#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/16/4001686.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_4001686 loop_ _publ_author_name 'Allenbaugh, Rachel J.' 'Schauer, Cynthia K.' 'Josey, Amanda' 'Martin, James D.' 'Anokhin, Denis V.' 'Ivanov, Dimitri A.' _publ_section_title ; Effect of Axial Interactions on the Formation of Mesophases: Comparison of the Phase Behavior of Dialkyl 2,2′-bipyridyl-4,4′-dicarboxylate Complexes of Pt(II), Pt(IV), and Pt(II)/Pt(IV) Molecular Alloys ; _journal_issue 23 _journal_name_full 'Chemistry of Materials' _journal_page_first 4517 _journal_paper_doi 10.1021/cm3018105 _journal_volume 24 _journal_year 2012 _chemical_formula_moiety 'C14 H12 Cl2 N2 O4 Pt1, C H2 Cl2' _chemical_formula_sum 'C15 H14 Cl4 N2 O4 Pt' _chemical_formula_weight 623.19 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 04-09-29 _audit_creation_method CRYSTALS_ver_12.39 _cell_angle_alpha 90 _cell_angle_beta 115.134(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.2723(16) _cell_length_b 6.7511(7) _cell_length_c 17.6663(17) _cell_measurement_reflns_used 1024 _cell_measurement_temperature 173 _cell_measurement_theta_max 27.0 _cell_measurement_theta_min 2.5 _cell_volume 1865.0(3) _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_collection 'SMART (Siemens, 1993)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_molecular_graphics 'CAMERON (Watkin et al 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al 2003)' _computing_structure_solution 'SIR92 (Altomare et al, 1994)' _diffrn_ambient_temperature 173 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method '\f & \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4073 _diffrn_reflns_theta_full 27.006 _diffrn_reflns_theta_max 27.006 _diffrn_reflns_theta_min 1.302 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.121 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_correction_T_min 0.29 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.219 _exptl_crystal_description needle _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_diff_density_max 4.68 _refine_diff_density_min -2.62 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 0.9072 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 4057 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0343 _refine_ls_shift/su_max 0.000175 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 47.5 76.0 43.6 16.5 2.67 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1060 _refine_ls_wR_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.1060 _reflns_limit_h_max 19 _reflns_limit_h_min -22 _reflns_limit_k_max 8 _reflns_limit_k_min 0 _reflns_limit_l_max 22 _reflns_limit_l_min 0 _reflns_number_gt 2998 _reflns_number_total 4073 _reflns_threshold_expression I>2.00u(I) _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _oxford_refine_ls_scale 0.136 _oxford_structure_analysis_title 'c04225 in P2(1)/c' _cod_data_source_file cm3018105_si_002.cif _cod_data_source_block CRYSTALS_cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius ; _cod_original_sg_symbol_H-M 'P 1 21/c 1 ' _cod_original_formula_sum 'C15 H14 Cl4 N2 O4 Pt1' _cod_database_code 4001686 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn Pt1 Pt -0.0253 0.0201 0.2394 0.0108 1.0000 Uani . Cl2 Cl -0.1310 0.0183 