# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 N4, 2(Br)' _chemical_formula_sum 'C20 H32 Br2 N4' _chemical_formula_weight 488.32 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 _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4538(6) _cell_length_b 10.1708(6) _cell_length_c 11.0501(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.582(4) _cell_angle_gamma 90.00 _cell_volume 1131.70(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 75 _exptl_crystal_description 'transparent block' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 500 _exptl_absorpt_coefficient_mu 4.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4301 _exptl_absorpt_correction_T_max 0.6554 _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 = 0.602489 ; _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 6067 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 72.09 _reflns_number_total 2128 _reflns_number_gt 2003 _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 , 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. The ratio of unique refelctions (2128) relative to the numbe of refined parameters (120) is high so that the slightly low (0.956) fraction of measured reflections is not significant. ; _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^)+(0.0500P)^2^+0.6005P] 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 2128 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.93913(2) 0.19806(2) 0.11458(2) 0.03020(13) Uani 1 1 d . . . N1 N 0.74361(18) 0.88703(19) 1.07708(17) 0.0227(4) Uani 1 1 d . . . N2 N 0.71002(18) 0.9925(2) 0.89916(17) 0.0224(4) Uani 1 1 d . . . C3 C 0.5941(2) 1.0063(2) 0.9373(2) 0.0199(4) Uani 1 1 d . . . C4 C 0.4767(2) 1.0695(2) 0.8791(2) 0.0198(4) Uani 1 1 d . . . H1 H 0.4616 1.1143 0.8011 0.024 Uiso 1 1 calc R . . C1 C 0.7959(2) 0.9228(2) 0.9846(2) 0.0255(5) Uani 1 1 d . . . H4 H 0.8831 0.9012 0.9807 0.031 Uiso 1 1 calc R . . C2 C 0.6170(2) 0.9396(2) 1.0528(2) 0.0201(4) Uani 1 1 d . . . C8 C 0.7345(2) 1.0491(3) 0.7852(2) 0.0267(5) Uani 1 1 d . . . H5A H 0.8314 1.0594 0.7979 0.032 Uiso 1 1 calc R . . H5B H 0.6938 1.1376 0.7708 0.032 Uiso 1 1 calc R . . C5 C 0.8129(2) 0.8147(2) 1.1905(2) 0.0273(5) Uani 1 1 d . . . H8A H 0.8887 0.7664 1.1740 0.033 Uiso 1 1 calc R . . H8B H 0.7515 0.7492 1.2105 0.033 Uiso 1 1 calc R . . C6 C 0.8632(2) 0.9039(2) 1.3019(2) 0.0280(5) Uani 1 1 d . . . H9A H 0.7879 0.9524 1.3190 0.034 Uiso 1 1 calc R . . H9B H 0.9257 0.9689 1.2830 0.034 Uiso 1 1 calc R . . C7 C 0.9335(3) 0.8242(3) 1.4171(3) 0.0400(7) Uani 1 1 d . . . H10A H 0.8716 0.7597 1.4356 0.060 Uiso 1 1 calc R . . H10B H 0.9645 0.8831 1.4892 0.060 Uiso 1 1 calc R . . H10C H 1.0096 0.7782 1.4009 0.060 Uiso 1 1 calc R . . C9 C 0.6789(3) 0.9653(3) 0.6708(2) 0.0336(6) Uani 1 1 d . . . H6A H 0.5833 0.9495 0.6613 0.040 Uiso 1 1 calc R . . H6B H 0.7246 0.8790 0.6821 0.040 Uiso 1 1 calc R . . C10 C 0.6966(3) 1.0308(3) 0.5534(2) 0.0398(6) Uani 1 1 d . . . H7A H 0.6500 1.1154 0.5413 0.060 Uiso 1 1 calc R . . H7B H 0.6599 0.9741 0.4807 0.060 Uiso 1 1 calc R . . H7C H 0.7914 1.0453 0.5623 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.03073(19) 0.03181(19) 0.0328(2) -0.00758(10) 0.01669(12) -0.00091(9) N1 0.0228(9) 0.0278(10) 0.0179(9) -0.0026(8) 0.0060(7) 0.0016(7) N2 0.0220(9) 0.0314(10) 0.0165(9) -0.0028(8) 0.0101(7) -0.0022(7) C3 0.0222(10) 0.0255(11) 0.0143(10) -0.0037(9) 0.0090(8) -0.0033(8) C4 0.0235(10) 0.0232(10) 0.0134(9) 0.0000(8) 0.0062(7) -0.0011(8) C1 0.0236(10) 0.0344(12) 0.0204(11) -0.0063(10) 0.0089(8) -0.0004(9) C2 0.0207(10) 0.0233(10) 0.0164(10) -0.0025(9) 0.0052(7) 0.0003(8) C8 0.0273(11) 0.0377(13) 0.0191(11) -0.0013(10) 0.0132(8) -0.0064(10) C5 0.0281(12) 0.0284(12) 0.0248(12) 0.0044(10) 0.0062(9) 0.0061(9) C6 0.0329(12) 0.0304(12) 0.0189(11) 0.0039(10) 0.0040(9) 0.0018(10) C7 0.0407(15) 0.0429(15) 0.0296(14) 0.0129(12) -0.0022(11) -0.0013(12) C9 0.0458(14) 0.0355(13) 0.0220(12) -0.0028(11) 0.0133(10) -0.0033(11) C10 0.0528(16) 0.0515(17) 0.0204(12) -0.0029(12) 0.0191(11) -0.0021(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 N1 C1 1.332(3) . ? N1 C2 1.385(3) . ? N1 C5 1.466(3) . ? N2 C1 1.321(3) . ? N2 C3 1.392(3) . ? N2 C8 1.469(3) . ? C3 C4 1.382(3) . ? C3 C2 1.408(3) . ? C4 C2 1.389(3) 3_677 ? C2 C4 1.389(3) 3_677 ? C8 C9 1.506(3) . ? C5 C6 1.506(3) . ? C6 C7 1.522(3) . ? C9 C10 1.513(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C2 108.26(19) . . ? C1 N1 C5 125.6(2) . . ? C2 N1 C5 125.89(19) . . ? C1 N2 C3 108.50(18) . . ? C1 N2 C8 125.58(19) . . ? C3 N2 C8 125.89(19) . . ? C4 C3 N2 130.0(2) . . ? C4 C3 C2 124.0(2) . . ? N2 C3 C2 106.02(19) . . ? C3 C4 C2 112.6(2) . 3_677 ? N2 C1 N1 110.8(2) . . ? N1 C2 C4 130.2(2) . 3_677 ? N1 C2 C3 106.40(19) . . ? C4 C2 C3 123.4(2) 3_677 . ? N2 C8 C9 112.3(2) . . ? N1 C5 C6 112.35(19) . . ? C5 C6 C7 110.3(2) . . ? C8 C9 C10 111.2(2) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 72.09 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.413 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.102 _database_code_depnum_ccdc_archive 'CCDC 947442' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 N4, 2(Br)' _chemical_formula_sum 'C20 H32 Br2 N4' _chemical_formula_weight 488.32 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 5.9373(7) _cell_length_b 21.744(2) _cell_length_c 17.7002(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.467(2) _cell_angle_gamma 90.00 _cell_volume 2278.2(4) _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 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 3.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7167 _exptl_absorpt_correction_T_max 0.9005 _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 = 0.789095 ; _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 22931 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.88 _reflns_number_total 5428 _reflns_number_gt 3870 _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. The terminal methyl groups of the i-Pr substituents show large ADPs (particularly C6 and C7. They do not appear to be disordered and such lage ADPs are not unusual for terminal methyl groups. ; _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^)+(0.0438P)^2^+0.3991P] 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 5428 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0785 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.47717(5) 0.478182(14) 0.211406(16) 0.03735(10) Uani 1 1 d . . . Br2 Br 0.31773(5) 0.205998(14) 0.027102(18) 0.04003(10) Uani 1 1 d . . . C1 C 0.1889(6) 0.62232(14) 0.47799(16) 0.0379(7) Uani 1 1 d . . . H1 H 0.0975 0.6581 0.4715 0.045 Uiso 1 1 calc R . . N1 N 0.2593(4) 0.58913(11) 0.42170(13) 0.0336(6) Uani 1 1 d . . . N2 N 0.2632(4) 0.59891(10) 0.54483(13) 0.0327(5) Uani 1 1 d . . . C2 C 0.3889(5) 0.54050(12) 0.45249(15) 0.0260(6) Uani 1 1 d . . . C3 C 0.3902(5) 0.54678(12) 0.53194(15) 0.0270(6) Uani 1 1 d . . . C4 C 0.5010(5) 0.50623(12) 0.58307(15) 0.0269(6) Uani 1 1 d . . . H4 H 0.5013 0.5102 0.6365 0.032 Uiso 1 1 calc R . . C5 C 0.2049(6) 0.60038(14) 0.33896(16) 0.0443(8) Uani 1 1 d . . . H5 H 0.3141 0.5769 0.3098 0.053 Uiso 1 1 calc R . . C6 C -0.0308(10) 0.5777(2) 0.3167(3) 0.107(2) Uani 1 1 d . . . H6A H -0.0481 0.5358 0.3359 0.161 Uiso 1 1 calc R . . H6B H -0.0569 0.5776 0.2613 0.161 Uiso 1 1 calc R . . H6C H -0.1408 0.6048 0.3383 0.161 Uiso 1 1 calc R . . C7 C 0.2238(8) 0.66747(18) 0.3208(2) 0.0689(12) Uani 1 1 d . . . H7A H 0.0964 0.6897 0.3399 0.103 Uiso 1 1 calc R . . H7B H 0.2216 0.6728 0.2657 0.103 Uiso 1 1 calc R . . H7C H 0.3658 0.6837 0.3448 0.103 Uiso 1 1 calc R . . C8 C 0.2077(6) 0.62146(13) 0.62091(16) 0.0374(7) Uani 1 1 d . . . H8 H 0.3136 0.6016 0.6603 0.045 Uiso 1 1 calc R . . C9 C 0.2414(6) 0.69049(15) 0.6258(2) 0.0494(9) Uani 1 1 d . . . H9A H 0.3935 0.7009 0.6121 0.074 Uiso 1 1 calc R . . H9B H 0.2233 0.7043 0.6777 0.074 Uiso 1 1 calc R . . H9C H 0.1291 0.7110 0.5909 0.074 Uiso 1 1 calc R . . C10 C -0.0304(6) 0.60181(17) 0.6339(2) 0.0540(9) Uani 1 1 d . . . H10A H -0.1375 0.6240 0.5989 0.081 Uiso 1 1 calc R . . H10B H -0.0617 0.6113 0.6862 0.081 Uiso 1 1 calc R . . H10C H -0.0462 0.5575 0.6252 0.081 Uiso 1 1 calc R . . C11 C 0.7826(5) 0.63618(13) 0.97479(16) 0.0307(6) Uani 1 1 d . . . H11 H 0.7210 0.6763 0.9678 0.037 Uiso 1 1 calc R . . N3 N 0.9050(4) 0.60759(10) 0.92563(12) 0.0275(5) Uani 1 1 d . . . N4 N 0.7582(4) 0.60081(10) 1.03511(13) 0.0304(5) Uani 1 1 d . . . C12 C 0.9673(4) 0.55035(12) 0.95551(15) 0.0257(6) Uani 1 1 d . . . C13 C 0.8727(4) 0.54580(12) 1.02592(15) 0.0256(6) Uani 1 1 d . . . C14 C 1.1000(5) 0.50488(12) 0.92691(15) 0.0266(6) Uani 1 1 d . . . H14 H 1.1656 0.5081 0.8798 0.032 Uiso 1 1 calc R . . C15 C 0.9806(5) 0.63352(13) 0.85395(15) 0.0298(6) Uani 1 1 d . . . H15 H 0.9961 0.5987 0.8178 0.036 Uiso 1 1 calc R . . C16 C 0.8070(5) 0.67783(14) 0.81831(17) 0.0387(7) Uani 1 1 d . . . H16A H 0.6629 0.6564 0.8076 0.058 Uiso 1 1 calc R . . H16B H 0.8591 0.6939 0.7710 0.058 Uiso 1 1 calc R . . H16C H 0.7865 0.7120 0.8533 0.058 Uiso 1 1 calc R . . C17 C 1.2112(5) 0.66235(16) 0.87025(19) 0.0463(8) Uani 1 1 d . . . H17A H 1.2004 0.6965 0.9059 0.070 Uiso 1 1 calc R . . H17B H 1.2658 0.6778 0.8230 0.070 Uiso 1 1 calc R . . H17C H 1.3167 0.6315 0.8925 0.070 Uiso 1 1 calc R . . C18 C 0.6367(5) 0.61877(13) 1.10271(16) 0.0328(7) Uani 1 1 d . . . H18 H 0.6470 0.5836 1.1393 0.039 Uiso 1 1 calc R . . C19 C 0.3922(6) 0.6301(2) 1.0799(2) 0.0652(12) Uani 1 1 d . . . H19A H 0.3776 0.6654 1.0455 0.098 Uiso 1 1 calc R . . H19B H 0.3121 0.6387 1.1251 0.098 Uiso 1 1 calc R . . H19C H 0.3267 0.5936 1.0542 0.098 Uiso 1 1 calc R . . C20 C 0.7507(6) 0.67394(15) 1.14147(18) 0.0449(8) Uani 1 1 d . . . H20A H 0.9115 0.6651 1.1531 0.067 Uiso 1 1 calc R . . H20B H 0.6801 0.6827 1.1885 0.067 Uiso 1 1 calc R . . H20C H 0.7342 0.7097 1.1078 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.04758(19) 0.04139(18) 0.02411(14) -0.00146(13) 0.00943(12) -0.00772(14) Br2 0.04709(19) 0.03165(16) 0.04137(18) 0.00052(13) 0.00350(14) -0.00080(14) C1 0.0521(19) 0.0336(16) 0.0281(15) -0.0003(13) 0.0033(14) 0.0163(14) N1 0.0493(15) 0.0279(12) 0.0236(12) 0.0019(10) 0.0024(11) 0.0096(11) N2 0.0444(15) 0.0307(13) 0.0232(12) -0.0011(10) 0.0042(10) 0.0093(11) C2 0.0345(15) 0.0221(13) 0.0214(13) 0.0031(10) 0.0026(11) 0.0006(11) C3 0.0352(15) 0.0245(13) 0.0218(13) -0.0014(11) 0.0048(12) -0.0007(12) C4 0.0351(15) 0.0251(14) 0.0211(13) 0.0013(10) 0.0052(11) -0.0015(12) C5 0.073(2) 0.0388(17) 0.0199(15) -0.0001(13) -0.0029(15) 0.0216(17) C6 0.146(5) 0.101(4) 0.064(3) 0.037(3) -0.060(3) -0.072(4) C7 0.094(3) 0.070(3) 0.039(2) 0.0166(19) -0.015(2) -0.026(2) C8 0.056(2) 0.0358(17) 0.0215(14) -0.0027(12) 0.0066(13) 0.0127(14) C9 0.064(2) 0.0433(19) 0.0427(19) -0.0161(15) 0.0169(17) -0.0066(17) C10 0.071(3) 0.055(2) 0.0386(19) -0.0001(16) 0.0216(18) -0.0138(19) C11 0.0351(16) 0.0267(14) 0.0314(15) 0.0026(12) 0.0096(12) 0.0025(12) N3 0.0329(13) 0.0267(12) 0.0243(12) 0.0035(9) 0.0099(10) 0.0019(10) N4 0.0381(14) 0.0274(12) 0.0272(13) 0.0029(10) 0.0132(10) 0.0054(11) C12 0.0301(15) 0.0252(13) 0.0224(13) 0.0027(11) 0.0059(11) -0.0018(11) C13 0.0288(14) 0.0250(13) 0.0238(13) -0.0025(11) 0.0062(11) -0.0011(11) C14 0.0290(15) 0.0298(14) 0.0219(13) 0.0008(11) 0.0080(11) -0.0022(12) C15 0.0379(16) 0.0304(14) 0.0223(14) 0.0056(11) 0.0101(12) 0.0013(12) C16 0.0487(19) 0.0399(17) 0.0285(15) 0.0100(13) 0.0102(14) 0.0040(15) C17 0.0426(18) 0.053(2) 0.0442(19) 0.0173(16) 0.0075(15) -0.0033(16) C18 0.0393(17) 0.0349(16) 0.0262(14) 0.0009(12) 0.0151(12) 0.0054(13) C19 0.037(2) 0.113(3) 0.047(2) -0.030(2) 0.0141(17) -0.003(2) C20 0.053(2) 0.053(2) 0.0294(16) -0.0038(15) 0.0066(15) -0.0020(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.324(4) . ? C1 N2 1.331(4) . ? N1 C2 1.394(3) . ? N1 C5 1.495(4) . ? N2 C3 1.390(3) . ? N2 C8 1.494(3) . ? C2 C4 1.385(4) 3_666 ? C2 C3 1.412(4) . ? C3 C4 1.392(4) . ? C4 C2 1.385(4) 3_666 ? C5 C7 1.500(5) . ? C5 C6 1.507(6) . ? C8 C10 1.512(5) . ? C8 C9 1.516(4) . ? C11 N3 1.331(3) . ? C11 N4 1.333(3) . ? N3 C12 1.391(3) . ? N3 C15 1.489(3) . ? N4 C13 1.392(3) . ? N4 C18 1.496(3) . ? C12 C14 1.385(4) . ? C12 C13 1.410(4) . ? C13 C14 1.384(4) 3_767 ? C14 C13 1.384(4) 3_767 ? C15 C16 1.512(4) . ? C15 C17 1.513(4) . ? C18 C19 1.497(5) . ? C18 C20 1.515(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 111.0(3) . . ? C1 N1 C2 108.4(2) . . ? C1 N1 C5 126.2(2) . . ? C2 N1 C5 125.3(2) . . ? C1 N2 C3 108.2(2) . . ? C1 N2 C8 126.5(2) . . ? C3 N2 C8 125.2(2) . . ? C4 C2 N1 130.1(2) 3_666 . ? C4 C2 C3 123.9(2) 3_666 . ? N1 C2 C3 106.0(2) . . ? N2 C3 C4 130.2(2) . . ? N2 C3 C2 106.3(2) . . ? C4 C3 C2 123.5(2) . . ? C2 C4 C3 112.7(2) 3_666 . ? N1 C5 C7 110.8(3) . . ? N1 C5 C6 109.2(3) . . ? C7 C5 C6 110.2(3) . . ? N2 C8 C10 108.6(3) . . ? N2 C8 C9 109.9(2) . . ? C10 C8 C9 113.1(3) . . ? N3 C11 N4 110.7(2) . . ? C11 N3 C12 108.2(2) . . ? C11 N3 C15 126.6(2) . . ? C12 N3 C15 125.0(2) . . ? C11 N4 C13 108.5(2) . . ? C11 N4 C18 125.4(2) . . ? C13 N4 C18 126.0(2) . . ? C14 C12 N3 129.9(2) . . ? C14 C12 C13 123.4(2) . . ? N3 C12 C13 106.7(2) . . ? C14 C13 N4 130.4(2) 3_767 . ? C14 C13 C12 123.6(2) 3_767 . ? N4 C13 C12 106.0(2) . . ? C13 C14 C12 113.0(2) 3_767 . ? N3 C15 C16 110.8(2) . . ? N3 C15 C17 108.8(2) . . ? C16 C15 C17 113.1(2) . . ? N4 C18 C19 110.2(3) . . ? N4 C18 C20 110.1(2) . . ? C19 C18 C20 112.4(3) . . ? 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 N2 C1 N1 C2 0.0(4) . . . . ? N2 C1 N1 C5 178.4(3) . . . . ? N1 C1 N2 C3 -0.3(4) . . . . ? N1 C1 N2 C8 -176.2(3) . . . . ? C1 N1 C2 C4 -179.8(3) . . . 3_666 ? C5 N1 C2 C4 1.7(5) . . . 3_666 ? C1 N1 C2 C3 0.3(3) . . . . ? C5 N1 C2 C3 -178.1(3) . . . . ? C1 N2 C3 C4 -179.4(3) . . . . ? C8 N2 C3 C4 -3.4(5) . . . . ? C1 N2 C3 C2 0.4(3) . . . . ? C8 N2 C3 C2 176.4(3) . . . . ? C4 C2 C3 N2 179.7(3) 3_666 . . . ? N1 C2 C3 N2 -0.4(3) . . . . ? C4 C2 C3 C4 -0.5(5) 3_666 . . . ? N1 C2 C3 C4 179.4(3) . . . . ? N2 C3 C4 C2 -179.8(3) . . . 3_666 ? C2 C3 C4 C2 0.5(4) . . . 3_666 ? C1 N1 C5 C7 43.7(5) . . . . ? C2 N1 C5 C7 -138.2(3) . . . . ? C1 N1 C5 C6 -77.9(4) . . . . ? C2 N1 C5 C6 100.3(4) . . . . ? C1 N2 C8 C10 75.1(4) . . . . ? C3 N2 C8 C10 -100.1(3) . . . . ? C1 N2 C8 C9 -49.0(4) . . . . ? C3 N2 C8 C9 135.7(3) . . . . ? N4 C11 N3 C12 -0.7(3) . . . . ? N4 C11 N3 C15 -175.9(3) . . . . ? N3 C11 N4 C13 0.6(3) . . . . ? N3 C11 N4 C18 178.0(3) . . . . ? C11 N3 C12 C14 -177.8(3) . . . . ? C15 N3 C12 C14 -2.4(5) . . . . ? C11 N3 C12 C13 0.5(3) . . . . ? C15 N3 C12 C13 175.8(2) . . . . ? C11 N4 C13 C14 178.9(3) . . . 3_767 ? C18 N4 C13 C14 1.5(5) . . . 3_767 ? C11 N4 C13 C12 -0.3(3) . . . . ? C18 N4 C13 C12 -177.7(3) . . . . ? C14 C12 C13 C14 -1.0(5) . . . 3_767 ? N3 C12 C13 C14 -179.4(3) . . . 3_767 ? C14 C12 C13 N4 178.3(3) . . . . ? N3 C12 C13 N4 -0.2(3) . . . . ? N3 C12 C14 C13 178.9(3) . . . 3_767 ? C13 C12 C14 C13 0.9(4) . . . 3_767 ? C11 N3 C15 C16 -33.4(4) . . . . ? C12 N3 C15 C16 152.2(3) . . . . ? C11 N3 C15 C17 91.6(3) . . . . ? C12 N3 C15 C17 -82.8(3) . . . . ? C11 N4 C18 C19 63.0(4) . . . . ? C13 N4 C18 C19 -120.0(3) . . . . ? C11 N4 C18 C20 -61.5(4) . . . . ? C13 N4 C18 C20 115.5(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.553 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 947443' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H40 N4, 2(Br)' _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 0.0181 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)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0896(5) _cell_length_b 14.1543(7) _cell_length_c 17.3476(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.306(3) _cell_angle_gamma 90.00 _cell_volume 2670.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(1) _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 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 3.