# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1820 # Synthesis, properties and structures of complexes of platinum # metal halides and Group 11 metals with two distibinomethane # ligands, R2SbCH2SbR2 (R = Me or Ph) # T. Even, A.R.J. Genge, A.M. Hill, N.J. Holmes, W. Levason and M. Webster # J. Chem. Soc., Dalton Trans. Paper reference no. 9/08296D ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 7 October 1991 ### ############################################################################## #============================================================================== data_global1 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof W Levason' _publ_contact_author_address ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; _publ_contact_author_phone '023 80 593792' _publ_contact_author_fax ? _publ_contact_author_email 'wxl@soton.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please note that this file is three separate CIFs edited into one file and it accompanies a paper submitted to J Chem Soc, Dalton Trans. (Ref. 9/08296D). ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, properties and structures of complexes of platinum metal halides and Group 11 metals with two distibinomethane ligands, R~2~SbCH~2~SbR~2~ (R = Me or Ph) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Even, Tina' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Genge, Anthony R. J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Hill, Angela M.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Holmes, Nicholas J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Levason, William' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Webster, Michael' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; #============================================================================== # 4. TEXT _publ_section_references ; Molecular Structure Corporation (1988) MSC/AFC Diffractometer Control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation (1995) teXsan - Crystal Structure Analysis Package (Version 1.8), MSC, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1997) SHELXL97, Program for the Refinement of Crystal Structures, University of G\"ottingen, Germany. ; #============================================================================== data_99lev002 #============================================================================== # 5. CHEMICAL DATA _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diiodotris(bisdiphenylstibinomethane)ruthenium(II) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C75 H66 I2 Ru Sb6' _chemical_formula_weight 2052.65 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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.8997(5) _cell_length_b 11.22890(10) _cell_length_c 25.5004(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.3400(9) _cell_angle_gamma 90.00 _cell_volume 6831.