# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_year ? _journal_page_first ? _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Heaton, B.' 'Berkei, Michael' 'Bickley, Jamie F.' 'Steiner, Alexander' _publ_contact_author_name 'Prof B Heaton' _publ_contact_author_address ; Prof B Heaton Department of Chemistry University of Liverpool PO Box 147 Liverpool L69 7ZD UNITED KINGDOM ; _publ_contact_author_email 'BTH@LIVERPOOL.AC.UK' _publ_section_title ; Polymeric Anionic Networks using Dibromine as a Crosslinker; the Preparation and Crystal Structure of [(C4H9)4N]2[Pt2Br10] (Br2)7 and [(C4H9)4N]2[PtBr4CI2] (Br2)6 ; data_mibe7m _database_code_CSD 187953 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 Br16 Cl2 N2 Pt' _chemical_formula_weight 2029.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.604(6) _cell_length_b 15.530(8) _cell_length_c 17.764(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.671(11) _cell_angle_gamma 90.00 _cell_volume 3033(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3479 _cell_measurement_theta_min 4.555 _cell_measurement_theta_max 48.038 _exptl_crystal_description Needle _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 12.966 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1122 _exptl_absorpt_correction_T_max 0.4236 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12055 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.1079 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 22.49 _reflns_number_total 3949 _reflns_number_gt 3367 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+126.5514P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3949 _refine_ls_number_parameters 243 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2059 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.58319(19) 0.14625(14) 0.01469(15) 0.0560(6) Uani 1 1 d . . . Br2 Br 0.70993(16) -0.05610(13) 0.03603(13) 0.0442(6) Uani 1 1 d . . . Br3 Br 0.9189(5) 0.2191(5) 0.2974(3) 0.078(2) Uiso 0.641(16) 1 d PD A 1 Br3' Br 0.9536(10) 0.1728(11) 0.2983(6) 0.101(5) Uiso 0.359(16) 1 d PD A 2 Br4 Br 0.7877(3) 0.1595(3) 0.18424(18) 0.1026(12) Uani 1 1 d D . . Br5 Br 0.72253(18) 0.76311(14) 0.04844(10) 0.0421(5) Uani 1 1 d D . . Br6 Br 0.7480(3) 0.61245(17) 0.05690(14) 0.0726(8) Uani 1 1 d D . . Br7 Br 1.0182(2) 0.18972(19) 0.97235(15) 0.0670(7) Uani 1 1 d D . . Br8 Br 0.8274(2) 0.16045(17) 0.98292(15) 0.0649(7) Uani 1 1 d D . . C1 C 0.7195(17) 0.6906(14) 0.7667(11) 0.042(5) Uani 1 1 d . C . H1A H 0.7602 0.7159 0.7307 0.050 Uiso 1 1 calc R . . H1B H 0.6734 0.6396 0.7395 0.050 Uiso 1 1 calc R . . C2 C 0.819(2) 0.6595(17) 0.8424(12) 0.061(6) Uani 1 1 d . . . H2A H 0.8634 0.7098 0.8719 0.073 Uiso 1 1 calc R . . H2B H 0.7801 0.6292 0.8771 0.073 Uiso 1 1 calc R . . C3 C 0.905(2) 0.6004(19) 0.8220(14) 0.073(8) Uani 1 1 d . . . H3A H 0.8595 0.5505 0.7925 0.088 Uiso 1 1 calc R . . H3B H 0.9419 0.6310 0.7863 0.088 Uiso 1 1 calc R . . C4 C 1.003(3) 0.569(2) 0.8912(16) 0.091(10) Uani 1 1 d . . . H4A H 1.0567 0.6169 0.9156 0.137 Uiso 1 1 calc R . . H4B H 1.0489 0.5244 0.8745 0.137 Uiso 1 1 calc R . . H4C H 0.9672 0.5449 0.9298 0.137 Uiso 1 1 calc R . . C5 C 0.693(2) 0.8334(14) 0.8239(11) 0.048(6) Uani 1 1 d . C . H5A H 0.7346 0.8152 0.8794 0.058 Uiso 1 1 calc R . . H5B H 0.6293 0.8756 0.8252 0.058 Uiso 1 1 calc R . . C6 C 0.786(2) 0.8796(15) 0.7924(12) 0.053(6) Uani 1 1 d . . . H6A H 0.8552 0.8405 0.7968 0.063 Uiso 1 1 calc R . . H6B H 0.7474 0.8939 0.7356 0.063 Uiso 1 1 calc R . . C7 C 