#------------------------------------------------------------------------------ #$Date: 2019-11-28 15:33:49 +0200 (Thu, 28 Nov 2019) $ #$Revision: 244041 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/55/7125564.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7125564 loop_ _publ_author_name 'Berkei, Michael' 'Bickley, Jamie F.' 'Heaton, Brian T.' 'Steiner, Alexander' _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[PtBr4Cl2].(Br2)6. ; _journal_issue 18 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 2180 _journal_page_last 2181 _journal_paper_doi 10.1039/b205712n _journal_year 2002 _chemical_formula_sum 'C32 H72 Br16 Cl2 N2 Pt' _chemical_formula_weight 2029.47 _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 108.671(11) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 11.604(6) _cell_length_b 15.530(8) _cell_length_c 17.764(9) _cell_measurement_reflns_used 3479 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 48.038 _cell_measurement_theta_min 4.555 _cell_volume 3033(3) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SHELXTL (Bruker, 2000)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Apex CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.1079 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 12055 _diffrn_reflns_theta_full 22.49 _diffrn_reflns_theta_max 22.49 _diffrn_reflns_theta_min 1.78 _exptl_absorpt_coefficient_mu 12.966 _exptl_absorpt_correction_T_max 0.4236 _exptl_absorpt_correction_T_min 0.1122 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 2000)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 1900 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 2.050 _refine_diff_density_min -2.314 _refine_diff_density_rms 0.265 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 243 _refine_ls_number_reflns 3949 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0822 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+126.5514P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1979 _refine_ls_wR_factor_ref 0.2059 _reflns_number_gt 3367 _reflns_number_total 3949 _reflns_threshold_expression >2sigma(I) _cod_data_source_file b205712n.txt _cod_data_source_block mibe7m _cod_depositor_comments ; The following automatic conversions were performed: data item '_symmetry_cell_setting' value 'Monoclinic' was changed to 'monoclinic' in accordance with the /home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7125564 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' 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) 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' 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 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_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 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_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 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)