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.996 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 3.497 _exptl_absorpt_correction_type 'multi-scan' # sortav _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_T_max 0.961 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector. Nonius CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75316 _diffrn_reflns_av_R_equivalents 0.1348 _diffrn_reflns_av_sigmaI/netI 0.1384 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _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 1.60 _diffrn_reflns_theta_max 27.49 _reflns_number_total 15670 _reflns_number_gt 8915 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (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 w=1/[\s^2^(Fo^2^)+(0.0494P)^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 15670 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.104 _refine_ls_shift/su_mean 0.005 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.26623(3) 0.19092(5) 0.19278(2) 0.02579(15) Uani 1 d . . . I2 I 0.12354(3) -0.17416(5) 0.23163(2) 0.02551(15) Uani 1 d . . . Sb1 Sb 0.14763(3) 0.13973(5) 0.28498(2) 0.02012(14) Uani 1 d . . . Sb2 Sb 0.11501(3) 0.13681(5) 0.16341(2) 0.01997(14) Uani 1 d . . . Sb3 Sb 0.26879(3) -0.06695(5) 0.28238(2) 0.02058(14) Uani 1 d . . . Sb4 Sb 0.40066(3) 0.10470(5) 0.27660(2) 0.02754(16) Uani 1 d . . . Sb5 Sb 0.21824(3) -0.10344(5) 0.13123(2) 0.02024(14) Uani 1 d . . . Sb6 Sb 0.35606(3) 0.00557(5) 0.08652(2) 0.02949(16) Uani 1 d . . . Ru1 Ru 0.19353(3) 0.01187(5) 0.21419(2) 0.01751(16) Uani 1 d . . . C1 C 0.1086(4) 0.2605(7) 0.2283(3) 0.025(2) Uani 1 d . . . H1A H 0.1300 0.3329 0.2241 0.037(3) Uiso 1 calc R . . H1B H 0.0701 0.2794 0.2354 0.037(3) Uiso 1 calc R . . C2 C 0.3264(4) 0.0608(7) 0.3169(3) 0.029(2) Uani 1 d . . . H2A H 0.3384 0.0321 0.3516 0.037(3) Uiso 1 calc R . . H2B H 0.3058 0.1341 0.3216 0.037(3) Uiso 1 calc R . . C3 C 0.2671(4) -0.0168(7) 0.0747(3) 0.025(2) Uani 1 d . . . H3A H 0.2513 0.0621 0.0692 0.037(3) Uiso 1 calc R . . H3B H 0.2606 -0.0597 0.0419 0.037(3) Uiso 1 calc R . . C11 C 0.1866(4) 0.2515(7) 0.3445(3) 0.020(2) Uani 1 d . . . C12 C 0.1747(4) 0.2359(7) 0.3962(3) 0.032(2) Uani 1 d . . . H12 H 0.1494 0.1775 0.4052 0.037(3) Uiso 1 calc R . . C13 C 0.2002(5) 0.3068(9) 0.4345(4) 0.045(3) Uani 1 d . . . H13 H 0.1920 0.2960 0.4694 0.037(3) Uiso 1 calc R . . C14 C 0.2373(5) 0.3923(8) 0.4220(4) 0.047(3) Uani 1 d . . . H14 H 0.2552 0.4378 0.4484 0.037(3) Uiso 1 calc R . . C15 C 0.2487(4) 0.4123(8) 0.3701(4) 0.040(3) Uani 1 d . . . H15 H 0.2730 0.4728 0.3612 0.037(3) Uiso 1 calc R . . C16 C 0.2234(4) 0.3410(7) 0.3320(4) 0.032(2) Uani 1 d . . . H16 H 0.2311 0.3530 0.2970 0.037(3) Uiso 1 calc R . . C21 C 0.0794(4) 0.0741(7) 0.3263(3) 0.023(2) Uani 1 d . . . C22 C 0.0262(5) 0.1224(8) 0.3175(4) 