0.832(3) 0.9600(17) 0.8380(15) 0.072(7) Uani 1 1 d . . . H7A H 0.8696 0.9457 0.8949 0.086 Uiso 1 1 calc R . . H7B H 0.7625 0.9993 0.8332 0.086 Uiso 1 1 calc R . . C8 C 0.924(3) 1.0046(18) 0.8075(18) 0.087(9) Uani 1 1 d . . . H8A H 0.9912 0.9651 0.8106 0.130 Uiso 1 1 calc R . . H8B H 0.9556 1.0557 0.8400 0.130 Uiso 1 1 calc R . . H8C H 0.8850 1.0221 0.7521 0.130 Uiso 1 1 calc R . . C9 C 0.549(2) 0.7161(15) 0.8244(12) 0.051(6) Uani 1 1 d . C . H9A H 0.6029 0.7008 0.8784 0.061 Uiso 1 1 calc R . . H9B H 0.4928 0.7613 0.8306 0.061 Uiso 1 1 calc R . . C10 C 0.478(2) 0.6408(18) 0.7905(16) 0.068(7) Uani 1 1 d D . . H10A H 0.5264 0.6057 0.7652 0.082 Uiso 1 1 calc R B 1 H10B H 0.4050 0.6608 0.7476 0.082 Uiso 1 1 calc R B 1 C11 C 0.435(6) 0.582(3) 0.844(3) 0.17(2) Uiso 0.86(5) 1 d PD C 1 H11A H 0.3794 0.5382 0.8100 0.205 Uiso 0.86(5) 1 calc PR C 1 H11B H 0.5059 0.5509 0.8794 0.205 Uiso 0.86(5) 1 calc PR C 1 C12 C 0.374(6) 0.624(4) 0.890(4) 0.17(3) Uiso 0.86(5) 1 d PD C 1 H12A H 0.3496 0.5815 0.9235 0.259 Uiso 0.86(5) 1 calc PR C 1 H12B H 0.3008 0.6527 0.8556 0.259 Uiso 0.86(5) 1 calc PR C 1 H12C H 0.4277 0.6667 0.9245 0.259 Uiso 0.86(5) 1 calc PR C 1 C11' C 0.368(6) 0.626(5) 0.818(6) 0.02(3) Uiso 0.14(5) 1 d PD C 2 H11C H 0.3697 0.6747 0.8543 0.019 Uiso 0.14(5) 1 calc PR C 2 H11D H 0.2971 0.6369 0.7698 0.019 Uiso 0.14(5) 1 calc PR C 2 C12' C 0.338(9) 0.553(5) 0.854(6) 0.02(3) Uiso 0.14(5) 1 d PD C 2 H12D H 0.2616 0.5633 0.8656 0.025 Uiso 0.14(5) 1 calc PR C 2 H12E H 0.4029 0.5405 0.9039 0.025 Uiso 0.14(5) 1 calc PR C 2 H12F H 0.3272 0.5031 0.8184 0.025 Uiso 0.14(5) 1 calc PR C 2 C13 C 0.5487(18) 0.7805(15) 0.6953(11) 0.046(5) Uani 1 1 d . C . H13A H 0.6008 0.8058 0.6665 0.056 Uiso 1 1 calc R . . H13B H 0.5128 0.7271 0.6669 0.056 Uiso 1 1 calc R . . C14 C 0.446(2) 0.8428(16) 0.6897(12) 0.057(6) Uani 1 1 d D . . H14A H 0.4791 0.8940 0.7227 0.068 Uiso 1 1 calc R . . H14B H 0.3864 0.8150 0.7110 0.068 Uiso 1 1 calc R . . C15 C 0.383(2) 0.8708(16) 0.6049(13) 0.063(6) Uani 1 1 d D . . H15A H 0.4422 0.9022 0.5853 0.075 Uiso 1 1 calc R . . H15B H 0.3570 0.8189 0.5714 0.075 Uiso 1 1 calc R . . C16 C 0.279(2) 0.9248(19) 0.5959(17) 0.081(8) Uani 1 1 d D . . H16A H 0.2217 0.8950 0.6168 0.122 Uiso 1 1 calc R . . H16B H 0.2402 0.9378 0.5395 0.122 Uiso 1 1 calc R . . H16C H 0.3056 0.9786 0.6253 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.5149(5) -0.0039(4) 0.1355(2) 0.0505(15) Uani 1 1 d . . . N1 N 0.6298(15) 0.7555(11) 0.7777(9) 0.040(4) Uani 1 1 d . . . Pt1 Pt 0.5000 0.0000 0.0000 0.0259(3) Uani 1 2 d S . . 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 0.0341(12) 0.0415(12) 0.0909(17) -0.0031(12) 0.0177(11) 0.0008(10) Br2 0.0208(10) 0.0470(12) 0.0642(13) 0.0038(10) 0.0126(9) 0.0088(9) Br4 0.070(2) 0.157(3) 0.0798(19) -0.054(2) 0.0230(15) -0.017(2) Br5 0.0420(12) 0.0585(13) 0.0295(9) 0.0073(9) 0.0164(8) 0.0175(10) Br6 0.109(2) 0.0600(15) 0.0524(14) 0.0097(12) 0.0309(14) 0.0306(15) Br7 0.0470(14) 0.0906(19) 0.0619(14) 0.0071(14) 0.0156(11) 0.0046(14) Br8 0.0526(15) 0.0695(16) 0.0749(16) 0.0049(13) 0.0236(12) -0.0023(13) C1 0.034(11) 0.054(13) 0.038(10) -0.008(10) 0.015(9) 0.014(10) C2 0.069(17) 0.081(17) 0.041(12) 0.005(12) 0.030(12) 0.009(14) C3 0.076(18) 0.090(19) 0.054(14) 0.017(14) 0.022(13) 0.045(16) C4 0.072(19) 0.12(3) 0.082(19) 0.030(18) 0.020(15) 0.058(19) C5 0.059(14) 0.061(14) 0.029(10) 0.002(10) 0.019(10) 0.015(12) C6 0.056(15) 0.058(14) 0.044(12) 0.002(11) 0.016(11) 0.013(12) C7 0.10(2) 0.069(17) 0.057(15) -0.006(13) 