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4030 _exptl_absorpt_correction_T_max 0.9249 _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 = 0.581303 ; _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 15352 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 69.99 _reflns_number_total 4924 _reflns_number_gt 3657 _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 , 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. One of the t-Bu methyl groups (atoms C7) shows large anisotropic movement. This atom is possibly disordered but was refined as one atom. The hydrogen atoms associatd with atom C7 were placed on calculated positions with U(eq)H= 1.3 U(eq)C and these hydrogen atoms consequently also feature a large U(eq). Large motion of terminal methyl groups are not unusual. ; _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^)+(0.0970P)^2^+2.7962P] 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 4924 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1847 _refine_ls_wR_factor_gt 0.1672 _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 Br1 Br 0.44492(5) 0.23132(4) 0.17591(3) 0.0522(2) Uani 1 1 d . . . C1 C 0.1553(4) 0.3626(3) 0.1338(3) 0.0342(10) Uani 1 1 d . . . H1 H 0.2006 0.3221 0.1726 0.041 Uiso 1 1 calc R . . N1 N 0.1056(3) 0.4444(3) 0.1484(2) 0.0329(8) Uani 1 1 d . . . N2 N 0.1323(4) 0.3454(3) 0.0567(2) 0.0346(8) Uani 1 1 d . . . C2 C 0.0463(4) 0.4833(3) 0.0766(2) 0.0313(9) Uani 1 1 d . . . C3 C 0.0628(4) 0.4190(3) 0.0183(3) 0.0319(9) Uani 1 1 d . . . C4 C 0.0182(4) 0.4328(3) -0.0613(3) 0.0324(10) Uani 1 1 d . . . H4 H 0.0304 0.3896 -0.1009 0.039 Uiso 1 1 calc R . . C5 C 0.1192(4) 0.4890(3) 0.2261(2) 0.0346(10) Uani 1 1 d . . . H5A H 0.1180 0.4393 0.2661 0.042 Uiso 1 1 calc R . . H5B H 0.0483 0.5313 0.2264 0.042 Uiso 1 1 calc R . . C6 C 0.2374(6) 0.5456(5) 0.2482(3) 0.0646(18) Uani 1 1 d . . . H6 H 0.2990 0.4936 0.2616 0.077 Uiso 1 1 calc R . . C7 C 0.2829(13) 0.5907(13) 0.1970(6) 0.260(12) Uani 1 1 d . . . H7A H 0.2867 0.6582 0.2099 0.390 Uiso 1 1 calc R . . H7B H 0.2309 0.5814 0.1449 0.390 Uiso 1 1 calc R . . H7C H 0.3659 0.5672 0.1967 0.390 Uiso 1 1 calc R . . C8 C 0.2422(6) 0.5892(5) 0.3283(3) 0.072(2) Uani 1 1 d . . . H8A H 0.3177 0.6265 0.3430 0.107 Uiso 1 1 calc R . . H8B H 0.2414 0.5391 0.3672 0.107 Uiso 1 1 calc R . . H8C H 0.1706 0.6303 0.3267 0.107 Uiso 1 1 calc R . . C9 C 0.1693(5) 0.2589(3) 0.0197(3) 0.0408(11) Uani 1 1 d . . . H9A H 0.2405 0.2300 0.0552 0.049 Uiso 1 1 calc R . . H9B H 0.1954 0.2759 -0.0299 0.049 Uiso 1 1 calc R . . C10 C 0.0630(8) 0.1857(4) 0.0019(5) 0.083(2) Uani 1 1 d . . . H10 H 0.0013 0.2117 -0.0429 0.099 Uiso 1 1 calc R . . C11 C 0.1212(9) 0.0982(5) -0.0299(6) 0.105(3) Uani 1 1 d . . . H11A H 0.1901 0.0755 0.0100 0.157 Uiso 1 1 calc R . . H11B H 0.1510 0.1156 -0.0776 0.157 Uiso 1 1 calc R . . H11C H 0.0593 0.0482 -0.0423 0.157 Uiso 1 1 calc R . . C12 C 0.0010(8) 0.1661(5) 0.0606(6) 0.112(4) Uani 1 1 d . . . H12A H -0.0600 0.1166 0.0431 0.169 Uiso 1 1 calc R . . H12B H -0.0408 0.2233 0.0735 0.169 Uiso 1 1 calc R . . H12C H 0.0591 0.1445 0.1072 0.169 Uiso 1 1 calc R . . Br2 Br 0.89070(5) 0.72558(4) 0.20660(3) 0.0465(2) Uani 1 1 d . . . C21 C 0.6089(4) 0.6256(4) 0.1547(3) 0.0401(11) Uani 1 1 d . . . H21 H 0.6403 0.6624 0.2000 0.048 Uiso 1 1 calc R . . N21 N 0.5711(4) 0.6611(3) 0.0829(2) 0.0403(9) Uani 1 1 d . . . N22 N 0.5972(4) 0.5320(3) 0.1550(2) 0.0400(9) Uani 1 1 d . . . C22 C 0.5312(5) 0.5857(3) 0.0323(3) 0.0377(10) Uani 1 1 d . . . C23 C 0.5476(5) 0.5032(3) 0.0782(3) 0.0392(11) Uani 1 1 d . . . C24 C 0.5152(4) 0.4141(3) 0.0484(3) 0.0381(11) Uani 1 1 d . . . H24 H 0.5238 0.3585 0.0796 0.046 Uiso 1 1 calc R . . C25 C 0.5636(5) 0.7617(3) 0.0639(3) 0.0453(12) Uani 1 1 d . . . H25A H 0.5653 0.7700 0.0075 0.054 Uiso 1 1 calc R . . H25B H 0.6364 0.7942 0.0947 0.054 Uiso 1 1 calc R . . C26 C 0.4467(5) 0.8077(4) 0.0815(4) 0.0536(14) Uani 1 1 d . . . H26 H 0.4456 0.7993 0.1386 0.064 Uiso 1 1 calc R . . C27 C 0.3310(6) 0.7645(5) 0.0336(4) 0.0677(18) Uani 1 1 d . . . H27A H 0.3332 0.7694 -0.0225 0.101 Uiso 1 1 calc R . . H27B H 0.2590 0.7983 0.0444 0.101 Uiso 1 1 calc R . . H27C H 0.3260 0.6978 0.0479 0.101 Uiso 1 1 calc R . . C28 C 0.4527(7) 0.9124(5) 0.0642(5) 0.081(2) Uani 1 1 d . . . H28A H 0.5248 0.9401 0.0984 0.122 Uiso 1 1 calc R . . H28B H 0.3780 0.9434 0.0738 0.122 Uiso 1 1 calc R . . H28C H 0.4591 0.9213 0.0091 0.122 Uiso 1 1 calc R . . C29 C 0.6364(5) 0.4718(4) 0.2239(3) 0.0478(13) Uani 1 1 d . . . H29A H 0.5845 0.4144 0.2186 0.057 Uiso 1 1 calc R . . H29B H 0.6238 0.5061 0.2715 0.057 Uiso 1 1 calc R . . C30 C 0.7708(5) 0.4430(5) 0.2343(3) 0.0544(15) Uani 1 1 d . . . H30 H 0.8214 0.5017 0.2360 0.065 Uiso 1 1 calc R . . C31 C 0.8093(7) 0.3918(6) 0.3128(4) 0.080(2) Uani 1 1 d . . . H31A H 0.8003 0.4346 0.3558 0.120 Uiso 1 1 calc R . . H31B H 0.8953 0.3719 0.3192 0.120 Uiso 1 1 calc R . . H31C H 0.7569 0.3362 0.3138 0.120 Uiso 1 1 calc R . . C32 C 0.7971(5) 0.3808(4) 0.1674(4) 0.0593(15) Uani 1 1 d . . . H32A H 0.7411 0.3265 0.1605 0.089 Uiso 1 1 calc R . . H32B H 0.8823 0.3584 0.1801 0.089 Uiso 1 1 calc R . . H32C H 0.7847 0.4176 0.1186 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0440(3) 0.0632(4) 0.0490(4) 0.0225(3) 0.0083(3) 0.0054(2) C1 0.037(2) 0.027(2) 0.036(2) 0.0077(19) 0.002(2) 0.0029(18) N1 0.038(2) 0.0296(19) 0.0285(19) 0.0018(16) 0.0007(16) 0.0005(15) N2 0.043(2) 0.0267(18) 0.035(2) 0.0019(16) 0.0077(17) 0.0042(16) C2 0.036(2) 0.030(2) 0.027(2) 0.0006(18) 0.0037(18) -0.0003(18) C3 0.036(2) 0.029(2) 0.031(2) 0.0001(18) 0.0051(19) -0.0009(17) C4 0.044(2) 0.025(2) 0.028(2) -0.0031(18) 0.0077(19) 0.0009(18) C5 0.040(2) 0.037(2) 0.026(2) 0.0030(19) 0.0040(19) -0.0009(19) C6 0.067(4) 0.086(5) 0.043(3) -0.023(3) 0.016(3) -0.040(4) C7 0.258(16) 0.44(3) 0.116(8) -0.159(13) 0.118(10) -0.285(18) C8 0.080(4) 0.086(5) 0.048(3) -0.021(3) 0.012(3) -0.035(4) C9 0.050(3) 0.031(2) 0.041(3) 0.001(2) 0.011(2) 0.012(2) C10 0.123(6) 0.037(3) 0.105(6) -0.014(4) 0.063(5) -0.010(4) C11 0.153(8) 0.035(3) 0.151(8) -0.023(4) 0.089(7) -0.010(4) C12 0.103(6) 0.061(5) 0.197(10) -0.051(6) 0.086(7) -0.031(4) Br2 0.0513(4) 0.0450(4) 0.0440(3) -0.0137(2) 0.0110(3) -0.0018(2) C21 0.044(3) 0.042(3) 0.033(2) -0.008(2) 0.004(2) -0.004(2) N21 0.048(2) 0.033(2) 0.039(2) -0.0029(18) 0.0063(18) -0.0018(17) N22 0.048(2) 0.041(2) 0.0287(19) -0.0010(17) 0.0034(17) -0.0009(18) C22 0.050(3) 0.032(2) 0.032(2) -0.0033(19) 0.009(2) 0.002(2) C23 0.050(3) 0.038(3) 0.029(2) -0.002(2) 0.006(2) 0.000(2) C24 0.049(3) 0.033(2) 0.031(2) 0.0037(19) 0.004(2) -0.002(2) C25 0.050(3) 0.032(2) 0.053(3) -0.004(2) 0.007(3) -0.004(2) C26 0.062(3) 0.046(3) 0.055(3) 0.001(3) 0.016(3) 0.006(3) C27 0.056(4) 0.077(5) 0.070(4) -0.015(4) 0.013(3) 0.007(3) C28 0.101(6) 0.052(4) 0.091(5) 0.011(4) 0.019(4) 0.015(4) C29 0.065(3) 0.046(3) 0.030(2) 0.002(2) 0.004(2) -0.003(3) C30 0.054(3) 0.055(4) 0.046(3) 0.006(3) -0.010(3) 0.001(3) C31 0.081(5) 0.099(6) 0.053(4) 0.020(4) -0.002(3) 0.021(4) C32 0.051(3) 0.059(4) 0.066(4) -0.003(3) 0.008(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.328(6) . ? C1 N2 1.334(6) . ? N1 C2 1.401(5) . ? N1 C5 1.469(5) . ? N2 C3 1.386(6) . ? N2 C9 1.476(6) . ? C2 C4 1.385(6) 3_565 ? C2 C3 1.399(6) . ? C3 C4 1.387(6) . ? C4 C2 1.385(6) 3_565 ? C5 C6 1.520(7) . ? C6 C7 1.275(12) . ? C6 C8 1.513(8) . ? C9 C10 1.554(9) . ? C10 C12 1.364(10) . ? C10 C11 1.547(9) . ? C21 N22 1.331(6) . ? C21 N21 1.333(6) . ? N21 C22 1.397(6) . ? N21 C25 1.460(6) . ? N22 C23 1.399(6) . ? N22 C29 1.463(6) . ? C22 C24 1.394(6) 3_665 ? C22 C23 1.405(7) . ? C23 C24 1.383(7) . ? C24 C22 1.394(6) 3_665 ? C25 C26 1.533(8) . ? C26 C27 1.514(9) . ? C26 C28 1.517(9) . ? C29 C30 1.522(8) . ? C30 C31 1.528(8) . ? C30 C32 1.530(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 110.2(4) . . ? C1 N1 C2 108.2(4) . . ? C1 N1 C5 125.3(4) . . ? C2 N1 C5 126.4(4) . . ? C1 N2 C3 108.8(4) . . ? C1 N2 C9 124.9(4) . . ? C3 N2 C9 126.2(4) . . ? C4 C2 C3 123.7(4) 3_565 . ? C4 C2 N1 129.9(4) 3_565 . ? C3 C2 N1 106.4(4) . . ? N2 C3 C4 129.9(4) . . ? N2 C3 C2 106.3(4) . . ? C4 C3 C2 123.8(4) . . ? C2 C4 C3 112.5(4) 3_565 . ? N1 C5 C6 112.7(4) . . ? C7 C6 C8 119.2(7) . . ? C7 C6 C5 121.9(7) . . ? C8 C6 C5 108.6(5) . . ? N2 C9 C10 112.0(4) . . ? C12 C10 C11 114.2(6) . . ? C12 C10 C9 117.5(7) . . ? C11 C10 C9 104.6(6) . . ? N22 C21 N21 111.4(4) . . ? C21 N21 C22 107.6(4) . . ? C21 N21 C25 124.8(4) . . ? C22 N21 C25 127.4(4) . . ? C21 N22 C23 107.9(4) . . ? C21 N22 C29 124.7(4) . . ? C23 N22 C29 127.3(4) . . ? C24 C22 N21 129.6(4) 3_665 . ? C24 C22 C23 123.5(4) 3_665 . ? N21 C22 C23 106.8(4) . . ? C24 C23 N22 130.4(4) . . ? C24 C23 C22 123.3(4) . . ? N22 C23 C22 106.2(4) . . ? C23 C24 C22 113.1(4) . 3_665 ? N21 C25 C26 112.5(4) . . ? C27 C26 C28 110.5(6) . . ? C27 C26 C25 112.2(5) . . ? C28 C26 C25 107.7(5) . . ? N22 C29 C30 112.3(4) . . ? C29 C30 C31 109.2(5) . . ? C29 C30 C32 113.1(4) . . ? C31 C30 C32 110.0(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.241 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.118 _database_code_depnum_ccdc_archive 'CCDC 947444' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H85 Br4 Cl6 N4 O0.50 P4 Pt2' _chemical_formula_weight 2096.87 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' 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' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 9.8875(5) _cell_length_b 39.2195(19) _cell_length_c 21.2620(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.0060(10) _cell_angle_gamma 90.00 _cell_volume 8143.4(7) _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 stick' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4100 _exptl_absorpt_coefficient_mu 5.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3945 _exptl_absorpt_correction_T_max 0.6905 _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 = 0.668580 ; _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 100747 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 58 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 31.97 _reflns_number_total 26445 _reflns_number_gt 19899 _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. Hydrogen atom positions attached to the disordered H2O molecule were not calculated. One of the terminal methyl groups (C20) and possibly the methylene group it is bonded too are disordered. Only the disorder of the methyl group has been considered. Bond angles involving the disordered Atom C20A have been delete. Large ADPs have been observed for terminal carbon atoms of n-butyl substituents and particularly if this atom is disordered as in the present case (C20/C20A). The largest residual density peak is found in the vicinity of a platinum atom. ; _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^)+(0.0906P)^2^+67.6732P] 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 26445 _refine_ls_number_parameters 872 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1707 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.34038(2) 0.765273(6) 0.135490(12) 0.02302(7) Uani 1 1 d . . . Pt2 Pt 0.30969(2) 0.500502(6) 0.226524(12) 0.02196(6) Uani 1 1 d . . . Br1 Br 0.58352(12) 0.75279(3) 0.16180(7) 0.0693(3) Uani 1 1 d . . . Br2 Br 0.54842(12) 0.51685(3) 0.24903(7) 0.0721(3) Uani 1 1 d . . . P1 P 0.11739(17) 0.77731(4) 0.11757(8) 0.0250(3) Uani 1 1 d . . . P2 P 0.37178(18) 0.82011(4) 0.10294(9) 0.0275(3) Uani 1 1 d . . . P3 P 0.08867(16) 0.48639(4) 0.21309(8) 0.0222(3) Uani 1 1 d . . . P4 P 0.35126(17) 0.44305(4) 0.23472(8) 0.0239(3) Uani 1 1 d . . . N1 N 0.2792(6) 0.69028(13) 0.1102(3) 0.0258(11) Uani 1 1 d . . . N2 N 0.3057(6) 0.70081(13) 0.2123(3) 0.0238(10) Uani 1 1 d . . . N4 N 0.2554(6) 0.56595(14) 0.1521(3) 0.0239(10) Uani 1 1 d . . . N3 N 0.2799(6) 0.57615(13) 0.2538(3) 0.0222(10) Uani 1 1 d . . . C1 C 0.3051(7) 0.71559(17) 0.1548(3) 0.0257(12) Uani 1 1 d . . . C2 C 0.2671(7) 0.65913(15) 0.1391(3) 0.0236(12) Uani 1 1 d . . . C3 C 0.2843(7) 0.66575(16) 0.2050(3) 0.0247(12) Uani 1 1 d . . . C4 C 0.2860(7) 0.64022(16) 0.2506(3) 0.0240(12) Uani 1 1 d . . . H4 H 0.2960 0.6445 0.2951 0.029 Uiso 1 1 calc R . . C5 C 0.2716(7) 0.60783(16) 0.2244(3) 0.0229(11) Uani 1 1 d . . . C6 C 0.2549(7) 0.60135(16) 0.1586(3) 0.0235(12) Uani 1 1 d . . . C7 C 0.2490(7) 0.62708(17) 0.1128(3) 0.0272(13) Uani 1 1 d . . . H7 H 0.2341 0.6229 0.0682 0.033 Uiso 1 1 calc R . . C9 C 0.2879(10) 0.6950(2) 0.0427(3) 0.0404(19) Uani 1 1 d . . . H9A H 0.2625 0.7187 0.0299 0.049 Uiso 1 1 calc R . . H9B H 0.2225 0.6794 0.0168 0.049 Uiso 1 1 calc R . . C10 C 0.4349(13) 0.6875(3) 0.0299(5) 0.058(3) Uani 1 1 d . . . H10A H 0.5012 0.7009 0.0599 0.069 Uiso 1 1 calc R . . H10B H 0.4557 0.6630 0.0376 0.069 Uiso 1 1 calc R . . C11 C 0.4503(19) 0.6963(5) -0.0373(7) 0.103(6) Uani 1 1 d . . . H11A H 0.3935 0.6810 -0.0668 0.155 Uiso 1 1 calc R . . H11B H 0.5464 0.6939 -0.0427 0.155 Uiso 1 1 calc R . . H11C H 0.4210 0.7200 -0.0462 0.155 Uiso 1 1 calc R . . C12 C 0.3303(8) 0.71810(18) 0.2736(3) 0.0286(13) Uani 1 1 d . . . H12A H 0.3698 0.7409 0.2679 0.034 Uiso 1 1 calc R . . H12B H 0.3987 0.7050 0.3030 0.034 Uiso 1 1 calc R . . C13 C 0.2021(9) 0.72234(18) 0.3037(3) 0.0332(15) Uani 1 1 d . . . H13A H 0.1610 0.6997 0.3093 0.040 Uiso 1 1 calc R . . H13B H 0.1341 0.7362 0.2756 0.040 Uiso 1 1 calc R . . C14 C 0.2387(11) 0.7400(3) 0.3688(4) 0.049(2) Uani 1 1 d . . . H14A H 0.2410 0.7230 0.4028 0.073 Uiso 1 1 calc R . . H14B H 0.1698 0.7574 0.3734 0.073 Uiso 1 1 calc R . . H14C H 0.3289 0.7508 0.3716 0.073 Uiso 1 1 calc R . . C8 C 0.2726(6) 0.55085(16) 0.2102(3) 0.0226(11) Uani 1 1 d . . . C18 C 0.2551(10) 0.54835(19) 0.0914(4) 0.0401(19) Uani 1 1 d . B . H18A H 0.1951 0.5605 0.0569 0.048 Uiso 1 1 calc R . . H18B H 0.2206 0.5248 0.0939 0.048 Uiso 1 1 calc R . . C19 C 0.4135(19) 0.5479(4) 0.0770(6) 0.118(7) Uani 1 1 d D . . H19A H 0.4388 0.5709 0.0638 0.142 Uiso 0.60 1 calc PR A 1 H19B H 0.4761 0.5417 0.1163 0.142 Uiso 0.60 1 calc PR A 1 H19C H 0.3933 0.5468 0.0299 0.142 Uiso 0.40 1 calc PR A 2 H19D H 0.4357 0.5722 0.0859 0.142 Uiso 0.40 1 calc PR A 2 C20 C 0.430(2) 0.5224(4) 0.0248(8) 0.063(5) Uani 0.60 1 d PD B 1 H20A H 0.3866 0.5315 -0.0164 0.095 Uiso 0.60 1 calc P C 1 H20B H 0.3860 0.5009 0.0333 0.095 Uiso 0.60 1 calc P D 1 H20C H 0.5274 0.5185 0.0240 0.095 Uiso 0.60 1 calc P E 1 C20A C 0.559(5) 0.534(3) 0.085(6) 0.29(5) Uiso 0.40 1 d PD B 2 H20D H 0.6235 0.5527 0.0984 0.430 Uiso 0.40 1 calc P F 2 H20E H 0.5769 0.5244 0.0452 0.430 Uiso 0.40 1 calc P G 2 H20F H 0.5697 0.5164 0.1184 0.430 Uiso 0.40 1 calc P H 2 C15 C 0.2980(7) 0.57114(17) 0.3234(3) 0.0260(13) Uani 1 1 d . . . H15A H 0.3698 0.5869 0.3439 0.031 Uiso 1 1 calc R . . H15B H 0.3299 0.5475 0.3334 0.031 Uiso 1 1 calc R . . C16 C 0.1673(8) 0.57727(19) 0.3509(3) 0.0307(14) Uani 1 1 d . . . H16A H 0.0978 0.5600 0.3341 0.037 Uiso 1 1 calc R . . H16B H 0.1302 0.6001 0.3381 0.037 Uiso 1 1 calc R . . C17 C 0.1973(11) 0.5749(3) 0.4236(4) 0.048(2) Uani 1 1 d . . . H17A H 0.2390 0.5528 0.4361 0.072 Uiso 1 1 calc R . . H17B H 0.1117 0.5773 0.4410 0.072 Uiso 1 1 calc R . . H17C H 0.2606 0.5932 0.4403 0.072 Uiso 1 1 calc R . . C21 C 0.0034(8) 0.7429(2) 0.0890(4) 0.0355(16) Uani 1 1 d . . . C22 C -0.0395(16) 0.7386(3) 0.0250(5) 0.083(5) Uani 1 1 d . . . H22 H -0.0180 0.7550 -0.0048 0.100 Uiso 1 1 calc R . . C23 C -0.117(2) 0.7090(5) 0.0043(7) 0.144(10) Uani 1 1 d . . . H23 H -0.1491 0.7056 -0.0398 0.173 Uiso 1 1 calc R . . C24 C -0.145(2) 0.6856(4) 0.0470(8) 0.125(8) Uani 1 1 d . . . H24 H -0.1966 0.6659 0.0325 0.150 Uiso 1 1 calc R . . C25 C -0.1007(11) 0.6895(3) 0.1099(6) 0.061(3) Uani 1 1 d . . . H25 H -0.1200 0.6725 0.1391 0.073 Uiso 1 1 calc R . . C26 C -0.0281(8) 0.7180(2) 0.1317(4) 