0.038(3) Uani 1 d . . . H22 H 0.0203 0.1849 0.2939 0.037(3) Uiso 1 calc R . . C23 C -0.0182(5) 0.0773(9) 0.3440(4) 0.052(3) Uani 1 d . . . H23 H -0.0540 0.1080 0.3375 0.037(3) Uiso 1 calc R . . C24 C -0.0093(4) -0.0124(8) 0.3798(4) 0.038(3) Uani 1 d . . . H24 H -0.0389 -0.0408 0.3982 0.037(3) Uiso 1 calc R . . C25 C 0.0434(4) -0.0609(8) 0.3886(3) 0.033(2) Uani 1 d . . . H25 H 0.0496 -0.1213 0.4132 0.037(3) Uiso 1 calc R . . C26 C 0.0866(4) -0.0192(7) 0.3608(3) 0.029(2) Uani 1 d . . . H26 H 0.1216 -0.0550 0.3654 0.037(3) Uiso 1 calc R . . C31 C 0.0306(4) 0.0781(7) 0.1524(3) 0.023(2) Uani 1 d . . . C32 C 0.0187(4) -0.0356(7) 0.1327(3) 0.027(2) Uani 1 d . . . H32 H 0.0476 -0.0846 0.1226 0.037(3) Uiso 1 calc R . . C33 C -0.0369(4) -0.0754(8) 0.1283(3) 0.030(2) Uani 1 d . . . H33 H -0.0446 -0.1505 0.1143 0.037(3) Uiso 1 calc R . . C34 C -0.0799(4) -0.0070(8) 0.1439(4) 0.035(2) Uani 1 d . . . H34 H -0.1165 -0.0357 0.1422 0.037(3) Uiso 1 calc R . . C35 C -0.0677(4) 0.1063(8) 0.1622(4) 0.040(3) Uani 1 d . . . H35 H -0.0968 0.1555 0.1717 0.037(3) Uiso 1 calc R . . C36 C -0.0139(4) 0.1476(8) 0.1667(4) 0.034(2) Uani 1 d . . . H36 H -0.0070 0.2240 0.1797 0.037(3) Uiso 1 calc R . . C41 C 0.1200(4) 0.2564(7) 0.0977(3) 0.021(2) Uani 1 d . . . C42 C 0.1565(4) 0.3515(7) 0.0998(3) 0.025(2) Uani 1 d . . . H42 H 0.1810 0.3623 0.1291 0.037(3) Uiso 1 calc R . . C43 C 0.1565(4) 0.4310(7) 0.0583(4) 0.031(2) Uani 1 d . . . H43 H 0.1810 0.4954 0.0601 0.037(3) Uiso 1 calc R . . C44 C 0.1213(4) 0.4163(7) 0.0152(3) 0.030(2) Uani 1 d . . . H44 H 0.1214 0.4710 -0.0122 0.037(3) Uiso 1 calc R . . C45 C 0.0852(4) 0.3202(7) 0.0118(3) 0.032(2) Uani 1 d . . . H45 H 0.0614 0.3099 -0.0180 0.037(3) Uiso 1 calc R . . C46 C 0.0845(4) 0.2390(7) 0.0528(3) 0.024(2) Uani 1 d . . . H46 H 0.0606 0.1736 0.0505 0.037(3) Uiso 1 calc R . . C51 C 0.2399(4) -0.1360(7) 0.3546(3) 0.027(2) Uani 1 d . . . C52 C 0.2431(4) -0.0668(7) 0.3996(3) 0.026(2) Uani 1 d . . . H52 H 0.2587 0.0090 0.3987 0.037(3) Uiso 1 calc R . . C53 C 0.2237(4) -0.1089(8) 0.4455(3) 0.031(2) Uani 1 d . . . H53 H 0.2266 -0.0615 0.4754 0.037(3) Uiso 1 calc R . . C54 C 0.2005(4) -0.2179(9) 0.4481(4) 0.039(3) Uani 1 d . . . H54 H 0.1874 -0.2448 0.4796 0.037(3) Uiso 1 calc R . . C55 C 0.1960(4) -0.2903(8) 0.4038(4) 0.030(2) Uani 1 d . . . H55 H 0.1806 -0.3662 0.4056 0.037(3) Uiso 1 calc R . . C56 C 0.2146(4) -0.2481(8) 0.3574(3) 0.028(2) Uani 1 d . . . H56 H 0.2104 -0.2948 0.3274 0.037(3) Uiso 1 calc R . . C61 C 0.3263(4) -0.2013(7) 0.2613(3) 0.025(2) Uani 1 d . . . C62 C 0.3360(4) -0.3080(8) 0.2885(3) 0.031(2) Uani 1 d . . . H62 H 0.3178 -0.3221 0.3192 0.037(3) Uiso 1 calc R . . C63 C 0.3722(4) -0.3928(8) 0.2706(4) 0.038(3) Uani 1 d . . . H63 H 0.3787 -0.4632 0.2892 0.037(3) Uiso 1 calc R . . C64 C 0.3984(4) -0.3723(8) 0.2251(4) 0.038(3) Uani 1 d . . . H64 H 0.4222 -0.4297 