590 0.3845 0.054 Uiso 1 1 calc R . . C7A C 0.3111(7) 0.8780(5) 0.3026(5) 0.031(3) Uani 1 1 d . . . C8A C 0.0521(8) 0.8573(6) 0.3103(6) 0.050(4) Uani 1 1 d . . . C9A C 0.3503(8) 0.9053(6) 0.1544(6) 0.043(3) Uani 1 1 d . . . H9D H 0.3963 0.9276 0.1457 0.052 Uiso 1 1 calc R . . H9E H 0.3032 0.9265 0.1386 0.052 Uiso 1 1 calc R . . C10A C 0.3514(9) 0.8479(6) 0.1261(6) 0.052(4) Uani 1 1 d . . . H10D H 0.3037 0.8268 0.1332 0.063 Uiso 1 1 calc R . . H10E H 0.3965 0.8260 0.1442 0.063 Uiso 1 1 calc R . . C11A C 0.3561(9) 0.8509(7) 0.0617(6) 0.061(4) Uani 1 1 d . . . H11D H 0.4000 0.8762 0.0546 0.073 Uiso 1 1 calc R . . H11E H 0.3079 0.8690 0.0433 0.073 Uiso 1 1 calc R . . C12A C 0.3667(12) 0.7941(8) 0.0324(7) 0.086(6) Uani 1 1 d . . . H12D H 0.4170 0.7776 0.0472 0.129 Uiso 1 1 calc R . . H12E H 0.3650 0.7999 -0.0094 0.129 Uiso 1 1 calc R . . H12F H 0.3249 0.7679 0.0406 0.129 Uiso 1 1 calc R . . C13A C 0.4413(7) 0.8813(6) 0.3632(6) 0.047(4) Uani 1 1 d . . . H13D H 0.4150 0.8976 0.3952 0.056 Uiso 1 1 calc R . . H13E H 0.4898 0.9031 0.3604 0.056 Uiso 1 1 calc R . . C14A C 0.4608(8) 0.8186(6) 0.3758(6) 0.053(4) Uani 1 1 d . . . H14D H 0.4122 0.7973 0.3797 0.063 Uiso 1 1 calc R . . H14E H 0.4851 0.8021 0.3430 0.063 Uiso 1 1 calc R . . C15A C 0.5149(9) 0.8116(7) 0.4301(7) 0.064(5) Uani 1 1 d . . . H15D H 0.5620 0.8349 0.4265 0.077 Uiso 1 1 calc R . . H15E H 0.4893 0.8273 0.4628 0.077 Uiso 1 1 calc R . . C16A C 0.5397(11) 0.7513(8) 0.4445(7) 0.092(6) Uani 1 1 d . . . H16D H 0.4951 0.7294 0.4552 0.137 Uiso 1 1 calc R . . H16E H 0.5808 0.7516 0.4770 0.137 Uiso 1 1 calc R . . H16F H 0.5595 0.7336 0.4108 0.137 Uiso 1 1 calc R . . C17A C 0.0260(7) 0.8762(6) 0.2060(6) 0.045(4) Uani 1 1 d . . . H17D H 0.0449 0.9090 0.1843 0.054 Uiso 1 1 calc R . . H17E H -0.0267 0.8858 0.2159 0.054 Uiso 1 1 calc R . . C18A C 0.0212(8) 0.8229(6) 0.1672(6) 0.050(4) Uani 1 1 d . . . H18D H 0.0739 0.8130 0.1573 0.060 Uiso 1 1 calc R . . H18E H 0.0017 0.7901 0.1885 0.060 Uiso 1 1 calc R . . C19A C -0.0318(8) 0.8325(6) 0.1123(6) 0.056(4) Uani 1 1 d . . . H19D H -0.0113 0.8648 0.0908 0.068 Uiso 1 1 calc R . . H19E H -0.0838 0.8436 0.1224 0.068 Uiso 1 1 calc R . . C20A C -0.0400(10) 0.7800(7) 0.0730(7) 0.071(5) Uani 1 1 d . . . H20D H 0.0113 0.7630 0.0704 0.106 Uiso 1 1 calc R . . H20E H -0.0628 0.7914 0.0343 0.106 Uiso 1 1 calc R . . H20F H -0.0738 0.7518 0.0890 0.106 Uiso 1 1 calc R . . C21A C 0.1187(9) 0.8381(7) 0.4115(5) 0.057(4) Uani 1 1 d . . . H21D H 0.0674 0.8471 0.4243 0.069 Uiso 1 1 calc R . . H21E H 0.1583 0.8618 0.4342 0.069 Uiso 1 1 calc R . . C22A C 0.1374(9) 0.7737(6) 0.4221(6) 0.055(4) Uani 1 1 d . . . H22D H 0.0979 0.7495 0.3999 0.066 Uiso 1 1 calc R . . H22E H 0.1891 0.7643 0.4101 0.066 Uiso 1 1 calc R . . C23A C 0.1363(10) 0.7636(7) 0.4874(7) 0.071(5) Uani 1 1 d . . . H23D H 0.1784 0.7864 0.5087 0.085 Uiso 1 1 calc R . . H23E H 0.0862 0.7773 0.4993 0.085 Uiso 1 1 calc R . . C24A C 0.1471(11) 0.7010(7) 0.5039(8) 0.087(6) Uani 1 1 d . . . H24D H 0.0971 0.6810 0.4970 0.130 Uiso 1 1 calc R . . H24E H 0.1665 0.6980 0.5449 0.130 Uiso 1 1 calc R . . H24F H 0.1846 0.6834 0.4805 0.130 Uiso 1 1 calc R . . C25A C 0.5552(10) 0.8382(7) 0.2275(8) 0.070(5) Uani 1 1 d . . . H25D H 0.5198 0.8072 0.2279 0.084 Uiso 1 1 calc R . . C26A C 0.5692(9) 0.8714(8) 0.1795(8) 0.076(5) Uani 1 1 d . . . H26D H 0.5490 0.8641 0.1406 0.091 Uiso 1 1 calc R . . C27A C 0.6174(9) 0.9166(7) 0.1980(8) 0.067(5) Uani 1 1 d . . . H27D H 0.6329 0.9474 0.1750 0.080 Uiso 1 1 calc R . . C28A C 0.6398(9) 0.9080(8) 0.2593(7) 0.067(5) Uani 1 1 d . . . H28D H 0.6733 0.9322 0.2835 0.080 Uiso 1 1 calc R . . C29A C 0.6053(9) 0.8605(7) 0.2761(8) 0.063(4) Uani 1 1 d . . . H29D H 0.6125 0.8442 0.3137 0.075 Uiso 1 1 calc R . . C30A C -0.0638(12) 0.7659(8) 0.3311(9) 0.086(6) Uani 1 1 d . . . H30D H -0.0194 0.7422 0.3299 0.103 Uiso 1 1 calc R . . C31A C -0.1143(10) 0.7860(8) 0.2834(9) 0.081(6) Uani 1 1 d . . . H31D H -0.1119 0.7758 0.2441 0.098 Uiso 1 1 calc R . . C32A C -0.1675(10) 0.8230(9) 0.3036(13) 0.099(7) Uani 1 1 d . . . H32D H -0.2062 0.8438 0.2802 0.118 Uiso 1 1 calc R . . C33A C -0.1556(13) 0.8249(10) 0.3627(14) 0.109(9) Uani 1 1 d . . . H33D H -0.1848 0.8475 0.3866 0.131 Uiso 1 1 calc R . . C34A C -0.0941(14) 0.7889(9) 0.3827(8) 0.091(7) Uani 1 1 d . . . H34D H -0.0756 0.7810 0.4218 0.109 Uiso 1 1 calc R . . Br1B Br 0.32978(9) 0.61807(6) 1.00343(6) 0.0541(4) Uani 1 1 d . . . Br2B Br 0.14159(9) 0.54789(6) 0.57665(6) 0.0534(4) Uani 1 1 d . . . Ni1B Ni 0.31155(10) 0.52236(7) 1.02612(7) 0.0405(5) Uani 1 1 d . . . Ni2B Ni 0.12850(10) 0.45051(8) 0.59354(7) 0.0435(5) Uani 1 1 d . . . N1B N 0.3216(6) 0.4883(5) 0.9077(4) 0.036(3) Uani 1 1 d . . . N2B N 0.2031(6) 0.5029(4) 0.9238(4) 0.038(3) Uani 1 1 d . . . N3B N 0.2339(6) 0.4558(4) 0.6986(4) 0.034(2) Uani 1 1 d . . . N4B N 0.1144(6) 0.4680(4) 0.7154(4) 0.040(3) Uani 1 1 d . . . C1B C 0.2797(8) 0.5013(6) 0.9501(6) 0.049(4) Uani 1 1 d . . . C2B C 0.2765(7) 0.4814(5) 0.8553(5) 0.036(3) Uani 1 1 d . . . C3B C 0.2983(8) 0.4711(5) 0.8005(5) 0.040(3) Uani 1 1 d . . . H3G H 0.3509 0.4672 0.7927 0.048 Uiso 1 1 calc R . . C4B C 0.2348(7) 0.4669(5) 0.7576(5) 0.035(3) Uani 1 1 d . . . C5B C 0.1602(7) 0.4749(5) 0.7687(6) 0.039(3) Uani 1 1 d . . . C6B C 0.1384(7) 0.4882(5) 0.8231(6) 0.038(3) Uani 1 1 d . . . H6G H 0.0861 0.4946 0.8305 0.045 Uiso 1 1 calc R . . C7B C 0.2011(7) 0.4911(5) 0.8653(5) 0.034(3) Uani 1 1 d . . . C8B C 0.1612(8) 0.4566(5) 0.6720(6) 0.040(3) Uani 1 1 d . . . C9B C 0.4055(7) 0.4808(6) 0.9183(5) 0.039(3) Uani 1 1 d . . . H9G H 0.4256 0.5056 0.9511 0.046 Uiso 1 1 calc R . . H9H H 0.4294 0.4938 0.8837 0.046 Uiso 1 1 calc R . . C10B C 0.4307(7) 0.4194(6) 0.9319(5) 0.044(3) Uani 1 1 d . . . H10G H 0.3982 0.4038 0.9607 0.053 Uiso 1 1 calc R . . H10H H 0.4852 0.4199 0.9499 0.053 Uiso 1 1 calc R . . C11B C 0.4254(8) 0.3779(6) 0.8792(6) 0.050(4) Uani 1 1 d . . . H11G H 0.3709 0.3763 0.8612 0.060 Uiso 1 1 calc R . . H11H H 0.4578 0.3930 0.8500 0.060 Uiso 1 1 calc R . . C12B C 0.4530(9) 0.3165(6) 0.8969(6) 0.063(4) Uani 1 1 d . . . H12G H 0.5081 0.3175 0.9119 0.094 Uiso 1 1 calc R . . H12H H 0.4460 0.2913 0.8631 0.094 Uiso 1 1 calc R . . H12I H 0.4224 0.3020 0.9269 0.094 Uiso 1 1 calc R . . C13B C 0.1353(7) 0.5159(5) 0.9553(5) 0.039(3) Uani 1 1 d . . . H13G H 0.0953 0.5354 0.9286 0.047 Uiso 1 1 calc R . . H13H H 0.1517 0.5429 0.9871 0.047 Uiso 1 1 calc R . . C14B C 0.0997(8) 0.4642(6) 0.9799(5) 0.045(4) Uani 1 1 d . . . H14G H 0.0661 0.4770 1.0093 0.054 Uiso 1 1 calc R . . H14H H 0.1419 0.4406 0.9999 0.054 Uiso 1 1 calc R . . C15B C 0.0515(8) 