0.0397(18) Uani 1 1 d . . . H26 H 0.0012 0.7209 0.1761 0.048 Uiso 1 1 calc R . . C27 C 0.0578(7) 0.79260(17) 0.1882(3) 0.0291(14) Uani 1 1 d . . . C28 C 0.1495(9) 0.80615(18) 0.2384(4) 0.0349(16) Uani 1 1 d . . . H28 H 0.2448 0.8065 0.2363 0.042 Uiso 1 1 calc R . . C29 C 0.1020(11) 0.8192(2) 0.2918(4) 0.045(2) Uani 1 1 d . . . H29 H 0.1647 0.8288 0.3256 0.054 Uiso 1 1 calc R . . C30 C -0.0346(11) 0.8183(2) 0.2958(5) 0.052(2) Uani 1 1 d . . . H30 H -0.0661 0.8267 0.3328 0.062 Uiso 1 1 calc R . . C31 C -0.1269(10) 0.8051(2) 0.2465(5) 0.050(2) Uani 1 1 d . . . H31 H -0.2219 0.8050 0.2491 0.060 Uiso 1 1 calc R . . C32 C -0.0806(8) 0.7919(2) 0.1926(4) 0.0364(16) Uani 1 1 d . . . H32 H -0.1441 0.7825 0.1590 0.044 Uiso 1 1 calc R . . C33 C 0.0933(7) 0.81277(18) 0.0613(4) 0.0305(14) Uani 1 1 d . . . H33A H 0.1037 0.8047 0.0182 0.037 Uiso 1 1 calc R . . H33B H 0.0003 0.8225 0.0595 0.037 Uiso 1 1 calc R . . C34 C 0.2003(7) 0.83974(18) 0.0835(4) 0.0333(15) Uani 1 1 d . . . H34A H 0.1767 0.8514 0.1217 0.040 Uiso 1 1 calc R . . H34B H 0.2012 0.8570 0.0497 0.040 Uiso 1 1 calc R . . C35 C 0.4543(7) 0.82381(18) 0.0328(4) 0.0319(15) Uani 1 1 d . . . C36 C 0.5961(9) 0.8172(3) 0.0401(4) 0.0446(19) Uani 1 1 d . . . H36 H 0.6428 0.8086 0.0793 0.054 Uiso 1 1 calc R . . C37 C 0.6667(9) 0.8233(2) -0.0098(5) 0.045(2) Uani 1 1 d . . . H37 H 0.7624 0.8190 -0.0046 0.054 Uiso 1 1 calc R . . C38 C 0.6004(11) 0.8355(2) -0.0666(5) 0.049(2) Uani 1 1 d . . . H38 H 0.6504 0.8397 -0.1005 0.059 Uiso 1 1 calc R . . C39 C 0.4612(10) 0.8417(2) -0.0749(4) 0.047(2) Uani 1 1 d . . . H39 H 0.4158 0.8500 -0.1146 0.056 Uiso 1 1 calc R . . C40 C 0.3868(9) 0.8357(2) -0.0252(4) 0.0384(17) Uani 1 1 d . . . H40 H 0.2909 0.8397 -0.0311 0.046 Uiso 1 1 calc R . . C41 C 0.4731(8) 0.8489(2) 0.1574(5) 0.045(2) Uani 1 1 d . . . C42 C 0.5100(11) 0.8808(2) 0.1340(7) 0.068(4) Uani 1 1 d . . . H42 H 0.4774 0.8868 0.0910 0.081 Uiso 1 1 calc R . . C43 C 0.5900(14) 0.9029(4) 0.1712(11) 0.099(6) Uani 1 1 d . . . H43 H 0.6117 0.9244 0.1549 0.118 Uiso 1 1 calc R . . C44 C 0.6377(12) 0.8946(4) 0.2299(11) 0.109(8) Uani 1 1 d . . . H44 H 0.6996 0.9099 0.2543 0.131 Uiso 1 1 calc R . . C45 C 0.6009(13) 0.8626(5) 0.2610(8) 0.106(7) Uani 1 1 d . . . H45 H 0.6318 0.8577 0.3047 0.127 Uiso 1 1 calc R . . C46 C 0.5152(10) 0.8397(3) 0.2198(6) 0.068(4) Uani 1 1 d . . . H46 H 0.4880 0.8185 0.2354 0.082 Uiso 1 1 calc R . . C47 C -0.0239(7) 0.51070(19) 0.1552(3) 0.0278(13) Uani 1 1 d . . . C48 C -0.0553(8) 0.5440(2) 0.1700(4) 0.0360(16) Uani 1 1 d . . . H48 H -0.0301 0.5523 0.2122 0.043 Uiso 1 1 calc R . . C49 C -0.1239(10) 0.5651(2) 0.1228(5) 0.050(2) Uani 1 1 d . . . H49 H -0.1472 0.5877 0.1331 0.060 Uiso 1 1 calc R . . C50 C -0.1582(12) 0.5533(3) 0.0610(5) 0.057(3) Uani 1 1 d . . . H50 H -0.1994 0.5682 0.0283 0.068 Uiso 1 1 calc R . . C51 C -0.1324(11) 0.5198(3) 0.0469(4) 0.052(2) Uani 1 1 d . . . H51 H -0.1620 0.5113 0.0052 0.062 Uiso 1 1 calc R . . C52 C -0.0630(9) 0.4981(2) 0.0936(4) 0.0380(17) Uani 1 1 d . . . H52 H -0.0429 0.4752 0.0835 0.046 Uiso 1 1 calc R . . C53 C 0.0228(7) 0.48889(18) 0.2880(3) 0.0274(13) Uani 1 1 d . . . C54 C -0.1159(8) 0.4926(2) 0.2906(4) 0.0327(15) Uani 1 1 d . . . H54 H -0.1795 0.4952 0.2525 0.039 Uiso 1 1 calc R . . C55 C -0.1608(9) 0.4925(3) 0.3490(4) 0.046(2) Uani 1 1 d . . . H55 H -0.2558 0.4949 0.3507 0.055 Uiso 1 1 calc R . . C56 C -0.0694(10) 0.4889(3) 0.4056(4) 0.049(2) Uani 1 1 d . . . H56 H -0.1018 0.4887 0.4453 0.059 Uiso 1 1 calc R . . C57 C 0.0670(9) 0.4855(2) 0.4032(4) 0.0422(19) Uani 1 1 d . . . H57 H 0.1298 0.4832 0.4416 0.051 Uiso 1 1 calc R . . C58 C 0.1150(8) 0.4856(2) 0.3452(4) 0.0354(16) Uani 1 1 d . . . H58 H 0.2103 0.4833 0.3441 0.042 Uiso 1 1 calc R . . C59 C 0.0747(7) 0.44133(17) 0.1901(4) 0.0291(13) Uani 1 1 d . . . H59A H -0.0171 0.4325 0.1946 0.035 Uiso 1 1 calc R . . H59B H 0.0874 0.4387 0.1451 0.035 Uiso 1 1 calc R . . C60 C 0.1856(7) 0.42127(17) 0.2336(4) 0.0298(14) Uani 1 1 d . . . H60A H 0.1910 0.3977 0.2174 0.036 Uiso 1 1 calc R . . H60B H 0.1628 0.4201 0.2772 0.036 Uiso 1 1 calc R . . C61 C 0.4603(6) 0.42674(16) 0.3045(3) 0.0235(12) Uani 1 1 d . . . C62 C 0.4883(9) 0.4467(2) 0.3589(4) 0.0377(17) Uani 1 1 d . . . H62 H 0.4567 0.4696 0.3586 0.045 Uiso 1 1 calc R . . C63 C 0.5642(10) 0.4326(3) 0.4145(4) 0.049(2) Uani 1 1 d . . . H63 H 0.5806 0.4457 0.4525 0.059 Uiso 1 1 calc R . . C64 C 0.6146(9) 0.3999(2) 0.4137(4) 0.0409(18) Uani 1 1 d . . . H64 H 0.6652 0.3904 0.4513 0.049 Uiso 1 1 calc R . . C65 C 0.5921(8) 0.38086(18) 0.3589(4) 0.0326(15) Uani 1 1 d . . . H65 H 0.6296 0.3586 0.3583 0.039 Uiso 1 1 calc R . . C66 C 0.5148(8) 0.39408(17) 0.3046(4) 0.0295(14) Uani 1 1 d . . . H66 H 0.4988 0.3807 0.2669 0.035 Uiso 1 1 calc R . . C67 C 0.4232(8) 0.42642(17) 0.1674(3) 0.0285(14) Uani 1 1 d . . . C68 C 0.3526(10) 0.4049(2) 0.1224(4) 0.0410(18) Uani 1 1 d . . . H68 H 0.2597 0.3993 0.1240 0.049 Uiso 1 1 calc R . . C69 C 0.4193(13) 0.3914(3) 0.0743(5) 0.056(3) Uani 1 1 d . . . H69 H 0.3718 0.3762 0.0438 0.067 Uiso 1 1 calc R . . C70 C 0.5534(13) 0.4001(3) 0.0711(5) 0.061(3) Uani 1 1 d . . . H70 H 0.5982 0.3907 0.0388 0.073 Uiso 1 1 calc R . . C71 C 0.6222(11) 0.4224(3) 0.1149(5) 0.053(2) Uani 1 1 d . . . H71 H 0.7143 0.4285 0.1127 0.064 Uiso 1 1 calc R . . C72 C 0.5561(9) 0.4358(2) 0.1621(4) 0.0417(18) Uani 1 1 d . . . H72 H 0.6027 0.4517 0.1914 0.050 Uiso 1 1 calc R . . Br11 Br 0.49968(9) 0.65014(2) 0.40557(4) 0.04238(19) Uani 1 1 d . . . Br12 Br 0.93766(14) 0.39413(4) 0.04856(6) 0.0779(4) Uani 1 1 d . . . C81 C 0.6348(11) 0.6139(3) 0.2559(5) 0.061(3) Uani 1 1 d . . . H81A H 0.5795 0.5937 0.2407 0.073 Uiso 1 1 calc R . . H81B H 0.5949 0.6240 0.2916 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.8035(3) 0.60101(9) 0.28406(15) 0.0706(8) Uani 1 1 d . . . Cl2 Cl 0.6248(4) 0.64327(14) 0.1950(2) 0.1116(17) Uani 1 1 d . . . C82 C 0.6509(12) 0.5638(3) 0.4210(5) 0.058(3) Uani 1 1 d . . . H82A H 0.6617 0.5599 0.3760 0.069 Uiso 1 1 calc R . . H82B H 0.5860 0.5829 0.4221 0.069 Uiso 1 1 calc R . . Cl3 Cl 0.8102(3) 0.57487(8) 0.4650(2) 0.0880(12) Uani 1 1 d . . . Cl4 Cl 0.5832(3) 0.52691(6) 0.45103(12) 0.0542(6) Uani 1 1 d . . . C83 C 0.6930(14) 0.7193(5) 0.3247(8) 0.101(6) Uani 1 1 d . . . H83A H 0.6776 0.6982 0.3482 0.121 Uiso 1 1 calc R . . H83B H 0.6312 0.7186 0.2833 0.121 Uiso 1 1 calc R . . Cl5 Cl 0.6491(9) 0.7541(3) 0.3677(4) 0.214(5) Uani 1 1 d . . . Cl6 Cl 0.8606(4) 0.7195(2) 0.3105(4) 0.188(4) Uani 1 1 d . . . O1 O 0.072(3) 0.3363(9) 0.1296(10) 0.155(14) 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 0.02407(12) 0.01779(11) 0.02714(12) 0.00140(9) 0.00384(9) 0.00186(8) Pt2 0.02090(11) 0.01661(10) 0.02853(12) -0.00253(9) 0.00434(8) 0.00046(8) Br1 0.0480(6) 0.0601(7) 0.0991(9) 0.0129(6) 0.0097(6) 0.0043(5) Br2 0.0483(6) 0.0623(7) 0.1030(10) -0.0006(6) 0.0035(6) 0.0004(5) P1 0.0222(7) 0.0229(7) 0.0291(8) 0.0049(6) 0.0019(6) -0.0006(6) P2 0.0248(8) 0.0196(7) 0.0386(9) 0.0012(7) 0.0071(7) -0.0001(6) P3 0.0206(7) 0.0216(7) 0.0243(7) -0.0022(6) 0.0034(6) 0.0001(6) P4 0.0251(8) 0.0185(7) 0.0283(8) -0.0034(6) 0.0049(6) 0.0016(6) N1 0.038(3) 0.016(2) 0.023(3) 0.0010(19) 0.005(2) 0.003(2) N2 0.030(3) 0.015(2) 0.026(3) 0.0015(19) 0.002(2) 0.0007(19) N4 0.029(3) 0.019(2) 0.024(2) -0.0039(19) 0.003(2) 0.003(2) N3 0.027(3) 0.016(2) 0.023(2) -0.0022(19) 0.000(2) 0.0014(19) C1 0.028(3) 0.022(3) 0.027(3) -0.002(2) 0.003(2) 0.004(2) C2 0.032(3) 0.016(3) 0.023(3) 0.002(2) 0.003(2) 0.004(2) C3 0.031(3) 0.019(3) 0.023(3) -0.002(2) -0.001(2) 0.001(2) C4 0.029(3) 0.018(3) 0.023(3) 0.000(2) 0.000(2) 0.004(2) C5 0.027(3) 0.017(3) 0.024(3) 0.000(2) 0.001(2) 0.002(2) C6 0.026(3) 0.019(3) 0.023(3) -0.003(2) -0.002(2) 0.002(2) C7 0.036(3) 0.022(3) 0.023(3) -0.002(2) 0.004(3) -0.002(3) C9 0.069(6) 0.030(4) 0.022(3) 0.002(3) 0.007(3) 0.009(4) C10 0.092(8) 0.046(5) 0.040(5) 0.002(4) 0.026(5) 0.017(5) C11 0.143(15) 0.117(13) 0.063(8) 0.033(8) 0.054(9) 0.054(11) C12 0.039(4) 0.024(3) 0.023(3) -0.004(2) 0.004(3) -0.003(3) C13 0.051(4) 0.021(3) 0.029(3) -0.003(3) 0.010(3) 0.002(3) C14 0.064(6) 0.052(5) 0.035(4) -0.007(4) 0.020(4) -0.006(4) C8 0.020(3) 0.020(3) 0.028(3) -0.004(2) 0.004(2) 0.000(2) C18 0.070(6) 0.022(3) 0.030(4) -0.010(3) 0.013(4) -0.008(3) C19 0.20(2) 0.116(13) 0.054(7) 0.003(8) 0.075(11) 0.060(13) C20 0.090(14) 0.044(9) 0.062(11) -0.011(8) 0.032(10) -0.003(9) C15 0.034(3) 0.022(3) 0.021(3) -0.003(2) 0.000(2) 0.001(2) C16 0.036(4) 0.029(3) 0.027(3) -0.001(3) 0.005(3) 0.002(3) C17 0.066(6) 0.051(5) 0.027(4) -0.008(3) 0.008(4) 0.008(4) C21 0.032(4) 0.030(4) 0.043(4) 0.000(3) 0.000(3) -0.005(3) C22 0.126(12) 0.069(8) 0.044(6) 0.013(5) -0.020(7) -0.049(8) C23 0.23(2) 0.104(12) 0.067(9) 0.021(8) -0.070(12) -0.104(15) C24 0.182(18) 0.086(10) 0.085(10) 0.017(8) -0.049(11) -0.096(12) C25 0.055(6) 0.043(5) 0.078(7) 0.013(5) -0.007(5) -0.027(4) C26 0.030(4) 0.036(4) 0.051(5) 0.005(3) 0.002(3) -0.006(3) C27 0.034(3) 0.019(3) 0.035(3) 0.008(3) 0.009(3) 0.005(2) C28 0.044(4) 0.023(3) 0.039(4) 0.002(3) 0.008(3) 0.007(3) C29 0.068(6) 0.032(4) 0.037(4) 0.004(3) 0.013(4) 0.008(4) C30 0.076(7) 0.039(5) 0.046(5) 0.007(4) 0.032(5) 0.013(4) C31 0.038(4) 0.045(5) 0.071(6) 0.008(4) 0.022(4) 0.006(4) C32 0.033(4) 0.030(4) 0.048(4) 0.009(3) 0.011(3) 0.007(3) C33 0.026(3) 0.031(3) 0.035(4) 0.011(3) 0.005(3) 0.003(3) C34 0.030(3) 0.023(3) 0.048(4) 0.009(3) 0.010(3) 0.005(3) C35 0.031(3) 0.022(3) 0.045(4) 0.005(3) 0.012(3) -0.001(3) C36 0.035(4) 0.055(5) 0.045(5) 0.002(4) 0.009(3) 0.008(4) C37 0.039(4) 0.049(5) 0.052(5) -0.003(4) 0.019(4) -0.003(4) C38 0.068(6) 0.036(4) 0.050(5) -0.005(4) 0.032(5) -0.007(4) C39 0.059(6) 0.044(5) 0.040(4) 0.005(4) 0.015(4) 0.007(4) C40 0.040(4) 0.033(4) 0.042(4) 0.003(3) 0.006(3) 0.005(3) C41 0.022(3) 0.038(4) 0.075(6) -0.028(4) 0.011(4) -0.004(3) C42 0.058(6) 0.031(4) 0.124(10) -0.030(5) 0.044(7) -0.015(4) C43 0.053(7) 0.058(8) 0.190(19) -0.068(11) 0.035(10) -0.017(6) C44 0.027(5) 0.094(11) 0.21(2) -0.106(14) 0.019(8) -0.009(6) C45 0.046(6) 0.141(15) 0.119(12) -0.086(12) -0.025(7) 0.042(8) C46 0.042(5) 0.075(7) 0.082(8) -0.048(6) -0.012(5) 0.018(5) C47 0.021(3) 0.031(3) 0.031(3) 0.000(3) 0.003(2) 0.000(2) C48 0.037(4) 0.032(4) 0.037(4) -0.005(3) -0.001(3) 0.005(3) C49 0.056(5) 0.043(5) 0.046(5) 0.002(4) -0.007(4) 0.016(4) C50 0.070(7) 0.050(6) 0.044(5) 0.013(4) -0.008(5) 0.017(5) C51 0.062(6) 0.065(6) 0.025(4) 0.000(4) -0.004(4) 0.007(5) C52 0.040(4) 0.043(4) 0.030(4) -0.006(3) 0.002(3) 0.004(3) C53 0.028(3) 0.026(3) 0.029(3) -0.002(3) 0.008(3) -0.001(2) C54 0.032(4) 0.039(4) 0.029(3) 0.005(3) 0.009(3) 0.006(3) C55 0.038(4) 0.058(6) 0.045(5) 0.005(4) 0.018(4) 0.015(4) C56 0.055(5) 0.067(6) 0.030(4) 0.003(4) 0.019(4) 0.019(5) C57 0.045(5) 0.054(5) 0.027(4) 0.005(3) 0.002(3) 0.007(4) C58 0.030(4) 0.043(4) 0.031(4) 0.001(3) 0.000(3) 0.005(3) C59 0.027(3) 0.023(3) 0.037(4) -0.007(3) 0.004(3) -0.004(2) C60 0.031(3) 0.018(3) 0.040(4) -0.005(3) 0.005(3) -0.002(2) C61 0.022(3) 0.020(3) 0.028(3) -0.002(2) 0.004(2) 0.003(2) C62 0.044(4) 0.032(4) 0.036(4) -0.011(3) 0.002(3) 0.015(3) C63 0.058(6) 0.052(5) 0.033(4) -0.013(4) -0.006(4) 0.017(4) C64 0.049(5) 0.039(4) 0.032(4) 0.005(3) -0.001(3) 0.011(4) C65 0.039(4) 0.019(3) 0.038(4) 0.004(3) 0.003(3) 0.002(3) C66 0.037(4) 0.017(3) 0.034(3) -0.004(2) 0.004(3) -0.001(2) C67 0.037(4) 0.024(3) 0.025(3) 0.004(2) 0.006(3) 0.013(3) C68 0.057(5) 0.034(4) 0.032(4) -0.007(3) 0.007(4) 0.001(4) C69 0.088(8) 0.042(5) 0.041(5) -0.013(4) 0.015(5) 0.007(5) C70 0.089(8) 0.061(6) 0.038(5) 0.002(4) 0.028(5) 0.022(6) C71 0.051(5) 0.070(7) 0.042(5) 0.004(4) 0.021(4) 0.014(5) C72 0.042(4) 0.049(5) 0.036(4) 0.000(3) 0.012(3) 0.009(4) Br11 0.0438(4) 0.0428(4) 0.0374(4) -0.0074(3) -0.0032(3) 0.0005(3) Br12 0.0780(8) 0.1018(10) 0.0534(6) -0.0318(6) 0.0090(6) -0.0140(7) C81 0.043(5) 0.081(8) 0.061(6) 0.001(6) 0.015(5) 0.004(5) Cl1 0.0548(15) 0.086(2) 0.0673(17) -0.0216(15) -0.0019(13) 0.0182(14) Cl2 0.0570(18) 0.165(4) 0.117(3) 0.080(3) 0.0265(19) 0.018(2) C82 0.068(7) 0.040(5) 0.058(6) 0.009(4) -0.012(5) 0.000(5) Cl3 0.0674(18) 0.0529(16) 0.129(3) 0.0203(18) -0.0290(19) -0.0142(14) Cl4 0.0635(14) 0.0452(12) 0.0587(14) -0.0087(10) 0.0247(11) -0.0069(10) C83 0.056(8) 0.142(15) 0.103(12) 0.039(11) 0.008(7) -0.029(9) Cl5 0.195(8) 0.288(11) 0.163(7) -0.090(7) 0.047(6) -0.139(8) Cl6 0.055(2) 0.242(7) 0.270(8) 0.188(7) 0.030(3) 0.016(3) O1 0.15(2) 0.25(3) 0.058(12) -0.044(16) -0.017(13) 0.14(2) _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 2.033(7) . ? Pt1 P1 2.2285(17) . ? Pt1 P2 2.2952(18) . ? Pt1 Br1 2.4312(12) . ? Pt2 C8 2.028(6) . ? Pt2 P3 2.2290(16) . ? Pt2 P4 2.2920(17) . ? Pt2 Br2 2.4204(12) . ? P1 C27 1.799(7) . ? P1 C21 1.802(8) . ? P1 C33 1.826(7) . ? P2 C41 1.804(8) . ? P2 C35 1.815(8) . ? P2 C34 1.849(7) . ? P3 C47 1.799(7) . ? P3 C53 1.815(7) . ? P3 C59 1.833(7) . ? P4 C61 1.809(7) . ? P4 C67 1.816(7) . ? P4 C60 1.844(7) . ? N1 C1 1.368(8) . ? N1 C2 1.381(8) . ? N1 C9 1.464(9) . ? N2 C1 1.354(9) . ? N2 C3 1.396(8) . ? N2 C12 1.455(8) . ? N4 C8 1.356(8) . ? N4 C6 1.395(8) . ? N4 C18 1.464(9) . ? N3 C8 1.353(8) . ? N3 C5 1.388(8) . ? N3 C15 1.474(8) . ? C2 C7 1.376(9) . ? C2 C3 1.409(9) . ? C3 C4 1.392(9) . ? C4 C5 1.386(9) . ? C5 C6 1.406(9) . ? C6 C7 1.397(9) . ? C9 C10 1.548(14) . ? C10 C11 1.502(15) . ? C12 C13 1.517(11) . ? C13 C14 1.539(11) . ? C18 C19 1.642(19) . ? C19 C20 1.5188(10) . ? C19 C20A 1.5190(12) . ? C15 C16 1.519(10) . ? C16 C17 1.530(11) . ? C21 C22 1.372(13) . ? C21 C26 1.402(11) . ? C22 C23 1.424(17) . ? C23 C24 1.35(2) . ? C24 C25 1.349(18) . ? C25 C26 1.368(12) . ? C27 C32 1.387(10) . ? C27 C28 1.394(11) . ? C28 C29 1.393(12) . ? C29 C30 1.367(14) . ? C30 C31 1.378(15) . ? C31 C32 1.397(13) . ? C33 C34 1.518(11) . ? C35 C40 1.387(11) . ? C35 C36 1.409(11) . ? C36 C37 1.379(12) . ? C37 C38 1.366(14) . ? C38 C39 1.382(14) . ? C39 C40 1.399(12) . ? C41 C46 1.373(17) . ? C41 C42 1.418(14) . ? C42 C43 1.345(17) . ? C43 C44 1.30(3) . ? C44 C45 1.49(3) . ? C45 C46 1.436(16) . ? C47 C48 1.388(10) . ? C47 C52 1.397(10) . ? C48 C49 1.394(11) . ? C49 C50 1.385(14) . ? C50 C51 1.381(15) . ? C51 C52 1.403(12) . ? C53 C54 1.389(10) . ? C53 C58 1.406(10) . ? C54 C55 1.383(11) . ? C55 C56 1.393(13) . ? C56 C57 1.363(13) . ? C57 C58 1.390(11) . ? C59 C60 1.536(10) . ? C61 C62 1.388(10) . ? C61 C66 1.389(9) . ? C62 C63 1.410(12) . ? C63 C64 1.379(12) . ? C64 C65 1.372(11) . ? C65 C66 1.382(10) . ? C67 C68 1.380(11) . ? C67 C72 1.386(12) . ? C68 C69 1.404(12) . ? C69 C70 1.381(17) . ? C70 C71 1.376(16) . ? C71 C72 1.383(12) . ? C81 Cl2 1.723(12) . ? C81 Cl1 1.756(11) . ? C82 Cl3 1.756(11) . ? C82 Cl4 1.756(11) . ? C83 Cl6 1.730(14) . ? C83 Cl5 1.73(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 Pt1 P1 92.4(2) . . ? C1 Pt1 P2 174.09(19) . . ? P1 Pt1 P2 85.81(6) . . ? C1 Pt1 Br1 87.43(19) . . ? P1 Pt1 Br1 176.56(6) . . ? P2 Pt1 Br1 94.73(5) . . ? C8 Pt2 P3 94.17(18) . . ? C8 Pt2 P4 174.55(19) . . ? P3 Pt2 P4 85.76(6) . . ? C8 Pt2 Br2 85.43(18) . . ? P3 Pt2 Br2 175.85(6) . . ? P4 Pt2 Br2 95.03(5) . . ? C27 P1 C21 105.2(4) . . ? C27 P1 C33 105.5(3) . . ? C21 P1 C33 109.8(4) . . ? C27 P1 Pt1 111.9(2) . . ? C21 P1 Pt1 116.7(3) . . ? C33 P1 Pt1 107.3(2) . . ? C41 P2 C35 101.6(4) . . ? C41 P2 C34 106.3(4) . . ? C35 P2 C34 107.3(4) . . ? C41 P2 Pt1 118.7(4) . . ? C35 P2 Pt1 115.0(2) . . ? C34 P2 Pt1 107.2(2) . . ? C47 P3 C53 107.7(3) . . ? C47 P3 C59 108.4(3) . . ? C53 P3 C59 105.3(3) . . ? C47 P3 Pt2 116.4(2) . . ? C53 P3 Pt2 110.7(2) . . ? C59 P3 Pt2 107.8(2) . . ? C61 P4 C67 105.2(3) . . ? C61 P4 C60 105.1(3) . . ? C67 P4 C60 106.2(3) . . ? C61 P4 Pt2 119.1(2) . . ? C67 P4 Pt2 112.4(2) . . ? C60 P4 Pt2 107.8(2) . . ? C1 N1 C2 110.7(5) . . ? C1 N1 C9 123.7(6) . . ? C2 N1 C9 124.7(6) . . ? C1 N2 C3 110.0(5) . . ? C1 N2 C12 125.9(5) . . ? C3 N2 C12 