0.2125 0.037(3) Uiso 1 calc R . . C65 C 0.3899(4) -0.2676(8) 0.1978(4) 0.034(2) Uani 1 d . . . H65 H 0.4084 -0.2538 0.1673 0.037(3) Uiso 1 calc R . . C66 C 0.3539(4) -0.1836(8) 0.2157(3) 0.026(2) Uani 1 d . . . H66 H 0.3480 -0.1134 0.1968 0.037(3) Uiso 1 calc R . . C71 C 0.4185(4) 0.2728(8) 0.3169(3) 0.033(2) Uani 1 d . . . C72 C 0.3882(5) 0.3202(8) 0.3568(4) 0.040(3) Uani 1 d . . . H72 H 0.3553 0.2834 0.3658 0.037(3) Uiso 1 calc R . . C73 C 0.4067(5) 0.4218(9) 0.3830(4) 0.050(3) Uani 1 d . . . H73 H 0.3859 0.4527 0.4096 0.037(3) Uiso 1 calc R . . C74 C 0.4552(5) 0.4777(9) 0.3707(4) 0.049(3) Uani 1 d . . . H74 H 0.4679 0.5445 0.3894 0.037(3) Uiso 1 calc R . . C75 C 0.4846(4) 0.4334(8) 0.3302(4) 0.045(3) Uani 1 d . . . H75 H 0.5169 0.4720 0.3206 0.037(3) Uiso 1 calc R . . C76 C 0.4664(4) 0.3316(8) 0.3036(4) 0.042(3) Uani 1 d . . . H76 H 0.4867 0.3025 0.2763 0.037(3) Uiso 1 calc R . . C81 C 0.4578(4) 0.0054(7) 0.3284(3) 0.030(2) Uani 1 d . . . C82 C 0.4908(4) 0.0563(9) 0.3704(4) 0.036(2) Uani 1 d . . . H82 H 0.4856 0.1360 0.3788 0.037(3) Uiso 1 calc R . . C83 C 0.5303(5) -0.0093(10) 0.3994(4) 0.049(3) Uani 1 d . . . H83 H 0.5502 0.0253 0.4279 0.037(3) Uiso 1 calc R . . C84 C 0.5402(5) -0.1255(10) 0.3862(4) 0.048(3) Uani 1 d . . . H84 H 0.5683 -0.1681 0.4047 0.037(3) Uiso 1 calc R . . C85 C 0.5085(5) -0.1809(8) 0.3450(4) 0.043(3) Uani 1 d . . . H85 H 0.5145 -0.2603 0.3366 0.037(3) Uiso 1 calc R . . C86 C 0.4675(4) -0.1136(8) 0.3171(4) 0.036(2) Uani 1 d . . . H86 H 0.4460 -0.1497 0.2900 0.037(3) Uiso 1 calc R . . C91 C 0.1492(4) -0.1378(7) 0.0753(3) 0.023(2) Uani 1 d . . . C92 C 0.1198(4) -0.2452(8) 0.0742(4) 0.033(2) Uani 1 d . . . H92 H 0.1291 -0.3037 0.0991 0.037(3) Uiso 1 calc R . . C93 C 0.0770(4) -0.2651(9) 0.0364(4) 0.039(3) Uani 1 d . . . H93 H 0.0579 -0.3373 0.0357 0.037(3) Uiso 1 calc R . . C94 C 0.0626(4) -0.1798(9) 0.0002(4) 0.042(3) Uani 1 d . . . H94 H 0.0339 -0.1942 -0.0252 0.037(3) Uiso 1 calc R . . C95 C 0.0903(4) -0.0723(8) 0.0011(4) 0.035(2) Uani 1 d . . . H95 H 0.0802 -0.0131 -0.0232 0.037(3) Uiso 1 calc R . . C96 C 0.1326(4) -0.0544(8) 0.0382(4) 0.032(2) Uani 1 d . . . H96 H 0.1514 0.0181 0.0384 0.037(3) Uiso 1 calc R . . C101 C 0.2528(4) -0.2774(7) 0.1301(3) 0.022(2) Uani 1 d . . . C102 C 0.2857(4) -0.3106(8) 0.0896(4) 0.031(2) Uani 1 d . . . H102 H 0.2904 -0.2578 0.0621 0.037(3) Uiso 1 calc R . . C103 C 0.3118(4) -0.4212(7) 0.0892(4) 0.033(2) Uani 1 d . . . H103 H 0.3346 -0.4420 0.0624 0.037(3) Uiso 1 calc R . . C104 C 0.3028(4) -0.4994(7) 0.1298(4) 0.037(3) Uani 1 d . . . H104 H 0.3190 -0.5747 0.1293 0.037(3) Uiso 1 calc R . . C105 C 0.2706(4) -0.4696(7) 0.1709(4) 0.034(2) Uani 1 d . . . H105 H 0.2660 -0.5233 0.1981 0.037(3) Uiso 1 calc R . . C106 C 0.2449(4) -0.3583(7) 0.1713(3) 0.025(2) Uani 1 d . . . H106 H 0.2227 -0.3375 0.1986 0.037(3) Uiso 1 calc R . . C111 C 0.3575(5) 