0.1051 0.0166 1.0000 Uani . Cl3 Cl -0.1304 0.0192 0.2868 0.0169 1.0000 Uani . N4 N 0.0730 0.0211 0.2067 0.0147 1.0000 Uani . C5 C 0.0660 0.0225 0.1284 0.0187 1.0000 Uani . C6 C 0.1378 0.0212 0.1110 0.0186 1.0000 Uani . C7 C 0.2185 0.0158 0.1778 0.0149 1.0000 Uani . C8 C 0.2253 0.0158 0.2585 0.0165 1.0000 Uani . C9 C 0.1514 0.0189 0.2719 0.0128 1.0000 Uani . C10 C 0.1521 0.0168 0.3552 0.0135 1.0000 Uani . C11 C 0.2247 0.0130 0.4295 0.0151 1.0000 Uani . C12 C 0.2169 0.0073 0.5044 0.0165 1.0000 Uani . C13 C 0.1359 0.0103 0.5033 0.0208 1.0000 Uani . C14 C 0.0647 0.0168 0.4257 0.0162 1.0000 Uani . N15 N 0.0726 0.0181 0.3533 0.0151 1.0000 Uani . C16 C 0.2984 0.0050 0.1636 0.0185 1.0000 Uani . O17 O 0.3674 -0.0287 0.2191 0.0305 1.0000 Uani . O18 O 0.2826 0.0388 0.0846 0.0290 1.0000 Uani . C19 C 0.3536 0.0188 0.0636 0.0335 1.0000 Uani . C20 C 0.2922 -0.0027 0.5879 0.0221 1.0000 Uani . O21 O 0.2846 -0.0149 0.6522 0.0497 1.0000 Uani . O22 O 0.3667 0.0004 0.5829 0.0221 1.0000 Uani . C23 C 0.4405 -0.0066 0.6620 0.0327 1.0000 Uani . C24 C 0.3506 -0.4110 0.3492 0.0380 1.0000 Uani . Cl25 Cl 0.4168 -0.2400 0.4243 0.0330 1.0000 Uani . Cl26 Cl 0.3979 -0.6485 0.3680 0.0532 1.0000 Uani . H14 H 0.0058 0.0181 0.4242 0.0221 1.0000 Uiso R H13 H 0.1288 0.0068 0.5574 0.0255 1.0000 Uiso R H11 H 0.2827 0.0137 0.4296 0.0182 1.0000 Uiso R H5 H 0.0077 0.0211 0.0806 0.0195 1.0000 Uiso R H6 H 0.1317 0.0246 0.0516 0.0235 1.0000 Uiso R H8 H 0.2831 0.0159 0.3069 0.0196 1.0000 Uiso R H232 H 0.4945 -0.0017 0.6526 0.0375 1.0000 Uiso R H231 H 0.4414 0.1115 0.6973 0.0375 1.0000 Uiso R H233 H 0.4411 -0.1301 0.6928 0.0375 1.0000 Uiso R H41 H 0.2934 -0.4212 0.3519 0.0426 1.0000 Uiso R H42 H 0.3406 -0.3679 0.2916 0.0426 1.0000 Uiso R H193 H 0.3340 0.0483 0.0019 0.0484 1.0000 Uiso R H192 H 0.3997 0.1165 0.0961 0.0484 1.0000 Uiso R H191 H 0.3772 -0.1178 0.0751 0.0484 1.0000 Uiso 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 0.0095 0.0117 0.0098 0.0001 0.0028 0.0003 Cl2 0.0132 0.0202 0.0120 -0.0004 0.0012 0.0006 Cl3 0.0127 0.0219 0.0179 0.0006 0.0082 0.0000 N4 0.0164 0.0164 0.0144 0.0005 0.0097 -0.0003 C5 0.0146 0.0280 0.0096 -0.0095 0.0014 -0.0022 C6 0.0178 0.0295 0.0098 0.0066 0.0071 0.0053 C7 0.0149 0.0197 0.0135 0.0038 0.0092 0.0003 C8 0.0119 0.0164 0.0177 0.0014 0.0028 0.0011 C9 0.0137 0.0110 0.0128 -0.0025 0.0049 -0.0004 C10 0.0178 0.0129 0.0099 0.0009 0.0061 -0.0007 C11 0.0112 0.0169 0.0186 -0.0023 0.0078 -0.0024 C12 0.0186 0.0149 0.0146 -0.0006 0.0057 -0.0005 C13 0.0241 0.0298 0.0104 0.0021 0.0090 0.0011 C14 0.0142 0.0251 0.0104 0.0021 0.0061 -0.0068 N15 0.0086 0.0197 0.0126 -0.0021 0.0004 -0.0007 C16 0.0198 0.0211 0.0176 -0.0013 0.0109 -0.0016 O17 0.0183 0.0558 0.0187 0.0044 0.0092 0.0066 O18 0.0232 0.0502 0.0180 0.0040 0.0129 0.0040 C19 0.0440 0.0366 0.0355 0.0050 0.0319 0.0063 C20 0.0207 0.0276 0.0155 0.0033 0.0051 0.0026 O21 0.0193 0.1154 0.0125 0.0052 0.0049 0.0042 O22 0.0148 0.0351 0.0158 0.0018 0.0060 0.0010 C23 0.0233 0.0461 0.0213 0.0054 0.0022 -0.0013 C24 0.0280 0.0463 0.0275 -0.0013 0.0000 0.0046 Cl25 0.0324 0.0400 0.0250 -0.0008 0.0106 -0.0037 Cl26 0.0524 0.0414 0.0564 -0.0062 0.0142 0.0062 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103 11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _oxford_twin_element_scale_factors 0.891 0.109