124.1(5) . . ? C8 N4 C6 110.3(5) . . ? C8 N4 C18 125.5(6) . . ? C6 N4 C18 123.8(6) . . ? C8 N3 C5 110.7(5) . . ? C8 N3 C15 125.1(5) . . ? C5 N3 C15 124.1(5) . . ? N2 C1 N1 106.8(6) . . ? N2 C1 Pt1 128.0(5) . . ? N1 C1 Pt1 125.1(5) . . ? C7 C2 N1 129.9(6) . . ? C7 C2 C3 124.1(6) . . ? N1 C2 C3 105.9(5) . . ? C4 C3 N2 130.2(6) . . ? C4 C3 C2 123.1(6) . . ? N2 C3 C2 106.6(5) . . ? C5 C4 C3 112.9(6) . . ? C4 C5 N3 130.1(6) . . ? C4 C5 C6 123.7(6) . . ? N3 C5 C6 106.1(5) . . ? N4 C6 C7 130.6(6) . . ? N4 C6 C5 106.0(5) . . ? C7 C6 C5 123.2(6) . . ? C2 C7 C6 112.8(6) . . ? N1 C9 C10 110.4(7) . . ? C11 C10 C9 111.1(10) . . ? N2 C12 C13 113.3(6) . . ? C12 C13 C14 109.5(7) . . ? N3 C8 N4 106.8(5) . . ? N3 C8 Pt2 127.5(5) . . ? N4 C8 Pt2 125.1(4) . . ? N4 C18 C19 107.4(7) . . ? C20 C19 C18 110.9(14) . . ? N3 C15 C16 112.8(6) . . ? C15 C16 C17 109.7(6) . . ? C22 C21 C26 119.5(8) . . ? C22 C21 P1 120.4(7) . . ? C26 C21 P1 119.7(6) . . ? C21 C22 C23 118.3(11) . . ? C24 C23 C22 120.2(12) . . ? C25 C24 C23 121.5(11) . . ? C24 C25 C26 120.0(10) . . ? C25 C26 C21 120.5(9) . . ? C32 C27 C28 119.0(7) . . ? C32 C27 P1 120.4(6) . . ? C28 C27 P1 120.5(6) . . ? C29 C28 C27 120.2(8) . . ? C30 C29 C28 120.2(9) . . ? C29 C30 C31 120.4(8) . . ? C30 C31 C32 120.0(8) . . ? C27 C32 C31 120.1(8) . . ? C34 C33 P1 108.3(5) . . ? C33 C34 P2 110.4(5) . . ? C40 C35 C36 119.5(7) . . ? C40 C35 P2 122.8(6) . . ? C36 C35 P2 117.5(6) . . ? C37 C36 C35 119.8(8) . . ? C38 C37 C36 120.7(9) . . ? C37 C38 C39 120.3(8) . . ? C38 C39 C40 120.3(9) . . ? C35 C40 C39 119.4(8) . . ? C46 C41 C42 121.0(10) . . ? C46 C41 P2 120.7(8) . . ? C42 C41 P2 118.3(9) . . ? C43 C42 C41 121.5(16) . . ? C44 C43 C42 119.6(17) . . ? C43 C44 C45 124.0(12) . . ? C46 C45 C44 114.6(15) . . ? C41 C46 C45 119.1(15) . . ? C48 C47 C52 120.5(7) . . ? C48 C47 P3 118.6(6) . . ? C52 C47 P3 120.3(6) . . ? C47 C48 C49 119.8(8) . . ? C50 C49 C48 120.2(9) . . ? C51 C50 C49 119.9(8) . . ? C50 C51 C52 120.7(8) . . ? C47 C52 C51 118.7(8) . . ? C54 C53 C58 119.1(7) . . ? C54 C53 P3 122.2(6) . . ? C58 C53 P3 118.7(5) . . ? C55 C54 C53 119.5(7) . . ? C54 C55 C56 121.3(8) . . ? C57 C56 C55 119.3(8) . . ? C56 C57 C58 120.6(8) . . ? C57 C58 C53 120.1(7) . . ? C60 C59 P3 108.4(5) . . ? C59 C60 P4 108.6(5) . . ? C62 C61 C66 119.5(6) . . ? C62 C61 P4 119.9(5) . . ? C66 C61 P4 120.6(5) . . ? C61 C62 C63 119.3(7) . . ? C64 C63 C62 120.0(8) . . ? C65 C64 C63 120.4(7) . . ? C64 C65 C66 120.0(7) . . ? C65 C66 C61 120.7(7) . . ? C68 C67 C72 119.2(7) . . ? C68 C67 P4 123.2(6) . . ? C72 C67 P4 117.6(6) . . ? C67 C68 C69 119.4(9) . . ? C70 C69 C68 120.4(9) . . ? C71 C70 C69 120.0(9) . . ? C70 C71 C72 119.4(10) . . ? C71 C72 C67 121.4(9) . . ? Cl2 C81 Cl1 112.9(6) . . ? Cl3 C82 Cl4 111.8(5) . . ? Cl6 C83 Cl5 114.4(10) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 31.97 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 4.387 _refine_diff_density_min -5.016 _refine_diff_density_rms 0.248 _database_code_depnum_ccdc_archive 'CCDC 947445' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H54 Br2 N4 P4 Pt2),2(Br), 0.5(C6 H14), 2(C H4 O)' _chemical_formula_sum 'C33 H69 Br4 N4 O2 P4 Pt2' _chemical_formula_weight 1387.62 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2551(6) _cell_length_b 12.2648(7) _cell_length_c 20.1873(12) _cell_angle_alpha 77.4950(10) _cell_angle_beta 81.3650(10) _cell_angle_gamma 86.3740(10) _cell_volume 2449.5(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 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1334 _exptl_absorpt_coefficient_mu 9.129 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1919 _exptl_absorpt_correction_T_max 0.4621 _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 = 0.413730 ; _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 28746 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 30.00 _reflns_number_total 14164 _reflns_number_gt 11213 _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. The asymmetric unit contains 1/2 hexane molecule related to the other half by an inversion center located on the midpont of the C41-C41* bond. This together with the free and unbound nature of the hexane molecule and the associated strong thermal motion might be responsible for the deviation of some C-C-C angels from 109 deg. ; _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^)+(0.0480P)^2^+9.6309P] 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 14164 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1065 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.752163(19) 0.812927(17) 0.332330(10) 0.01850(6) Uani 1 1 d . . . Br1 Br 0.91872(6) 0.78611(6) 0.23382(3) 0.03444(15) Uani 1 1 d . . . P2 P 0.65121(16) 0.96063(13) 0.26751(8) 0.0257(3) Uani 1 1 d . . . P1 P 0.59552(15) 0.83418(14) 0.41771(8) 0.0271(3) Uani 1 1 d . . . C1 C 0.8429(5) 0.6909(4) 0.3959(3) 0.0193(10) Uani 1 1 d . . . N1 N 0.9396(5) 0.7087(4) 0.4315(2) 0.0208(9) Uani 1 1 d . . . N2 N 0.8213(4) 0.5803(4) 0.4126(2) 0.0191(9) Uani 1 1 d . . . C2 C 0.9823(5) 0.6080(4) 0.4697(3) 0.0194(10) Uani 1 1 d . . . C3 C 0.9064(5) 0.5255(5) 0.4579(3) 0.0201(10) Uani 1 1 d . . . C4 C 0.9206(5) 0.4130(4) 0.4874(3) 0.0186(10) Uani 1 1 d . . . H4 H 0.8696 0.3565 0.4792 0.022 Uiso 1 1 calc R . . C5 C 1.0004(6) 0.8166(5) 0.4252(3) 0.0267(12) Uani 1 1 d . . . H5A H 1.0117 0.8269 0.4713 0.032 Uiso 1 1 calc R . . H5B H 0.9416 0.8779 0.4050 0.032 Uiso 1 1 calc R . . C6 C 1.1335(6) 0.8216(5) 0.3805(4) 0.0333(14) Uani 1 1 d . . . H6A H 1.1931 0.7631 0.4017 0.050 Uiso 1 1 calc R . . H6B H 1.1709 0.8949 0.3758 0.050 Uiso 1 1 calc R . . H6C H 1.1225 0.8100 0.3352 0.050 Uiso 1 1 calc R . . C7 C 0.7299(6) 0.5234(5) 0.3835(3) 0.0249(12) Uani 1 1 d . . . H7A H 0.6601 0.5776 0.3670 0.030 Uiso 1 1 calc R . . H7B H 0.6870 0.4637 0.4199 0.030 Uiso 1 1 calc R . . C8 C 0.7976(7) 0.4725(6) 0.3247(4) 0.0380(15) Uani 1 1 d . . . H8A H 0.8307 0.5321 0.2862 0.057 Uiso 1 1 calc R . . H8B H 0.7343 0.4290 0.3102 0.057 Uiso 1 1 calc R . . H8C H 0.8715 0.4235 0.3397 0.057 Uiso 1 1 calc R . . C14 C 0.7326(9) 1.0900(6) 0.2583(5) 0.051(2) Uani 1 1 d . . . H14A H 0.8192 1.0869 0.2305 0.077 Uiso 1 1 calc R . . H14B H 0.7438 1.1015 0.3036 0.077 Uiso 1 1 calc R . . H14C H 0.6790 1.1520 0.2357 0.077 Uiso 1 1 calc R . . C13 C 0.6243(6) 0.9532(5) 0.1823(3) 0.0289(13) Uani 1 1 d . . . H13A H 0.5855 1.0244 0.1602 0.043 Uiso 1 1 calc R . . H13B H 0.5641 0.8929 0.1851 0.043 Uiso 1 1 calc R . . H13C H 0.7087 0.9383 0.1554 0.043 Uiso 1 1 calc R . . C12 C 0.4861(7) 0.9789(7) 0.3178(4) 0.0414(17) Uani 1 1 d . . . H12A H 0.4495 1.0550 0.3017 0.050 Uiso 1 1 calc R . . H12B H 0.4248 0.9244 0.3109 0.050 Uiso 1 1 calc R . . C11 C 0.4991(7) 0.9613(6) 0.3920(4) 0.0404(16) Uani 1 1 d . . . H11A H 0.4105 0.9559 0.4195 0.048 Uiso 1 1 calc R . . H11B H 0.5428 1.0257 0.4004 0.048 Uiso 1 1 calc R . . C9 C 0.6499(8) 0.8473(7) 0.4973(4) 0.0438(17) Uani 1 1 d . . . H9A H 0.5735 0.8443 0.5331 0.066 Uiso 1 1 calc R . . H9B H 0.6930 0.9187 0.4904 0.066 Uiso 1 1 calc R . . H9C H 0.7125 0.7858 0.5112 0.066 Uiso 1 1 calc R . . C10 C 0.4847(7) 0.7190(6) 0.4446(4) 0.0398(16) Uani 1 1 d . . . H10A H 0.4131 0.7366 0.4790 0.060 Uiso 1 1 calc R . . H10B H 0.5333 0.6514 0.4644 0.060 Uiso 1 1 calc R . . H10C H 0.4477 0.7065 0.4049 0.060 Uiso 1 1 calc R . . Br2 Br 0.76492(8) 0.15486(8) 0.43891(4) 0.0516(2) Uani 1 1 d . . . Pt21 Pt 0.34806(2) 0.631531(17) 0.183537(10) 0.01885(6) Uani 1 1 d . . . Br21 Br 0.48629(7) 0.67032(6) 0.26597(4) 0.03714(15) Uani 1 1 d . . . P22 P 0.26750(15) 0.47853(13) 0.26116(8) 0.0246(3) Uani 1 1 d . . . P21 P 0.22058(15) 0.58759(13) 0.11430(8) 0.0239(3) Uani 1 1 d . . . C21 C 0.4091(5) 0.7717(5) 0.1140(3) 0.0213(11) Uani 1 1 d . . . N21 N 0.5175(4) 0.7823(4) 0.0662(2) 0.0201(9) Uani 1 1 d . . . N22 N 0.3445(4) 0.8731(4) 0.1061(2) 0.0192(9) Uani 1 1 d . . . C22 C 0.5249(5) 0.8908(4) 0.0274(3) 0.0187(10) Uani 1 1 d . . . C23 C 0.4137(5) 0.9499(4) 0.0531(3) 0.0189(10) Uani 1 1 d . . . C24 C 0.3845(5) 1.0614(4) 0.0272(3) 0.0190(10) Uani 1 1 d . . . H24 H 0.3096 1.1010 0.0452 0.023 Uiso 1 1 calc R . . C25 C 0.6154(6) 0.6929(5) 0.0565(3) 0.0256(12) Uani 1 1 d . . . H25A H 0.6357 0.6927 0.0070 0.031 Uiso 1 1 calc R . . H25B H 0.5775 0.6201 0.0801 0.031 Uiso 1 1 calc R . . C26 C 0.7416(6) 0.7057(6) 0.0836(4) 0.0346(15) Uani 1 1 d . . . H26A H 0.7773 0.7792 0.0621 0.052 Uiso 1 1 calc R . . H26B H 0.8060 0.6472 0.0730 0.052 Uiso 1 1 calc R . . H26C H 0.7235 0.6989 0.1334 0.052 Uiso 1 1 calc R . . C27 C 0.2237(5) 0.9002(5) 0.1481(3) 0.0224(11) Uani 1 1 d . . . H27A H 0.1798 0.8301 0.1722 0.027 Uiso 1 1 calc R . . H27B H 0.1631 0.9447 0.1180 0.027 Uiso 1 1 calc R . . C28 C 0.2485(7) 0.9650(6) 0.2002(3) 0.0355(15) Uani 1 1 d . . . H28A H 0.2977 0.9173 0.2342 0.053 Uiso 1 1 calc R . . H28B H 0.1639 0.9891 0.2232 0.053 Uiso 1 1 calc R . . H28C H 0.2998 1.0306 0.1772 0.053 Uiso 1 1 calc R . . C34 C 0.3799(7) 0.3729(6) 0.2987(4) 0.0394(16) Uani 1 1 d . . . H34A H 0.4486 0.4083 0.3149 0.059 Uiso 1 1 calc R . . H34B H 0.4206 0.3310 0.2643 0.059 Uiso 1 1 calc R . . H34C H 0.3316 0.3217 0.3375 0.059 Uiso 1 1 calc R . . C33 C 0.1625(7) 0.5176(6) 0.3331(3) 0.0377(16) Uani 1 1 d . . . H33A H 0.1277 0.4502 0.3649 0.057 Uiso 1 1 calc R . . H33B H 0.0891 0.5658 0.3167 0.057 Uiso 1 1 calc R . . H33C H 0.2137 0.5579 0.3568 0.057 Uiso 1 1 calc R . . C32 C 0.1627(7) 0.4065(5) 0.2193(4) 0.0336(14) Uani 1 1 d . . . H32A H 0.2167 0.3523 0.1961 0.040 Uiso 1 1 calc R . . H32B H 0.0945 0.3651 0.2540 0.040 Uiso 1 1 calc R . . C31 C 0.0969(7) 0.4932(6) 0.1670(4) 0.0342(14) Uani 1 1 d . . . H31A H 0.0275 0.5362 0.1910 0.041 Uiso 1 1 calc R . . H31B H 0.0548 0.4551 0.1375 0.041 Uiso 1 1 calc R . . C29 C 0.3094(7) 0.5170(6) 0.0504(4) 0.0383(16) Uani 1 1 d . . . H29A H 0.2469 0.4944 0.0241 0.057 Uiso 1 1 calc R . . H29B H 0.3566 0.4507 0.0731 0.057 Uiso 1 1 calc R . . H29C H 0.3729 0.5677 0.0195 0.057 Uiso 1 1 calc R . . C30 C 0.1277(7) 0.6996(6) 0.0661(4) 0.0360(15) Uani 1 1 d . . . H30A H 0.1887 0.7497 0.0330 0.054 Uiso 1 1 calc R . . H30B H 0.0754 0.7416 0.0976 0.054 Uiso 1 1 calc R . . H30C H 0.0687 0.6682 0.0417 0.054 Uiso 1 1 calc R . . Br22 Br 0.46862(11) 0.24644(7) 0.13347(6) 0.0659(3) Uani 1 1 d . . . C41 C 0.9580(12) 0.0118(10) 0.0303(6) 0.0780(18) Uiso 1 1 d . . 3 C42 C 1.0351(12) 0.0995(10) 0.0403(6) 0.0780(18) Uiso 1 1 d . A 3 C43 C 0.9603(12) 0.1331(10) 0.1024(6) 0.0780(18) Uiso 1 1 d . A 3 O44 O 1.0478(14) 0.2252(12) 0.1230(7) 0.068(3) Uiso 0.50 1 d P B 1 C44 C 1.009(2) 0.3075(18) 0.0766(11) 0.068(3) Uiso 0.50 1 d P B 1 O45 O 0.0642(6) 0.2340(5) 0.3768(4) 0.068(2) Uani 1 1 d . C 1 H45 H -0.0170 0.2385 0.3741 0.102 Uiso 1 1 calc R . . C45 C 0.1170(11) 0.1311(8) 0.3629(7) 0.078(3) Uani 1 1 d . . . H45A H 0.0884 0.0706 0.4018 0.118 Uiso 1 1 calc R C 1 H45B H 0.2136 0.1327 0.3554 0.118 Uiso 1 1 calc R C 1 H45C H 0.0858 0.1183 0.3217 0.118 Uiso 1 1 calc R C 1 O46 O 0.7281(9) 0.4101(8) 0.1727(5) 0.0364(17) Uiso 0.50 1 d P D 2 C46 C 0.7398(14) 0.3758(12) 0.1120(7) 0.0364(17) Uiso 0.50 1 d P D 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 Pt1 0.01792(10) 0.01795(10) 0.01791(10) -0.00055(7) -0.00299(7) 0.00250(7) Br1 0.0260(3) 0.0468(4) 0.0255(3) -0.0027(3) 0.0033(2) 0.0039(3) P2 0.0311(8) 0.0199(7) 0.0259(7) -0.0019(6) -0.0099(6) 0.0048(6) P1 0.0258(7) 0.0277(8) 0.0259(8) -0.0064(6) 0.0016(6) 0.0036(6) C1 0.019(2) 0.018(2) 0.019(2) -0.002(2) -0.0007(19) 0.0011(19) N1 0.025(2) 0.018(2) 0.018(2) 0.0021(17) -0.0052(17) 0.0014(18) N2 0.021(2) 0.016(2) 0.020(2) -0.0003(17) -0.0065(17) 0.0016(17) C2 0.022(2) 0.017(2) 0.019(2) -0.0019(19) -0.0052(19) 0.002(2) C3 0.018(2) 0.023(3) 0.017(2) -0.001(2) -0.0014(19) 0.003(2) C4 0.022(2) 0.017(2) 0.017(2) -0.0023(19) -0.0038(19) -0.002(2) C5 0.035(3) 0.016(3) 0.029(3) -0.002(2) -0.012(2) -0.001(2) C6 0.034(3) 0.026(3) 0.039(4) -0.002(3) -0.004(3) -0.011(3) C7 0.027(3) 0.024(3) 0.026(3) -0.004(2) -0.013(2) -0.002(2) C8 0.041(4) 0.039(4) 0.040(4) -0.021(3) -0.009(3) 0.000(3) C14 0.074(6) 0.028(4) 0.057(5) -0.001(3) -0.033(4) -0.010(4) C13 0.028(3) 0.030(3) 0.027(3) -0.001(2) -0.009(2) 0.006(2) C12 0.038(4) 0.045(4) 0.043(4) -0.017(3) -0.009(3) 0.023(3) C11 0.036(4) 0.035(4) 0.047(4) -0.013(3) 0.001(3) 0.013(3) C9 0.045(4) 0.058(5) 0.032(4) -0.018(3) -0.003(3) -0.001(4) C10 0.032(3) 0.044(4) 0.039(4) -0.009(3) 0.012(3) -0.008(3) Br2 0.0416(4) 0.0672(6) 0.0534(5) -0.0330(4) 0.0046(3) -0.0135(4) Pt21 0.02112(10) 0.01623(10) 0.01725(10) 0.00035(7) -0.00155(7) -0.00189(7) Br21 0.0450(4) 0.0331(3) 0.0351(3) -0.0001(3) -0.0189(3) -0.0083(3) P22 0.0286(7) 0.0192(7) 0.0226(7) 0.0008(5) 0.0007(6) -0.0036(6) P21 0.0284(7) 0.0215(7) 0.0226(7) -0.0042(6) -0.0065(6) 0.0001(6) C21 0.022(3) 0.018(3) 0.023(3) -0.001(2) -0.005(2) -0.001(2) N21 0.021(2) 0.018(2) 0.018(2) 0.0004(17) 0.0026(17) -0.0008(17) N22 0.020(2) 0.015(2) 0.019(2) 0.0012(17) 0.0019(17) -0.0009(17) C22 0.021(2) 0.015(2) 0.020(2) -0.0039(19) -0.0031(19) -0.0004(19) C23 0.019(2) 0.016(2) 0.020(2) -0.0012(19) -0.0021(19) -0.0044(19) C24 0.020(2) 0.017(2) 0.020(2) -0.003(2) -0.0019(19) -0.0015(19) C25 0.027(3) 0.017(3) 0.030(3) 0.000(2) -0.003(2) 0.004(2) C26 0.028(3) 0.030(3) 0.046(4) -0.006(3) -0.011(3) 0.007(3) C27 0.018(2) 0.023(3) 0.022(3) -0.001(2) 0.005(2) -0.001(2) C28 0.032(3) 0.046(4) 0.027(3) -0.006(3) 0.001(3) -0.001(3) C34 0.042(4) 0.027(3) 0.043(4) 0.009(3) -0.006(3) -0.005(3) C33 0.038(4) 0.041(4) 0.029(3) -0.002(3) 0.007(3) -0.008(3) C32 0.036(3) 0.025(3) 0.040(4) -0.006(3) -0.004(3) -0.010(3) C31 0.037(3) 0.032(3) 0.037(4) -0.008(3) -0.010(3) -0.009(3) C29 0.048(4) 0.035(4) 0.034(4) -0.015(3) -0.011(3) 0.015(3) C30 0.042(4) 0.034(4) 0.036(4) -0.011(3) -0.016(3) 0.005(3) Br22 0.0925(7) 0.0396(4) 0.0811(7) -0.0254(4) -0.0531(6) 0.0222(5) O45 0.054(4) 0.032(3) 0.104(5) -0.009(3) 0.026(4) -0.002(3) C45 0.068(6) 0.044(5) 0.117(10) -0.024(6) 0.014(6) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.026(5) . ? Pt1 P1 2.2202(15) . ? Pt1 P2 2.2823(15) . ? Pt1 Br1 2.4845(6) . ? P2 C14 1.800(8) . ? P2 C13 1.804(6) . ? P2 C12 1.866(7) . ? P1 C10 1.808(7) . ? P1 C11 1.813(7) . ? P1 C9 1.819(7) . ? C1 N2 1.349(7) . ? C1 N1 1.362(7) . ? N1 C2 1.390(7) . ? N1 C5 1.471(7) . ? N2 C3 1.396(6) . ? N2 C7 1.461(7) . ? C2 C4 1.392(7) 2_766 ? C2 C3 1.396(8) . ? C3 C4 1.387(7) . ? C4 C2 1.392(7) 2_766 ? C5 C6 1.516(9) . ? C7 C8 1.517(9) . ? C12 C11 1.491(10) . ? Pt21 C21 2.036(5) . ? Pt21 P21 2.2174(15) . ? Pt21 P22 2.2788(14) . ? Pt21 Br21 2.4782(7) . ? P22 C34 1.797(7) . ? P22 C33 1.807(7) . ? P22 C32 1.834(7) . ? P21 C29 1.809(7) . ? P21 C30 1.810(7) . ? P21 C31 1.824(7) . ? C21 N21 1.351(7) . ? C21 N22 1.361(7) . ? N21 C22 1.391(7) . ? N21 C25 1.465(7) . ? N22 C23 1.399(6) . ? N22 C27 1.455(7) . ? C22 C24 1.379(7) 2_675 ? C22 C23 1.406(7) . ? C23 C24 1.386(7) . ? C24 C22 1.379(7) 2_675 ? C25 C26 1.509(9) . ? C27 C28 1.506(9) . ? C32 C31 1.529(9) . ? C41 C42 1.440(16) . ? C41 C41 1.46(2) 2_755 ? C42 C43 1.491(16) . ? O44 C44 1.30(2) . ? O45 C45 1.409(11) . ? O46 C46 1.366(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 C1 Pt1 P1 90.78(15) . . ? C1 Pt1 P2 174.80(16) . . ? P1 Pt1 P2 86.28(6) . . ? C1 Pt1 Br1 90.52(15) . . ? P1 Pt1 Br1 177.08(5) . . ? P2 Pt1 Br1 92.61(4) . . ? C14 P2 C13 105.7(4) . . ? C14 P2 C12 105.4(4) . . ? C13 P2 C12 107.3(3) . . ? C14 P2 Pt1 112.7(3) . . ? C13 P2 Pt1 119.3(2) . . ? C12 P2 Pt1 105.4(2) . . ? C10 P1 C11 108.4(4) . . ? C10 P1 C9 103.2(4) . . ? C11 P1 C9 104.9(4) . . ? C10 P1 Pt1 113.4(2) . . ? C11 P1 Pt1 109.5(2) . . ? C9 P1 Pt1 116.7(3) . . ? N2 C1 N1 106.8(4) . . ? N2 C1 Pt1 128.9(4) . . ? N1 C1 Pt1 124.3(4) . . ? C1 N1 C2 110.2(5) . . ? C1 N1 C5 125.2(4) . . ? C2 N1 C5 124.3(5) . . ? C1 N2 C3 110.4(5) . . ? C1 N2 C7 125.3(4) . . ? C3 N2 C7 124.1(5) . . ? N1 C2 C4 129.7(5) . 