0.1634(8) 0.0374(4) 0.035(2) Uani 1 d . . . C112 C 0.3155(5) 0.2460(8) 0.0367(4) 0.042(3) Uani 1 d . . . H112 H 0.2851 0.2350 0.0573 0.037(3) Uiso 1 calc R . . C113 C 0.3182(6) 0.3467(9) 0.0049(5) 0.059(3) Uani 1 d . . . H113 H 0.2882 0.3995 0.0032 0.037(3) Uiso 1 calc R . . C114 C 0.3623(7) 0.3698(10) -0.0230(4) 0.060(4) Uani 1 d . . . H114 H 0.3645 0.4402 -0.0419 0.037(3) Uiso 1 calc R . . C115 C 0.4035(6) 0.2881(12) -0.0229(4) 0.068(4) Uani 1 d . . . H115 H 0.4339 0.3012 -0.0434 0.037(3) Uiso 1 calc R . . C116 C 0.4018(5) 0.1838(10) 0.0071(4) 0.053(3) Uani 1 d . . . H116 H 0.4307 0.1286 0.0064 0.037(3) Uiso 1 calc R . . C121 C 0.3793(4) -0.1173(7) 0.0253(4) 0.032(2) Uani 1 d . . . C122 C 0.4289(5) -0.1796(9) 0.0314(4) 0.052(3) Uani 1 d . . . H122 H 0.4531 -0.1661 0.0606 0.037(3) Uiso 1 calc R . . C123 C 0.4426(5) -0.2621(11) -0.0060(5) 0.070(4) Uani 1 d . . . H123 H 0.4757 -0.3051 -0.0010 0.037(3) Uiso 1 calc R . . C124 C 0.4092(5) -0.2817(9) -0.0494(4) 0.047(3) Uani 1 d . . . H124 H 0.4200 -0.3362 -0.0743 0.037(3) Uiso 1 calc R . . C125 C 0.3600(5) -0.2229(8) -0.0571(4) 0.041(3) Uani 1 d . . . H125 H 0.3363 -0.2382 -0.0865 0.037(3) Uiso 1 calc R . . C126 C 0.3458(5) -0.1388(9) -0.0201(4) 0.044(3) Uani 1 d . . . H126 H 0.3128 -0.0956 -0.0259 0.037(3) Uiso 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 I1 0.0272(4) 0.0223(3) 0.0278(3) 0.0051(2) 0.0012(3) -0.0047(2) I2 0.0290(4) 0.0230(3) 0.0247(3) 0.0017(2) 0.0036(3) -0.0056(2) Sb1 0.0225(4) 0.0206(3) 0.0174(3) -0.0008(2) 0.0024(3) 0.0000(2) Sb2 0.0213(4) 0.0203(3) 0.0182(3) 0.0024(2) 0.0003(3) 0.0001(2) Sb3 0.0210(4) 0.0236(3) 0.0171(3) 0.0033(2) 0.0007(3) 0.0015(2) Sb4 0.0244(4) 0.0325(3) 0.0260(4) 0.0024(3) 0.0037(3) -0.0003(3) Sb5 0.0237(4) 0.0204(3) 0.0169(3) 0.0003(2) 0.0032(3) 0.0006(2) Sb6 0.0300(4) 0.0345(3) 0.0241(4) 0.0014(3) 0.0025(3) -0.0024(3) Ru1 0.0200(4) 0.0178(3) 0.0148(4) 0.0011(3) 0.0017(3) -0.0004(3) C1 0.031(6) 0.020(4) 0.022(5) 0.001(4) -0.001(4) 0.003(4) C2 0.025(6) 0.031(5) 0.029(5) 0.000(4) 0.000(4) -0.005(4) C3 0.026(6) 0.029(5) 0.020(5) 0.007(4) -0.001(4) 0.001(4) C11 0.027(6) 0.020(4) 0.015(5) -0.006(3) 0.001(4) 0.004(4) C12 0.040(7) 0.023(5) 0.031(6) -0.004(4) -0.005(5) -0.012(4) C13 0.056(8) 0.048(6) 0.028(6) 0.002(5) -0.005(5) -0.009(6) C14 0.058(9) 0.039(6) 0.043(7) -0.016(5) -0.018(6) -0.005(5) C15 0.038(7) 0.031(5) 0.052(7) -0.008(5) 0.006(6) -0.015(5) C16 0.034(6) 0.027(5) 0.036(6) -0.005(4) 0.013(5) -0.006(4) C21 0.024(6) 0.018(4) 0.025(5) -0.003(4) 0.002(4) 0.001(4) C22 0.053(8) 0.030(5) 0.030(6) 0.017(4) 0.008(5) 0.009(5) C23 0.035(7) 0.063(7) 0.059(8) 0.013(6) 0.021(6) 0.011(6) C24 0.027(6) 0.042(6) 0.047(7) 0.002(5) 0.021(5) -0.005(5) C25 0.043(7) 0.032(5) 0.027(6) 0.008(4) 0.015(5) -0.005(5) C26 0.037(7) 0.027(5) 0.023(5) -0.007(4) 0.003(5) 0.011(4) C31 0.022(6) 0.025(5) 0.020(5) 0.004(4) 