0.038(15) -0.004(16) C8 0.11(2) 0.072(19) 0.084(19) -0.023(16) 0.033(18) -0.008(17) C9 0.046(13) 0.073(16) 0.044(12) 0.017(11) 0.031(10) 0.017(12) C10 0.046(15) 0.089(19) 0.085(18) -0.004(16) 0.043(13) -0.005(14) C13 0.040(12) 0.069(15) 0.032(10) -0.002(10) 0.014(9) 0.009(11) C14 0.051(14) 0.075(16) 0.048(12) 0.009(12) 0.022(11) 0.034(13) C15 0.052(15) 0.069(16) 0.061(14) 0.005(13) 0.009(12) 0.005(13) C16 0.040(15) 0.10(2) 0.09(2) 0.018(17) 0.009(13) 0.024(16) Cl1 0.058(3) 0.081(4) 0.015(2) 0.005(2) 0.015(2) 0.048(3) N1 0.046(10) 0.051(10) 0.032(8) -0.007(8) 0.026(8) 0.009(8) Pt1 0.0189(5) 0.0326(6) 0.0276(5) -0.0005(4) 0.0093(4) 0.0048(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Pt1 2.449(2) . ? Br2 Pt1 2.471(2) . ? Br3 Br4 2.293(5) . ? Br3' Br4 2.314(9) . ? Br5 Br6 2.357(3) . ? Br7 Br8 2.326(4) . ? C1 N1 1.51(2) . ? C1 C2 1.54(3) . ? C2 C3 1.49(3) . ? C3 C4 1.46(3) . ? C5 N1 1.51(3) . ? C5 C6 1.55(3) . ? C6 C7 1.49(3) . ? C7 C8 1.52(4) . ? C9 C10 1.45(3) . ? C9 N1 1.56(2) . ? C10 C11 1.51(3) . ? C10 C11' 1.51(3) . ? C11 C12 1.42(3) . ? C11' C12' 1.42(3) . ? C13 C14 1.51(3) . ? C13 N1 1.52(2) . ? C14 C15 1.51(3) . ? C15 C16 1.43(3) . ? Cl1 Pt1 2.358(4) . ? Pt1 Cl1 2.358(4) 3_655 ? Pt1 Br1 2.449(2) 3_655 ? Pt1 Br2 2.471(2) 3_655 ? 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 Br3 Br4 Br3' 20.6(3) . . ? N1 C1 C2 116.7(15) . . ? C3 C2 C1 110.8(17) . . ? C4 C3 C2 114(2) . . ? N1 C5 C6 116.5(15) . . ? C7 C6 C5 111.2(18) . . ? C6 C7 C8 111(2) . . ? C10 C9 N1 117.1(17) . . ? C9 C10 C11 119(3) . . ? C9 C10 C11' 114(4) . . ? C11 C10 C11' 40(4) . . ? C12 C11 C10 114(4) . . ? C12' C11' C10 129(7) . . ? C14 C13 N1 117.4(15) . . ? C13 C14 C15 111.7(17) . . ? C16 C15 C14 114(2) . . ? C1 N1 C5 111.9(16) . . ? C1 N1 C13 106.6(13) . . ? C5 N1 C13 111.2(16) . . ? C1 N1 C9 111.3(16) . . ? C5 N1 C9 107.0(14) . . ? C13 N1 C9 108.8(16) . . ? Cl1 Pt1 Cl1 180.0(4) . 3_655 ? Cl1 Pt1 Br1 90.99(16) . . ? Cl1 Pt1 Br1 89.01(16) 3_655 . ? Cl1 Pt1 Br1 89.01(16) . 3_655 ? Cl1 Pt1 Br1 90.99(16) 3_655 3_655 ? Br1 Pt1 Br1 180.00(4) . 3_655 ? Cl1 Pt1 Br2 90.99(13) . 3_655 ? Cl1 Pt1 Br2 89.01(13) 3_655 3_655 ? Br1 Pt1 Br2 91.31(8) . 3_655 ? Br1 Pt1 Br2 88.69(8) 3_655 3_655 ? Cl1 Pt1 Br2 89.01(13) . . ? Cl1 Pt1 Br2 90.99(13) 3_655 . ? Br1 Pt1 Br2 88.69(8) . . ? Br1 Pt1 Br2 91.31(8) 3_655 . ? Br2 Pt1 Br2 180.00(13) 3_655 . ? 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 N1 C1 C2 C3 -176(2) . . . . ? C1 C2 C3 C4 179(2) . . . . ? N1 C5 C6 C7 174.2(19) . . . . ? C5 C6 C7 C8 179(2) . . . . ? N1 C9 C10 C11 158(3) . . . . ? N1 C9 C10 C11' -157(4) . . . . ? C9 C10 C11 C12 52(6) . . . . ? C11' C10 C11 C12 -42(7) . . . . ? C9 C10 C11' C12' -124(9) . . . . ? C11 C10 C11' C12' -17(8) . . . . ? N1 C13 C14 C15 173(2) . . . . ? C13 C14 C15 C16 176(2) . . . . ? C2 C1 N1 C5 54(2) . . . . ? C2 C1 N1 C13 175.9(19) . . . . ? C2 C1 N1 C9 -66(2) . . . . ? C6 C5 N1 C1 53(2) . . . . ? C6 C5 N1 C13 -66(2) . . . . ? C6 C5 N1 C9 175.4(17) . . . . ? C14 C13 N1 C1 177(2) . . . . ? C14 C13 N1 C5 -60(2) . . . . ? C14 C13 N1 C9 57(2) . . . . ? C10 C9 N1 C1 -58(2) . . . . ? C10 C9 N1 C5 178.9(19) . . . . ? C10 C9 N1 C13 59(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.050 _refine_diff_density_min -2.314 _refine_diff_density_rms 0.265 data_mibe5m _database_code_CSD 187954 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 Br24 N2 Pt2' _chemical_formula_weight 2792.94 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' '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3186(12) _cell_length_b 17.1659(19) _cell_length_c 18.743(2) _cell_angle_alpha 103.257(2) _cell_angle_beta 101.864(2) _cell_angle_gamma 93.605(2) _cell_volume 3445.