2_766 ? N1 C2 C3 106.3(5) . . ? C4 C2 C3 124.0(5) 2_766 . ? C4 C3 C2 123.4(5) . . ? C4 C3 N2 130.4(5) . . ? C2 C3 N2 106.2(5) . . ? C3 C4 C2 112.7(5) . 2_766 ? N1 C5 C6 110.8(5) . . ? N2 C7 C8 112.7(5) . . ? C11 C12 P2 109.7(5) . . ? C12 C11 P1 110.0(5) . . ? C21 Pt21 P21 92.01(16) . . ? C21 Pt21 P22 176.70(16) . . ? P21 Pt21 P22 86.20(6) . . ? C21 Pt21 Br21 91.42(16) . . ? P21 Pt21 Br21 176.56(4) . . ? P22 Pt21 Br21 90.37(4) . . ? C34 P22 C33 104.9(4) . . ? C34 P22 C32 105.6(3) . . ? C33 P22 C32 106.2(3) . . ? C34 P22 Pt21 119.7(2) . . ? C33 P22 Pt21 111.5(2) . . ? C32 P22 Pt21 108.0(2) . . ? C29 P21 C30 104.5(3) . . ? C29 P21 C31 107.8(4) . . ? C30 P21 C31 105.2(3) . . ? C29 P21 Pt21 113.4(3) . . ? C30 P21 Pt21 117.8(2) . . ? C31 P21 Pt21 107.5(2) . . ? N21 C21 N22 106.9(5) . . ? N21 C21 Pt21 127.6(4) . . ? N22 C21 Pt21 125.5(4) . . ? C21 N21 C22 110.8(4) . . ? C21 N21 C25 125.2(5) . . ? C22 N21 C25 124.1(4) . . ? C21 N22 C23 110.1(4) . . ? C21 N22 C27 125.5(5) . . ? C23 N22 C27 124.3(4) . . ? C24 C22 N21 130.9(5) 2_675 . ? C24 C22 C23 122.9(5) 2_675 . ? N21 C22 C23 106.1(4) . . ? C24 C23 N22 130.1(5) . . ? C24 C23 C22 123.9(5) . . ? N22 C23 C22 106.0(4) . . ? C22 C24 C23 113.2(5) 2_675 . ? N21 C25 C26 112.6(5) . . ? N22 C27 C28 112.6(5) . . ? C31 C32 P22 108.9(4) . . ? C32 C31 P21 109.5(5) . . ? C42 C41 C41 96.9(12) . 2_755 ? C41 C42 C43 103.3(10) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.753 _refine_diff_density_min -2.115 _refine_diff_density_rms 0.200 _database_code_depnum_ccdc_archive 'CCDC 947446' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H62 Br2 N4 P4 Pt2, 6(C H4 O), Br2, (O H2)' _chemical_formula_sum 'C38 H88 Br4 N4 O7 P4 Pt2' _chemical_formula_weight 1546.82 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' 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' 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 _symmetry_space_group_name_Hall '-P 2yn' 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 12.9311(15) _cell_length_b 10.7309(13) _cell_length_c 20.245(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.749(2) _cell_angle_gamma 90.00 _cell_volume 2776.6(6) _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 plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 8.070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2476 _exptl_absorpt_correction_T_max 0.8553 _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 = 0.563518 ; _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 25425 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 30.00 _reflns_number_total 8000 _reflns_number_gt 6054 _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. The asmmetric unit contains 1/2 water molcule of crystallization. This water molecule is located about 2 A from one of the bromine counter ions indicating the possibility of hydrogen bonding between the the bromine atom and the water moelcule. The SOF of the water molcule is 0.5. ; _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^)+(0.0749P)^2^+8.9217P] 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 8000 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 Pt1 Pt 0.909664(17) 0.22184(2) 0.760842(12) 0.02711(8) Uani 1 1 d . . . Br1 Br 0.75474(5) 0.08436(7) 0.72701(4) 0.04076(17) Uani 1 1 d . . . P1 P 1.04602(12) 0.34957(15) 0.78314(9) 0.0299(3) Uani 1 1 d . . . P2 P 0.88018(13) 0.31623(16) 0.65864(8) 0.0299(3) Uani 1 1 d . . . C1 C 0.9430(5) 0.1378(6) 0.8531(3) 0.0296(12) Uani 1 1 d . . . N1 N 1.0066(4) 0.0363(5) 0.8670(3) 0.0303(11) Uani 1 1 d . . . N2 N 0.9095(4) 0.1703(5) 0.9097(3) 0.0295(11) Uani 1 1 d . . . C2 C 1.0113(5) 0.0040(6) 0.9340(3) 0.0298(13) Uani 1 1 d . . . C3 C 0.9485(5) 0.0909(5) 0.9617(3) 0.0272(12) Uani 1 1 d . . . C4 C 0.9330(5) 0.0896(5) 1.0284(3) 0.0301(13) Uani 1 1 d . . . H4 H 0.8886 0.1469 1.0463 0.036 Uiso 1 1 calc R . . C5 C 1.0564(5) -0.0345(6) 0.8178(3) 0.0297(12) Uani 1 1 d . . . H5A H 1.1273 -0.0608 0.8386 0.036 Uiso 1 1 calc R . . H5B H 1.0639 0.0202 0.7794 0.036 Uiso 1 1 calc R . . C6 C 0.9935(6) -0.1481(7) 0.7930(4) 0.0390(15) Uani 1 1 d . . . H6A H 0.9214 -0.1227 0.7740 0.047 Uiso 1 1 calc R . . H6B H 0.9892 -0.2054 0.8307 0.047 Uiso 1 1 calc R . . C7 C 1.0440(8) -0.2141(8) 0.7401(5) 0.053(2) Uani 1 1 d . . . H7A H 1.0640 -0.1528 0.7085 0.079 Uiso 1 1 calc R . . H7B H 0.9943 -0.2736 0.7162 0.079 Uiso 1 1 calc R . . H7C H 1.1064 -0.2587 0.7614 0.079 Uiso 1 1 calc R . . C8 C 0.8328(5) 0.2711(6) 0.9146(4) 0.0324(13) Uani 1 1 d . . . H8A H 0.8378 0.3337 0.8794 0.039 Uiso 1 1 calc R . . H8B H 0.8501 0.3130 0.9585 0.039 Uiso 1 1 calc R . . C9 C 0.7222(6) 0.2218(7) 0.9071(4) 0.0428(16) Uani 1 1 d . . . H9A H 0.7172 0.1591 0.9423 0.051 Uiso 1 1 calc R . . H9B H 0.7049 0.1801 0.8632 0.051 Uiso 1 1 calc R . . C10 C 0.6437(7) 0.3256(10) 0.9123(5) 0.064(3) Uani 1 1 d . . . H10A H 0.6636 0.3709 0.9543 0.096 Uiso 1 1 calc R . . H10B H 0.5738 0.2896 0.9113 0.096 Uiso 1 1 calc R . . H10C H 0.6431 0.3830 0.8746 0.096 Uiso 1 1 calc R . . C11 C 1.0284(6) 0.4702(6) 0.8422(4) 0.0375(15) Uani 1 1 d . . . H11A H 1.0204 0.4323 0.8852 0.056 Uiso 1 1 calc R . . H11B H 0.9656 0.5185 0.8255 0.056 Uiso 1 1 calc R . . H11C H 1.0895 0.5253 0.8481 0.056 Uiso 1 1 calc R . . C12 C 1.1704(5) 0.2788(7) 0.8138(4) 0.0438(17) Uani 1 1 d . . . H12A H 1.2242 0.3437 0.8223 0.066 Uiso 1 1 calc R . . H12B H 1.1892 0.2203 0.7804 0.066 Uiso 1 1 calc R . . H12C H 1.1657 0.2340 0.8554 0.066 Uiso 1 1 calc R . . C13 C 1.0667(5) 0.4293(6) 0.7065(4) 0.0359(14) Uani 1 1 d . . . H13A H 1.1056 0.5078 0.7178 0.043 Uiso 1 1 calc R . . H13B H 1.1089 0.3759 0.6809 0.043 Uiso 1 1 calc R . . C14 C 0.9609(5) 0.4581(6) 0.6636(4) 0.0353(14) Uani 1 1 d . . . H14A H 0.9715 0.4844 0.6183 0.042 Uiso 1 1 calc R . . H14B H 0.9254 0.5266 0.6841 0.042 Uiso 1 1 calc R . . C15 C 0.7505(5) 0.3663(7) 0.6250(4) 0.0376(15) Uani 1 1 d . . . H15A H 0.7490 0.3932 0.5786 0.056 Uiso 1 1 calc R . . H15B H 0.7301 0.4359 0.6515 0.056 Uiso 1 1 calc R . . H15C H 0.7015 0.2970 0.6264 0.056 Uiso 1 1 calc R . . C16 C 0.9240(6) 0.2188(7) 0.5955(4) 0.0419(16) Uani 1 1 d . . . H16A H 0.8848 0.1403 0.5920 0.063 Uiso 1 1 calc R . . H16B H 0.9988 0.2014 0.6078 0.063 Uiso 1 1 calc R . . H16C H 0.9120 0.2620 0.5523 0.063 Uiso 1 1 calc R . . Br2 Br 0.23963(8) 0.21377(11) 0.61389(6) 0.0721(3) Uani 1 1 d . . . C21 C 0.3934(10) 0.8767(10) 0.4714(5) 0.080(3) Uani 1 1 d . . . H21A H 0.4175 0.9549 0.4936 0.120 Uiso 1 1 calc R . . H21B H 0.3399 0.8947 0.4329 0.120 Uiso 1 1 calc R . . H21C H 0.4526 0.8341 0.4562 0.120 Uiso 1 1 calc R . . O21 O 0.3508(7) 0.8000(7) 0.5165(4) 0.082(2) Uani 1 1 d . . . C22 C 0.1024(12) 0.9239(14) 0.5647(7) 0.106(5) Uani 1 1 d . . . H22A H 0.1001 0.9337 0.6126 0.159 Uiso 1 1 calc R . . H22B H 0.0817 0.8388 0.5509 0.159 Uiso 1 1 calc R . . H22C H 0.0541 0.9833 0.5395 0.159 Uiso 1 1 calc R . . O22 O 0.2057(7) 0.9469(8) 0.5518(5) 0.089(2) Uani 1 1 d . . . C23 C 0.1105(9) 0.4515(17) 0.5311(6) 0.097(5) Uani 1 1 d . . . H23A H 0.1124 0.3831 0.5633 0.145 Uiso 1 1 calc R . . H23B H 0.1426 0.4243 0.4927 0.145 Uiso 1 1 calc R . . H23C H 0.0377 0.4758 0.5159 0.145 Uiso 1 1 calc R . . O23 O 0.1661(11) 0.5539(16) 0.5617(7) 0.164(5) Uani 1 1 d . . . O1 O 0.1838(11) 0.0856(15) 0.6677(7) 0.074(4) 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 0.02902(12) 0.02007(12) 0.02988(14) 0.00118(9) -0.00307(9) -0.00178(9) Br1 0.0409(4) 0.0371(4) 0.0401(4) 0.0051(3) -0.0071(3) -0.0143(3) P1 0.0300(8) 0.0232(7) 0.0339(9) -0.0018(6) -0.0036(6) -0.0032(6) P2 0.0330(8) 0.0248(7) 0.0301(8) -0.0001(6) -0.0010(6) 0.0001(6) C1 0.033(3) 0.024(3) 0.030(3) 0.001(2) -0.002(2) 0.000(2) N1 0.036(3) 0.022(2) 0.031(3) 0.002(2) 0.000(2) -0.001(2) N2 0.033(3) 0.022(2) 0.030(3) 0.003(2) -0.006(2) 0.005(2) C2 0.033(3) 0.022(3) 0.032(3) -0.002(2) -0.003(3) 0.000(2) C3 0.031(3) 0.016(2) 0.031(3) -0.001(2) -0.007(2) 0.003(2) C4 0.032(3) 0.019(3) 0.037(3) -0.003(2) -0.003(3) 0.003(2) C5 0.032(3) 0.026(3) 0.031(3) 0.000(2) 0.004(2) 0.003(2) C6 0.045(4) 0.031(3) 0.040(4) -0.006(3) 0.003(3) 0.003(3) C7 0.062(5) 0.037(4) 0.058(5) -0.011(4) 0.005(4) 0.001(4) C8 0.035(3) 0.020(3) 0.040(4) 0.002(3) 0.000(3) 0.003(2) C9 0.039(4) 0.037(4) 0.051(4) -0.005(3) 0.002(3) 0.000(3) C10 0.053(5) 0.072(6) 0.061(6) -0.007(5) -0.009(4) 0.025(5) C11 0.043(4) 0.027(3) 0.040(4) -0.008(3) 0.001(3) -0.004(3) C12 0.031(3) 0.038(4) 0.060(5) 0.002(3) -0.001(3) -0.001(3) C13 0.032(3) 0.030(3) 0.044(4) 0.003(3) 0.003(3) -0.004(3) C14 0.039(3) 0.026(3) 0.040(4) 0.003(3) 0.003(3) -0.004(3) C15 0.036(3) 0.038(4) 0.036(4) 0.002(3) -0.006(3) 0.004(3) C16 0.053(4) 0.035(4) 0.038(4) -0.008(3) 0.007(3) 0.005(3) Br2 0.0513(5) 0.0780(7) 0.0868(8) -0.0205(6) 0.0099(5) -0.0047(5) C21 0.108(9) 0.059(6) 0.064(7) 0.005(5) -0.015(6) -0.017(6) O21 0.120(7) 0.065(5) 0.060(4) 0.014(4) 0.009(4) -0.003(4) C22 0.141(13) 0.090(10) 0.089(10) -0.016(8) 0.022(9) -0.034(9) O22 0.091(6) 0.059(5) 0.115(7) 0.008(5) 0.012(5) 0.000(4) C23 0.065(7) 0.156(15) 0.063(7) -0.020(8) -0.007(6) 0.021(8) O23 0.141(11) 0.189(14) 0.159(13) 0.064(11) 0.017(9) 0.022(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 Pt1 C1 2.060(6) . ? Pt1 P1 2.2246(16) . ? Pt1 P2 2.2831(17) . ? Pt1 Br1 2.4983(7) . ? P1 C11 1.800(7) . ? P1 C12 1.802(7) . ? P1 C13 1.827(7) . ? P2 C15 1.794(7) . ? P2 C16 1.808(7) . ? P2 C14 1.840(7) . ? C1 N2 1.333(8) . ? C1 N1 1.368(8) . ? N1 C2 1.391(8) . ? N1 C5 1.477(8) . ? N2 C3 1.388(7) . ? N2 C8 1.480(8) . ? C2 C4 1.394(8) 3_757 ? C2 C3 1.408(9) . ? C3 C4 1.394(9) . ? C4 C2 1.394(8) 3_757 ? C5 C6 1.508(9) . ? C6 C7 1.512(11) . ? C8 C9 1.510(10) . ? C9 C10 1.521(11) . ? C13 C14 1.536(9) . ? C21 O21 1.403(13) . ? C22 O22 1.422(16) . ? C23 O23 1.404(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 92.03(18) . . ? C1 Pt1 P2 177.54(18) . . ? P1 Pt1 P2 85.90(6) . . ? C1 Pt1 Br1 92.22(17) . . ? P1 Pt1 Br1 175.70(5) . . ? P2 Pt1 Br1 89.84(5) . . ? C11 P1 C12 105.7(4) . . ? C11 P1 C13 106.1(3) . . ? C12 P1 C13 104.6(4) . . ? C11 P1 Pt1 113.6(2) . . ? C12 P1 Pt1 116.7(2) . . ? C13 P1 Pt1 109.3(2) . . ? C15 P2 C16 106.2(4) . . ? C15 P2 C14 105.2(3) . . ? C16 P2 C14 106.3(4) . . ? C15 P2 Pt1 119.7(3) . . ? C16 P2 Pt1 110.9(3) . . ? C14 P2 Pt1 107.6(2) . . ? N2 C1 N1 107.2(5) . . ? N2 C1 Pt1 127.9(4) . . ? N1 C1 Pt1 124.9(5) . . ? C1 N1 C2 109.6(5) . . ? C1 N1 C5 125.5(5) . . ? C2 N1 C5 124.8(5) . . ? C1 N2 C3 111.3(5) . . ? C1 N2 C8 123.9(5) . . ? C3 N2 C8 124.6(5) . . ? N1 C2 C4 130.9(6) . 3_757 ? N1 C2 C3 106.3(5) . . ? C4 C2 C3 122.7(6) 3_757 . ? N2 C3 C4 130.6(5) . . ? N2 C3 C2 105.6(5) . . ? C4 C3 C2 123.8(5) . . ? C2 C4 C3 113.5(6) 3_757 . ? N1 C5 C6 111.8(5) . . ? C5 C6 C7 110.2(6) . . ? N2 C8 C9 111.8(5) . . ? C8 C9 C10 111.6(7) . . ? C14 C13 P1 109.9(4) . . ? C13 C14 P2 108.3(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.075 _refine_diff_density_min -2.841 _refine_diff_density_rms 0.212 _database_code_depnum_ccdc_archive 'CCDC 947447' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H62 Br2 N4 P4 Pt2, 4(C H2 Cl2),2(Br)' _chemical_formula_sum 'C36 H70 Br4 Cl8 N4 P4 Pt2' _chemical_formula_weight 1676.26 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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_hall '-P 2ybc' 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 16.8861(12) _cell_length_b 11.9102(9) _cell_length_c 14.9781(11) _cell_angle_alpha 90.00 _cell_angle_beta 101.4310(10) _cell_angle_gamma 90.00 _cell_volume 2952.6(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 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 7.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3455 _exptl_absorpt_correction_T_max 0.6473 _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 = 0.490346 ; _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 34130 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 30.50 _reflns_number_total 8959 _reflns_number_gt 6977 _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. The Cl14-C22-Cl13 angle of one of the dichloromethane molecules is large (119.5(9) deg) but falls in the range C1 molecules bearing two large and two small substituents. ; _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^)+(0.0462P)^2^+12.9439P] 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 8959 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.735238(11) 0.771305(18) 0.032936(14) 0.02181(6) Uani 1 1 d . . . Br1 Br 0.81502(4) 0.61624(6) -0.01785(7) 0.0523(2) Uani 1 1 d . . . P1 P 0.65658(8) 0.90045(13) 0.07835(9) 0.0245(3) Uani 1 1 d . . . P2 P 0.62553(8) 0.65618(13) 0.01863(10) 0.0252(3) Uani 1 1 d . . . C1 C 0.8325(3) 0.8745(5) 0.0292(4) 0.0241(10) Uani 1 1 d . . . N1 N 0.8990(2) 0.8912(4) 0.0934(3) 0.0241(9) Uani 1 1 d . . . N2 N 0.8447(2) 0.9229(4) -0.0500(3) 0.0217(9) Uani 1 1 d . . . C2 C 0.9572(3) 0.9478(5) 0.0563(4) 0.0248(11) Uani 1 1 d . . . C3 C 0.9223(3) 0.9669(5) -0.0360(3) 0.0235(10) Uani 1 1 d . . . C4 C 0.9638(3) 1.0196(5) -0.0957(4) 0.0255(11) Uani 1 1 d . . . H4 H 0.9406 1.0325 -0.1580 0.031 Uiso 1 1 calc R . . C5 C 0.9073(3) 0.8513(6) 0.1877(4) 0.0311(12) Uani 1 1 d . . . H5 H 0.8550 0.8147 0.1923 0.037 Uiso 1 1 calc R . . C6 C 0.9721(4) 0.7629(7) 0.2117(5) 0.0446(17) Uani 1 1 d . . . H6A H 0.9593 0.6990 0.1701 0.067 Uiso 1 1 calc R . . H6B H 0.9746 0.7377 0.2744 0.067 Uiso 1 1 calc R . . H6C H 1.0244 0.7947 0.2060 0.067 Uiso 1 1 calc R . . C7 C 0.9179(5) 0.9515(7) 0.2526(5) 0.0484(18) Uani 1 1 d . . . H7A H 0.9683 0.9907 0.2493 0.073 Uiso 1 1 calc R . . H7B H 0.9200 0.9251 0.3150 0.073 Uiso 1 1 calc R . . H7C H 0.8722 1.0031 0.2351 0.073 Uiso 1 1 calc R . . C8 C 0.7834(3) 0.9273(5) -0.1346(4) 0.0242(10) Uani 1 1 d . . . H8 H 0.7319 0.8982 -0.1198 0.029 Uiso 1 1 calc R . . C9 C 0.8048(4) 0.8508(6) -0.2068(4) 0.0358(13) Uani 1 1 d . . . H9A H 0.8520 0.8809 -0.2277 0.054 Uiso 1 1 calc R . . H9B H 0.7590 0.8463 -0.2584 0.054 Uiso 1 1 calc R . . H9C H 0.8173 0.7757 -0.1812 0.054 Uiso 1 1 calc R . . C10 C 0.7675(4) 1.0475(5) -0.1670(4) 0.0330(13) Uani 1 1 d . . . H10A H 0.7616 1.0952 -0.1154 0.050 Uiso 1 1 calc R . . H10B H 0.7177 1.0504 -0.2135 0.050 Uiso 1 1 calc R . . H10C H 0.8128 1.0744 -0.1931 0.050 Uiso 1 1 calc R . . C11 C 0.6598(4) 1.0400(5) 0.0312(4) 0.0341(13) Uani 1 1 d . . . H11A H 0.6200 1.0879 0.0522 0.051 Uiso 1 1 calc R . . H11B H 0.6473 1.0358 -0.0354 0.051 Uiso 1 1 calc R . . H11C H 0.7140 1.0718 0.0514 0.051 Uiso 1 1 calc R . . C12 C 0.6735(5) 0.9183(7) 0.1998(4) 0.0443(16) Uani 1 1 d . . . H12A H 0.7271 0.9509 0.2215 0.066 Uiso 1 1 calc R . . H12B H 0.6703 0.8452 0.2289 0.066 Uiso 1 1 calc R . . H12C H 0.6322 0.9686 0.2152 0.066 Uiso 1 1 calc R . . C13 C 0.5512(3) 0.8549(6) 0.0454(4) 0.0318(12) Uani 1 1 d . . . H13A H 0.5172 0.8968 0.0807 0.038 Uiso 1 1 calc R . . H13B H 0.5308 0.8699 -0.0201 0.038 Uiso 1 1 calc R . . C14 C 0.5469(3) 0.7294(5) 0.0643(4) 0.0332(13) Uani 1 1 d . . . H14A H 0.4931 0.7000 0.0354 0.040 Uiso 1 1 calc R . . H14B H 0.5548 0.7164 0.1308 0.040 Uiso 1 1 calc R . . C15 C 0.5853(4) 0.6312(6) -0.0999(4) 0.0396(15) Uani 1 1 d . . . H15A H 0.6267 0.5962 -0.1281 0.059 Uiso 1 1 calc R . . H15B H 0.5686 0.7027 -0.1304 0.059 Uiso 1 1 calc R . . H15C H 0.5384 0.5812 -0.1061 0.059 Uiso 1 1 calc R . . C16 C 0.6364(4) 0.5199(5) 0.0732(5) 0.0373(14) Uani 1 1 d . . . H16A H 0.5886 0.4741 0.0495 0.056 Uiso 1 1 calc R . . H16B H 0.6417 0.5293 0.1391 0.056 Uiso 1 1 calc R . . H16C H 0.6847 0.4825 0.0605 0.056 Uiso 1 1 calc R . . C21 C 0.6058(5) 0.2511(7) 0.2873(6) 0.0512(19) Uani 1 1 d . . . H21A H 0.5535 0.2114 0.2705 0.061 Uiso 1 1 calc R . . H21B H 0.5944 0.3298 0.3018 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.66351(13) 0.1874(2) 0.38511(18) 0.0685(6) Uani 1 1 d . . . Cl2 Cl 0.6542(2) 0.2494(2) 0.19424(19) 0.0847(9) Uani 1 1 d . . . C22 C 0.8763(7) 0.1861(12) 0.5093(14) 