0.000(4) -0.005(4) C32 0.028(6) 0.025(5) 0.027(5) 0.002(4) -0.005(4) 0.004(4) C33 0.029(6) 0.028(5) 0.034(6) 0.001(4) -0.001(5) -0.002(4) C34 0.020(6) 0.040(6) 0.047(6) -0.001(5) 0.001(5) -0.010(4) C35 0.026(7) 0.039(6) 0.056(7) -0.014(5) 0.006(5) 0.002(5) C36 0.037(7) 0.022(5) 0.043(6) -0.005(4) -0.004(5) 0.001(4) C41 0.018(5) 0.019(4) 0.027(5) 0.000(4) 0.003(4) 0.002(4) C42 0.023(6) 0.029(5) 0.024(5) 0.002(4) 0.001(4) -0.002(4) C43 0.031(6) 0.025(5) 0.037(6) 0.007(4) 0.013(5) 0.001(4) C44 0.042(7) 0.029(5) 0.021(5) 0.008(4) 0.008(5) 0.001(5) C45 0.036(7) 0.036(5) 0.022(5) 0.004(4) -0.004(5) 0.003(5) C46 0.019(5) 0.025(5) 0.027(5) -0.005(4) -0.003(4) 0.003(4) C51 0.028(6) 0.030(5) 0.023(5) 0.005(4) 0.002(4) 0.001(4) C52 0.027(6) 0.030(5) 0.020(5) 0.004(4) 0.000(4) -0.001(4) C53 0.028(6) 0.039(5) 0.026(5) -0.002(4) 0.005(4) -0.005(4) C54 0.027(6) 0.056(7) 0.033(6) 0.011(5) 0.007(5) 0.004(5) C55 0.026(6) 0.032(5) 0.032(6) 0.009(4) 0.005(5) -0.003(4) C56 0.023(6) 0.036(5) 0.025(5) -0.005(4) -0.006(4) 0.003(4) C61 0.031(6) 0.021(4) 0.022(5) 0.000(4) -0.004(4) 0.002(4) C62 0.030(6) 0.042(5) 0.021(5) 0.009(4) 0.006(4) 0.010(5) C63 0.032(7) 0.040(6) 0.042(6) 0.003(5) 0.007(5) 0.013(5) C64 0.023(6) 0.047(6) 0.043(7) -0.019(5) 0.000(5) 0.009(5) C65 0.028(6) 0.048(6) 0.027(6) -0.012(5) 0.005(5) -0.007(5) C66 0.019(6) 0.038(5) 0.020(5) -0.002(4) 0.000(4) -0.001(4) C71 0.042(7) 0.033(5) 0.025(5) 0.009(4) -0.004(5) 0.005(5) C72 0.045(7) 0.037(6) 0.039(6) -0.004(5) 0.013(5) -0.010(5) C73 0.068(9) 0.039(6) 0.044(7) -0.004(5) 0.012(6) -0.004(6) C74 0.067(9) 0.044(6) 0.035(7) 0.007(5) -0.009(6) 0.001(6) C75 0.032(7) 0.033(6) 0.068(8) 0.018(5) -0.005(6) -0.004(5) C76 0.027(7) 0.038(6) 0.062(8) 0.006(5) 0.010(6) 0.000(5) C81 0.033(6) 0.033(5) 0.022(5) 0.000(4) 0.002(4) 0.002(4) C82 0.034(7) 0.042(6) 0.032(6) -0.002(5) 0.007(5) -0.004(5) C83 0.050(8) 0.063(8) 0.034(7) 0.003(5) -0.005(6) -0.007(6) C84 0.041(8) 0.063(8) 0.040(7) 0.023(6) 0.000(6) 0.015(6) C85 0.054(8) 0.033(6) 0.040(7) 0.002(5) -0.002(6) 0.006(5) C86 0.028(6) 0.044(6) 0.036(6) 0.002(5) 0.001(5) -0.002(5) C91 0.030(6) 0.022(4) 0.019(5) 0.001(4) 0.007(4) 0.005(4) C92 0.034(7) 0.031(5) 0.035(6) -0.001(4) 0.009(5) 0.005(5) C93 0.029(7) 0.039(6) 0.049(7) -0.021(5) -0.009(5) -0.004(5) C94 0.030(7) 0.053(7) 0.039(6) -0.027(5) -0.018(5) 0.010(5) C95 0.038(7) 0.042(6) 0.025(6) 0.000(4) 0.001(5) 0.019(5) C96 0.033(6) 0.027(5) 0.037(6) 0.000(4) 0.006(5) 0.003(4) C101 0.019(5) 0.024(4) 0.020(5) -0.005(4) -0.006(4) 0.004(4) C102 0.028(6) 0.034(5) 0.031(6) -0.001(4) 0.006(5) 0.000(4) C103 0.026(6) 0.033(5) 0.041(6) -0.011(4) 0.003(5) 0.008(4) C104 0.047(7) 0.021(5) 0.044(7) -0.005(4) 0.004(5) 0.007(4) C105 0.049(7) 0.018(5) 0.034(6) 0.006(4) -0.003(5) -0.001(4) C106 0.034(6) 0.026(5) 0.016(5) -0.001(4) 0.002(4) 0.002(4) C111 0.046(7) 0.029(5) 0.029(6) -0.007(4) 