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 _exptl_absorpt_coefficient_mu 17.997 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0616 _exptl_absorpt_correction_T_max 0.2942 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8953 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1990 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 22.49 _reflns_number_total 8953 _reflns_number_gt 5409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SMART' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8953 _refine_ls_number_parameters 534 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _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 0.64155(18) 1.05184(12) 0.02961(11) 0.0270(5) Uani 1 1 d . . . Br2 Br 0.6137(2) 0.83812(13) -0.01406(11) 0.0360(6) Uani 1 1 d . . . Br3 Br 0.7185(2) 0.94636(13) 0.16893(11) 0.0341(6) Uani 1 1 d . . . Br4 Br 0.4284(2) 0.84112(13) 0.11132(12) 0.0365(6) Uani 1 1 d . . . Br5 Br 0.4620(2) 1.04683(12) 0.16036(11) 0.0302(6) Uani 1 1 d . . . Br6 Br 1.0891(2) 0.66212(13) 0.39566(12) 0.0357(6) Uani 1 1 d . . . Br7 Br 1.09365(19) 0.45623(13) 0.35336(11) 0.0328(6) Uani 1 1 d . . . Br8 Br 0.87010(19) 0.43739(12) 0.45685(11) 0.0290(5) Uani 1 1 d . . . Br9 Br 0.82343(19) 0.53384(13) 0.30627(11) 0.0342(6) Uani 1 1 d . . . Br10 Br 0.85975(19) 0.64740(13) 0.48776(11) 0.0306(6) Uani 1 1 d . . . Br11 Br 0.8110(2) 0.78405(15) 0.40010(13) 0.0468(7) Uani 1 1 d . . . Br12 Br 0.7628(3) 0.8819(2) 0.3382(2) 0.0798(10) Uani 1 1 d . . . Br13 Br 0.4719(3) 0.95128(19) 0.40913(14) 0.0646(9) Uani 1 1 d . . . Br14 Br 0.4683(2) 0.98910(14) 0.29860(12) 0.0395(6) Uani 1 1 d . . . Br15 Br 0.1818(2) 0.90482(15) 0.68230(15) 0.0554(8) Uani 1 1 d . . . Br16 Br 0.0656(3) 0.79932(17) 0.58968(15) 0.0677(9) Uani 1 1 d . . . Br17 Br 0.5782(2) 0.57418(15) 0.43062(14) 0.0475(7) Uani 1 1 d . . . Br18 Br 0.3714(2) 0.53105(14) 0.40074(13) 0.0429(7) Uani 1 1 d . . . Br19 Br 0.1070(2) 0.49357(13) 0.20576(12) 0.0371(6) Uani 1 1 d . . . Br20 Br 0.1236(2) 0.51918(16) 0.09103(14) 0.0542(8) Uani 1 1 d . . . Br21 Br -0.0254(3) 0.0362(2) 0.1249(2) 0.0894(12) Uani 1 1 d . . . Br22 Br 0.1780(2) 0.03713(16) 0.12613(16) 0.0590(8) Uani 1 1 d . . . Br23 Br 0.2079(3) 0.57025(17) 0.91981(19) 0.0826(11) Uani 1 1 d . . . Br24 Br 0.3173(2) 0.68735(14) 0.99874(13) 0.0430(7) Uani 1 1 d . . . C1 C 0.091(2) 0.8634(13) 0.2403(12) 0.042(7) Uani 1 1 d . . . H1A H 0.0270 0.8940 0.2199 0.051 Uiso 1 1 calc R . . H1B H 0.1675 0.8831 0.2286 0.051 Uiso 1 1 calc R . . C2 C 0.109(2) 0.8848(12) 0.3247(14) 0.056(8) Uani 1 1 d D . . H2A H 0.1815 0.8618 0.3472 0.067 Uiso 1 1 calc R . . H2B H 0.0376 0.8606 0.3382 0.067 Uiso 1 1 calc R . . C3 C 0.125(2) 0.9750(12) 0.3569(12) 0.063(9) Uani 1 1 d D . . H3A H 0.1972 0.9988 0.3440 0.076 Uiso 1 1 calc R . . H3B H 0.0532 0.9978 0.3335 0.076 Uiso 1 1 calc R . . C4 C 0.140(3) 0.9973(18) 0.4391(12) 0.087(11) Uani 1 1 d D . . H4A H 0.0640 0.9812 0.4519 0.131 Uiso 1 1 calc R . . H4B H 0.1608 1.0558 0.4579 0.131 Uiso 1 1 calc R . . H4C H 0.2054 0.9700 0.4623 0.131 Uiso 1 1 calc R . . C5 C 0.150(2) 0.7267(13) 0.2325(13) 0.044(7) Uani 1 1 d . . . H5A H 0.1438 0.7310 0.2851 0.053 Uiso 1 1 calc R . . H5B H 0.1260 0.6697 0.2046 0.053 Uiso 1 1 calc R . . C6 C 0.280(2) 0.7474(13) 0.2329(12) 0.049(7) Uani 1 1 d D . . H6A