0.4265(6) 0.9358(6) 0.045(3) Uani 1 1 d . . . H15G H 0.0861 0.4103 0.9086 0.053 Uiso 1 1 calc R . . H15H H 0.0123 0.4506 0.9131 0.053 Uiso 1 1 calc R . . C16B C 0.0098(9) 0.3771(7) 0.9635(6) 0.064(4) Uani 1 1 d . . . H16G H 0.0479 0.3543 0.9879 0.095 Uiso 1 1 calc R . . H16H H -0.0163 0.3527 0.9331 0.095 Uiso 1 1 calc R . . H16I H -0.0287 0.3928 0.9872 0.095 Uiso 1 1 calc R . . C17B C 0.3024(8) 0.4434(6) 0.6688(5) 0.046(4) Uani 1 1 d . . . H17G H 0.3452 0.4690 0.6844 0.055 Uiso 1 1 calc R . . H17H H 0.2901 0.4526 0.6273 0.055 Uiso 1 1 calc R . . C18B C 0.3320(12) 0.3785(8) 0.6746(9) 0.115(8) Uani 1 1 d . . . H18G H 0.3592 0.3719 0.6398 0.138 Uiso 1 1 calc R . . H18H H 0.3730 0.3788 0.7077 0.138 Uiso 1 1 calc R . . C19B C 0.2946(12) 0.3334(8) 0.6805(9) 0.13(2) Uani 0.50 1 d PR . . H19G H 0.2660 0.3229 0.6429 0.155 Uiso 0.50 1 calc PR . . H19H H 0.2558 0.3404 0.7081 0.155 Uiso 0.50 1 calc PR . . C19C C 0.340(3) 0.353(2) 0.7239(19) 0.097(13) Uiso 0.50 1 d P . . C20B C 0.3464(15) 0.2831(8) 0.7024(11) 0.144(10) Uani 1 1 d . . . H20G H 0.3987 0.2886 0.6908 0.216 Uiso 1 1 calc R . . H20H H 0.3244 0.2473 0.6859 0.216 Uiso 1 1 calc R . . H20I H 0.3493 0.2813 0.7447 0.216 Uiso 1 1 calc R . . C21B C 0.0291(7) 0.4711(6) 0.7065(6) 0.052(4) Uani 1 1 d . . . H21G H 0.0130 0.4850 0.6668 0.063 Uiso 1 1 calc R . . H21H H 0.0107 0.4991 0.7339 0.063 Uiso 1 1 calc R . . C22B C -0.0101(9) 0.4111(7) 0.7153(7) 0.075(5) Uani 1 1 d . . . H22G H -0.0659 0.4138 0.7011 0.090 Uiso 1 1 calc R . . H22H H 0.0136 0.3824 0.6912 0.090 Uiso 1 1 calc R . . C23B C -0.0033(11) 0.3902(8) 0.7751(8) 0.082(5) Uani 1 1 d . . . H23G H -0.0234 0.4195 0.8005 0.098 Uiso 1 1 calc R . . H23H H 0.0520 0.3829 0.7888 0.098 Uiso 1 1 calc R . . C24B C -0.0513(11) 0.3335(7) 0.7776(9) 0.098(7) Uani 1 1 d . . . H24G H -0.1041 0.3396 0.7589 0.147 Uiso 1 1 calc R . . H24H H -0.0535 0.3224 0.8180 0.147 Uiso 1 1 calc R . . H24I H -0.0262 0.3029 0.7574 0.147 Uiso 1 1 calc R . . C25B C 0.3881(10) 0.4665(7) 1.0772(6) 0.059(4) Uani 1 1 d . . . H25G H 0.4341 0.4494 1.0661 0.071 Uiso 1 1 calc R . . C26B C 0.3820(9) 0.5159(7) 1.1081(6) 0.055(4) Uani 1 1 d . . . H26G H 0.4237 0.5407 1.1213 0.066 Uiso 1 1 calc R . . C27B C 0.2997(9) 0.5240(7) 1.1176(6) 0.062(4) Uani 1 1 d . . . H27G H 0.2795 0.5556 1.1370 0.074 Uiso 1 1 calc R . . C28B C 0.2571(9) 0.4787(7) 1.0940(6) 0.053(4) Uani 1 1 d . . . H28G H 0.2037 0.4713 1.0970 0.063 Uiso 1 1 calc R . . C29B C 0.3071(8) 0.4457(7) 1.0648(6) 0.054(4) Uani 1 1 d . . . H29G H 0.2915 0.4143 1.0403 0.064 Uiso 1 1 calc R . . C30B C 0.1132(12) 0.3642(7) 0.5878(7) 0.070(5) Uani 1 1 d . . . H30G H 0.1235 0.3423 0.6222 0.084 Uiso 1 1 calc R . . C31B C 0.1638(11) 0.3767(7) 0.5499(8) 0.073(5) Uani 1 1 d . . . H31G H 0.2148 0.3614 0.5507 0.088 Uiso 1 1 calc R . . C32B C 0.1303(11) 0.4158(7) 0.5090(7) 0.069(5) Uani 1 1 d . . . H32G H 0.1558 0.4343 0.4799 0.083 Uiso 1 1 calc R . . C33B C 0.0522(10) 0.4228(8) 0.5189(7) 0.071(5) Uani 1 1 d . . . H33G H 0.0147 0.4457 0.4968 0.086 Uiso 1 1 calc R . . C34B C 0.0400(11) 0.3901(8) 0.5666(7) 0.075(5) Uani 1 1 d . . . H34G H -0.0079 0.3855 0.5826 0.090 Uiso 1 1 calc R . . C1 C 0.7459(19) 0.4482(15) 0.7487(12) 0.080 Uiso 0.50 1 d PD . . H1A H 0.6891 0.4514 0.7432 0.120 Uiso 0.50 1 calc P . . H1B H 0.7669 0.4765 0.7774 0.120 Uiso 0.50 1 calc P . . H1C H 0.7606 0.4096 0.7625 0.120 Uiso 0.50 1 calc P . . C2 C 0.7781(17) 0.4591(11) 0.6926(12) 0.080 Uiso 0.50 1 d PD . . C3 C 0.8225(17) 0.5075(12) 0.6889(13) 0.080 Uiso 0.50 1 d PD . . H3 H 0.8323 0.5348 0.7191 0.096 Uiso 0.50 1 calc PR . . C4 C 0.851(2) 0.5115(14) 0.6361(12) 0.080 Uiso 0.50 1 d PD . . H4 H 0.8819 0.5436 0.6276 0.096 Uiso 0.50 1 calc PR . . C5 C 0.8351(18) 0.4689(12) 0.5958(14) 0.080 Uiso 0.50 1 d PD . . H5 H 0.8574 0.4745 0.5606 0.096 Uiso 0.50 1 calc PR . . C6 C 0.7921(17) 0.4196(13) 0.5981(13) 0.080 Uiso 0.50 1 d PD . . H6 H 0.7851 0.3911 0.5688 0.096 Uiso 0.50 1 calc PR . . C7 C 0.7611(19) 0.4187(13) 0.6501(12) 0.080 Uiso 0.50 1 d PD . . H7 H 0.7262 0.3887 0.6570 0.096 Uiso 0.50 1 calc PR . . C11 C 0.4517(14) 0.5666(16) 0.4075(14) 0.080 Uiso 0.50 1 d PD . . H11A H 0.4630 0.5576 0.3681 0.120 Uiso 0.50 1 calc P . . H11B H 0.4285 0.6049 0.4081 0.120 Uiso 0.50 1 calc P . . H11C H 0.4152 0.5383 0.4201 0.120 Uiso 0.50 1 calc P . . C12 C 0.5253(15) 0.5653(10) 0.4474(13) 0.080 Uiso 0.50 1 d PD . . C13 C 0.5413(15) 0.6072(13) 0.4885(12) 0.080 Uiso 0.50 1 d PD . . H13 H 0.5057 0.6378 0.4915 0.096 Uiso 0.50 1 calc PR . . C14 C 0.6090(14) 0.6046(14) 0.5250(13) 0.080 Uiso 0.50 1 d PD . . H14 H 0.6218 0.6344 0.5522 0.096 Uiso 0.50 1 calc PR . . C15 C 0.6582(19) 0.5587(12) 0.5221(14) 0.080 Uiso 0.50 1 d PD . . H15 H 0.7047 0.5550 0.5474 0.096 Uiso 0.50 1 calc PR . . C16 C 0.6363(15) 0.5184(14) 0.4804(13) 0.080 Uiso 0.50 1 d PD . . H16 H 0.6728 0.4888 0.4758 0.096 Uiso 0.50 1 calc PR . . C17 C 0.5678(15) 0.5158(12) 0.4446(13) 0.080 Uiso 0.50 1 d PD . . H17 H 0.5518 0.4838 0.4210 0.096 Uiso 0.50 1 calc PR . . C21 C 0.2111(13) 0.7062(16) 0.1338(11) 0.080 Uiso 0.50 1 d PD . . H21A H 0.2233 0.6868 0.0985 0.120 Uiso 0.50 1 calc P . . H21B H 0.1971 0.7462 0.1249 0.120 Uiso 0.50 1 calc P . . H21C H 0.1673 0.6868 0.1490 0.120 Uiso 0.50 1 calc P . . C22 C 0.2804(8) 0.7045(6) 0.1779(5) 0.080 Uiso 0.50 1 d PRD . . C23 C 0.3501(8) 0.6767(6) 0.1755(5) 0.080 Uiso 0.50 1 d PRD . . H23 H 0.3617 0.6595 0.1404 0.096 Uiso 0.50 1 calc PR . . C24 C 0.4030(8) 0.6738(6) 0.2239(5) 0.080 Uiso 0.50 1 d PRD . . H24 H 0.4511 0.6546 0.2223 0.096 Uiso 0.50 1 calc PR . . C25 C 0.3862(8) 0.6986(6) 0.2747(5) 0.080 Uiso 0.50 1 d PRD . . H25 H 0.4227 0.6966 0.3081 0.096 Uiso 0.50 1 calc PR . . C26 C 0.3165(8) 0.7264(6) 0.2771(5) 0.080 Uiso 0.50 1 d PRD . . H26 H 0.3051 0.7439 0.3121 0.096 Uiso 0.50 1 calc PR . . C27 C 0.2634(8) 0.7290(6) 0.2288(5) 0.080 Uiso 0.50 1 d PRD . . H27 H 0.2149 0.7477 0.2306 0.096 Uiso 0.50 1 calc PR . . C31 C 0.7657(8) 0.7221(6) -0.0183(5) 0.080 Uiso 0.50 1 d PD . . H31A H 0.7156 0.7335 -0.0386 0.120 Uiso 0.50 1 calc P . . H31B H 0.7803 0.6843 -0.0319 0.120 Uiso 0.50 1 calc P . . H31C H 0.8055 0.7501 -0.0259 0.120 Uiso 0.50 1 calc P . . C32 C 0.7593(11) 0.7196(8) 0.0453(5) 0.080 Uiso 0.50 1 d PRD . . C33 C 0.7747(11) 0.6707(8) 0.0774(5) 0.080 Uiso 0.50 1 d PRD . . H33 H 0.7803 0.6355 0.0577 0.096 Uiso 0.50 1 calc PR . . C34 C 0.7822(11) 0.6707(8) 0.1368(5) 0.080 Uiso 0.50 1 d PD . . H34 H 0.7994 0.6380 0.1589 0.096 Uiso 0.50 1 calc PR . . C35 C 0.7632(19) 0.7213(8) 0.1621(13) 0.080 Uiso 0.50 1 d PD . . H35 H 0.7603 0.7216 0.2026 0.096 Uiso 0.50 1 calc PR . . C36 C 0.748(2) 0.7716(13) 0.1321(11) 0.080 Uiso 0.50 1 d PD . . H36 H 0.7393 0.8063 0.1518 0.096 Uiso 0.50 1 calc PR . . C37 C 0.746(2) 0.7701(10) 0.0729(11) 0.080 Uiso 0.50 1 d PD . . H37 H 0.7349 0.8041 0.0510 0.096 Uiso 0.50 1 calc PR . . 