0.139(7) Uani 1 1 d . . . H22A H 0.8539 0.1094 0.5098 0.166 Uiso 1 1 calc R . . H22B H 0.8514 0.2203 0.4502 0.166 Uiso 1 1 calc R . . Cl3 Cl 0.97444(19) 0.1735(3) 0.5114(2) 0.0995(10) Uani 1 1 d . . . Cl4 Cl 0.8453(3) 0.2591(5) 0.5906(3) 0.163(2) Uani 1 1 d . . . Br2 Br 0.55368(4) 0.94231(6) 0.79623(4) 0.03414(14) 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 Pt1 0.01707(9) 0.02349(10) 0.02729(10) 0.00032(8) 0.01021(7) -0.00285(8) Br1 0.0425(4) 0.0309(3) 0.0946(6) -0.0071(4) 0.0409(4) 0.0018(3) P1 0.0223(6) 0.0298(7) 0.0230(6) -0.0020(5) 0.0082(5) 0.0001(5) P2 0.0231(6) 0.0282(7) 0.0269(7) -0.0014(5) 0.0112(5) -0.0069(5) C1 0.021(2) 0.028(3) 0.024(2) 0.005(2) 0.0071(19) 0.002(2) N1 0.0166(19) 0.032(3) 0.025(2) 0.0067(18) 0.0060(16) -0.0067(17) N2 0.0165(19) 0.027(2) 0.022(2) 0.0019(17) 0.0054(15) -0.0045(16) C2 0.020(2) 0.032(3) 0.025(2) 0.005(2) 0.0096(19) -0.007(2) C3 0.016(2) 0.031(3) 0.024(2) 0.005(2) 0.0039(18) -0.0049(19) C4 0.023(2) 0.033(3) 0.021(2) 0.004(2) 0.0053(19) -0.006(2) C5 0.029(3) 0.044(4) 0.022(3) 0.008(2) 0.009(2) -0.009(2) C6 0.032(3) 0.060(5) 0.042(4) 0.023(3) 0.008(3) -0.005(3) C7 0.054(4) 0.060(5) 0.035(4) 0.002(3) 0.017(3) -0.010(4) C8 0.018(2) 0.031(3) 0.023(2) -0.002(2) 0.0037(18) -0.003(2) C9 0.034(3) 0.042(4) 0.033(3) -0.007(3) 0.010(2) 0.000(3) C10 0.027(3) 0.035(3) 0.035(3) 0.006(2) 0.002(2) 0.001(2) C11 0.036(3) 0.030(3) 0.039(3) -0.005(2) 0.015(3) 0.000(2) C12 0.057(4) 0.048(4) 0.031(3) -0.002(3) 0.015(3) 0.013(3) C13 0.021(2) 0.044(4) 0.033(3) -0.001(3) 0.011(2) 0.001(2) C14 0.023(3) 0.042(3) 0.039(3) -0.001(3) 0.017(2) -0.005(2) C15 0.037(3) 0.052(4) 0.030(3) -0.009(3) 0.007(3) -0.015(3) C16 0.040(3) 0.033(3) 0.041(3) 0.003(3) 0.013(3) -0.008(3) C21 0.052(4) 0.043(4) 0.062(5) -0.005(3) 0.020(4) -0.008(3) Cl1 0.0502(11) 0.0659(14) 0.0865(16) 0.0229(12) 0.0062(11) -0.0087(10) Cl2 0.137(3) 0.0593(14) 0.0751(16) -0.0301(12) 0.0622(17) -0.0365(15) C22 0.059(7) 0.086(9) 0.28(2) -0.089(12) 0.065(10) -0.020(6) Cl3 0.0763(18) 0.122(3) 0.104(2) 0.024(2) 0.0264(16) 0.0067(18) Cl4 0.101(3) 0.257(6) 0.121(3) -0.052(4) -0.004(2) 0.086(3) Br2 0.0331(3) 0.0401(3) 0.0292(3) -0.0011(2) 0.0060(2) -0.0061(2) _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 2.061(5) . ? Pt1 P1 2.2251(14) . ? Pt1 P2 2.2805(14) . ? Pt1 Br1 2.4921(7) . ? P1 C12 1.797(6) . ? P1 C11 1.810(6) . ? P1 C13 1.833(6) . ? P2 C15 1.796(6) . ? P2 C16 1.810(7) . ? P2 C14 1.831(6) . ? C1 N1 1.341(7) . ? C1 N2 1.369(6) . ? N1 C2 1.396(6) . ? N1 C5 1.470(7) . ? N2 C3 1.389(6) . ? N2 C8 1.470(6) . ? C2 C4 1.401(7) 3_775 ? C2 C3 1.409(7) . ? C3 C4 1.392(7) . ? C4 C2 1.401(7) 3_775 ? C5 C6 1.508(10) . ? C5 C7 1.528(10) . ? C8 C9 1.512(8) . ? C8 C10 1.518(8) . ? C13 C14 1.525(9) . ? C21 Cl2 1.751(9) . ? C21 Cl1 1.761(9) . ? C22 Cl3 1.657(11) . ? C22 Cl4 1.664(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pt1 P1 97.08(16) . . ? C1 Pt1 P2 173.15(15) . . ? P1 Pt1 P2 85.49(5) . . ? C1 Pt1 Br1 87.24(15) . . ? P1 Pt1 Br1 175.69(4) . . ? P2 Pt1 Br1 90.23(4) . . ? C12 P1 C11 106.0(3) . . ? C12 P1 C13 105.0(3) . . ? C11 P1 C13 105.7(3) . . ? C12 P1 Pt1 114.0(2) . . ? C11 P1 Pt1 116.7(2) . . ? C13 P1 Pt1 108.6(2) . . ? C15 P2 C16 106.4(3) . . ? C15 P2 C14 106.7(3) . . ? C16 P2 C14 105.9(3) . . ? C15 P2 Pt1 109.5(2) . . ? C16 P2 Pt1 119.3(2) . . ? C14 P2 Pt1 108.3(2) . . ? N1 C1 N2 108.1(4) . . ? N1 C1 Pt1 128.8(4) . . ? N2 C1 Pt1 122.1(4) . . ? C1 N1 C2 110.0(4) . . ? C1 N1 C5 123.3(4) . . ? C2 N1 C5 126.7(4) . . ? C1 N2 C3 109.1(4) . . ? C1 N2 C8 124.1(4) . . ? C3 N2 C8 126.8(4) . . ? N1 C2 C4 130.7(5) . 3_775 ? N1 C2 C3 106.1(4) . . ? C4 C2 C3 123.2(4) 3_775 . ? N2 C3 C4 130.9(5) . . ? N2 C3 C2 106.6(4) . . ? C4 C3 C2 122.5(4) . . ? C3 C4 C2 114.4(5) . 3_775 ? N1 C5 C6 112.4(5) . . ? N1 C5 C7 109.6(5) . . ? C6 C5 C7 114.0(6) . . ? N2 C8 C9 111.6(5) . . ? N2 C8 C10 111.1(4) . . ? C9 C8 C10 113.0(5) . . ? C14 C13 P1 108.6(4) . . ? C13 C14 P2 109.4(4) . . ? Cl2 C21 Cl1 112.9(5) . . ? Cl3 C22 Cl4 119.5(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.784 _refine_diff_density_min -1.680 _refine_diff_density_rms 0.183 _database_code_depnum_ccdc_archive 'CCDC 947448' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H70 Br2 N4 P4 Pt2, 4(C H4 O), 2(Br)' _chemical_formula_sum 'C40 H86 Br4 N4 O4 P4 Pt2' _chemical_formula_weight 1520.83 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' 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' 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 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.4288(8) _cell_length_b 10.7546(7) _cell_length_c 24.7631(17) _cell_angle_alpha 90.00 _cell_angle_beta 99.2950(10) _cell_angle_gamma 90.00 _cell_volume 3003.7(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 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.682 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 7.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1989 _exptl_absorpt_correction_T_max 0.3817 _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 = 0.414348 ; _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 27935 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7936 _reflns_number_gt 6397 _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^)+(0.0545P)^2^+10.5957P] 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 7936 _refine_ls_number_parameters 306 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0535 _refine_ls_R_factor_gt 0.0394 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.051 _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 0.693618(17) 0.279247(18) 0.867170(8) 0.02384(7) Uani 1 1 d . B . Br1 Br 0.68890(6) 0.13652(7) 0.78803(3) 0.04761(17) Uani 1 1 d . . . P1 P 0.69556(14) 0.41742(14) 0.93405(6) 0.0317(3) Uani 1 1 d D . . P2 P 0.56104(14) 0.40697(15) 0.81648(7) 0.0353(3) Uani 1 1 d D . . N1 N 0.9291(4) 0.1751(5) 0.9222(2) 0.0349(11) Uani 1 1 d . B . N2 N 0.7830(4) 0.0778(4) 0.9497(2) 0.0302(10) Uani 1 1 d . B . C1 C 0.8105(5) 0.1683(5) 0.9162(2) 0.0290(11) Uani 1 1 d . . . C2 C 0.9809(5) 0.0893(6) 0.9612(3) 0.0381(14) Uani 1 1 d . . . C3 C 0.8856(5) 0.0257(6) 0.9785(3) 0.0348(13) Uani 1 1 d . B . C4 C 0.9010(5) -0.0655(6) 1.0187(3) 0.0391(15) Uani 1 1 d . . . H4 H 0.8371 -0.1073 1.0310 0.047 Uiso 1 1 calc R B . C5 C 0.9964(6) 0.2546(6) 0.8898(3) 0.0412(15) Uani 1 1 d . . . H5A H 1.0695 0.2839 0.9134 0.049 Uiso 1 1 calc R B . H5B H 0.9482 0.3285 0.8769 0.049 Uiso 1 1 calc R . . C6 C 1.0294(7) 0.1871(8) 0.8413(3) 0.0557(19) Uani 1 1 d D A . C7 C 1.0872(11) 0.2672(15) 0.8034(5) 0.053(4) Uani 0.55 1 d PD A 1 C8 C 1.000(2) 0.361(2) 0.7739(9) 0.146(12) Uani 0.55 1 d PD A 1 C7A C 1.091(3) 0.0613(17) 0.8452(14) 0.139(12) Uiso 0.45 1 d PD A 2 C8A C 1.106(4) 0.044(4) 0.7858(14) 0.168(16) Uiso 0.45 1 d PD A 2 C9 C 0.6621(5) 0.0354(5) 0.9527(2) 0.0291(11) Uani 1 1 d . . . H9A H 0.6057 0.1040 0.9415 0.035 Uiso 1 1 calc R B . H9B H 0.6566 0.0137 0.9911 0.035 Uiso 1 1 calc R . . C10 C 0.6276(6) -0.0759(6) 0.9167(3) 0.0461(17) Uani 1 1 d . B . H10A H 0.6832 -0.1451 0.9282 0.055 Uiso 1 1 calc R . . H10B H 0.6334 -0.0546 0.8784 0.055 Uiso 1 1 calc R . . C11 C 0.4988(6) -0.1183(6) 0.9203(4) 0.055(2) Uani 1 1 d . . . H11A H 0.4825 -0.1970 0.8996 0.066 Uiso 1 1 calc R B . H11B H 0.4928 -0.1355 0.9590 0.066 Uiso 1 1 calc R . . C12 C 0.4060(6) -0.0248(8) 0.8982(3) 0.0544(19) Uani 1 1 d . B . H12A H 0.4142 0.0491 0.9217 0.082 Uiso 1 1 calc R . . H12B H 0.3272 -0.0611 0.8975 0.082 Uiso 1 1 calc R . . H12C H 0.4161 -0.0011 0.8610 0.082 Uiso 1 1 calc R . . C13 C 0.6469(7) 0.3643(7) 0.9944(3) 0.0478(17) Uani 1 1 d . B . H13A H 0.7007 0.2994 1.0115 0.072 Uiso 1 1 calc R . . H13B H 0.5666 0.3303 0.9852 0.072 Uiso 1 1 calc R . . H13C H 0.6465 0.4339 1.0200 0.072 Uiso 1 1 calc R . . C14 C 0.8216(11) 0.5121(15) 0.9463(6) 0.046(3) Uani 0.55 1 d P B 1 C14A C 0.8556(13) 0.4594(18) 0.9690(7) 0.041(4) Uani 0.45 1 d P B 2 C15 C 0.5696(12) 0.5278(10) 0.9087(5) 0.037(2) Uani 0.55 1 d PD B 1 C16 C 0.5573(14) 0.5580(10) 0.8485(6) 0.044(3) Uani 0.55 1 d PD B 1 C15A C 0.6334(14) 0.5642(11) 0.9102(6) 0.037(3) Uani 0.45 1 d PD B 2 C16A C 0.5256(14) 0.5267(12) 0.8663(7) 0.041(4) Uani 0.45 1 d PD B 2 C17 C 0.5931(14) 0.4370(18) 0.7447(6) 0.054(4) Uani 0.55 1 d P B 1 C17A C 0.6221(15) 0.4957(19) 0.7683(8) 0.051(5) Uani 0.45 1 d P B 2 C18 C 0.4158(6) 0.3433(7) 0.7967(4) 0.057(2) Uani 1 1 d . B . H18A H 0.3835 0.3187 0.8295 0.085 Uiso 1 1 calc R . . H18B H 0.4203 0.2703 0.7734 0.085 Uiso 1 1 calc R . . H18C H 0.3641 0.4059 0.7764 0.085 Uiso 1 1 calc R . . Br2 Br 0.67980(8) 0.69287(8) 0.05436(4) 0.0622(2) Uani 1 1 d . . . O21 O 0.1421(8) 0.5503(10) 0.8860(4) 0.127(3) Uani 1 1 d . . . C21 C 0.2018(10) 0.6074(15) 0.8486(5) 0.110(5) Uani 1 1 d . . . O31 O 0.908(3) 0.799(3) 0.8602(13) 0.183(7) Uiso 0.488(12) 1 d P C 3 C31 C 0.978(5) 0.784(5) 0.899(2) 0.183(7) Uiso 0.488(12) 1 d P C 3 O31A O 1.034(3) 0.703(3) 0.8542(12) 0.183(7) Uiso 0.512(12) 1 d P C 4 C31A C 0.906(4) 0.637(4) 0.8646(17) 0.183(7) Uiso 0.512(12) 1 d P C 4 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 0.02368(10) 0.02054(10) 0.02632(11) 0.00341(8) 0.00107(7) 0.00285(8) Br1 0.0505(4) 0.0460(4) 0.0461(4) -0.0180(3) 0.0072(3) -0.0054(3) P1 0.0365(8) 0.0270(7) 0.0325(8) -0.0027(6) 0.0084(6) -0.0046(6) P2 0.0315(7) 0.0331(8) 0.0395(8) 0.0123(7) 0.0001(6) 0.0069(6) N1 0.023(2) 0.035(3) 0.047(3) 0.025(2) 0.005(2) 0.005(2) N2 0.023(2) 0.030(2) 0.037(3) 0.014(2) 0.0023(19) 0.0038(18) C1 0.024(2) 0.026(3) 0.037(3) 0.009(2) 0.004(2) 0.001(2) C2 0.025(3) 0.041(3) 0.050(4) 0.025(3) 0.009(2) 0.006(2) C3 0.022(3) 0.035(3) 0.047(3) 0.019(3) 0.004(2) 0.004(2) C4 0.023(3) 0.042(3) 0.052(4) 0.026(3) 0.005(2) 0.002(2) C5 0.032(3) 0.041(3) 0.052(4) 0.029(3) 0.012(3) 0.005(3) C6 0.044(4) 0.070(5) 0.057(5) 0.013(4) 0.022(3) -0.005(4) C7 0.042(7) 0.079(10) 0.040(7) 0.031(7) 0.012(5) -0.008(7) C8 0.25(4) 0.12(2) 0.085(16) 0.021(15) 0.07(2) -0.05(2) C9 0.022(2) 0.030(3) 0.037(3) 0.009(2) 0.009(2) 0.004(2) C10 0.040(3) 0.022(3) 0.082(5) -0.005(3) 0.025(3) 0.001(2) C11 0.049(4) 0.027(3) 0.094(6) -0.017(4) 0.031(4) -0.010(3) C12 0.035(3) 0.062(5) 0.064(5) -0.019(4) 0.000(3) -0.006(3) C13 0.070(5) 0.039(4) 0.036(3) 0.001(3) 0.012(3) 0.004(3) C14 0.028(6) 0.055(9) 0.055(9) -0.016(7) 0.005(6) -0.016(6) C14A 0.029(7) 0.056(10) 0.035(8) -0.010(7) -0.008(6) -0.015(7) C15 0.050(7) 0.021(5) 0.038(7) 0.004(5) 0.002(6) 0.011(5) C16 0.063(9) 0.016(6) 0.051(8) 0.018(5) 0.003(7) -0.003(5) C15A 0.035(7) 0.019(6) 0.053(9) 0.002(6) -0.006(7) -0.007(6) C16A 0.032(8) 0.012(6) 0.074(14) 0.016(7) -0.010(8) 0.005(5) C17 0.053(9) 0.083(13) 0.028(7) 0.021(7) 0.009(6) 0.016(8) C17A 0.041(9) 0.062(12) 0.046(10) 0.042(9) -0.005(8) 0.003(8) C18 0.035(3) 0.050(4) 0.077(5) -0.004(4) -0.015(3) 0.003(3) Br2 0.0657(5) 0.0526(4) 0.0768(5) -0.0299(4) 0.0371(4) -0.0338(4) O21 0.111(7) 0.152(9) 0.117(7) -0.002(7) 0.019(6) -0.001(7) C21 0.078(7) 0.160(13) 0.100(9) 0.042(9) 0.041(7) -0.002(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.039(5) . ? Pt1 P1 2.2225(15) . ? Pt1 P2 2.2680(15) . ? Pt1 Br1 2.4831(7) . ? P1 C14 1.750(12) . ? P1 C13 1.772(7) . ? P1 C15A 1.791(11) . ? P1 C15 1.893(10) . ? P1 C14A 1.946(14) . ? P2 C17A 1.757(16) . ? P2 C18 1.789(7) . ? P2 C16 1.811(11) . ? P2 C16A 1.872(13) . ? P2 C17 1.900(13) . ? N1 C1 1.342(7) . ? N1 C2 1.396(7) . ? N1 C5 1.472(7) . ? N2 C1 1.348(7) . ? N2 C3 1.389(7) . ? N2 C9 1.469(7) . ? C2 C4 1.385(8) 3_757 ? C2 C3 1.411(8) . ? C3 C4 1.387(8) . ? C4 C2 1.385(8) 3_757 ? C5 C6 1.503(11) . ? C6 C7 1.503(13) . ? C6 C7A 1.5208(10) . ? C7 C8 1.5211(10) . ? C7A C8A 1.5211(10) . ? C9 C10 1.506(9) . ? C10 C11 1.557(9) . ? C11 C12 1.499(11) . ? C15 C16 1.510(18) . ? C15A C16A 1.56(2) . ? O21 C21 1.380(14) . ? O31 C31 1.17(5) . ? O31A C31A 1.68(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 P1 91.21(17) . . ? C1 Pt1 P2 177.13(17) . . ? P1 Pt1 P2 86.15(6) . . ? C1 Pt1 Br1 92.10(17) . . ? P1 Pt1 Br1 176.17(4) . . ? P2 Pt1 Br1 90.58(5) . . ? C14 P1 C13 113.7(6) . . ? C14 P1 C15A 79.4(8) . . ? C13 P1 C15A 113.6(6) . . ? C14 P1 C15 104.7(7) . . ? C13 P1 C15 99.0(5) . . ? C15A P1 C15 25.6(5) . . ? C14 P1 C14A 25.8(6) . . ? C13 P1 C14A 95.8(6) . . ? C15A P1 C14A 103.7(8) . . ? C15 P1 C14A 127.7(7) . . ? C14 P1 Pt1 115.3(5) . . ? C13 P1 Pt1 116.5(2) . . ? C15A P1 Pt1 112.8(5) . . ? C15 P1 Pt1 104.9(4) . . ? C14A P1 Pt1 112.4(5) . . ? C17A P2 C18 118.3(7) . . ? C17A P2 C16 81.4(9) . . ? C18 P2 C16 112.1(6) . . ? C17A P2 C16A 103.0(10) . . ? C18 P2 C16A 98.8(6) . . ? C16 P2 C16A 21.8(5) . . ? C17A P2 C17 27.7(8) . . ? C18 P2 C17 96.9(6) . . ? C16 P2 C17 106.2(8) . . ? C16A P2 C17 126.5(8) . . ? C17A P2 Pt1 113.7(6) . . ? C18 P2 Pt1 115.3(3) . . ? C16 P2 Pt1 111.2(5) . . ? C16A P2 Pt1 104.4(5) . . ? C17 P2 Pt1 114.1(5) . . ? C1 N1 C2 110.4(5) . . ? C1 N1 C5 125.4(5) . . ? C2 N1 C5 124.1(5) . . ? C1 N2 C3 110.3(4) . . ? C1 N2 C9 124.8(4) . . ? C3 N2 C9 124.8(5) . . ? N1 C1 N2 107.6(5) . . ? N1 C1 Pt1 125.9(4) . . ? N2 C1 Pt1 126.4(4) . . ? C4 C2 N1 130.7(5) 3_757 . ? C4 C2 C3 123.7(5) 3_757 . ? N1 C2 C3 105.6(5) . . ? C4 C3 N2 130.8(5) . . ? C4 C3 C2 123.1(5) . . ? N2 C3 C2 106.1(5) . . ? C2 C4 C3 113.2(5) 3_757 . ? N1 C5 C6 112.1(6) . . ? C5 C6 C7 114.5(9) . . ? C5 C6 C7A 123.4(14) . . ? C7 C6 C7A 107.7(15) . . ? C6 C7 C8 111.2(11) . . ? C6 C7A C8A 100(2) . . ? N2 C9 C10 112.0(5) . . ? C9 C10 C11 111.1(5) . . ? C12 C11 C10 113.7(6) . . ? C16 C15 P1 114.0(8) . . ? C15 C16 P2 103.5(8) . . ? C16A C15A P1 103.2(9) . . ? C15A C16A P2 114.0(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.145 _refine_diff_density_min -2.264 _refine_diff_density_rms 0.167 _database_code_depnum_ccdc_archive 'CCDC 947449' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H70 Br2 N4 P4 Pt2, C H4 O, 2(Br)' _chemical_formula_sum 'C37 H74 Br4 N4 O P4 Pt2' _chemical_formula_weight 1424.70 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' 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' 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 _symmetry_space_group_name_hall '-P 2ybc' 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 11.4812(5) _cell_length_b 10.8653(5) _cell_length_c 21.0825(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.9670(10) _cell_angle_gamma 90.00 _cell_volume 2623.7(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 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 8.524 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2942 _exptl_absorpt_correction_T_max 0.6752 _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 = 0.466055 ; _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 28853 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.00 _reflns_number_total 7577 _reflns_number_gt 6316 _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. Some large ADPs for terminal methyl groups are observed which are not untypical for this type of compound. ; _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^)+(0.0471P)^2^+5.4912P] 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 7577 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.22125(5) 0.32935(5) 0.75940(2) 0.03247(12) Uani 1 1 d . . . Pt1 Pt 0.219954(14) 0.199382(15) 0.857739(8) 0.01979(6) Uani 1 1 d . . . P1 P 0.20769(11) 0.07189(11) 0.93951(6) 0.0265(3) Uani 1 1 d . . . P2 P 0.08952(11) 0.07106(11) 0.80453(6) 0.0262(2) Uani 1 1 d . . . C1 C 0.3290(4) 0.3149(4) 0.9099(2) 0.0222(9) Uani 1 1 d . . . N1 N 0.2945(3) 0.4103(3) 0.94631(18) 0.0209(7) Uani 1 1 d . . . N2 N 0.4475(3) 0.3093(3) 0.91820(19) 0.0230(8) Uani 1 1 d . . . C2 C 0.3902(4) 0.4674(4) 0.9773(2) 0.0202(8) Uani 1 1 d . . . C3 C 0.4897(4) 0.4026(4) 0.9592(2) 0.0201(8) Uani 1 1 d . . . C4 C 0.6028(4) 0.4328(4) 0.9808(2) 0.0200(8) Uani 1 1 d . . . H4 H 0.6694 0.3898 0.9682 0.024 Uiso 1 1 calc R . . C5 C 0.1731(4) 