H 0.3051 0.8052 0.2575 0.059 Uiso 1 1 calc R . . H6B H 0.2907 0.7372 0.1806 0.059 Uiso 1 1 calc R . . C7 C 0.3580(19) 0.6966(13) 0.2752(12) 0.039(6) Uani 1 1 d D . . H7A H 0.3496 0.7089 0.3280 0.047 Uiso 1 1 calc R . . H7B H 0.3291 0.6389 0.2522 0.047 Uiso 1 1 calc R . . C8 C 0.487(2) 0.7120(18) 0.2739(19) 0.091(11) Uani 1 1 d D . . H8A H 0.4974 0.6933 0.2222 0.137 Uiso 1 1 calc R . . H8B H 0.5364 0.6829 0.3062 0.137 Uiso 1 1 calc R . . H8C H 0.5141 0.7699 0.2922 0.137 Uiso 1 1 calc R . . C9 C -0.0690(19) 0.7509(13) 0.2054(12) 0.040(6) Uani 1 1 d . . . H9A H -0.0685 0.7596 0.2596 0.048 Uiso 1 1 calc R . . H9B H -0.1250 0.7865 0.1849 0.048 Uiso 1 1 calc R . . C10 C -0.1179(19) 0.6676(13) 0.1679(13) 0.045(7) Uani 1 1 d D . . H10A H -0.0722 0.6314 0.1945 0.054 Uiso 1 1 calc R . . H10B H -0.1061 0.6554 0.1158 0.054 Uiso 1 1 calc R . . C11 C -0.2514(17) 0.6513(13) 0.1658(13) 0.045(7) Uani 1 1 d D . . H11A H -0.2732 0.5922 0.1540 0.054 Uiso 1 1 calc R . . H11B H -0.2645 0.6741 0.2167 0.054 Uiso 1 1 calc R . . C12 C -0.335(2) 0.6836(14) 0.1116(15) 0.060(8) Uani 1 1 d D . . H12A H -0.3210 0.7426 0.1261 0.089 Uiso 1 1 calc R . . H12B H -0.4190 0.6660 0.1115 0.089 Uiso 1 1 calc R . . H12C H -0.3201 0.6638 0.0612 0.089 Uiso 1 1 calc R . . C13 C 0.065(2) 0.7650(15) 0.1169(13) 0.048(7) Uani 1 1 d . . . H13A H 0.0515 0.7065 0.0926 0.058 Uiso 1 1 calc R . . H13B H 0.1478 0.7851 0.1146 0.058 Uiso 1 1 calc R . . C14 C -0.029(3) 0.8082(18) 0.0714(13) 0.081(11) Uani 1 1 d D . . H14A H -0.1116 0.7927 0.0775 0.097 Uiso 1 1 calc R . . H14B H -0.0100 0.8673 0.0911 0.097 Uiso 1 1 calc R . . C15 C -0.027(3) 0.7851(18) -0.0118(14) 0.101(12) Uiso 1 1 d D . . H15A H -0.0620 0.8265 -0.0360 0.122 Uiso 1 1 calc R . . H15B H 0.0589 0.7847 -0.0164 0.122 Uiso 1 1 calc R . . C16 C -0.093(3) 0.7065(19) -0.0516(16) 0.118(15) Uani 1 1 d D . . H16A H -0.0596 0.6652 -0.0276 0.177 Uiso 1 1 calc R . . H16B H -0.0860 0.6940 -0.1041 0.177 Uiso 1 1 calc R . . H16C H -0.1792 0.7073 -0.0499 0.177 Uiso 1 1 calc R . . C17 C 0.505(2) 0.3873(11) 0.2529(12) 0.036(6) Uani 1 1 d . . . H17A H 0.5860 0.4183 0.2753 0.043 Uiso 1 1 calc R . . H17B H 0.4472 0.4142 0.2807 0.043 Uiso 1 1 calc R . . C18 C 0.467(2) 0.3941(11) 0.1694(12) 0.048(7) Uani 1 1 d D . . H18A H 0.5222 0.3665 0.1402 0.057 Uiso 1 1 calc R . . H18B H 0.3834 0.3664 0.1468 0.057 Uiso 1 1 calc R . . C19 C 0.470(2) 0.4792(12) 0.1645(11) 0.041(6) Uani 1 1 d D . . H19A H 0.5504 0.5080 0.1926 0.049 Uiso 1 1 calc R . . H19B H 0.4081 0.5047 0.1896 0.049 Uiso 1 1 calc R . . C20 C 0.447(2) 0.4901(16) 0.0855(12) 0.059(8) Uani 1 1 d D . . H20A H 0.5161 0.4751 0.0635 0.089 Uiso 1 1 calc R . . H20B H 0.4364 0.5465 0.0866 0.089 Uiso 1 1 calc R . . H20C H 0.3730 0.4557 0.0550 0.089 Uiso 1 1 calc R . . C21 C 0.590(2) 0.2565(13) 0.2222(13) 0.043(7) Uani 1 1 d . . . H21A H 0.5862 0.2022 0.2320 0.052 Uiso 1 1 calc R . . H21B H 0.5542 0.2499 0.1680 0.052 Uiso 1 1 calc R . . C22 C 0.721(2) 0.2907(13) 0.2388(14) 0.049(7) Uani 1 1 d D . . H22A H 0.7265 0.3461 0.2316 0.059 Uiso 1 1 calc R . . H22B H 0.7602 0.2935 0.2918 0.059 Uiso 1 1 calc R . . C23 C 0.7865(19) 0.2393(12) 0.1879(11) 0.041(6) Uani 1 1 d D . . H23A H 0.7524 0.2420 0.1356 0.049 Uiso 1 1 calc R . . H23B H 0.7707 0.1827 0.1904 0.049 Uiso 1 1 calc R . . C24 C 0.922(2) 0.2624(15) 0.2059(17) 0.077(10) Uani 1 1 d D . . H24A H 0.9389 0.3143 0.1945 0.115 Uiso 1 1 calc R . . H24B H 0.9593 0.2211 0.1753 0.115 Uiso 1 1 calc R . . H24C H 0.9553 0.2667 0.2593 0.115 Uiso 1 1 calc