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 Br1A 0.0423(8) 0.0460(8) 0.0565(9) -0.0006(7) 0.0045(6) 0.0000(7) Br2A 0.0462(9) 0.0490(9) 0.0753(11) -0.0091(8) 0.0159(8) -0.0033(7) Ni1A 0.0373(10) 0.0447(11) 0.0498(11) -0.0025(9) 0.0018(8) 0.0022(8) Ni2A 0.0431(11) 0.0485(12) 0.0593(12) -0.0076(9) 0.0117(9) -0.0070(9) N4A 0.032(6) 0.053(7) 0.035(6) 0.003(5) 0.004(5) -0.009(5) N1A 0.045(7) 0.041(7) 0.027(6) -0.002(5) -0.001(5) -0.001(5) N2A 0.042(7) 0.041(7) 0.043(7) 0.002(5) 0.000(5) 0.000(5) N3A 0.049(7) 0.045(7) 0.043(7) 0.002(6) 0.011(6) -0.010(6) C1A 0.040(8) 0.035(8) 0.045(8) -0.008(6) -0.011(7) -0.003(6) C2A 0.045(8) 0.031(7) 0.032(7) -0.009(6) 0.008(6) 0.001(6) C3A 0.044(8) 0.033(7) 0.035(7) -0.004(6) -0.008(6) -0.004(6) C4A 0.029(7) 0.039(8) 0.053(9) -0.006(7) 0.001(6) 0.003(6) C5A 0.041(8) 0.029(7) 0.051(9) -0.004(6) 0.012(7) -0.003(6) C6A 0.037(8) 0.049(9) 0.048(8) -0.002(7) -0.005(7) 0.012(7) C7A 0.030(7) 0.032(7) 0.032(7) -0.009(6) 0.002(6) 0.003(6) C8A 0.044(9) 0.047(9) 0.058(10) -0.008(7) 0.006(8) -0.008(7) C9A 0.035(8) 0.044(9) 0.052(9) 0.008(7) 0.011(6) 0.001(6) C10A 0.063(10) 0.053(10) 0.040(8) -0.008(7) 0.000(7) -0.002(8) C11A 0.067(11) 0.065(11) 0.048(9) 0.008(8) -0.002(8) -0.020(9) C12A 0.127(17) 0.086(14) 0.048(10) -0.016(10) 0.026(10) 0.000(12) C13A 0.031(8) 0.060(10) 0.047(8) -0.002(7) -0.009(6) -0.009(7) C14A 0.053(9) 0.055(10) 0.048(9) 0.007(7) -0.006(7) 0.004(8) C15A 0.065(11) 0.056(10) 0.067(11) 0.007(8) -0.020(8) 0.006(8) C16A 0.107(16) 0.099(16) 0.064(12) -0.004(11) -0.014(11) 0.030(13) C17A 0.028(7) 0.050(9) 0.056(9) 0.014(7) -0.003(6) -0.005(6) C18A 0.056(9) 0.044(9) 0.048(9) 0.003(7) 0.001(7) -0.001(7) C19A 0.048(9) 0.064(11) 0.054(9) -0.001(8) -0.010(7) -0.001(8) C20A 0.069(11) 0.076(12) 0.066(11) -0.028(9) 0.001(9) -0.010(9) C21A 0.057(10) 0.088(13) 0.030(8) -0.012(8) 0.020(7) -0.007(9) C22A 0.056(10) 0.048(10) 0.060(10) 0.002(8) 0.005(8) 0.002(8) C23A 0.073(12) 0.064(11) 0.076(12) 0.026(10) 0.011(9) 0.005(9) C24A 0.087(14) 0.080(14) 0.091(14) 0.028(11) -0.001(11) -0.007(11) C25A 0.070(12) 0.049(11) 0.093(14) 0.001(10) 0.015(11) 0.017(9) C26A 0.051(11) 0.089(14) 0.088(14) -0.035(12) 0.012(9) 0.017(10) C27A 0.056(10) 0.066(12) 0.084(13) -0.017(10) 0.037(9) 0.003(9) C28A 0.040(9) 0.091(14) 0.068(11) -0.026(10) -0.003(8) 0.009(9) C29A 0.050(10) 0.045(10) 0.092(13) 0.018(9) 0.006(9) 0.005(8) C30A 0.085(14) 0.056(12) 0.116(17) 0.004(12) 0.008(13) -0.037(10) C31A 0.038(10) 0.091(14) 0.114(16) -0.044(12) 0.007(10) -0.019(10) C32A 0.038(11) 0.085(16) 0.18(2) -0.009(17) 0.023(14) -0.019(10) C33A 0.076(16) 0.077(16) 0.19(3) -0.011(19) 0.085(18) -0.013(12) C34A 0.125(19) 0.084(15) 0.070(13) -0.013(11) 0.039(13) -0.036(14) Br1B 0.0723(11) 0.0477(9) 0.0406(8) -0.0017(7) -0.0027(7) -0.0057(8) Br2B 0.0687(10) 0.0424(9) 0.0448(8) 0.0026(7) -0.0141(7) -0.0026(8) Ni1B 0.0388(10) 0.0457(11) 0.0355(9) -0.0016(8) -0.0026(7) -0.0021(8) Ni2B 0.0493(11) 0.0399(10) 0.0383(10) -0.0003(8) -0.0088(8) -0.0049(9) N1B 0.028(6) 0.049(7) 0.031(6) 0.001(5) -0.005(5) 0.004(5) N2B 0.033(6) 0.043(7) 0.039(6) -0.001(5) 0.004(5) -0.004(5) N3B 0.038(6) 0.036(6) 0.028(6) 0.005(5) -0.006(5) 0.003(5) N4B 0.044(7) 0.040(7) 0.034(6) 0.007(5) -0.011(5) -0.013(5) C1B 0.051(9) 0.047(9) 0.046(9) 0.001(7) -0.002(7) 0.008(7) C2B 0.034(8) 0.029(7) 0.045(8) 0.000(6) -0.001(6) 0.003(6) C3B 0.041(8) 0.036(8) 0.043(8) 0.001(6) -0.002(6) -0.004(6) C4B 0.038(8) 0.027(7) 0.040(8) 0.008(6) 0.007(6) 0.001(6) C5B 0.036(8) 0.026(7) 0.054(9) 0.005(6) -0.005(7) -0.004(6) C6B 0.028(7) 0.033(8) 0.052(9) -0.004(6) 0.004(6) 0.000(6) C7B 0.039(8) 0.031(7) 0.032(7) 0.002(6) 0.001(6) 0.003(6) C8B 0.039(8) 0.029(7) 0.048(8) 0.015(6) -0.005(7) -0.005(6) C9B 0.030(7) 0.045(8) 0.040(8) 0.004(6) 0.002(6) -0.009(6) C10B 0.031(7) 0.058(10) 0.041(8) -0.003(7) -0.004(6) 0.004(7) C11B 0.047(9) 0.051(9) 0.051(9) 0.005(7) 0.007(7) 0.014(7) C12B 0.074(11) 0.057(10) 0.055(10) 0.001(8) -0.004(8) 0.001(9) C13B 0.040(8) 0.033(8) 0.043(8) 0.002(6) -0.003(6) 0.006(6) C14B 0.041(8) 0.051(9) 0.040(8) 0.013(7) -0.008(6) 0.015(7) C15B 0.042(8) 0.047(9) 0.045(8) 0.005(7) 0.009(7) -0.002(7) C16B 0.066(11) 0.069(11) 0.058(10) 0.004(9) 0.017(8) -0.015(9) C17B 0.055(9) 0.054(9) 0.027(7) 0.002(7) 0.000(6) 0.013(7) C18B 0.14(2) 0.064(14) 0.13(2) 0.002(14) 0.012(16) 0.018(15) C19B 0.13(4) 0.012(18) 0.23(6) 0.03(2) -0.06(4) -0.03(2) C20B 0.19(3) 0.053(13) 0.19(3) -0.005(15) 0.02(2) 0.037(15) C21B 0.026(8) 0.071(11) 0.056(9) 0.008(8) -0.007(6) 0.002(7) C22B 0.056(11) 0.085(13) 0.082(13) 0.022(10) -0.008(9) -0.036(10) C23B 0.075(13) 0.088(14) 0.083(13) 0.005(11) 0.008(10) -0.007(11) C24B 0.095(15) 0.057(12) 0.148(19) 0.035(12) 0.037(13) -0.025(11) C25B 0.071(11) 0.059(11) 0.046(9) 0.001(8) -0.007(8) 0.008(9) C26B 0.062(11) 0.057(10) 0.040(8) 0.010(8) -0.017(7) -0.018(8) C27B 0.067(11) 0.077(12) 0.038(8) 0.002(8) -0.008(8) 0.006(9) C28B 0.046(9) 0.071(11) 0.041(8) 0.003(8) 0.000(7) -0.004(8) C29B 0.046(9) 0.059(10) 0.052(9) 0.019(8) -0.012(7) -0.004(8) C30B 0.100(15) 0.056(11) 0.050(10) -0.002(8) -0.011(10) -0.023(10) C31B 0.078(13) 0.056(11) 0.084(13) -0.009(10) -0.002(11) 0.011(10) C32B 0.082(13) 0.075(12) 0.049(10) -0.007(9) 0.005(9) -0.015(10) C33B 0.067(12) 0.082(13) 0.058(11) -0.037(10) -0.026(9) 0.020(10) C34B 0.084(14) 0.085(13) 0.053(11) -0.014(10) -0.004(9) -0.047(11) _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 Br1A Ni1A 2.321(2) . ? Br2A Ni2A 2.306(2) . ? Ni1A C1A 1.876(13) . ? Ni1A C25A 2.031(15) . ? Ni1A C26A 2.101(16) . ? Ni1A C27A 2.109(15) . ? Ni1A C29A 2.139(15) . ? Ni1A C28A 2.140(15) . ? Ni1A Ni2A 10.342(3) . ? Ni2A C8A 1.871(14) . ? Ni2A C30A 2.038(17) . ? Ni2A C31A 2.123(16) . ? Ni2A C34A 2.131(18) . ? Ni2A C33A 2.157(18) . ? Ni2A C32A 2.164(18) . ? N4A C8A 1.336(16) . ? N4A C4A 1.371(15) . ? N4A C17A 1.452(15) . ? N1A C1A 1.368(15) . ? N1A C2A 1.392(16) . ? N1A C9A 1.459(15) . ? N2A C1A 1.359(16) . ? N2A C7A 1.372(15) . ? N2A C13A 1.484(15) . ? N3A C5A 1.368(16) . ? N3A C8A 1.377(17) . ? N3A C21A 1.497(16) . ? C2A C3A 1.383(17) . ? C2A C7A 1.413(16) . ? C3A C4A 1.421(18) . ? C4A C5A 1.392(18) . ? C5A C6A 1.414(17) . ? C6A C7A 1.400(17) . ? C9A C10A 1.494(17) . ? C10A C11A 1.510(18) . ? C11A C12A 1.51(2) . ? C13A C14A 1.522(18) . ? C14A C15A 1.499(18) . ? C15A C16A 1.50(2) . ? C17A C18A 1.536(18) . ? C18A