0.4532(4) 0.9491(2) 0.0237(9) Uani 1 1 d . . . H5A H 0.1660 0.4983 0.9895 0.028 Uiso 1 1 calc R . . H5B H 0.1207 0.3808 0.9492 0.028 Uiso 1 1 calc R . . C6 C 0.1332(4) 0.5372(4) 0.8936(2) 0.0255(9) Uani 1 1 d . . . H6 H 0.1218 0.4851 0.8545 0.031 Uiso 1 1 calc R . . C7 C 0.2221(5) 0.6356(5) 0.8810(3) 0.0350(11) Uani 1 1 d . . . H7A H 0.2363 0.6868 0.9191 0.052 Uiso 1 1 calc R . . H7B H 0.1923 0.6871 0.8454 0.052 Uiso 1 1 calc R . . H7C H 0.2953 0.5967 0.8705 0.052 Uiso 1 1 calc R . . C8 C 0.0149(5) 0.5914(5) 0.9074(3) 0.0351(11) Uani 1 1 d . . . H8A H 0.0231 0.6395 0.9468 0.053 Uiso 1 1 calc R . . H8B H -0.0412 0.5246 0.9122 0.053 Uiso 1 1 calc R . . H8C H -0.0131 0.6449 0.8721 0.053 Uiso 1 1 calc R . . C9 C 0.5209(4) 0.2209(5) 0.8862(3) 0.0308(11) Uani 1 1 d . . . H9A H 0.4864 0.1378 0.8892 0.037 Uiso 1 1 calc R . . H9B H 0.5992 0.2189 0.9090 0.037 Uiso 1 1 calc R . . C10 C 0.5345(5) 0.2502(8) 0.8172(3) 0.0501(17) Uani 1 1 d . . . H10 H 0.4569 0.2388 0.7934 0.060 Uiso 1 1 calc R . . C11 C 0.5732(8) 0.3800(10) 0.8078(4) 0.080(3) Uani 1 1 d . . . H11A H 0.5151 0.4367 0.8233 0.121 Uiso 1 1 calc R . . H11B H 0.5812 0.3948 0.7624 0.121 Uiso 1 1 calc R . . H11C H 0.6486 0.3935 0.8315 0.121 Uiso 1 1 calc R . . C12 C 0.6203(7) 0.1575(11) 0.7914(4) 0.087(3) Uani 1 1 d . . . H12A H 0.6901 0.1518 0.8208 0.131 Uiso 1 1 calc R . . H12B H 0.6427 0.1849 0.7496 0.131 Uiso 1 1 calc R . . H12C H 0.5830 0.0765 0.7872 0.131 Uiso 1 1 calc R . . C13 C 0.3281(7) -0.0272(9) 0.9562(5) 0.088(3) Uani 1 1 d . . . H13A H 0.3952 0.0209 0.9735 0.132 Uiso 1 1 calc R . . H13B H 0.3480 -0.0682 0.9170 0.132 Uiso 1 1 calc R . . H13C H 0.3079 -0.0891 0.9874 0.132 Uiso 1 1 calc R . . C14 C 0.1800(8) 0.1380(7) 1.0143(3) 0.063(2) Uani 1 1 d . . . H14A H 0.1709 0.0723 1.0454 0.095 Uiso 1 1 calc R . . H14B H 0.1084 0.1871 1.0098 0.095 Uiso 1 1 calc R . . H14C H 0.2457 0.1909 1.0288 0.095 Uiso 1 1 calc R . . C15 C 0.0833(9) -0.0270(8) 0.9224(4) 0.090(4) Uani 1 1 d . . . H15A H 0.0989 -0.1065 0.9444 0.108 Uiso 1 1 calc R . . H15B H 0.0151 0.0107 0.9411 0.108 Uiso 1 1 calc R . . C16 C 0.0528(7) -0.0516(6) 0.8584(3) 0.0572(19) Uani 1 1 d . . . H16A H -0.0324 -0.0667 0.8531 0.069 Uiso 1 1 calc R . . H16B H 0.0927 -0.1279 0.8462 0.069 Uiso 1 1 calc R . . C17 C 0.1401(5) -0.0088(6) 0.7368(3) 0.0437(14) Uani 1 1 d . . . H17A H 0.0755 -0.0559 0.7159 0.066 Uiso 1 1 calc R . . H17B H 0.2034 -0.0650 0.7509 0.066 Uiso 1 1 calc R . . H17C H 0.1688 0.0510 0.7068 0.066 Uiso 1 1 calc R . . C18 C -0.0445(4) 0.1435(5) 0.7768(3) 0.0320(11) Uani 1 1 d . . . H18A H -0.0972 0.0820 0.7566 0.048 Uiso 1 1 calc R . . H18B H -0.0285 0.2077 0.7459 0.048 Uiso 1 1 calc R . . H18C H -0.0812 0.1805 0.8129 0.048 Uiso 1 1 calc R . . C21 C 0.4285(12) 0.2214(12) 0.6286(5) 0.047(3) Uani 0.50 1 d P . . H21A H 0.4769 0.1836 0.6634 0.071 Uiso 0.50 1 calc PR . . H21B H 0.4636 0.2062 0.5882 0.071 Uiso 0.50 1 calc PR . . H21C H 0.3500 0.1854 0.6269 0.071 Uiso 0.50 1 calc PR . . O1 O 0.4217(9) 0.3386(10) 0.6381(5) 0.058(3) Uani 0.50 1 d P . . H1 H 0.4419 0.3763 0.6059 0.088 Uiso 0.50 1 calc PR . . Br2 Br 0.85893(5) 0.24575(5) 0.93659(3) 0.03547(12) 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 0.0354(3) 0.0327(2) 0.0293(3) 0.00556(19) 0.0017(2) 0.0010(2) Pt1 0.01679(8) 0.01948(8) 0.02260(9) -0.00139(6) -0.00224(6) -0.00032(6) P1 0.0256(6) 0.0249(6) 0.0282(6) 0.0040(5) -0.0048(5) -0.0010(5) P2 0.0243(6) 0.0248(6) 0.0283(6) -0.0024(5) -0.0062(5) -0.0029(5) C1 0.019(2) 0.025(2) 0.022(2) 0.0029(17) 0.0026(16) -0.0007(17) N1 0.0157(17) 0.0224(17) 0.0242(19) -0.0009(14) -0.0011(14) 0.0006(14) N2 0.0159(17) 0.0265(19) 0.0263(19) -0.0064(15) -0.0004(14) 0.0001(14) C2 0.0156(19) 0.022(2) 0.023(2) -0.0005(16) 0.0003(15) 0.0018(16) C3 0.020(2) 0.0193(18) 0.022(2) -0.0041(16) 0.0030(16) 0.0007(16) C4 0.0159(19) 0.021(2) 0.023(2) -0.0039(16) 0.0008(15) 0.0007(15) C5 0.0140(19) 0.027(2) 0.030(2) -0.0009(18) -0.0013(16) -0.0001(16) C6 0.023(2) 0.026(2) 0.027(2) -0.0031(18) -0.0022(18) 0.0033(18) C7 0.037(3) 0.032(3) 0.035(3) 0.005(2) -0.004(2) 0.001(2) C8 0.028(3) 0.039(3) 0.038(3) -0.003(2) -0.003(2) 0.009(2) C9 0.021(2) 0.031(2) 0.041(3) -0.016(2) 0.004(2) 0.0019(18) C10 0.028(3) 0.089(5) 0.033(3) -0.019(3) 0.003(2) 0.004(3) C11 0.080(6) 0.118(8) 0.046(4) 0.016(5) 0.023(4) -0.014(6) C12 0.051(4) 0.152(9) 0.057(5) -0.057(6) -0.002(4) 0.036(5) C13 0.055(5) 0.105(7) 0.107(7) 0.076(6) 0.031(5) 0.047(5) C14 0.105(6) 0.049(4) 0.039(4) 0.003(3) 0.025(4) -0.010(4) C15 0.125(8) 0.078(6) 0.061(5) 0.034(4) -0.038(5) -0.076(6) C16 0.061(4) 0.055(4) 0.052(4) 0.022(3) -0.020(3) -0.034(3) C17 0.042(3) 0.040(3) 0.048(4) -0.017(3) -0.006(3) 0.009(3) C18 0.021(2) 0.042(3) 0.032(3) -0.006(2) -0.0019(19) 0.001(2) C21 0.057(8) 0.064(8) 0.019(5) -0.020(5) -0.006(5) 0.033(6) O1 0.057(6) 0.078(7) 0.042(5) -0.004(5) 0.019(5) 0.003(5) Br2 0.0340(3) 0.0391(3) 0.0331(3) -0.0034(2) 0.0014(2) 0.0120(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Pt1 2.5093(5) . ? Pt1 C1 2.040(5) . ? Pt1 P1 2.2235(13) . ? Pt1 P2 2.2831(12) . ? P1 C13 1.768(7) . ? P1 C14 1.781(7) . ? P1 C15 1.804(7) . ? P2 C18 1.790(5) . ? P2 C17 1.801(6) . ? P2 C16 1.819(6) . ? C1 N2 1.361(6) . ? C1 N1 1.364(6) . ? N1 C2 1.385(5) . ? N1 C5 1.475(5) . ? N2 C3 1.398(5) . ? N2 C9 1.472(6) . ? C2 C4 1.398(6) 3_667 ? C2 C3 1.415(6) . ? C3 C4 1.385(6) . ? C4 C2 1.398(6) 3_667 ? C5 C6 1.529(6) . ? C6 C7 1.515(7) . ? C6 C8 1.527(7) . ? C9 C10 1.508(9) . ? C10 C11 1.497(12) . ? C10 C12 1.535(10) . ? C15 C16 1.395(10) . ? C21 O1 1.292(16) . ? 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 91.98(13) . . ? C1 Pt1 P2 176.20(13) . . ? P1 Pt1 P2 85.75(5) . . ? C1 Pt1 Br1 93.49(12) . . ? P1 Pt1 Br1 174.53(3) . . ? P2 Pt1 Br1 88.79(4) . . ? C13 P1 C14 104.7(5) . . ? C13 P1 C15 105.9(5) . . ? C14 P1 C15 103.3(4) . . ? C13 P1 Pt1 116.3(3) . . ? C14 P1 Pt1 117.4(2) . . ? C15 P1 Pt1 107.9(2) . . ? C18 P2 C17 105.7(3) . . ? C18 P2 C16 107.1(3) . . ? C17 P2 C16 104.1(4) . . ? C18 P2 Pt1 114.30(18) . . ? C17 P2 Pt1 116.6(2) . . ? C16 P2 Pt1 108.2(2) . . ? N2 C1 N1 106.8(4) . . ? N2 C1 Pt1 127.7(3) . . ? N1 C1 Pt1 125.4(3) . . ? C1 N1 C2 110.7(4) . . ? C1 N1 C5 125.1(4) . . ? C2 N1 C5 124.1(4) . . ? C1 N2 C3 110.3(4) . . ? C1 N2 C9 124.7(4) . . ? C3 N2 C9 124.9(4) . . ? N1 C2 C4 130.9(4) . 3_667 ? N1 C2 C3 106.2(4) . . ? C4 C2 C3 122.9(4) 3_667 . ? C4 C3 N2 130.7(4) . . ? C4 C3 C2 123.4(4) . . ? N2 C3 C2 106.0(4) . . ? C3 C4 C2 113.8(4) . 3_667 ? N1 C5 C6 113.0(4) . . ? C7 C6 C8 112.3(4) . . ? C7 C6 C5 112.7(4) . . ? C8 C6 C5 107.9(4) . . ? N2 C9 C10 113.9(5) . . ? C11 C10 C9 112.2(5) . . ? C11 C10 C12 111.6(7) . . ? C9 C10 C12 108.4(6) . . ? C16 C15 P1 116.7(6) . . ? C15 C16 P2 114.2(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 2.314 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 947450' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H68 N6 P4 Pt2, 4(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C40 H74 F24 N8 P8 Pt2' _chemical_formula_weight 1761.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6793(7) _cell_length_b 11.7676(7) _cell_length_c 12.7644(7) _cell_angle_alpha 95.7770(10) _cell_angle_beta 96.0150(10) _cell_angle_gamma 113.0340(10) _cell_volume 1586.20(16) _cell_formula_units_Z 1 _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 0.09 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 862 _exptl_absorpt_coefficient_mu 4.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6763 _exptl_absorpt_correction_T_max 0.8715 _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 = 0.696262 ; _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 18755 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9164 _reflns_number_gt 8243 _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^)+(0.0436P)^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 9164 _refine_ls_number_parameters 378 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.431603(10) 0.259130(10) 0.266784(8) 0.01675(4) Uani 1 1 d . . . P2 P 0.62700(7) 0.36489(7) 0.36933(6) 0.01931(15) Uani 1 1 d . . . P1 P 0.46023(8) 0.08608(7) 0.29037(6) 0.01992(15) Uani 1 1 d . . . N1 N 0.1476(2) 0.1077(2) 0.19284(19) 0.0196(5) Uani 1 1 d . . . N2 N 0.2530(2) 0.1311(2) 0.05960(19) 0.0195(5) Uani 1 1 d . . . N3 N 0.4016(2) 0.4189(3) 0.2483(2) 0.0235(5) Uani 1 1 d . . . C1 C 0.2647(3) 0.1579(3) 0.1671(2) 0.0196(6) Uani 1 1 d . . . C2 C 0.0585(3) 0.0481(3) 0.1020(2) 0.0188(5) Uani 1 1 d . . . C3 C 0.1268(3) 0.0629(3) 0.0157(2) 0.0190(6) Uani 1 1 d . . . C4 C 0.0703(3) 0.0164(3) -0.0902(2) 0.0196(6) Uani 1 1 d . . . H4 H 0.1161 0.0280 -0.1484 0.024 Uiso 1 1 calc R . . C5 C 0.1149(3) 0.1260(3) 0.2995(2) 0.0241(6) Uani 1 1 d . . . H5A H 0.1898 0.1467 0.3541 0.029 Uiso 1 1 calc R . . H5B H 0.0480 0.0475 0.3120 0.029 Uiso 1 1 calc R . . C6 C 0.0690(4) 0.2317(4) 0.3104(3) 0.0358(8) Uani 1 1 d . . . H6A H 0.1380 0.3111 0.3024 0.043 Uiso 1 1 calc R . . H6B H -0.0020 0.2135 0.2525 0.043 Uiso 1 1 calc R . . C7 C 0.0264(4) 0.2469(5) 0.4176(3) 0.0457(10) Uani 1 1 d . . . H7A H -0.0461 0.1706 0.4235 0.068 Uiso 1 1 calc R . . H7B H 0.0023 0.3179 0.4232 0.068 Uiso 1 1 calc R . . H7C H 0.0955 0.2618 0.4751 0.068 Uiso 1 1 calc R . . C8 C 0.3571(3) 0.1746(3) -0.0027(2) 0.0240(6) Uani 1 1 d . . . H8A H 0.3294 0.1248 -0.0750 0.029 Uiso 1 1 calc R . . H8B H 0.4290 0.1599 0.0317 0.029 Uiso 1 1 calc R . . C9 C 0.4005(3) 0.3126(4) -0.0121(3) 0.0322(8) Uani 1 1 d . . . H9A H 0.4455 0.3628 0.0581 0.039 Uiso 1 1 calc R . . H9B H 0.4611 0.3332 -0.0633 0.039 Uiso 1 1 calc R . . C10 C 0.2940(4) 0.3498(4) -0.0485(3) 0.0428(9) Uani 1 1 d . . . H10A H 0.2492 0.3012 -0.1184 0.064 Uiso 1 1 calc R . . H10B H 0.3285 0.4391 -0.0541 0.064 Uiso 1 1 calc R . . H10C H 0.2354 0.3332 0.0033 0.064 Uiso 1 1 calc R . . C17 C 0.3691(3) 0.4946(3) 0.2287(3) 0.0276(7) Uani 1 1 d . . . C18 C 0.3249(4) 0.5884(4) 0.2015(3) 0.0410(9) Uani 1 1 d . . . H18A H 0.2950 0.5731 0.1246 0.062 Uiso 1 1 calc R . . H18B H 0.3940 0.6714 0.2211 0.062 Uiso 1 1 calc R . . H18C H 0.2556 0.5842 0.2403 0.062 Uiso 1 1 calc R . . C16 C 0.6286(3) 0.4370(3) 0.5022(3) 0.0278(7) Uani 1 1 d . . . H16A H 0.7132 0.4664 0.5434 0.042 Uiso 1 1 calc R . . H16B H 0.5681 0.3756 0.5377 0.042 Uiso 1 1 calc R . . H16C H 0.6053 0.5079 0.4973 0.042 Uiso 1 1 calc R . . C15 C 0.7382(3) 0.4859(3) 0.3112(3) 0.0307(7) Uani 1 1 d . . . H15A H 0.7079 0.5518 0.3028 0.046 Uiso 1 1 calc R . . H15B H 0.7472 0.4506 0.2412 0.046 Uiso 1 1 calc R . . H15C H 0.8200 0.5213 0.3578 0.046 Uiso 1 1 calc R . . C14 C 0.6940(3) 0.2505(3) 0.3880(3) 0.0269(7) Uani 1 1 d . . . H14A H 0.7336 0.2375 0.3256 0.032 Uiso 1 1 calc R . . H14B H 0.7594 0.2810 0.4523 0.032 Uiso 1 1 calc R . . C13 C 0.5882(3) 0.1277(3) 0.4008(3) 0.0276(7) Uani 1 1 d . . . H13A H 0.5578 0.1373 0.4693 0.033 Uiso 1 1 calc R . . H13B H 0.6197 0.0609 0.4009 0.033 Uiso 1 1 calc R . . C12 C 0.3272(4) -0.0398(3) 0.3236(3) 0.0321(7) Uani 1 1 d . . . H12A H 0.2565 -0.0678 0.2648 0.048 Uiso 1 1 calc R . . H12B H 0.3024 -0.0105 0.3885 0.048 Uiso 1 1 calc R . . H12C H 0.3503 -0.1096 0.3356 0.048 Uiso 1 1 calc R . . C11 C 0.5041(3) 0.0174(3) 0.1774(3) 0.0271(7) Uani 1 1 d . . . H11A H 0.5233 -0.0526 0.1964 0.041 Uiso 1 1 calc R . . H11B H 0.5786 0.0804 0.1566 0.041 Uiso 1 1 calc R . . H11C H 0.4342 -0.0130 0.1177 0.041 Uiso 1 1 calc R . . P3 P 0.30293(9) 0.17163(9) 0.63324(7) 0.02728(18) Uani 1 1 d . . . F1 F 0.4345(2) 0.1627(2) 0.6175(2) 0.0440(6) Uani 1 1 d . . . F2 F 0.2304(3) 0.0556(2) 0.5424(2) 0.0512(6) Uani 1 1 d . . . F3 F 0.3228(3) 0.2636(3) 0.5476(2) 0.0538(7) Uani 1 1 d . . . F4 F 0.1749(2) 0.1823(3) 0.6518(2) 0.0500(6) Uani 1 1 d . . . F5 F 0.2848(3) 0.0789(3) 0.7188(2) 0.0567(7) Uani 1 1 d . . . F6 F 0.3785(3) 0.2885(3) 0.7242(2) 0.0637(8) Uani 1 1 d . . . P4 P 0.19210(10) 0.72972(10) 0.95882(8) 0.0348(2) Uani 1 1 d . . . F7 F 0.1558(4) 0.6884(5) 0.8362(2) 0.1118(17) Uani 1 1 d . . . F8 F 0.0572(2) 0.7298(3) 0.9646(2) 0.0528(7) Uani 1 1 d . . . F9 F 0.1428(3) 0.5900(3) 0.9768(3) 0.0843(11) Uani 1 1 d . . . F10 F 0.3284(3) 0.7291(3) 0.9519(3) 0.0651(8) Uani 1 1 d . . . F11 F 0.2472(4) 0.8713(3) 0.9441(4) 0.1082(17) Uani 1 1 d . . . F12 F 0.2321(3) 0.7698(4) 1.0846(3) 0.0803(11) Uani 1 1 d . . . N21 N 0.8802(4) 0.3701(5) 0.6406(3) 0.0716(14) Uani 1 1 d . . . C21 C 0.9356(4) 0.3451(5) 0.7057(4) 0.0478(11) Uani 1 1 d . . . C22 C 1.0069(4) 0.3129(5) 0.7888(4) 0.0489(11) Uani 1 1 d . . . H22A H 0.9488 0.2487 0.8238 0.073 Uiso 1 1 calc R . . H22B H 1.0567 0.3875 0.8415 0.073 Uiso 1 1 calc R . . H22C H 1.0633 0.2807 0.7573 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01506(6) 0.01904(6) 0.01448(6) -0.00038(4) -0.00262(4) 0.00710(4) P2 0.0165(3) 0.0206(4) 0.0190(3) -0.0006(3) -0.0025(3) 0.0077(3) P1 0.0210(4) 0.0194(4) 0.0184(3) 0.0002(3) -0.0001(3) 0.0086(3) N1 0.0161(11) 0.0259(13) 0.0138(11) -0.0012(9) -0.0024(9) 0.0075(10) N2 0.0139(11) 0.0252(13) 0.0156(11) -0.0009(9) -0.0003(9) 0.0055(10) N3 0.0200(12) 0.0272(14) 0.0213(12) 0.0006(10) -0.0023(10) 0.0096(11) C1 0.0179(13) 0.0220(14) 0.0175(13) 0.0010(11) -0.0007(11) 0.0080(11) C2 0.0181(13) 0.0228(14) 0.0127(12) -0.0009(10) -0.0020(10) 0.0075(11) C3 0.0152(13) 0.0248(15) 0.0153(13) -0.0001(11) 0.0001(10) 0.0076(11) C4 0.0175(13) 0.0263(15) 0.0143(12) 0.0003(11) 0.0012(10) 0.0092(12) C5 0.0202(14) 0.0375(18) 0.0117(13) -0.0023(12) 0.0007(11) 0.0106(13) C6 0.038(2) 0.050(2) 0.0262(17) -0.0002(16) 0.0031(15) 0.0269(18) C7 0.041(2) 0.063(3) 0.038(2) -0.005(2) 0.0092(18) 0.029(2) C8 0.0158(13) 0.0348(18) 0.0185(14) 0.0022(12) 0.0038(11) 0.0074(13) C9 0.0272(17) 0.038(2) 0.0254(16) 0.0078(14) 0.0059(13) 0.0059(15) C10 0.051(3) 0.041(2) 0.040(2) 0.0133(18) 0.0082(19) 0.020(2) C17 0.0295(17) 0.0334(18) 0.0250(16) 0.0054(13) 0.0040(13) 0.0180(15) C18 0.049(2) 0.045(2) 0.045(2) 0.0131(18) 0.0071(19) 0.035(2) C16 0.0259(16) 0.0324(18) 0.0211(15) -0.0026(13) -0.0021(12) 0.0104(14) C15 0.0260(17) 0.0280(17) 0.0345(18) 0.0033(14) 0.0053(14) 0.0074(14) C14 0.0219(15) 0.0302(17) 0.0292(16) -0.0051(13) -0.0074(12) 0.0163(13) C13 0.0311(17) 0.0287(17) 0.0237(15) 0.0005(13) -0.0066(13) 0.0165(14) C12 0.0340(19) 0.0265(17) 0.0338(18) 0.0072(14) 0.0088(15) 0.0089(15) C11 0.0330(17) 0.0260(16) 0.0236(15) -0.0018(12) 0.0040(13) 0.0147(14) P3 0.0356(5) 0.0286(4) 0.0220(4) 0.0023(3) 0.0044(3) 0.0181(4) F1 0.0431(13) 0.0421(13) 0.0584(15) 0.0113(12) 0.0196(12) 0.0257(11) F2 0.0575(16) 0.0398(14) 0.0415(14) -0.0119(11) 0.0070(12) 0.0086(12) F3 0.0557(16) 0.0508(16) 0.0629(17) 0.0352(14) 0.0094(13) 0.0237(13) F4 0.0422(14) 0.0622(17) 0.0565(16) 0.0043(13) 0.0093(12) 0.0336(13) F5 0.0650(18) 0.080(2) 0.0490(15) 0.0397(15) 0.0257(13) 0.0430(16) F6 0.0594(18) 0.0632(18) 0.0570(17) -0.0304(14) -0.0123(14) 0.0274(15) P4 0.0403(5) 0.0355(5) 0.0343(5) 0.0084(4) 0.0101(4) 0.0199(4) F7 0.130(3) 0.220(5) 0.0355(16) 0.000(2) 0.0084(19) 0.130(4) F8 0.0452(14) 0.0696(18) 0.0539(16) 0.0180(14) 0.0162(12) 0.0300(14) F9 0.060(2) 0.0439(17) 0.136(3) 0.0267(19) -0.011(2) 0.0109(15) F10 0.0487(16) 0.070(2) 0.097(2) 0.0271(18) 0.0265(16) 0.0392(15) F11 0.090(3) 0.067(2) 0.219(5) 0.084(3) 0.091(3) 0.055(2) F12 0.063(2) 0.110(3) 0.0518(18) -0.0184(18) -0.0024(15) 0.029(2) N21 0.055(3) 0.121(4) 0.046(2) 0.004(3) -0.004(2) 0.049(3) C21 0.031(2) 0.071(3) 0.039(2) 0.000(2) 0.0098(18) 0.019(2) C22 0.033(2) 0.066(3) 0.043(2) 0.013(2) 0.0058(18) 0.013(2) _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 2.049(3) . ? Pt1 N3 2.073(3) . ? Pt1 P1 2.2326(8) . ? Pt1 P2 2.3007(8) . ? P2 C15 1.798(4) . ? P2 C16 1.813(3) . ? P2 C14 1.826(3) . ? P1 C11 1.800(3) . ? P1 C12 1.804(4) . ? P1 C13 1.818(3) . ? N1 C1 1.352(4) . ? N1 C2 1.390(3) . ? N1 C5 1.470(4) . ? N2 C1 1.356(4) . ? N2 C3 1.394(4) . ? N2 C8 1.472(4) . ? N3 C17 1.136(4) . ? C2 C4 1.378(4) 2 ? C2 C3 1.412(4) . ? C3 C4 1.394(4) . ? C4 C2 1.378(4) 2 ? C5 C6 1.536(5) . ? C6 C7 1.522(5) . ? C8 C9 1.523(5) . ? C9 C10 1.517(5) . ? C17 C18 1.447(5) . ? C14 C13 1.528(5) . ? P3 F2 1.580(3) . ? P3 F3 1.586(3) . ? P3 F4 1.588(3) . ? P3 F6 1.591(3) . ? P3 F5 1.593(3) . ? P3 F1 1.613(2) . ? P4 F7 1.553(3) . ? P4 F9 1.565(3) . ? P4 F11 1.573(3) . ? P4 F8 1.586(3) . ? P4 F12 1.593(3) . ? P4 F10 1.607(3) . ? N21 C21 1.132(6) . ? C21 C22 1.450(6) . ? 