R . . C25 C 0.558(2) 0.3203(13) 0.3481(12) 0.040(6) Uani 1 1 d . . . H25A H 0.5031 0.3527 0.3743 0.048 Uiso 1 1 calc R . . H25B H 0.6386 0.3526 0.3620 0.048 Uiso 1 1 calc R . . C26 C 0.571(2) 0.2430(14) 0.3771(10) 0.047(7) Uani 1 1 d D . . H26A H 0.4922 0.2087 0.3605 0.057 Uiso 1 1 calc R . . H26B H 0.6311 0.2125 0.3541 0.057 Uiso 1 1 calc R . . C27 C 0.611(2) 0.2598(15) 0.4600(10) 0.067(9) Uani 1 1 d D . . H27A H 0.5518 0.2918 0.4825 0.080 Uiso 1 1 calc R . . H27B H 0.6904 0.2934 0.4761 0.080 Uiso 1 1 calc R . . C28 C 0.622(3) 0.1861(15) 0.4911(13) 0.064(8) Uani 1 1 d D . . H28A H 0.5414 0.1626 0.4916 0.096 Uiso 1 1 calc R . . H28B H 0.6725 0.2016 0.5425 0.096 Uiso 1 1 calc R . . H28C H 0.6603 0.1464 0.4593 0.096 Uiso 1 1 calc R . . C29 C 0.388(2) 0.2581(13) 0.2417(13) 0.045(7) Uani 1 1 d . . . H29A H 0.3964 0.2053 0.2538 0.054 Uiso 1 1 calc R . . H29B H 0.3636 0.2478 0.1862 0.054 Uiso 1 1 calc R . . C30 C 0.284(2) 0.2945(16) 0.2746(13) 0.058(8) Uani 1 1 d D . . H30A H 0.3089 0.3532 0.2942 0.069 Uiso 1 1 calc R . . H30B H 0.2130 0.2878 0.2319 0.069 Uiso 1 1 calc R . . C31 C 0.241(4) 0.2668(17) 0.3330(19) 0.125(14) Uiso 1 1 d D . . H31A H 0.1629 0.2884 0.3365 0.151 Uiso 1 1 calc R . . H31B H 0.2996 0.2916 0.3812 0.151 Uiso 1 1 calc R . . C32 C 0.222(3) 0.1777(15) 0.3264(15) 0.073(9) Uiso 1 1 d D . . H32A H 0.1596 0.1520 0.2809 0.109 Uiso 1 1 calc R . . H32B H 0.1956 0.1684 0.3707 0.109 Uiso 1 1 calc R . . H32C H 0.2984 0.1547 0.3233 0.109 Uiso 1 1 calc R . . N1 N 0.0591(16) 0.7772(9) 0.1984(9) 0.031(5) Uani 1 1 d . . . N2 N 0.5109(15) 0.3061(10) 0.2669(9) 0.031(5) Uani 1 1 d . . . Pt1 Pt 0.53785(7) 0.94341(5) 0.07153(4) 0.0232(3) Uani 1 1 d . . . Pt2 Pt 0.97681(7) 0.55083(5) 0.42192(4) 0.0246(3) 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 0.0214(12) 0.0219(12) 0.0316(11) -0.0006(10) 0.0022(9) -0.0044(9) Br2 0.0458(16) 0.0272(13) 0.0318(11) -0.0018(10) 0.0092(11) 0.0132(11) Br3 0.0286(14) 0.0363(14) 0.0310(11) 0.0019(10) -0.0016(10) 0.0072(11) Br4 0.0441(16) 0.0231(13) 0.0359(12) -0.0036(10) 0.0099(11) -0.0068(11) Br5 0.0336(14) 0.0215(12) 0.0300(11) -0.0047(10) 0.0073(10) 0.0031(10) Br6 0.0280(14) 0.0319(14) 0.0452(13) 0.0080(11) 0.0078(11) -0.0037(10) Br7 0.0247(13) 0.0317(13) 0.0373(12) -0.0010(10) 0.0071(10) 0.0046(10) Br8 0.0194(12) 0.0259(12) 0.0354(11) 0.0024(10) -0.0002(10) -0.0053(10) Br9 0.0237(13) 0.0373(14) 0.0332(11) 0.0027(11) -0.0043(10) -0.0004(10) Br10 0.0226(13) 0.0270(13) 0.0377(11) 0.0021(10) 0.0030(10) 0.0035(10) Br11 0.0437(17) 0.0407(15) 0.0503(14) 0.0042(12) 0.0041(12) 0.0115(12) Br12 0.067(2) 0.081(2) 0.124(3) 0.063(2) 0.043(2) 0.0432(18) Br13 0.062(2) 0.091(2) 0.0410(14) 0.0187(15) 0.0122(14) 0.0006(17) Br14 0.0403(16) 0.0402(15) 0.0314(11) -0.0037(11) 0.0089(11) -0.0001(12) Br15 0.0450(18) 0.0345(15) 0.0720(17) -0.0043(13) 0.0001(14) 0.0055(12) Br16 0.062(2) 0.0535(18) 0.0656(17) -0.0162(15) -0.0010(15) 0.0145(15) Br17 0.0310(15) 0.0423(16) 0.0628(15) -0.0001(13) 0.0106(13) 0.0044(12) Br18 0.0284(14) 0.0406(15) 0.0501(14) -0.0072(12) 0.0083(12) 0.0030(11) Br19 0.0301(14) 0.0336(14) 0.0411(12) 0.0001(11) 0.0055(11) -0.0013(11) Br20 0.0599(19) 0.0544(18) 0.0469(14) 0.0053(13) 0.0173(13) 0.0062(14) Br21 0.044(2) 0.073(2) 0.151(3) 0.017(2) 0.031(2) 0.0153(17) Br22 0.0480(18) 0.0488(17) 0.0797(18) 0.0032(15) 0.0280(15) 0.0047(14) Br23 0.061(2) 0.0490(19) 0.101(2) -0.0291(18) -0.0048(18) -0.0122(15) Br24 0.0343(15) 0.0351(14) 0.0487(13) -0.0018(12) 0.0003(12) -0.0012(11) C1 0.033(15) 