C19A 1.508(17) . ? C19A C20A 1.527(19) . ? C21A C22A 1.55(2) . ? C22A C23A 1.539(19) . ? C23A C24A 1.52(2) . ? C25A C26A 1.40(2) . ? C25A C29A 1.45(2) . ? C26A C27A 1.38(2) . ? C27A C28A 1.45(2) . ? C28A C29A 1.34(2) . ? C30A C31A 1.42(2) . ? C30A C34A 1.46(3) . ? C31A C32A 1.38(3) . ? C32A C33A 1.37(3) . ? C33A C34A 1.40(3) . ? Br1B Ni1B 2.325(2) . ? Br2B Ni2B 2.322(2) . ? Ni1B C1B 1.862(14) . ? Ni1B C29B 2.007(14) . ? Ni1B C25B 2.129(14) . ? Ni1B C26B 2.157(13) . ? Ni1B C27B 2.160(14) . ? Ni1B C28B 2.175(15) . ? Ni1B Ni2B 10.361(2) . ? Ni2B C8B 1.858(13) . ? Ni2B C30B 2.035(16) . ? Ni2B C31B 2.123(17) . ? Ni2B C34B 2.127(15) . ? Ni2B C32B 2.131(15) . ? Ni2B C33B 2.166(14) . ? N1B C1B 1.319(16) . ? N1B C2B 1.386(15) . ? N1B C9B 1.456(15) . ? N2B C7B 1.386(15) . ? N2B C1B 1.400(16) . ? N2B C13B 1.479(16) . ? N3B C8B 1.342(15) . ? N3B C4B 1.396(15) . ? N3B C17B 1.464(16) . ? N4B C8B 1.386(17) . ? N4B C5B 1.407(15) . ? N4B C21B 1.470(16) . ? C2B C7B 1.368(17) . ? C2B C3B 1.389(17) . ? C3B C4B 1.407(17) . ? C4B C5B 1.356(17) . ? C5B C6B 1.394(18) . ? C6B C7B 1.385(16) . ? C9B C10B 1.522(17) . ? C10B C11B 1.557(18) . ? C11B C12B 1.553(19) . ? C13B C14B 1.497(17) . ? C14B C15B 1.531(17) . ? C15B C16B 1.538(18) . ? C17B C18B 1.60(2) . ? C18B C19B 1.2524 . ? C19B C20B 1.53(2) . ? C21B C22B 1.58(2) . ? C22B C23B 1.47(2) . ? C23B C24B 1.57(2) . ? C25B C26B 1.37(2) . ? C25B C29B 1.48(2) . ? C26B C27B 1.48(2) . ? C27B C28B 1.37(2) . ? C28B C29B 1.39(2) . ? C30B C31B 1.34(2) . ? C30B C34B 1.44(2) . ? C31B C32B 1.40(2) . ? C32B C33B 1.40(2) . ? C33B C34B 1.38(2) . ? C1 C2 1.4949(10) . ? C2 C7 1.3750(10) . ? C2 C3 1.3751(11) . ? C3 C4 1.3749(11) . ? C4 C5 1.3749(10) . ? C5 C6 1.3749(10) . ? C6 C7 1.3749(10) . ? C11 C12 1.4949(11) . ? C12 C17 1.3748(10) . ? C12 C13 1.3749(10) . ? C13 C14 1.3749(11) . ? C14 C15 1.3750(10) . ? C15 C16 1.3749(10) . ? C16 C17 1.3749(10) . ? C21 C22 1.4948(10) . ? C22 C23 1.3750 . ? C22 C27 1.3752 . ? C23 C24 1.3750 . ? C24 C25 1.3750 . ? C25 C26 1.3750 . ? C26 C27 1.3750 . ? C31 C32 1.4949(10) . ? C32 C37 1.3749(10) . ? C32 C33 1.3749 . ? C33 C34 1.3746 . ? C34 C35 1.3749(10) . ? C35 C36 1.3749(10) . ? C36 C37 1.3749(10) . ? 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 C1A Ni1A C25A 98.5(7) . . ? C1A Ni1A C26A 119.3(6) . . ? C25A Ni1A C26A 39.6(6) . . ? C1A Ni1A C27A 157.2(6) . . ? C25A Ni1A C27A 66.3(7) . . ? C26A Ni1A C27A 38.4(6) . . ? C1A Ni1A C29A 115.7(6) . . ? C25A Ni1A C29A 40.5(6) . . ? C26A Ni1A C29A 65.1(7) . . ? C27A Ni1A C29A 64.5(7) . . ? C1A Ni1A C28A 150.5(7) . . ? C25A Ni1A C28A 65.6(7) . . ? C26A Ni1A C28A 65.0(6) . . ? C27A Ni1A C28A 40.0(6) . . ? C29A Ni1A C28A 36.4(6) . . ? C1A Ni1A Br1A 94.1(4) . . ? C25A Ni1A Br1A 167.3(5) . . ? C26A Ni1A Br1A 131.5(6) . . ? C27A Ni1A Br1A 101.4(5) . . ? C29A Ni1A Br1A 132.7(5) . . ? C28A Ni1A Br1A 103.3(5) . . ? C1A Ni1A Ni2A 4.7(4) . . ? C25A Ni1A Ni2A 103.2(5) . . ? C26A Ni1A Ni2A 123.1(5) . . ? C27A Ni1A Ni2A 160.2(5) . . ? C29A Ni1A Ni2A 119.3(4) . . ? C28A Ni1A Ni2A 152.9(5) . . ? Br1A Ni1A Ni2A 89.42(6) . . ? C8A Ni2A C30A 100.3(7) . . ? C8A Ni2A C31A 112.6(6) . . ? C30A Ni2A C31A 39.8(7) . . ? C8A Ni2A C34A 125.6(9) . . ? C30A Ni2A C34A 41.0(7) . . ? C31A Ni2A C34A 65.4(8) . . ? C8A Ni2A C33A 163.5(9) . . ? C30A Ni2A C33A 65.9(8) . . ? C31A Ni2A C33A 63.1(8) . . ? C34A Ni2A C33A 38.0(8) . . ? C8A Ni2A C32A 147.0(8) . . ? C30A Ni2A C32A 65.4(8) . . ? C31A Ni2A C32A 37.6(7) . . ? C34A Ni2A C32A 63.7(9) . . ? C33A Ni2A C32A 36.9(8) . . ? C8A Ni2A Br2A 93.6(4) . . ? C30A Ni2A Br2A 164.1(6) . . ? C31A Ni2A Br2A 139.2(6) . . ? C34A Ni2A Br2A 123.6(6) . . ? C33A Ni2A Br2A 99.1(6) . . ? C32A Ni2A Br2A 106.1(6) . . ? C8A Ni2A Ni1A 5.5(4) . . ? C30A Ni2A Ni1A 105.5(6) . . ? C31A Ni2A Ni1A 117.8(5) . . ? C34A Ni2A Ni1A 128.5(7) . . ? C33A Ni2A Ni1A 166.2(8) . . ? C32A Ni2A Ni1A 151.1(7) . . ? Br2A Ni2A Ni1A 88.26(6) . . ? C8A N4A C4A 111.1(11) . . ? C8A N4A C17A 123.7(11) . . ? C4A N4A C17A 125.2(11) . . ? C1A N1A C2A 110.4(10) . . ? C1A N1A C9A 126.1(11) . . ? C2A N1A C9A 123.2(10) . . ? C1A N2A C7A 111.1(10) . . ? C1A N2A C13A 124.3(11) . . ? C7A N2A C13A 124.6(11) . . ? C5A N3A C8A 110.7(11) . . ? C5A N3A C21A 124.5(11) . . ? C8A N3A C21A 124.8(12) . . ? N2A C1A N1A 106.2(11) . . ? N2A C1A Ni1A 127.7(9) . . ? N1A C1A Ni1A 126.1(10) . . ? C3A C2A N1A 130.3(11) . . ? C3A C2A C7A 124.0(12) . . ? N1A C2A C7A 105.7(10) . . ? C2A C3A C4A 113.0(11) . . ? N4A C4A C5A 106.9(11) . . ? N4A C4A C3A 130.2(12) . . ? C5A C4A C3A 122.8(12) . . ? N3A C5A C4A 105.7(11) . . ? N3A C5A C6A 129.7(13) . . ? C4A C5A C6A 124.6(12) . . ? C7A C6A C5A 112.0(12) . . ? N2A C7A C6A 129.6(11) . . ? N2A C7A C2A 106.6(11) . . ? C6A C7A C2A 123.7(11) . . ? N4A C8A N3A 105.6(11) . . ? N4A C8A Ni2A 128.6(10) . . ? N3A C8A Ni2A 125.8(11) . . ? N1A C9A C10A 111.1(11) . . ? C9A C10A C11A 113.6(12) . . ? C10A C11A C12A 115.4(13) . . ? N2A C13A C14A 110.4(11) . . ? C15A C14A C13A 112.0(12) . . ? C16A C15A C14A 115.5(13) . . ? N4A C17A C18A 112.8(11) . . ? C19A C18A C17A 111.5(11) . . ? C18A C19A C20A 113.3(13) . . ? N3A C21A C22A 110.1(11) . . ? C23A C22A C21A 106.4(12) . . ? C24A C23A C22A 112.5(14) . . ? C26A C25A C29A 106.5(16) . . ? C26A C25A Ni1A 72.9(10) . . ? C29A C25A Ni1A 73.7(9) . . ? C27A C26A C25A 108.9(17) . . ? C27A C26A Ni1A 71.1(9) . . ? C25A C26A Ni1A 67.5(9) . . ? C26A C27A C28A 106.8(16) . . ? C26A C27A Ni1A 70.5(9) . . ? C28A C27A Ni1A 71.2(9) . . ? C29A C28A C27A 108.8(15) . . ? C29A C28A Ni1A 71.7(9) . . ? C27A C28A Ni1A 68.9(8) . . ? C28A C29A C25A 108.5(16) . . ? C28A C29A Ni1A 71.9(9) . . ? C25A C29A Ni1A 65.7(8) . . ? C31A C30A C34A 106.0(19) . . ? C31A C30A Ni2A 73.3(11) . . ? C34A C30A Ni2A 73.0(11) . . ? C32A C31A C30A 109(2) . . ? C32A C31A Ni2A 72.8(11) . . ? C30A C31A Ni2A 66.9(9) . . ? C33A C32A C31A 109(2) . . ? C33A C32A Ni2A 71.3(12) . . ? C31A C32A Ni2A 69.6(10) . . ? C32A C33A C34A 110(2) . . ? C32A C33A Ni2A 71.8(11) . . ? C34A C33A Ni2A 70.0(11) . . ? C33A C34A C30A 106(2) . . ? C33A C34A Ni2A 72.0(12) . . ? C30A C34A Ni2A 66.1(9) . . ? C1B Ni1B C29B 99.7(6) . . ? C1B Ni1B C25B 118.1(6) . . ? C29B Ni1B C25B 41.9(6) . . ? C1B Ni1B C26B 154.7(6) . . ? C29B Ni1B C26B 65.6(6) . . ? C25B Ni1B C26B 37.2(5) . . ? C1B Ni1B C27B 153.0(7) . . ? C29B Ni1B C27B 64.1(6) . . ? C25B Ni1B C27B 65.2(6) . . ? C26B Ni1B C27B 40.0(5) . . ? C1B Ni1B C28B 117.3(6) . . ? C29B Ni1B C28B 38.5(6) . . ? C25B Ni1B C28B 66.4(6) . . ? C26B Ni1B C28B 64.7(5) . . ? C27B Ni1B C28B 36.9(5) . . ? C1B Ni1B Br1B 94.1(4) . . ? C29B Ni1B Br1B 166.1(4) . . ? C25B