0.003(5) -0.013(5) C112 0.052(8) 0.036(6) 0.036(6) 0.004(5) -0.002(5) -0.015(5) C113 0.078(11) 0.040(7) 0.057(8) -0.002(6) -0.020(7) 0.004(6) C114 0.095(12) 0.044(7) 0.040(7) 0.007(5) 0.008(7) -0.001(7) C115 0.074(11) 0.096(10) 0.036(7) 0.005(7) 0.016(7) -0.043(9) C116 0.049(8) 0.060(7) 0.049(7) 0.008(6) 0.010(6) -0.014(6) C121 0.034(7) 0.029(5) 0.033(6) 0.006(4) 0.001(5) -0.003(4) C122 0.035(8) 0.067(8) 0.052(8) -0.013(6) -0.016(6) 0.003(6) C123 0.042(9) 0.076(9) 0.093(11) -0.022(8) 0.009(8) 0.022(7) C124 0.057(9) 0.043(6) 0.045(7) -0.012(5) 0.030(7) 0.001(6) C125 0.043(8) 0.043(6) 0.038(6) -0.008(5) 0.004(5) -0.007(5) C126 0.035(7) 0.058(7) 0.038(7) 0.013(5) 0.002(5) 0.009(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 I1 Ru1 2.7331(8) . ? I2 Ru1 2.7287(8) . ? Sb1 C21 2.123(8) . ? Sb1 C11 2.141(8) . ? Sb1 C1 2.155(8) . ? Sb1 Ru1 2.5988(8) . ? Sb1 Sb2 3.1526(8) . ? Sb2 C31 2.126(9) . ? Sb2 C41 2.156(8) . ? Sb2 C1 2.173(8) . ? Sb2 Ru1 2.6238(9) . ? Sb3 C61 2.131(8) . ? Sb3 C2 2.141(8) . ? Sb3 C51 2.148(8) . ? Sb3 Ru1 2.5841(9) . ? Sb4 C81 2.154(9) . ? Sb4 C2 2.160(8) . ? Sb4 C71 2.179(9) . ? Sb5 C101 2.122(8) . ? Sb5 C3 2.142(8) . ? Sb5 C91 2.153(9) . ? Sb5 Ru1 2.5780(8) . ? Sb6 C3 2.144(9) . ? Sb6 C111 2.171(9) . ? Sb6 C121 2.180(9) . ? C11 C12 1.375(11) . ? C11 C16 1.386(11) . ? C12 C13 1.375(12) . ? C13 C14 1.358(14) . ? C14 C15 1.385(13) . ? C15 C16 1.372(12) . ? C21 C26 1.373(11) . ? C21 C22 1.389(13) . ? C22 C23 1.387(13) . ? C23 C24 1.366(13) . ? C24 C25 1.379(13) . ? C25 C26 1.368(12) . ? C31 C36 1.384(12) . ? C31 C32 1.395(11) . ? C32 C33 1.401(12) . ? C33 C34 1.362(12) . ? C34 C35 1.380(12) . ? C35 C36 1.367(13) . ? C41 C42 1.378(11) . ? C41 C46 1.398(11) . ? C42 C43 1.384(11) . ? C43 C44 1.356(13) . ? C44 C45 1.380(12) . ? C45 C46 1.390(11) . ? C51 C52 1.385(11) . ? C51 C56 1.400(12) . ? C52 C53 1.368(11) . ? C53 C54 1.347(12) . ? C54 C55 1.390(12) . ? C55 C56 1.373(11) . ? C61 C66 1.384(11) . ? C61 C62 1.397(11) . ? C62 C63 1.383(12) . ? C63 C64 1.369(13) . ? C64 C65 1.375(13) . ? C65 C66 1.372(12) . ? C71 C76 1.381(13) . ? C71 C72 1.389(13) . ? C72 C73 1.384(13) . ? C73 C74 1.370(15) . ? C74 C75 1.376(14) . ? C75 C76 1.387(13) . ? C81 C86 1.389(11) . ? C81 C82 1.414(13) . ? C82 C83 1.378(14) . ? C83 C84 1.372(13) . ? C84 C85 1.404(14) . ? C85 C86 1.399(13) . ? C91 C96 1.373(11) . ? C91 C92 1.395(12) . ? C92 C93 1.383(13) . ? C93 C94 1.359(13) . ? C94 C95 1.377(13) . ? C95 C96 1.358(13) . ? C101 C102 1.386(11) . ? C101 C106 1.410(11) . ? C102 C103 1.389(12) . ? C103 C104 1.385(12) . ? C104 C105 1.377(13) . ? C105 C106 1.392(11) . ? C111 C116 1.365(14) . ? C111 C112 1.367(14) . ? C112 C113 1.395(13) . ? C113 C114 1.330(16) . ? C114 C115 1.346(17) . ? C115 C116 1.401(14) . ? C121 C122 1.378(14) . ? C121 C126 1.387(13) . ? C122 C123 1.382(15) . ? C123 C124 1.345(15) . ? C124 