0.037(15) 0.048(14) -0.004(12) 0.011(12) -0.009(12) C2 0.047(18) 0.033(16) 0.075(18) -0.003(14) 0.006(15) 0.000(13) C3 0.06(2) 0.039(17) 0.071(18) -0.017(15) 0.004(15) 0.014(14) C4 0.07(2) 0.09(2) 0.07(2) -0.026(18) -0.010(17) 0.016(18) C5 0.061(19) 0.021(13) 0.055(15) 0.006(12) 0.025(14) 0.005(13) C6 0.053(19) 0.045(17) 0.044(14) -0.005(13) 0.021(14) -0.013(14) C7 0.041(17) 0.027(14) 0.053(14) 0.020(12) 0.007(13) -0.003(12) C8 0.06(2) 0.09(3) 0.12(3) 0.03(2) 0.03(2) 0.04(2) C9 0.022(14) 0.049(16) 0.046(13) 0.008(13) 0.009(11) -0.011(12) C10 0.07(2) 0.024(14) 0.048(14) 0.011(12) 0.013(14) 0.012(13) C11 0.030(16) 0.022(13) 0.079(18) -0.003(13) 0.024(14) -0.009(11) C12 0.021(16) 0.042(17) 0.10(2) 0.024(16) -0.026(15) -0.012(12) C13 0.025(15) 0.062(18) 0.067(17) 0.039(15) 0.004(13) 0.004(13) C14 0.10(3) 0.08(2) 0.058(17) -0.011(17) 0.037(18) -0.036(19) C16 0.13(3) 0.13(3) 0.058(19) -0.03(2) 0.03(2) -0.01(3) C17 0.038(15) 0.006(12) 0.061(15) -0.001(11) 0.014(12) 0.006(10) C18 0.07(2) 0.023(14) 0.046(14) -0.005(12) 0.009(13) -0.001(12) C19 0.020(14) 0.038(15) 0.058(15) -0.003(13) 0.008(12) 0.007(11) C20 0.06(2) 0.07(2) 0.065(17) 0.050(16) 0.012(15) 0.034(16) C21 0.045(17) 0.026(14) 0.056(15) 0.002(12) 0.014(13) 0.002(12) C22 0.048(18) 0.025(14) 0.070(17) -0.007(13) 0.027(14) -0.008(12) C23 0.062(19) 0.019(13) 0.035(12) -0.001(11) 0.006(12) -0.008(12) C24 0.08(3) 0.032(17) 0.11(2) -0.014(17) 0.03(2) 0.010(16) C25 0.044(16) 0.032(14) 0.043(13) -0.002(12) 0.019(12) 0.006(12) C26 0.051(18) 0.042(16) 0.034(12) -0.014(12) -0.006(12) 0.029(13) C27 0.06(2) 0.07(2) 0.040(14) -0.021(15) 0.016(14) -0.023(16) C28 0.09(2) 0.06(2) 0.032(13) 0.016(14) 0.000(14) -0.010(17) C29 0.07(2) 0.025(14) 0.046(14) 0.016(12) 0.018(14) 0.008(13) C30 0.08(2) 0.053(18) 0.056(15) 0.028(14) 0.012(15) 0.056(16) N1 0.047(13) 0.007(9) 0.041(10) 0.007(8) 0.010(10) 0.005(9) N2 0.023(11) 0.019(10) 0.038(10) -0.003(9) -0.002(9) -0.009(8) Pt1 0.0221(5) 0.0162(5) 0.0255(4) -0.0032(4) 0.0027(4) -0.0006(4) Pt2 0.0164(5) 0.0214(5) 0.0303(4) 0.0007(4) 0.0003(4) -0.0023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Pt1 2.496(2) 2_675 ? Br1 Pt1 2.497(2) . ? Br2 Pt1 2.451(2) . ? Br3 Pt1 2.434(2) . ? Br4 Pt1 2.425(2) . ? Br5 Pt1 2.4668(19) . ? Br6 Pt2 2.427(2) . ? Br7 Pt2 2.459(2) . ? Br8 Pt2 2.509(2) . ? Br8 Pt2 2.517(2) 2_766 ? Br9 Pt2 2.428(2) . ? Br10 Pt2 2.457(2) . ? Br11 Br12 2.283(4) . ? Br13 Br14 2.302(4) . ? Br15 Br16 2.311(4) . ? Br17 Br18 2.322(3) . ? Br19 Br20 2.333(3) . ? Br21 Br22 2.297(4) . ? Br23 Br24 2.309(3) . ? C1 N1 1.49(2) . ? C1 C2 1.51(3) . ? C2 C3 1.512(19) . ? C3 C4 1.47(2) . ? C5 C6 1.49(3) . ? C5 N1 1.52(3) . ? C6 C7 1.514(19) . ? C7 C8 1.48(2) . ? C9 C10 1.46(3) . ? C9 N1 1.53(3) . ? C10 C11 1.511(19) . ? C11 C12 1.47(2) . ? C13 N1 1.51(3) . ? C13 C14 1.56(4) . ? C14 C15 1.52(2) . ? C15 C16 1.46(2) . ? C17 N2 1.48(3) . ? C17 C18 1.57(3) . ? C18 C19 1.485(19) . ? C19 C20 1.51(2) . ? C21 C22 1.51(3) . ? C21 N2 1.51(2) . ? C22 C23 1.489(19) . ? C23 C24 1.51(2) . ? C25 N2 1.46(3) . ? C25 C26 1.55(3) . ? C26 C27 1.480(19) . ? C27 C28 1.51(2) . ? C29 N2 1.50(3) . ? C29 C30 1.54(3) . ? C30 C31 1.44(2) . ? C31 C32 1.50(2) . ? Pt1 Br1 2.496(2) 2_675 ? Pt2 Br8 2.517(2) 2_766 ? 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 Pt1 Br1 Pt1 94.08(7) 2_675 . ? Pt2 Br8 Pt2 94.94(7) . 