Ni1B Br1B 128.6(4) . . ? C26B Ni1B Br1B 101.0(4) . . ? C27B Ni1B Br1B 103.6(5) . . ? C28B Ni1B Br1B 134.0(4) . . ? C1B Ni1B Ni2B 6.0(4) . . ? C29B Ni1B Ni2B 105.6(4) . . ? C25B Ni1B Ni2B 123.4(4) . . ? C26B Ni1B Ni2B 159.0(5) . . ? C27B Ni1B Ni2B 155.3(4) . . ? C28B Ni1B Ni2B 121.2(4) . . ? Br1B Ni1B Ni2B 88.27(5) . . ? C8B Ni2B C30B 99.5(6) . . ? C8B Ni2B C31B 117.3(6) . . ? C30B Ni2B C31B 37.5(6) . . ? C8B Ni2B C34B 118.3(6) . . ? C30B Ni2B C34B 40.4(7) . . ? C31B Ni2B C34B 63.6(7) . . ? C8B Ni2B C32B 154.6(7) . . ? C30B Ni2B C32B 65.0(7) . . ? C31B Ni2B C32B 38.4(6) . . ? C34B Ni2B C32B 63.7(7) . . ? C8B Ni2B C33B 155.1(7) . . ? C30B Ni2B C33B 65.6(7) . . ? C31B Ni2B C33B 63.6(6) . . ? C34B Ni2B C33B 37.6(6) . . ? C32B Ni2B C33B 38.1(6) . . ? C8B Ni2B Br2B 93.8(4) . . ? C30B Ni2B Br2B 166.5(5) . . ? C31B Ni2B Br2B 132.5(6) . . ? C34B Ni2B Br2B 132.8(6) . . ? C32B Ni2B Br2B 101.8(5) . . ? C33B Ni2B Br2B 102.6(5) . . ? C8B Ni2B Ni1B 4.9(4) . . ? C30B Ni2B Ni1B 104.4(5) . . ? C31B Ni2B Ni1B 121.5(5) . . ? C34B Ni2B Ni1B 122.0(5) . . ? C32B Ni2B Ni1B 157.7(5) . . ? C33B Ni2B Ni1B 157.6(6) . . ? Br2B Ni2B Ni1B 88.89(5) . . ? C1B N1B C2B 112.4(11) . . ? C1B N1B C9B 121.3(10) . . ? C2B N1B C9B 126.3(11) . . ? C7B N2B C1B 110.3(11) . . ? C7B N2B C13B 126.1(10) . . ? C1B N2B C13B 123.6(11) . . ? C8B N3B C4B 111.3(11) . . ? C8B N3B C17B 123.4(10) . . ? C4B N3B C17B 125.3(10) . . ? C8B N4B C5B 110.3(11) . . ? C8B N4B C21B 124.1(10) . . ? C5B N4B C21B 125.6(12) . . ? N1B C1B N2B 104.5(11) . . ? N1B C1B Ni1B 129.7(10) . . ? N2B C1B Ni1B 125.4(11) . . ? C7B C2B N1B 106.8(11) . . ? C7B C2B C3B 122.8(11) . . ? N1B C2B C3B 130.3(12) . . ? C2B C3B C4B 113.3(12) . . ? C5B C4B N3B 107.5(11) . . ? C5B C4B C3B 122.9(12) . . ? N3B C4B C3B 129.5(12) . . ? C4B C5B C6B 123.9(12) . . ? C4B C5B N4B 106.0(12) . . ? C6B C5B N4B 130.1(12) . . ? C7B C6B C5B 112.8(11) . . ? C2B C7B C6B 124.2(12) . . ? C2B C7B N2B 106.0(10) . . ? C6B C7B N2B 129.9(12) . . ? N3B C8B N4B 104.9(11) . . ? N3B C8B Ni2B 128.7(10) . . ? N4B C8B Ni2B 126.2(9) . . ? N1B C9B C10B 114.0(10) . . ? C9B C10B C11B 115.5(11) . . ? C12B C11B C10B 112.0(11) . . ? N2B C13B C14B 113.8(11) . . ? C13B C14B C15B 115.1(11) . . ? C14B C15B C16B 113.4(11) . . ? N3B C17B C18B 114.6(13) . . ? C19B C18B C17B 129.9(9) . . ? C18B C19B C20B 113.0(13) . . ? N4B C21B C22B 112.1(12) . . ? C23B C22B C21B 115.3(14) . . ? C22B C23B C24B 109.1(15) . . ? C26B C25B C29B 104.6(14) . . ? C26B C25B Ni1B 72.5(9) . . ? C29B C25B Ni1B 64.7(8) . . ? C25B C26B C27B 108.5(14) . . ? C25B C26B Ni1B 70.2(8) . . ? C27B C26B Ni1B 70.1(7) . . ? C28B C27B C26B 109.0(15) . . ? C28B C27B Ni1B 72.2(9) . . ? C26B C27B Ni1B 69.9(8) . . ? C27B C28B C29B 106.8(14) . . ? C27B C28B Ni1B 71.0(9) . . ? C29B C28B Ni1B 64.2(8) . . ? C28B C29B C25B 110.4(14) . . ? C28B C29B Ni1B 77.3(9) . . ? C25B C29B Ni1B 73.4(8) . . ? C31B C30B C34B 107.3(16) . . ? C31B C30B Ni2B 74.8(10) . . ? C34B C30B Ni2B 73.2(9) . . ? C30B C31B C32B 109.7(17) . . ? C30B C31B Ni2B 67.7(10) . . ? C32B C31B Ni2B 71.1(10) . . ? C31B C32B C33B 107.5(16) . . ? C31B C32B Ni2B 70.5(9) . . ? C33B C32B Ni2B 72.3(9) . . ? C34B C33B C32B 107.4(16) . . ? C34B C33B Ni2B 69.7(8) . . ? C32B C33B Ni2B 69.5(9) . . ? C33B C34B C30B 107.6(16) . . ? C33B C34B Ni2B 72.8(9) . . ? C30B C34B Ni2B 66.4(8) . . ? C7 C2 C3 127(3) . . ? C7 C2 C1 116(3) . . ? C3 C2 C1 117(3) . . ? C4 C3 C2 112(3) . . ? C3 C4 C5 120(3) . . ? C6 C5 C4 131(3) . . ? C7 C6 C5 108(3) . . ? C6 C7 C2 123(3) . . ? C17 C12 C13 124(3) . . ? C17 C12 C11 114(2) . . ? C13 C12 C11 121(2) . . ? C12 C13 C14 120(3) . . ? C13 C14 C15 120(3) . . ? C16 C15 C14 116(3) . . ? C17 C16 C15 128(3) . . ? C12 C17 C16 111(3) . . ? C23 C22 C27 120.0 . . ? C23 C22 C21 128.9(14) . . ? C27 C22 C21 110.5(14) . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.0 . . ? C37 C32 C33 119.3(13) . . ? C37 C32 C31 117.6(17) . . ? C33 C32 C31 122.6(9) . . ? C34 C33 C32 122.6 . . ? C33 C34 C35 115.4(15) . . ? C34 C35 C36 124(3) . . ? C37 C36 C35 118(3) . . ? C32 C37 C36 120(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 24.18 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.715 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.166 # Attachment 'cif-5.cif' data_sad7 _database_code_depnum_ccdc_archive 'CCDC 716393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C94 H124 B4 F16 N12 Ni4 O2' _chemical_formula_weight 2036.13 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' B B 0.0013 0.0007 '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' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.368(2) _cell_length_b 16.892(2) _cell_length_c 18.687(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.086(2) _cell_angle_gamma 90.00 _cell_volume 5087.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour orange-brown _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7274 _exptl_absorpt_correction_T_max 0.9683 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.808197 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42223 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0696 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.87 _reflns_number_total 9730 _reflns_number_gt 5168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _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. The Uij of the disordered butyl groups were refined through one common FVAR. The bond distance of one BF4 and of the disordered C3H6O was fixed through Dfix and Dang command. ; _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^)+(0.1754P)^2^+25.2287P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9730 _refine_ls_number_parameters 630 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1664 _refine_ls_R_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.3302 _refine_ls_wR_factor_gt 0.2650 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni -0.22924(5) 0.37957(6) 0.03924(6) 0.0473(3) Uani 1 1 d . . . Ni2 Ni 0.38784(6) 0.24638(6) 0.02963(7) 0.0571(4) Uani 1 1 d . . . N1 N -0.0772(3) 0.3649(4) -0.0196(4) 0.0461(15) Uani 1 1 d . . . N2 N -0.0567(3) 0.3429(4) 0.0960(4) 0.0460(15) Uani 1 1 d . B . N3 N 0.2192(3) 0.2983(4) -0.0253(4) 0.0496(17) Uani 1 1 d . . . N4 N 0.2414(3) 0.2811(4) 0.0914(4) 0.0500(16) Uani 1 1 d . . . N5 N -0.2591(3) 0.2700(4) 0.0306(4) 0.0437(15) Uani 1 1 d . . . N6 N 0.3626(4) 0.1366(4) 0.0165(4) 0.0545(18) Uani 1 1 d . . . C1 C -0.1162(4) 0.3617(4) 0.0387(5) 0.0458(18) Uani 1 1 d . . . C2 C 0.0070(4) 0.3451(4) 0.0002(4) 0.0439(18) Uani 1 1 d . . . C3 C 0.0669(4) 0.3364(5) -0.0418(5) 