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 N3 88.21(11) . . ? C1 Pt1 P1 91.57(9) . . ? N3 Pt1 P1 178.32(8) . . ? C1 Pt1 P2 175.11(8) . . ? N3 Pt1 P2 94.70(8) . . ? P1 Pt1 P2 85.64(3) . . ? C15 P2 C16 105.60(17) . . ? C15 P2 C14 106.57(17) . . ? C16 P2 C14 105.85(16) . . ? C15 P2 Pt1 115.25(12) . . ? C16 P2 Pt1 115.85(12) . . ? C14 P2 Pt1 106.99(11) . . ? C11 P1 C12 105.06(17) . . ? C11 P1 C13 106.91(16) . . ? C12 P1 C13 106.53(17) . . ? C11 P1 Pt1 114.40(12) . . ? C12 P1 Pt1 115.71(13) . . ? C13 P1 Pt1 107.65(11) . . ? C1 N1 C2 110.7(2) . . ? C1 N1 C5 125.4(2) . . ? C2 N1 C5 123.5(2) . . ? C1 N2 C3 110.1(2) . . ? C1 N2 C8 125.2(2) . . ? C3 N2 C8 124.6(2) . . ? C17 N3 Pt1 169.8(3) . . ? N1 C1 N2 107.2(2) . . ? N1 C1 Pt1 128.2(2) . . ? N2 C1 Pt1 124.6(2) . . ? C4 C2 N1 130.8(3) 2 . ? C4 C2 C3 123.3(3) 2 . ? N1 C2 C3 105.8(3) . . ? C4 C3 N2 130.4(3) . . ? C4 C3 C2 123.4(3) . . ? N2 C3 C2 106.2(2) . . ? C2 C4 C3 113.2(3) 2 . ? N1 C5 C6 110.8(3) . . ? C7 C6 C5 111.8(3) . . ? N2 C8 C9 112.6(3) . . ? C10 C9 C8 113.7(3) . . ? N3 C17 C18 178.4(4) . . ? C13 C14 P2 108.4(2) . . ? C14 C13 P1 108.7(2) . . ? F2 P3 F3 90.38(16) . . ? F2 P3 F4 91.14(15) . . ? F3 P3 F4 90.84(15) . . ? F2 P3 F6 178.92(16) . . ? F3 P3 F6 89.49(18) . . ? F4 P3 F6 89.93(15) . . ? F2 P3 F5 89.49(16) . . ? F3 P3 F5 179.12(16) . . ? F4 P3 F5 90.04(15) . . ? F6 P3 F5 90.62(17) . . ? F2 P3 F1 90.24(14) . . ? F3 P3 F1 89.70(14) . . ? F4 P3 F1 178.52(15) . . ? F6 P3 F1 88.69(15) . . ? F5 P3 F1 89.43(14) . . ? F7 P4 F9 90.7(3) . . ? F7 P4 F11 90.9(3) . . ? F9 P4 F11 177.5(2) . . ? F7 P4 F8 89.97(18) . . ? F9 P4 F8 90.83(18) . . ? F11 P4 F8 91.07(17) . . ? F7 P4 F12 178.2(2) . . ? F9 P4 F12 88.3(2) . . ? F11 P4 F12 90.0(3) . . ? F8 P4 F12 91.57(17) . . ? F7 P4 F10 89.52(19) . . ? F9 P4 F10 89.12(18) . . ? F11 P4 F10 88.99(17) . . ? F8 P4 F10 179.49(19) . . ? F12 P4 F10 88.94(18) . . ? N21 C21 C22 179.8(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.053 _refine_diff_density_min -0.960 _refine_diff_density_rms 0.143 _database_code_depnum_ccdc_archive 'CCDC 947451' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H78 N8 P4 Pt2, 4(F6 P)' _chemical_formula_sum 'C52 H78 F24 N8 P8 Pt2' _chemical_formula_weight 1909.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-C 2yc' 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 29.1083(11) _cell_length_b 10.4000(4) _cell_length_c 24.5042(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.2170(10) _cell_angle_gamma 90.00 _cell_volume 7250.1(5) _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 prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3752 _exptl_absorpt_coefficient_mu 4.133 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5953 _exptl_absorpt_correction_T_max 0.7896 _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 = 0.687153 ; _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 41939 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 30.50 _reflns_number_total 11040 _reflns_number_gt 9155 _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. A large solvent accessible void is present due to the odd shape of the molecule. The compound does not contain any solvent of crystallizaton so the void remains empty. ; _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^)+(0.0497P)^2^+12.7847P] 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 11040 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.325631(4) 0.431241(12) 0.380712(5) 0.02231(4) Uani 1 1 d . . . P2 P 0.24720(3) 0.42286(9) 0.34038(4) 0.02701(17) Uani 1 1 d . . . P1 P 0.30199(3) 0.48303(9) 0.45920(4) 0.02605(17) Uani 1 1 d . . . C1 C 0.39432(11) 0.4495(3) 0.42198(13) 0.0234(6) Uani 1 1 d . . . N1 N 0.42139(9) 0.3624(3) 0.45537(11) 0.0232(5) Uani 1 1 d . . . N2 N 0.41918(9) 0.5601(2) 0.42564(12) 0.0229(5) Uani 1 1 d . . . C2 C 0.46385(11) 0.4178(3) 0.48178(14) 0.0234(6) Uani 1 1 d . . . C3 C 0.46274(11) 0.5454(3) 0.46253(13) 0.0222(6) Uani 1 1 d . . . C4 C 0.49874(11) 0.6325(3) 0.47998(13) 0.0238(6) Uani 1 1 d . . . H4 H 0.4978 0.7186 0.4669 0.029 Uiso 1 1 calc R . . C5 C 0.41073(12) 0.2253(3) 0.46069(15) 0.0276(7) Uani 1 1 d . . . H5A H 0.3775 0.2090 0.4428 0.033 Uiso 1 1 calc R . . H5B H 0.4151 0.2027 0.5007 0.033 Uiso 1 1 calc R . . C6 C 0.44245(13) 0.1404(3) 0.43347(16) 0.0330(7) Uani 1 1 d . . . H6A H 0.4323 0.1457 0.3923 0.040 Uiso 1 1 calc R . . H6B H 0.4752 0.1717 0.4440 0.040 Uiso 1 1 calc R . . C7 C 0.44026(18) 0.0024(4) 0.4519(3) 0.0600(14) Uani 1 1 d . . . H7A H 0.4534 -0.0040 0.4921 0.090 Uiso 1 1 calc R . . H7B H 0.4585 -0.0518 0.4316 0.090 Uiso 1 1 calc R . . H7C H 0.4075 -0.0265 0.4440 0.090 Uiso 1 1 calc R . . C8 C 0.40419(11) 0.6773(3) 0.39406(14) 0.0262(6) Uani 1 1 d . . . H8A H 0.4094 0.7518 0.4198 0.031 Uiso 1 1 calc R . . H8B H 0.3701 0.6719 0.3778 0.031 Uiso 1 1 calc R . . C9 C 0.43035(14) 0.6991(4) 0.34759(15) 0.0373(8) Uani 1 1 d . . . H9A H 0.4271 0.6221 0.3233 0.045 Uiso 1 1 calc R . . H9B H 0.4642 0.7116 0.3639 0.045 Uiso 1 1 calc R . . C10 C 0.4114(2) 0.8165(5) 0.3126(2) 0.0605(14) Uani 1 1 d . . . H10A H 0.3784 0.8019 0.2945 0.091 Uiso 1 1 calc R . . H10B H 0.4298 0.8306 0.2840 0.091 Uiso 1 1 calc R . . H10C H 0.4137 0.8923 0.3367 0.091 Uiso 1 1 calc R . . C15 C 0.22528(15) 0.2879(4) 0.29616(18) 0.0425(9) Uani 1 1 d . . . H15A H 0.1909 0.2873 0.2888 0.064 Uiso 1 1 calc R . . H15B H 0.2374 0.2078 0.3149 0.064 Uiso 1 1 calc R . . H15C H 0.2357 0.2953 0.2608 0.064 Uiso 1 1 calc R . . N3 N 0.34662(9) 0.3798(3) 0.30461(12) 0.0265(6) Uani 1 1 d . . . C16 C 0.22672(16) 0.5616(4) 0.29796(18) 0.0416(9) Uani 1 1 d . . . H16A H 0.2415 0.5633 0.2655 0.062 Uiso 1 1 calc R . . H16B H 0.2351 0.6400 0.3201 0.062 Uiso 1 1 calc R . . H16C H 0.1925 0.5570 0.2852 0.062 Uiso 1 1 calc R . . C14 C 0.21543(12) 0.4252(4) 0.39660(17) 0.0369(9) Uani 1 1 d . . . H14A H 0.1825 0.4522 0.3820 0.044 Uiso 1 1 calc R . . H14B H 0.2151 0.3380 0.4127 0.044 Uiso 1 1 calc R . . C13 C 0.23948(13) 0.5190(4) 0.44151(16) 0.0371(8) Uani 1 1 d . . . H13A H 0.2259 0.5108 0.4751 0.045 Uiso 1 1 calc R . . H13B H 0.2345 0.6084 0.4276 0.045 Uiso 1 1 calc R . . C12 C 0.30870(15) 0.3515(4) 0.50813(16) 0.0411(9) Uani 1 1 d . . . H12A H 0.3421 0.3392 0.5247 0.062 Uiso 1 1 calc R . . H12B H 0.2959 0.2728 0.4887 0.062 Uiso 1 1 calc R . . H12C H 0.2917 0.3710 0.5376 0.062 Uiso 1 1 calc R . . C11 C 0.32968(15) 0.6191(5) 0.49824(17) 0.0427(9) Uani 1 1 d . . . H11A H 0.3150 0.6347 0.5301 0.064 Uiso 1 1 calc R . . H11B H 0.3258 0.6952 0.4741 0.064 Uiso 1 1 calc R . . H11C H 0.3632 0.6014 0.5117 0.064 Uiso 1 1 calc R . . C17 C 0.36170(14) 0.2661(4) 0.29789(16) 0.0381(8) Uani 1 1 d . . . H17 H 0.3602 0.2021 0.3251 0.046 Uiso 1 1 calc R . . C18 C 0.38030(15) 0.2339(4) 0.25154(17) 0.0400(9) Uani 1 1 d . . . H18 H 0.3908 0.1490 0.2468 0.048 Uiso 1 1 calc R . . C19 C 0.38307(14) 0.3296(4) 0.21225(16) 0.0365(8) Uani 1 1 d . . . C20 C 0.36700(15) 0.4521(4) 0.22133(17) 0.0392(9) Uani 1 1 d . . . H20 H 0.3682 0.5194 0.1955 0.047 Uiso 1 1 calc R . . C21 C 0.34928(14) 0.4745(4) 0.26825(16) 0.0367(8) Uani 1 1 d . . . H21 H 0.3388 0.5584 0.2750 0.044 Uiso 1 1 calc R . . C22 C 0.40289(15) 0.3019(4) 0.16210(17) 0.0392(8) Uani 1 1 d . . . C23 C 0.3947(2) 0.1872(5) 0.1338(2) 0.0569(13) Uani 1 1 d . . . H23 H 0.3760 0.1227 0.1460 0.068 Uiso 1 1 calc R . . C24 C 0.4138(2) 0.1664(5) 0.0871(2) 0.0620(14) Uani 1 1 d . . . H24 H 0.4080 0.0864 0.0682 0.074 Uiso 1 1 calc R . . N4 N 0.43989(15) 0.2529(4) 0.06772(17) 0.0529(10) Uani 1 1 d . . . C25 C 0.44744(17) 0.3641(5) 0.0955(2) 0.0499(11) Uani 1 1 d . . . H25 H 0.4661 0.4274 0.0825 0.060 Uiso 1 1 calc R . . C26 C 0.42961(17) 0.3920(5) 0.1421(2) 0.0467(10) Uani 1 1 d . . . H26 H 0.4358 0.4729 0.1601 0.056 Uiso 1 1 calc R . . P3 P 0.08331(4) 0.71191(12) 0.86406(5) 0.0454(3) Uani 1 1 d . . . F1 F 0.09608(15) 0.6036(3) 0.82406(13) 0.0855(12) Uani 1 1 d . . . F2 F 0.12891(11) 0.7893(3) 0.85740(14) 0.0703(9) Uani 1 1 d . . . F3 F 0.11420(9) 0.6363(3) 0.91613(10) 0.0476(6) Uani 1 1 d . . . F4 F 0.05326(14) 0.7887(3) 0.81301(14) 0.0863(11) Uani 1 1 d . . . F5 F 0.07259(13) 0.8204(3) 0.90535(14) 0.0742(10) Uani 1 1 d . . . F6 F 0.03872(12) 0.6342(4) 0.8735(2) 0.1080(15) Uani 1 1 d . . . P4 P 0.28168(4) 0.05475(11) 0.88403(5) 0.0407(2) Uani 1 1 d . . . F7 F 0.29794(13) 0.1894(3) 0.86417(16) 0.0771(10) Uani 1 1 d . . . F8 F 0.31890(15) 0.0696(3) 0.94115(16) 0.0903(13) Uani 1 1 d . . . F9 F 0.24542(13) 0.0413(4) 0.82640(15) 0.0798(10) Uani 1 1 d . . . F10 F 0.31895(14) -0.0184(4) 0.85743(17) 0.0878(11) Uani 1 1 d . . . F11 F 0.26593(19) -0.0789(4) 0.90421(18) 0.1041(16) Uani 1 1 d . . . F12 F 0.24454(13) 0.1263(5) 0.91106(18) 0.1016(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 Pt1 0.01899(6) 0.02771(7) 0.02082(6) 0.00106(5) 0.00552(4) -0.00301(4) P2 0.0211(4) 0.0332(4) 0.0256(4) 0.0029(3) 0.0024(3) -0.0036(3) P1 0.0225(4) 0.0342(4) 0.0224(4) 0.0017(3) 0.0067(3) -0.0005(3) C1 0.0237(14) 0.0261(15) 0.0220(14) 0.0001(11) 0.0085(12) -0.0010(11) N1 0.0197(12) 0.0214(13) 0.0284(13) -0.0002(10) 0.0046(10) -0.0015(10) N2 0.0185(11) 0.0246(13) 0.0259(13) 0.0026(10) 0.0051(10) 0.0001(10) C2 0.0208(14) 0.0236(15) 0.0268(15) -0.0005(12) 0.0074(12) -0.0015(11) C3 0.0175(13) 0.0247(15) 0.0246(14) 0.0028(11) 0.0047(11) 0.0013(11) C4 0.0212(14) 0.0208(14) 0.0303(16) 0.0008(12) 0.0072(12) -0.0012(11) C5 0.0270(15) 0.0230(15) 0.0333(17) 0.0009(13) 0.0077(13) -0.0053(12) C6 0.0318(17) 0.0274(17) 0.040(2) -0.0033(14) 0.0080(15) 0.0017(14) C7 0.048(3) 0.031(2) 0.102(4) 0.000(2) 0.019(3) 0.0019(19) C8 0.0234(14) 0.0259(16) 0.0283(16) 0.0065(12) 0.0033(12) 0.0013(12) C9 0.0384(19) 0.045(2) 0.0294(18) 0.0088(16) 0.0086(15) -0.0064(17) C10 0.073(3) 0.065(3) 0.042(2) 0.025(2) 0.008(2) -0.003(3) C15 0.038(2) 0.041(2) 0.044(2) -0.0055(18) -0.0014(17) -0.0067(17) N3 0.0197(12) 0.0326(15) 0.0283(14) 0.0033(12) 0.0073(10) -0.0042(11) C16 0.040(2) 0.044(2) 0.038(2) 0.0098(17) 0.0019(17) 0.0033(17) C14 0.0204(15) 0.054(2) 0.037(2) 0.0080(17) 0.0085(14) -0.0027(15) C13 0.0265(17) 0.055(2) 0.0319(18) 0.0013(17) 0.0101(14) 0.0039(16) C12 0.046(2) 0.051(2) 0.0312(19) 0.0131(17) 0.0184(17) 0.0060(18) C11 0.043(2) 0.054(2) 0.034(2) -0.0124(18) 0.0126(17) -0.0098(19) C17 0.040(2) 0.044(2) 0.0321(18) 0.0053(16) 0.0123(16) -0.0118(17) C18 0.046(2) 0.034(2) 0.044(2) 0.0020(16) 0.0198(18) -0.0018(17) C19 0.0370(19) 0.041(2) 0.0348(19) -0.0020(16) 0.0150(15) -0.0076(16) C20 0.045(2) 0.042(2) 0.034(2) 0.0059(16) 0.0158(17) -0.0004(17) C21 0.039(2) 0.041(2) 0.0325(19) -0.0006(16) 0.0112(16) 0.0031(16) C22 0.043(2) 0.042(2) 0.037(2) 0.0001(17) 0.0181(17) -0.0011(17) C23 0.081(4) 0.042(2) 0.061(3) -0.008(2) 0.046(3) -0.014(2) C24 0.088(4) 0.049(3) 0.061(3) -0.012(2) 0.044(3) -0.008(3) N4 0.063(3) 0.053(2) 0.053(2) -0.0004(18) 0.035(2) 0.0021(19) C25 0.056(3) 0.052(3) 0.051(3) 0.000(2) 0.032(2) -0.003(2) C26 0.052(3) 0.047(2) 0.047(2) -0.001(2) 0.024(2) -0.005(2) P3 0.0418(6) 0.0504(6) 0.0440(6) 0.0043(5) 0.0091(5) 0.0125(5) F1 0.134(3) 0.068(2) 0.0456(17) -0.0086(15) -0.0014(19) 0.036(2) F2 0.0629(19) 0.068(2) 0.088(2) 0.0300(17) 0.0345(17) 0.0112(15) F3 0.0487(14) 0.0529(15) 0.0436(14) 0.0085(12) 0.0153(11) 0.0125(12) F4 0.100(3) 0.079(2) 0.065(2) 0.0109(18) -0.0148(19) 0.035(2) F5 0.101(3) 0.067(2) 0.0640(19) 0.0072(15) 0.0395(18) 0.0389(18) F6 0.0429(18) 0.089(3) 0.185(5) 0.036(3) 0.008(2) -0.0035(18) P4 0.0409(6) 0.0460(6) 0.0382(5) -0.0094(4) 0.0152(4) -0.0076(4) F7 0.079(2) 0.0562(19) 0.096(3) 0.0024(17) 0.0181(19) -0.0221(17) F8 0.088(3) 0.104(3) 0.064(2) -0.0200(19) -0.017(2) 0.012(2) F9 0.068(2) 0.102(3) 0.060(2) -0.0121(18) -0.0085(16) -0.0140(19) F10 0.093(3) 0.094(3) 0.087(3) -0.013(2) 0.044(2) 0.033(2) F11 0.159(4) 0.078(3) 0.084(3) 0.007(2) 0.044(3) -0.050(3) F12 0.072(2) 0.142(4) 0.104(3) -0.036(3) 0.049(2) 0.013(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 Pt1 C1 2.049(3) . ? Pt1 N3 2.149(3) . ? Pt1 P1 2.2411(9) . ? Pt1 P2 2.2894(9) . ? P2 C16 1.805(4) . ? P2 C15 1.806(4) . ? P2 C14 1.815(4) . ? P1 C11 1.800(4) . ? P1 C12 1.802(4) . ? P1 C13 1.818(4) . ? C1 N2 1.352(4) . ? C1 N1 1.356(4) . ? N1 C2 1.393(4) . ? N1 C5 1.471(4) . ? N2 C3 1.401(4) . ? N2 C8 1.460(4) . ? C2 C4 1.380(4) 5_666 ? C2 C3 1.406(4) . ? C3 C4 1.382(4) . ? C4 C2 1.380(4) 5_666 ? C5 C6 1.529(5) . ? C6 C7 1.510(6) . ? C8 C9 1.515(5) . ? C9 C10 1.527(6) . ? N3 C17 1.284(5) . ? N3 C21 1.341(5) . ? C14 C13 1.526(6) . ? C17 C18 1.399(5) . ? C18 C19 1.399(5) . ? C19 C20 1.391(6) . ? C19 C22 1.492(5) . ? C20 C21 1.376(5) . ? C22 C26 1.373(6) . ? C22 C23 1.375(6) . ? C23 C24 1.393(6) . ? C24 N4 1.328(6) . ? N4 C25 1.335(6) . ? C25 C26 1.381(6) . ? P3 F4 1.582(3) . ? P3 F6 1.587(4) . ? P3 F1 1.588(3) . ? P3 F5 1.590(3) . ? P3 F2 1.590(3) . ? P3 F3 1.603(3) . ? P4 F12 1.570(3) . ? P4 F10 1.575(3) . ? P4 F11 1.576(3) . ? P4 F9 1.580(3) . ? P4 F8 1.586(4) . ? P4 F7 1.588(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 N3 91.40(11) . . ? C1 Pt1 P1 89.94(9) . . ? N3 Pt1 P1 178.61(7) . . ? C1 Pt1 P2 174.93(9) . . ? N3 Pt1 P2 93.24(8) . . ? P1 Pt1 P2 85.43(3) . . ? C16 P2 C15 104.1(2) . . ? C16 P2 C14 105.5(2) . . ? C15 P2 C14 107.1(2) . . ? C16 P2 Pt1 113.33(15) . . ? C15 P2 Pt1 118.82(15) . . ? C14 P2 Pt1 107.08(13) . . ? C11 P1 C12 105.6(2) . . ? C11 P1 C13 106.1(2) . . ? C12 P1 C13 106.09(19) . . ? C11 P1 Pt1 117.44(13) . . ? C12 P1 Pt1 112.27(14) . . ? C13 P1 Pt1 108.57(13) . . ? N2 C1 N1 107.1(3) . . ? N2 C1 Pt1 124.4(2) . . ? N1 C1 Pt1 128.2(2) . . ? C1 N1 C2 110.5(3) . . ? C1 N1 C5 126.5(3) . . ? C2 N1 C5 122.9(3) . . ? C1 N2 C3 110.4(3) . . ? C1 N2 C8 125.4(3) . . ? C3 N2 C8 124.1(3) . . ? C4 C2 N1 130.8(3) 5_666 . ? C4 C2 C3 122.9(3) 5_666 . ? N1 C2 C3 106.2(3) . . ? C4 C3 N2 130.6(3) . . ? C4 C3 C2 123.5(3) . . ? N2 C3 C2 105.8(3) . . ? C2 C4 C3 113.5(3) 5_666 . ? N1 C5 C6 111.3(3) . . ? C7 C6 C5 110.5(3) . . ? N2 C8 C9 112.4(3) . . ? C8 C9 C10 111.2(4) . . ? C17 N3 C21 121.4(3) . . ? C17 N3 Pt1 120.5(2) . . ? C21 N3 Pt1 117.4(3) . . ? C13 C14 P2 109.0(2) . . ? C14 C13 P1 108.9(3) . . ? N3 C17 C18 121.7(4) . . ? C17 C18 C19 118.5(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 C22 120.7(4) . . ? C18 C19 C22 121.2(4) . . ? C21 C20 C19 119.2(4) . . ? N3 C21 C20 121.0(4) . . ? C26 C22 C23 117.6(4) . . ? C26 C22 C19 120.7(4) . . ? C23 C22 C19 121.7(4) . . ? C22 C23 C24 119.4(4) . . ? N4 C24 C23 123.2(5) . . ? C24 N4 C25 116.7(4) . . ? N4 C25 C26 123.5(4) . . ? C22 C26 C25 119.5(4) . . ? F4 P3 F6 92.3(2) . . ? F4 P3 F1 91.85(19) . . ? F6 P3 F1 92.0(3) . . ? F4 P3 F5 89.73(18) . . ? F6 P3 F5 89.5(2) . . ? F1 P3 F5 177.8(2) . . ? F4 P3 F2 89.8(2) . . ? F6 P3 F2 177.5(2) . . ? F1 P3 F2 89.2(2) . . ? F5 P3 F2 89.2(2) . . ? F4 P3 F3 179.0(2) . . ? F6 P3 F3 88.41(19) . . ? F1 P3 F3 88.76(16) . . ? F5 P3 F3 89.65(16) . . ? F2 P3 F3 89.42(16) . . ? F12 P4 F10 179.3(3) . . ? F12 P4 F11 90.8(3) . . ? F10 P4 F11 88.6(3) . . ? F12 P4 F9 91.7(2) . . ? F10 P4 F9 88.6(2) . . ? F11 P4 F9 91.1(2) . . ? F12 P4 F8 89.1(2) . . ? F10 P4 F8 90.6(2) . . ? F11 P4 F8 89.9(2) . . ? F9 P4 F8 178.7(2) . . ? F12 P4 F7 89.3(2) . . ? F10 P4 F7 91.3(2) . . ? F11 P4 F7 179.5(3) . . ? F9 P4 F7 89.5(2) . . ? F8 P4 F7 89.6(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.548 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.146 # end of data set CCDC 947452 _database_code_depnum_ccdc_archive 'CCDC 947452'