2_766 ? N1 C1 C2 118.7(19) . . ? C1 C2 C3 112(2) . . ? C4 C3 C2 113(2) . . ? C6 C5 N1 116.9(19) . . ? C5 C6 C7 110(2) . . ? C8 C7 C6 112(2) . . ? C10 C9 N1 116.2(17) . . ? C9 C10 C11 112.4(18) . . ? C12 C11 C10 116(2) . . ? N1 C13 C14 113.8(19) . . ? C15 C14 C13 110(3) . . ? C16 C15 C14 113(2) . . ? N2 C17 C18 118.4(16) . . ? C19 C18 C17 111.9(16) . . ? C18 C19 C20 114.5(19) . . ? C22 C21 N2 115.6(16) . . ? C23 C22 C21 110.2(17) . . ? C22 C23 C24 114.6(18) . . ? N2 C25 C26 114.8(16) . . ? C27 C26 C25 113.1(18) . . ? C26 C27 C28 115(2) . . ? N2 C29 C30 117.7(19) . . ? C31 C30 C29 122(2) . . ? C30 C31 C32 119(3) . . ? C1 N1 C13 111.6(18) . . ? C1 N1 C5 109.4(17) . . ? C13 N1 C5 106.7(16) . . ? C1 N1 C9 107.6(15) . . ? C13 N1 C9 111.1(17) . . ? C5 N1 C9 110.5(17) . . ? C25 N2 C17 105.1(16) . . ? C25 N2 C29 111.8(17) . . ? C17 N2 C29 110.9(17) . . ? C25 N2 C21 112.2(18) . . ? C17 N2 C21 112.5(17) . . ? C29 N2 C21 104.6(15) . . ? Br4 Pt1 Br3 91.49(8) . . ? Br4 Pt1 Br2 90.09(8) . . ? Br3 Pt1 Br2 89.11(8) . . ? Br4 Pt1 Br5 88.52(7) . . ? Br3 Pt1 Br5 89.93(7) . . ? Br2 Pt1 Br5 178.30(8) . . ? Br4 Pt1 Br1 91.97(8) . 2_675 ? Br3 Pt1 Br1 176.46(8) . 2_675 ? Br2 Pt1 Br1 91.64(7) . 2_675 ? Br5 Pt1 Br1 89.40(7) . 2_675 ? Br4 Pt1 Br1 177.29(8) . . ? Br3 Pt1 Br1 90.60(8) . . ? Br2 Pt1 Br1 91.67(8) . . ? Br5 Pt1 Br1 89.75(7) . . ? Br1 Pt1 Br1 85.92(7) 2_675 . ? Br6 Pt2 Br9 91.54(8) . . ? Br6 Pt2 Br10 89.11(8) . . ? Br9 Pt2 Br10 89.47(8) . . ? Br6 Pt2 Br7 89.70(8) . . ? Br9 Pt2 Br7 89.54(7) . . ? Br10 Pt2 Br7 178.44(9) . . ? Br6 Pt2 Br8 176.40(8) . . ? Br9 Pt2 Br8 92.05(8) . . ? Br10 Pt2 Br8 90.64(7) . . ? Br7 Pt2 Br8 90.60(7) . . ? Br6 Pt2 Br8 91.36(8) . 2_766 ? Br9 Pt2 Br8 177.11(8) . 2_766 ? Br10 Pt2 Br8 90.57(7) . 2_766 ? Br7 Pt2 Br8 90.47(7) . 2_766 ? Br8 Pt2 Br8 85.06(7) . 2_766 ? 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 N1 C1 C2 C3 -173(2) . . . . ? C1 C2 C3 C4 179(2) . . . . ? N1 C5 C6 C7 174.7(17) . . . . ? C5 C6 C7 C8 177(2) . . . . ? N1 C9 C10 C11 -169.7(19) . . . . ? C9 C10 C11 C12 75(3) . . . . ? N1 C13 C14 C15 -174(2) . . . . ? C13 C14 C15 C16 80(4) . . . . ? N2 C17 C18 C19 -177.6(18) . . . . ? C17 C18 C19 C20 174(2) . . . . ? N2 C21 C22 C23 -176(2) . . . . ? C21 C22 C23 C24 -173(2) . . . . ? N2 C25 C26 C27 -176(2) . . . . ? C25 C26 C27 C28 179(2) . . . . ? N2 C29 C30 C31 -103(3) . . . . ? C29 C30 C31 C32 -44(5) . . . . ? C2 C1 N1 C13 -171(2) . . . . ? C2 C1 N1 C5 -53(3) . . . . ? C2 C1 N1 C9 67(3) . . . . ? C14 C13 N1 C1 -64(3) . . . . ? C14 C13 N1 C5 176(2) . . . . ? C14 C13 N1 C9 56(3) . . . . ? C6 C5 N1 C1 -59(2) . . . . ? C6 C5 N1 C13 62(2) . . . . ? C6 C5 N1 C9 -177.5(17) . . . . ? C10 C9 N1 C1 -180(2) . . . . ? C10 C9 N1 C13 58(3) . . . . ? C10 C9 N1 C5 -61(2) . . . . ? C26 C25 N2 C17 179.3(19) . . . . ? C26 C25 N2 C29 59(2) . . . . ? C26 C25 N2 C21 -58(2) . . . . ? C18 C17 N2 C25 176(2) . . . . ? C18 C17 N2 C29 -63(2) . . . . ? C18 C17 N2 C21 53(3) . . . . ? C30 C29 N2 C25 61(3) . . . . ? C30 C29 N2 C17 -56(2) . . . . ? C30 C29 N2 C21 -177.4(19) . . . . ? C22 C21 N2 C25 -57(3) . . . . ? C22 C21 N2 C17 61(3) . . . . ? C22 C21 N2 C29 -178(2) . . . . ? Pt1 Br1 Pt1 Br4 -39.0(15) 2_675 . . . ? Pt1 Br1 Pt1 Br3 -179.34(7) 2_675 . . . ? Pt1 Br1 Pt1 Br2 91.53(7) 2_675 . . . ? Pt1 Br1 Pt1 Br5 -89.41(7) 2_675 . . . ? Pt1 Br1 Pt1 Br1 0.0 2_675 . . 2_675 ? Pt2 Br8 Pt2 Br6 -4.4(12) 2_766 . . . ? Pt2 Br8 Pt2 Br9 179.98(8) 2_766 . . . ? Pt2 Br8 Pt2 Br10 -90.52(7) 2_766 . . . ? Pt2 Br8 Pt2 Br7 90.42(8) 2_766 . . . ? Pt2 Br8 Pt2 Br8 0.0 2_766 . . 2_766 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.175 _refine_diff_density_min -2.529 _refine_diff_density_rms 0.325