0.0479(19) Uani 1 1 d . . . H3 H 0.0573 0.3446 -0.0929 0.057 Uiso 1 1 calc R . . C4 C 0.1435(4) 0.3143(4) -0.0022(5) 0.0452(18) Uani 1 1 d . . . C5 C 0.1579(4) 0.3024(4) 0.0728(5) 0.0475(19) Uani 1 1 d . . . C6 C 0.0969(4) 0.3095(5) 0.1151(5) 0.052(2) Uani 1 1 d . . . H6 H 0.1062 0.3004 0.1660 0.062 Uiso 1 1 calc R . . C7 C 0.0197(4) 0.3315(4) 0.0746(4) 0.0452(18) Uani 1 1 d . . . C8 C 0.2776(5) 0.2782(5) 0.0326(5) 0.053(2) Uani 1 1 d . . . C9 C -0.1163(4) 0.3838(5) -0.0926(5) 0.051(2) Uani 1 1 d . . . H9A H -0.1772 0.3805 -0.0958 0.061 Uiso 1 1 calc R . . H9B H -0.1000 0.3437 -0.1260 0.061 Uiso 1 1 calc R . . C10 C -0.0942(5) 0.4658(5) -0.1177(5) 0.062(2) Uani 1 1 d . . . H10A H -0.1006 0.5049 -0.0796 0.074 Uiso 1 1 calc R . . H10B H -0.0353 0.4659 -0.1235 0.074 Uiso 1 1 calc R . . C11 C -0.1457(7) 0.4908(7) -0.1867(6) 0.093(4) Uani 1 1 d D . . H11A H -0.1282 0.5444 -0.1991 0.111 Uiso 1 1 calc R . . H11B H -0.2043 0.4941 -0.1799 0.111 Uiso 1 1 calc R . . C12 C -0.1406(9) 0.4354(8) -0.2506(6) 0.117(5) Uani 1 1 d D . . H12A H -0.1000 0.3935 -0.2348 0.176 Uiso 1 1 calc R . . H12B H -0.1235 0.4655 -0.2902 0.176 Uiso 1 1 calc R . . H12C H -0.1952 0.4115 -0.2676 0.176 Uiso 1 1 calc R . . C13 C -0.0716(5) 0.3279(5) 0.1720(5) 0.060(2) Uani 1 1 d D . . H13A H -0.1232 0.3548 0.1795 0.072 Uiso 0.50 1 calc PR A 3 H13B H -0.0249 0.3493 0.2077 0.072 Uiso 0.50 1 calc PR A 3 H13C H -0.0512 0.2744 0.1876 0.072 Uiso 0.50 1 calc PR A 4 H13D H -0.1320 0.3294 0.1723 0.072 Uiso 0.50 1 calc PR A 4 C14 C -0.0793(9) 0.2386(6) 0.1829(8) 0.061(5) Uani 0.50 1 d PD B 3 H14A H -0.1180 0.2161 0.1412 0.073 Uiso 0.50 1 calc PR B 3 H14B H -0.0244 0.2135 0.1843 0.073 Uiso 0.50 1 calc PR B 3 C15 C -0.1109(12) 0.2198(10) 0.2534(8) 0.070(5) Uani 0.50 1 d PD B 3 H15A H -0.0714 0.2415 0.2949 0.084 Uiso 0.50 1 calc PR B 3 H15B H -0.1649 0.2465 0.2524 0.084 Uiso 0.50 1 calc PR B 3 C16 C -0.1216(14) 0.1311(10) 0.2654(15) 0.084(7) Uani 0.50 1 d PD B 3 H16A H -0.1602 0.1089 0.2242 0.126 Uiso 0.50 1 calc PR B 3 H16B H -0.1438 0.1229 0.3103 0.126 Uiso 0.50 1 calc PR B 3 H16C H -0.0677 0.1046 0.2694 0.126 Uiso 0.50 1 calc PR B 3 C14A C -0.0259(11) 0.3923(13) 0.2286(8) 0.070(5) Uani 0.50 1 d PD B 4 H14C H 0.0349 0.3888 0.2312 0.084 Uiso 0.50 1 calc PR B 4 H14D H -0.0440 0.4462 0.2123 0.084 Uiso 0.50 1 calc PR B 4 C15A C -0.0479(11) 0.3762(15) 0.3036(7) 0.105(9) Uani 0.50 1 d PD B 4 H15C H -0.0939 0.4110 0.3120 0.126 Uiso 0.50 1 calc PR B 4 H15D H -0.0653 0.3204 0.3071 0.126 Uiso 0.50 1 calc PR B 4 C16A C 0.0301(11) 0.3931(17) 0.3596(10) 0.094(8) Uani 0.50 1 d PD B 4 H16D H 0.0616 0.3440 0.3709 0.142 Uiso 0.50 1 calc PR B 4 H16E H 0.0141 0.4141 0.4041 0.142 Uiso 0.50 1 calc PR B 4 H16F H 0.0646 0.4321 0.3399 0.142 Uiso 0.50 1 calc PR B 4 C17 C 0.2294(6) 0.2959(9) -0.1003(6) 0.100(4) Uani 1 1 d D . . H17A H 0.2887 0.2981 -0.1049 0.120 Uiso 1 1 calc R . . H17B H 0.1994 0.3399 -0.1285 0.120 Uiso 1 1 calc R . . C18 C 0.191(2) 0.2157(12) -0.1251(17) 0.290(10) Uiso 1 1 d D . . H18A H 0.2164 0.1736 -0.0916 0.348 Uiso 1 1 calc R . . H18B H 0.1307 0.2167 -0.1246 0.348 Uiso 1 1 calc R . . C19 C 0.206(2) 0.199(2) -0.2021(17) 0.290(10) Uiso 1 1 d D . . H19A H 0.2664 0.2003 -0.2045 0.348 Uiso 1 1 calc R . . H19B H 0.1766 0.2372 -0.2376 0.348 Uiso 1 1 calc R . . C20 C 0.171(2) 0.1155(19) -0.2147(18) 0.290(10) Uiso 1 1 d D . . H20A H 0.1788 0.0867 -0.1684 0.435 Uiso 1 1 calc R . . H20B H 0.1992 0.0875 -0.2491 0.435 Uiso 1 1 calc R . . H20C H 0.1113 0.1187 -0.2345 0.435 Uiso 1 1 calc R . . C21 C 0.2833(5) 0.2661(6) 0.1664(5) 0.063(2) Uani 1 1 d . . . H21A H 0.3364 0.2385 0.1652 0.076 Uiso 1 1 calc R . . H21B H 0.2482 0.2306 0.1903 0.076 Uiso 1 1 calc R . . C22 C 0.3009(6) 0.3407(7) 0.2114(5) 0.075(3) Uani 1 1 d D D . H22A H 0.2477 0.3674 0.2142 0.090 Uiso 1 1 calc R . . H22B H 0.3342 0.3772 0.1866 0.090 Uiso 1 1 calc R . . C23 C 0.3473(6) 0.3249(8) 0.2884(5) 0.106(4) Uani 1 1 d D . . H23A H 0.3984 0.2944 0.2860 0.128 Uiso 0.50 1 calc PR C 1 H23B H 0.3120 0.2927 0.3150 0.128 Uiso 0.50 1 calc PR C 1 H23C H 0.3431 0.3730 0.3180 0.128 Uiso 0.50 1 calc PR C 2 H23D H 0.3183 0.2817 0.3096 0.128 Uiso 0.50 1 calc PR C 2 C24 C 0.370(2) 0.4022(13) 0.3298(16) 0.159(15) Uani 0.50 1 d PD D 1 H24A H 0.3973 0.3901 0.3797 0.238 Uiso 0.50 1 calc PR D 1 H24B H 0.3202 0.4334 0.3307 0.238 Uiso 0.50 1 calc PR D 1 H24C H 0.4088 0.4325 0.3055 0.238 Uiso 0.50 1 calc PR D 1 C24A C 0.4390(7) 0.3026(16) 0.2965(16) 0.110(9) Uani 0.50 1 d PD D 2 H24D H 0.4631 0.2981 0.3482 0.164 Uiso 0.50 1 calc PR D 2 H24E H 0.4686 0.3435 0.2740 0.164 Uiso 0.50 1 calc PR D 2 H24F H 0.4442 0.2517 0.2724 0.164 Uiso 0.50 1 calc PR D 2 C25 C -0.2734(8) 0.4864(7) -0.0154(8) 0.090(4) Uani 1 1 d . . . H25 H -0.2632 0.5056 -0.0608 0.108 Uiso 1 1 calc R . . C26 C -0.3427(6) 0.4399(6) -0.0038(7) 0.083(3) Uani 1 1 d . . . H26 H -0.3853 0.4191 -0.0400 0.099 Uiso 1 1 calc R . . C27 C -0.3353(5) 0.4309(6) 0.0717(7) 0.074(3) Uani 1 1 d . . . H27 H -0.3725 0.4020 0.0955 0.089 Uiso 1 1 calc R . . C28 C -0.2657(6) 0.4705(6) 0.1061(7) 0.078(3) Uani 1 1 d . . . H28 H -0.2496 0.4775 0.1570 0.094 Uiso 1 1 calc R . . C29 C -0.2232(6) 0.4985(6) 0.0523(8) 0.080(3) Uani 1 1 d . . . H29 H -0.1695 0.5217 0.0605 0.095 Uiso 1 1 calc R . . C30 C 0.4438(8) 0.3500(8) 0.0057(16) 0.120(7) Uani 1 1 d . . . H30 H 0.4123 0.3915 -0.0201 0.144 Uiso 1 1 calc R . . C31 C 0.4805(10) 0.2961(14) -0.0243(8) 0.110(5) Uani 1 1 d . . . H31 H 0.4841 0.2915 -0.0743 0.132 Uiso 1 1 calc R . . C32 C 0.5148(7) 0.2451(8) 0.0325(18) 0.132(8) Uani 1 1 d . . . H32 H 0.5423 0.1965 0.0268 0.158 Uiso 1 1 calc R . . C33 C 0.5021(11) 0.2766(18) 0.0975(12) 0.148(9) Uani 1 1 d . . . H33 H 0.5219 0.2574 0.1452 0.177 Uiso 1 1 calc R . . C34 C 0.4548(11) 0.3411(13) 0.0779(17) 0.138(9) Uani 1 1 d . . . H34 H 0.4327 0.3750 0.1104 0.166 Uiso 1 1 calc R . . C35 C -0.2667(6) 0.2348(6) -0.0329(5) 0.062(2) Uani 1 1 d . . . H35 H -0.2580 0.2650 -0.0738 0.074 Uiso 1 1 calc R . . C36 C -0.2870(6) 0.1553(5) -0.0427(5) 0.061(2) Uani 1 1 d . . . H36 H -0.2923 0.1326 -0.0897 0.073 Uiso 1 1 calc R . . C37 C -0.2994(4) 0.1099(4) 0.0140(5) 0.0446(18) Uani 1 1 d . . . C38 C -0.2908(5) 0.1460(5) 0.0811(5) 0.054(2) Uani 1 1 d . . . H38 H -0.2983 0.1164 0.1227 0.065 Uiso 1 1 calc R . . C39 C -0.2715(5) 0.2254(5) 0.0875(5) 0.058(2) Uani 1 1 d . . . H39 H -0.2666 0.2496 0.1339 0.069 Uiso 1 1 calc R . . C40 C -0.3213(4) 0.0250(5) 0.0043(5) 0.0483(19) Uani 1 1 d . . . C41 C 0.3102(10) 0.1005(7) 0.0518(10) 0.127(6) Uani 1 1 d . . . H41 H 0.2835 0.1307 0.0839 0.152 Uiso 1 1 calc R . . C42 C 0.2923(10) 0.0192(7) 0.0441(8) 0.114(5) Uani 1 1 d . . . H42 H 0.2584 -0.0046 0.0744 0.137 Uiso 1 1 calc R . . C43 C 0.3901(8) 0.0939(7) -0.0330(7) 0.098(4) Uani 1 1 d . . . H43 H 0.4254 0.1186 -0.0617 0.117 Uiso 1 1 calc R . . C44 C 0.3702(9) 0.0147(7) -0.0457(7) 0.100(4) Uani 1 1 d . . . H44 H 0.3905 -0.0126 -0.0834 0.120 Uiso 1 1 calc R . . B1 B 0.1252(9) 0.1911(15) 0.2958(8) 0.115(7) Uani 1 1 d . . . F1 F 0.0796(7) 0.1795(12) 0.3458(7) 0.275(10) Uani 1 1 d . . . F2 F 0.2000(6) 0.1580(7) 0.3182(5) 0.170(5) Uani 1 1 d . . . F3 F 0.1366(6) 0.2717(6) 0.2909(4) 0.138(3) Uani 1 1 d . . . F4 F 0.0982(9) 0.1609(8) 0.2261(6) 0.236(8) Uani 1 1 d . . . B2 B 0.8913(6) 0.6072(8) 0.2609(5) 0.200(13) Uiso 1 1 d D . . F5 F 0.8477(12) 0.6728(9) 0.2708(10) 0.281(9) Uani 1 1 d D . . F6 F 0.9508(6) 0.5986(7) 0.3201(5) 0.155(4) Uani 1 1 d D . . F7 F 0.9193(6) 0.5848(10) 0.2002(5) 0.238(8) Uani 1 1 d D . . F8 F 0.8296(7) 0.5555(8) 0.2655(5) 0.174(4) Uani 1 1 d D . . O51 O -0.0620(15) 0.1442(19) 0.0008(16) 0.185(12) Uani 0.50 1 d PD . . C51 C 0.0731(15) 0.1150(17) 0.025(2) 0.166(19) Uani 0.50 1 d PD . . H51A H 0.0832 0.1681 0.0071 0.249 Uiso 0.50 1 calc PR . . H51B H 0.0752 0.0762 -0.0137 0.249 Uiso 0.50 1 calc PR . . H51C H 0.1158 0.1024 0.0670 0.249 Uiso 0.50 1 calc PR . . C52 C -0.0096(16) 0.1127(16) 0.0463(16) 0.20(3) Uani 0.50 1 d PD . . C53 C -0.043(2) 0.0479(18) 0.086(2) 0.20(2) Uani 0.50 1 d PD . . H53A H -0.1042 0.0477 0.0726 0.301 Uiso 0.50 1 calc PR . . H53B H -0.0273 0.0560 0.1380 0.301 Uiso 0.50 1 calc PR . . H53C H -0.0216 -0.0028 0.0719 0.301 Uiso 0.50 1 calc PR . . O51A O -0.121(2) 0.113(2) 0.283(2) 0.234(12) Uiso 0.50 1 d PD E 5 C51A C -0.110(3) 0.038(3) 0.181(3) 0.234(12) Uiso 0.50 1 d PD E 5 H51D H -0.1686 0.0265 0.1813 0.351 Uiso 0.50 1 calc P F 5 H51E H -0.0799 -0.0112 0.1769 0.351 Uiso 0.50 1 calc P G 5 H51F H -0.1054 0.0728 0.1399 0.351 Uiso 0.50 1 calc P H 5 C52A C -0.0740(18) 0.079(3) 0.2497(18) 0.234(12) Uiso 0.50 1 d PD E 5 C53A C -0.013(3) 0.028(3) 0.297(3) 0.234(12) Uiso 0.50 1 d PD E 5 H53D H 0.0043 -0.0151 0.2675 0.351 Uiso 0.50 1 calc P I 5 H53E H -0.0392 0.0053 0.3355 0.351 Uiso 0.50 1 calc P J 5 H53F H 0.0350 0.0595 0.3178 0.351 Uiso 0.50 1 calc P K 5 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 0.0211(5) 0.0453(6) 0.0762(7) -0.0063(5) 0.0107(4) -0.0017(4) Ni2 0.0218(5) 0.0426(6) 0.1074(10) -0.0029(6) 0.0127(5) 0.0000(4) N1 0.022(3) 0.048(4) 0.066(4) -0.006(3) 0.003(3) -0.001(3) N2 0.024(3) 0.053(4) 0.062(4) 0.001(3) 0.010(3) 0.002(3) N3 0.025(3) 0.052(4) 0.074(5) -0.003(3) 0.016(3) 0.000(3) N4 0.023(3) 0.052(4) 0.075(5) 0.003(3) 0.007(3) 0.006(3) N5 0.025(3) 0.044(3) 0.064(4) -0.002(3) 0.010(3) -0.003(2) N6 0.031(3) 0.045(4) 0.089(5) -0.008(4) 0.013(3) -0.002(3) C1 0.029(4) 0.041(4) 0.069(5) -0.009(4) 0.013(4) -0.006(3) C2 0.023(3) 0.045(4) 0.062(5) -0.002(4) 0.005(3) 0.000(3) C3 0.027(4) 0.052(5) 0.065(5) -0.003(4) 0.008(3) -0.006(3) C4 0.019(3) 0.048(4) 0.068(5) -0.006(4) 0.007(3) -0.001(3) C5 0.022(3) 0.042(4) 0.077(6) 0.001(4) 0.007(3) 0.002(3) C6 0.028(4) 0.053(5) 0.074(6) 0.004(4) 0.008(4) 0.004(3) C7 0.025(3) 0.047(4) 0.064(5) 0.001(4) 0.008(3) 0.003(3) C8 0.028(4) 0.037(4) 0.093(7) -0.001(4) 0.007(4) -0.002(3) C9 0.026(3) 0.060(5) 0.066(5) -0.009(4) 0.006(3) 0.000(3) C10 0.038(4) 0.063(5) 0.082(6) 0.002(5) 0.005(4) 0.000(4) C11 0.073(7) 0.088(8) 0.105(9) 0.007(7) -0.020(6) 0.013(6) C12 0.107(11) 0.144(13) 0.091(9) 0.028(9) -0.007(8) -0.011(9) C13 0.039(4) 0.079(6) 0.066(6) -0.006(5) 0.018(4) -0.003(4) C14 0.029(8) 0.081(13) 0.074(12) 0.014(10) 0.015(8) 0.011(8) C15 0.057(11) 0.107(16) 0.051(11) 0.017(10) 0.022(9) 0.011(11) C16 0.056(12) 0.099(17) 0.092(17) 0.050(14) 0.001(11) 0.000(11) C14A 0.047(10) 0.091(15) 0.069(12) 0.013(11) 0.004(9) 0.006(10) C15A 0.17(3) 0.091(17) 0.072(15) 0.013(13) 0.058(17) -0.013(17) C16A 0.058(12) 0.19(3) 0.035(10) 0.006(13) -0.005(8) -0.013(14) C17 0.033(5) 0.175(13) 0.095(9) -0.011(8) 0.021(5) 0.014(6) C21 0.027(4) 0.071(6) 0.090(7) 0.021(5) 0.004(4) 0.014(4) C22 0.043(5) 0.089(7) 0.084(7) -0.006(6) -0.012(5) 0.005(5) C23 0.063(7) 0.118(11) 0.126(11) 0.006(8) -0.020(7) 0.002(7) C24 0.14(3) 0.24(4) 0.09(2) -0.07(2) -0.004(19) -0.05(3) C24A 0.044(11) 0.12(2) 0.16(3) 0.012(18) -0.015(13) -0.002(12) C25 0.088(8) 0.072(7) 0.122(10) 0.018(7) 0.049(8) 0.045(6) C26 0.047(5) 0.070(7) 0.122(10) -0.014(6) -0.011(6) 0.030(5) C27 0.038(5) 0.057(6) 0.134(10) -0.006(6) 0.033(6) 0.008(4) C28 0.063(6) 0.068(6) 0.105(8) -0.026(6) 0.019(6) 0.016(5) C29 0.037(5) 0.053(5) 0.153(11) -0.005(6) 0.026(6) -0.004(4) C30 0.053(7) 0.049(7) 0.25(2) 0.019(11) -0.002(12) -0.015(6) C31 0.064(8) 0.157(15) 0.117(11) -0.030(11) 0.036(8) -0.063(10) C32 0.022(5) 0.064(7) 0.31(3) -0.030(13) 0.035(10) -0.006(5) C33 0.058(9) 0.22(2) 0.148(15) 0.071(15) -0.042(10) -0.087(12) C34 0.071(11) 0.125(15) 0.24(2) -0.097(17) 0.073(14) -0.061(10) C35 0.064(6) 0.064(6) 0.058(6) -0.001(4) 0.012(4) -0.018(4) C36 0.061(5) 0.060(5) 0.068(6) -0.015(5) 0.025(5) -0.016(4) C37 0.025(3) 0.041(4) 0.070(5) 0.004(4) 0.014(3) 0.003(3) C38 0.045(4) 0.053(5) 0.067(6) 0.005(4) 0.014(4) 0.003(4) C39 0.059(5) 0.046(5) 0.070(6) -0.005(4) 0.018(4) -0.003(4) C40 0.030(4) 0.048(4) 0.069(5) 0.000(4) 0.015(4) 0.001(3) C41 0.118(11) 0.063(7) 0.217(17) -0.017(9) 0.082(12) -0.012(7) C42 0.144(13) 0.074(8) 0.139(12) -0.012(8) 0.065(10) -0.024(8) C43 0.100(9) 0.077(8) 0.125(11) 0.006(7) 0.046(8) -0.016(7) C44 0.134(11) 0.066(7) 0.110(10) -0.005(6) 0.048(8) -0.013(7) B1 0.064(8) 0.20(2) 0.069(9) 0.045(11) -0.007(7) -0.045(11) F1 0.135(9) 0.49(3) 0.196(12) 0.176(15) 0.028(8) -0.064(13) F2 0.137(7) 0.241(11) 0.118(7) -0.018(7) -0.023(6) 0.106(8) F3 0.185(10) 0.144(8) 0.088(5) 0.012(5) 0.036(6) 0.029(7) F4 0.314(16) 0.217(12) 0.123(8) 0.072(8) -0.105(9) -0.155(11) F5 0.34(2) 0.249(19) 0.267(18) -0.015(14) 0.092(16) 0.096(17) F6 0.115(7) 0.233(11) 0.114(6) -0.025(7) 0.012(5) -0.008(7) F7 0.114(7) 0.51(2) 0.102(6) 0.102(10) 0.050(5) 0.098(11) F8 0.166(10) 0.247(13) 0.115(7) -0.039(7) 0.036(6) -0.028(9) O51 0.16(2) 0.23(3) 0.17(2) 0.03(2) 0.016(19) -0.07(2) C51 0.11(2) 0.075(19) 0.32(6) -0.10(3) 0.06(3) -0.012(16) C52 0.45(9) 0.051(16) 0.08(2) 0.016(14) -0.01(3) -0.06(3) C53 0.10(2) 0.27(6) 0.24(5) -0.13(5) 0.04(3) 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 C1 1.876(7) . ? Ni1 N5 1.913(6) . ? Ni1 C29 2.024(10) . ? Ni1 C27 2.122(8) . ? Ni1 C28 2.130(9) . ? Ni1 C25 2.136(11) . ? Ni1 C26 2.147(9) . ? Ni1 Ni2 10.3804(18) . ? Ni2 C8 1.892(7) . ? Ni2 N6 1.906(7) . ? Ni2 C34 2.057(13) . ? Ni2 C30 2.060(13) . ? Ni2 C32 2.069(10) . ? Ni2 C33 2.129(12) . ? Ni2 C31 2.136(11) . ? Ni2 Ni1 10.910(2) 3 ? N1 C1 1.358(10) . ? N1 C2 1.403(9) . ? N1 C9 1.436(10) . ? N2 C1 1.353(10) . ? N2 C7 1.391(9) . ? N2 C13 1.504(11) . ? N3 C8 1.356(10) . ? N3 C4 1.409(9) . ? N3 C17 1.441(13) . ? N4 C8 1.338(11) . ? N4 C5 1.397(9) . ? N4 C21 1.471(11) . ? N5 C35 1.315(11) . ? N5 C39 1.347(11) . ? N6 C43 1.313(14) . ? N6 C41 1.320(14) . ? C2 C3 1.367(10) . ? C2 C7 1.390(11) . ? C3 C4 1.389(10) . ? C4 C5 1.394(11) . ? C5 C6 1.383(11) . ? C6 C7 1.404(10) . ? C9 C10 1.526(12) . ? C10 C11 1.473(13) . ? C11 C12 1.5297(10) . ? C13 C14 1.5302(11) . ? C13 C14A 1.61(2) . ? C14 C15 1.5300(10) . ? C15 C16 1.5300(11) . ? C14A C15A 1.5300(10) . ? C15A C16A 1.5299(11) . ? C17 C18 1.5302(10) . ? C18 C19 1.5299(11) . ? C19 C20 1.5301(11) . ? C21 C22 1.514(14) . ? C22 C23 1.5300(10) . ? C23 C24A 1.5297(11) . ? C23 C24 1.5300(11) . ? C25 C29 1.398(16) . ? C25 C26 1.428(16) . ? C26 C27 1.403(15) . ? C27 C28 1.379(14) . ? C28 C29 1.401(15) . ? C30 C31 1.27(2) . ? C30 C34 1.34(2) . ? C31 C32 1.41(2) . ? C32 C33 1.38(3) . ? C33 C34 1.35(3) . ? C35 C36 1.387(12) . ? C36 C37 1.351(12) . ? C37 C38 1.380(12) . ? C37 C40 1.483(10) . ? C38 C39 1.377(12) . ? C40 C42 1.323(15) 3 ? C40 C44 1.380(14) 3 ? C41 C42 1.406(16) . ? C42 C40 1.323(15) 3 ? C43 C44 1.388(16) . ? C44 C40 1.380(14) 3 ? B1 F1 1.309(17) . ? B1 F2 1.344(19) . ? B1 F3 1.38(2) . ? B1 F4 1.40(2) . ? B2 F6 1.3489(10) . ? B2 F7 1.3490(10) . ? B2 F8 1.3490(10) . ? B2 F5 1.3492(10) . ? O51 C52 1.2198(10) . ? C51 C52 1.4778(11) . ? C52 C53 1.4780(10) . ? O51A C52A 1.2199(10) . ? C51A C52A 1.4779(11) . ? C52A C53A 1.4780(10) . ? 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 C1 Ni1 N5 94.6(3) . . ? C1 Ni1 C29 97.7(3) . . ? N5 Ni1 C29 167.5(3) . . ? C1 Ni1 C27 157.5(4) . . ? N5 Ni1 C27 102.1(3) . . ? C29 Ni1 C27 65.5(4) . . ? C1 Ni1 C28 119.8(4) . . ? N5 Ni1 C28 130.8(4) . . ? C29 Ni1 C28 39.3(4) . . ? C27 Ni1 C28 37.8(4) . . ? C1 Ni1 C25 112.6(4) . . ? N5 Ni1 C25 135.8(5) . . ? C29 Ni1 C25 39.2(4) . . ? C27 Ni1 C25 64.3(4) . . ? C28 Ni1 C25 64.2(5) . . ? C1 Ni1 C26 149.7(5) . . ? N5 Ni1 C26 103.7(4) . . ? C29 Ni1 C26 66.1(4) . . ? C27 Ni1 C26 38.4(4) . . ? C28 Ni1 C26 64.2(4) . . ? C25 Ni1 C26 38.9(4) . . ? C1 Ni1 Ni2 3.3(2) . . ? N5 Ni1 Ni2 91.35(17) . . ? C29 Ni1 Ni2 101.0(3) . . ? C27 Ni1 Ni2 160.2(3) . . ? C28 Ni1 Ni2 122.7(3) . . ? C25 Ni1 Ni2 115.1(3) . . ? C26 Ni1 Ni2 151.3(4) . . ? C8 Ni2 N6 95.4(3) . . ? C8 Ni2 C34 101.8(6) . . ? N6 Ni2 C34 154.2(10) . . ? C8 Ni2 C30 103.2(5) . . ? N6 Ni2 C30 153.2(8) . . ? C34 Ni2 C30 37.9(7) . . ? C8 Ni2 C32 163.8(4) . . ? N6 Ni2 C32 100.8(4) . . ? C34 Ni2 C32 62.7(6) . . ? C30 Ni2 C32 62.1(6) . . ? C8 Ni2 C33 131.0(11) . . ? N6 Ni2 C33 117.2(9) . . ? C34 Ni2 C33 37.6(7) . . ? C30 Ni2 C33 63.2(6) . . ? C32 Ni2 C33 38.2(7) . . ? C8 Ni2 C31 131.4(7) . . ? N6 Ni2 C31 118.5(6) . . ? C34 Ni2 C31 62.1(6) . . ? C30 Ni2 C31 35.3(6) . . ? C32 Ni2 C31 39.0(7) . . ? C33 Ni2 C31 64.2(6) . . ? C8 Ni2 Ni1 4.0(2) . . ? N6 Ni2 Ni1 91.36(19) . . ? C34 Ni2 Ni1 105.6(5) . . ? C30 Ni2 Ni1 106.9(4) . . ? C32 Ni2 Ni1 167.8(3) . . ? C33 Ni2 Ni1 133.9(10) . . ? C31 Ni2 Ni1 134.2(7) . . ? C8 Ni2 Ni1 94.0(2) . 3 ? N6 Ni2 Ni1 1.5(2) . 3 ? C34 Ni2 Ni1 154.6(10) . 3 ? C30 Ni2 Ni1 154.6(8) . 3 ? C32 Ni2 Ni1 102.1(3) . 3 ? C33 Ni2 Ni1 118.0(8) . 3 ? C31 Ni2 Ni1 120.0(6) . 3 ? Ni1 Ni2 Ni1 89.997(11) . 3 ? C1 N1 C2 110.9(7) . . ? C1 N1 C9 125.2(6) . . ? C2 N1 C9 123.8(6) . . ? C1 N2 C7 111.3(6) . . ? C1 N2 C13 125.0(6) . . ? C7 N2 C13 123.4(6) . . ? C8 N3 C4 109.8(7) . . ? C8 N3 C17 125.8(7) . . ? C4 N3 C17 124.1(7) . . ? C8 N4 C5 111.1(7) . . ? C8 N4 C21 125.2(6) . . ? C5 N4 C21 123.7(7) . . ? C35 N5 C39 117.1(7) . . ? C35 N5 Ni1 119.8(6) . . ? C39 N5 Ni1 123.1(6) . . ? C43 N6 C41 115.5(9) . . ? C43 N6 Ni2 122.2(7) . . ? C41 N6 Ni2 122.0(7) . . ? N2 C1 N1 105.7(6) . . ? N2 C1 Ni1 127.4(6) . . ? N1 C1 Ni1 126.9(6) . . ? C3 C2 C7 124.0(7) . . ? C3 C2 N1 130.2(8) . . ? C7 C2 N1 105.8(6) . . ? C2 C3 C4 113.2(8) . . ? C3 C4 C5 123.5(7) . . ? C3 C4 N3 130.4(8) . . ? C5 C4 N3 106.1(6) . . ? C6 C5 C4 123.4(7) . . ? C6 C5 N4 130.7(8) . . ? C4 C5 N4 105.9(6) . . ? C5 C6 C7 112.7(8) . . ? C2 C7 N2 106.3(6) . . ? C2 C7 C6 123.1(7) . . ? N2 C7 C6 130.6(8) . . ? N4 C8 N3 107.1(6) . . ? N4 C8 Ni2 126.7(6) . . ? N3 C8 Ni2 126.2(7) . . ? N1 C9 C10 113.8(7) . . ? C11 C10 C9 113.6(8) . . ? C10 C11 C12 114.0(9) . . ? N2 C13 C14 108.8(7) . . ? N2 C13 C14A 112.0(8) . . ? C14 C13 C14A 128.2(11) . . ? C15 C14 C13 111.6(10) . . ? C16 C15 C14 113.3(14) . . ? C15A C14A C13 109.0(14) . . ? C16A C15A C14A 107.0(14) . . ? N3 C17 C18 101.9(15) . . ? C19 C18 C17 109(2) . . ? C18 C19 C20 101(2) . . ? N4 C21 C22 113.4(7) . . ? C21 C22 C23 113.1(9) . . ? C24A C23 C22 116.9(13) . . ? C24A C23 C24 90.5(18) . . ? C22 C23 C24 111.4(15) . . ? C29 C25 C26 107.4(10) . . ? C29 C25 Ni1 66.1(6) . . ? C26 C25 Ni1 70.9(6) . . ? C27 C26 C25 106.3(10) . . ? C27 C26 Ni1 69.8(5) . . ? C25 C26 Ni1 70.1(6) . . ? C28 C27 C26 109.6(10) . . ? C28 C27 Ni1 71.4(5) . . ? C26 C27 Ni1 71.8(5) . . ? C27 C28 C29 107.6(11) . . ? C27 C28 Ni1 70.7(5) . . ? C29 C28 Ni1 66.3(6) . . ? C25 C29 C28 108.3(9) . . ? C25 C29 Ni1 74.8(6) . . ? C28 C29 Ni1 74.4(6) . . ? C31 C30 C34 111.9(17) . . ? C31 C30 Ni2 75.6(8) . . ? C34 C30 Ni2 70.9(9) . . ? C30 C31 C32 105.2(16) . . ? C30 C31 Ni2 69.1(8) . . ? C32 C31 Ni2 67.9(7) . . ? C33 C32 C31 109.1(14) . . ? C33 C32 Ni2 73.3(7) . . ? C31 C32 Ni2 73.0(7) . . ? C34 C33 C32 103.9(16) . . ? C34 C33 Ni2 68.3(8) . . ? C32 C33 Ni2 68.5(7) . . ? C30 C34 C33 109.5(18) . . ? C30 C34 Ni2 71.2(9) . . ? C33 C34 Ni2 74.1(9) . . ? N5 C35 C36 122.6(8) . . ? C37 C36 C35 120.8(8) . . ? C36 C37 C38 117.1(7) . . ? C36 C37 C40 121.3(8) . . ? C38 C37 C40 121.5(7) . . ? C39 C38 C37 119.6(8) . . ? N5 C39 C38 122.8(8) . . ? C42 C40 C44 115.0(9) 3 3 ? C42 C40 C37 121.4(8) 3 . ? C44 C40 C37 123.6(8) 3 . ? N6 C41 C42 122.8(12) . . ? C40 C42 C41 121.9(12) 3 . ? N6 C43 C44 123.5(11) . . ? C40 C44 C43 120.9(11) 3 . ? F1 B1 F2 108.5(14) . . ? F1 B1 F3 107(2) . . ? F2 B1 F3 107.8(12) . . ? F1 B1 F4 118.9(15) . . ? F2 B1 F4 105.1(18) . . ? F3 B1 F4 108.8(12) . . ? F6 B2 F7 110.9(9) . . ? F6 B2 F8 108.6(10) . . ? F7 B2 F8 103.9(9) . . ? F6 B2 F5 107.4(12) . . ? F7 B2 F5 127.8(13) . . ? F8 B2 F5 95.9(12) . . ? O51 C52 C51 111(3) . . ? O51 C52 C53 113(3) . . ? C51 C52 C53 127(3) . . ? O51A C52A C51A 118.0(16) . . ? O51A C52A C53A 113.1(15) . . ? C51A C52A C53A 112(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.552 _refine_diff_density_min -0.780 _refine_diff_density_rms 0.138