C125 1.352(14) . ? C125 C126 1.392(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Sb1 C11 99.6(3) . . ? C21 Sb1 C1 103.7(3) . . ? C11 Sb1 C1 105.1(3) . . ? C21 Sb1 Ru1 121.3(2) . . ? C11 Sb1 Ru1 129.3(2) . . ? C1 Sb1 Ru1 93.8(2) . . ? C21 Sb1 Sb2 109.3(2) . . ? C11 Sb1 Sb2 140.9(2) . . ? C1 Sb1 Sb2 43.5(2) . . ? Ru1 Sb1 Sb2 53.23(2) . . ? C31 Sb2 C41 100.7(3) . . ? C31 Sb2 C1 101.0(3) . . ? C41 Sb2 C1 101.7(3) . . ? C31 Sb2 Ru1 123.1(2) . . ? C41 Sb2 Ru1 130.3(2) . . ? C1 Sb2 Ru1 92.6(2) . . ? C31 Sb2 Sb1 108.2(2) . . ? C41 Sb2 Sb1 137.4(2) . . ? C1 Sb2 Sb1 43.0(2) . . ? Ru1 Sb2 Sb1 52.51(2) . . ? C61 Sb3 C2 99.8(3) . . ? C61 Sb3 C51 101.8(3) . . ? C2 Sb3 C51 96.9(3) . . ? C61 Sb3 Ru1 120.4(2) . . ? C2 Sb3 Ru1 116.9(2) . . ? C51 Sb3 Ru1 117.0(2) . . ? C81 Sb4 C2 95.7(3) . . ? C81 Sb4 C71 93.4(3) . . ? C2 Sb4 C71 96.8(3) . . ? C101 Sb5 C3 100.4(3) . . ? C101 Sb5 C91 96.3(3) . . ? C3 Sb5 C91 93.6(3) . . ? C101 Sb5 Ru1 125.5(2) . . ? C3 Sb5 Ru1 119.0(2) . . ? C91 Sb5 Ru1 115.5(2) . . ? C3 Sb6 C111 93.6(4) . . ? C3 Sb6 C121 96.7(4) . . ? C111 Sb6 C121 95.2(3) . . ? Sb5 Ru1 Sb3 101.33(3) . . ? Sb5 Ru1 Sb1 166.80(4) . . ? Sb3 Ru1 Sb1 91.56(3) . . ? Sb5 Ru1 Sb2 93.15(3) . . ? Sb3 Ru1 Sb2 164.81(3) . . ? Sb1 Ru1 Sb2 74.26(2) . . ? Sb5 Ru1 I2 85.47(2) . . ? Sb3 Ru1 I2 92.15(3) . . ? Sb1 Ru1 I2 91.27(3) . . ? Sb2 Ru1 I2 93.56(3) . . ? Sb5 Ru1 I1 91.54(3) . . ? Sb3 Ru1 I1 87.75(3) . . ? Sb1 Ru1 I1 91.80(3) . . ? Sb2 Ru1 I1 87.30(2) . . ? I2 Ru1 I1 176.93(3) . . ? Sb1 C1 Sb2 93.5(3) . . ? Sb3 C2 Sb4 118.9(4) . . ? Sb5 C3 Sb6 122.2(4) . . ? C12 C11 C16 118.9(8) . . ? C12 C11 Sb1 120.0(6) . . ? C16 C11 Sb1 121.1(6) . . ? C11 C12 C13 119.9(9) . . ? C14 C13 C12 120.7(10) . . ? C13 C14 C15 120.5(9) . . ? C16 C15 C14 118.6(9) . . ? C15 C16 C11 121.3(9) . . ? C26 C21 C22 118.6(8) . . ? C26 C21 Sb1 120.8(7) . . ? C22 C21 Sb1 120.5(6) . . ? C23 C22 C21 119.9(9) . . ? C24 C23 C22 120.0(10) . . ? C23 C24 C25 120.3(9) . . ? C26 C25 C24 119.3(9) . . ? C25 C26 C21 121.6(9) . . ? C36 C31 C32 117.9(8) . . ? C36 C31 Sb2 121.8(6) . . ? C32 C31 Sb2 120.2(6) . . ? C31 C32 C33 119.6(8) . . ? C34 C33 C32 121.7(8) . . ? C33 C34 C35 118.1(9) . . ? C36 C35 C34 121.4(9) . . ? C35 C36 C31 121.3(8) . . ? C42 C41 C46 119.5(8) . . ? C42 C41 Sb2 121.1(6) . . ? C46 C41 Sb2 119.4(6) . . ? C41 C42 C43 119.9(9) . . ? C44 C43 C42 120.9(9) . . ? C43 C44 C45 120.1(8) . . ? C44 C45 C46 120.0(9) . . ? C45 C46 C41 119.4(8) . . ? C52 C51 C56 117.6(8) . . ? C52 C51 Sb3 120.2(6) . . ? C56 C51 Sb3 122.1(6) . . ? C53 C52 C51 120.7(8) . . ? C54 C53 C52 121.1(9) . . ? C53 C54 C55 120.3(9) . . ? C56 C55 C54 118.9(8) . . ? C55 C56 C51 121.3(8) . . ? C66 C61 C62 117.9(8) . . ? C66 C61 Sb3 117.2(6) . . ? C62 C61 Sb3 124.9(6) . . ? C63 C62 C61 120.9(8) . . ? C64 C63 C62 119.4(9) . . ? C63 C64 C65 120.8(9) . . ? C66 C65 C64 119.7(9) . . ? C65 C66 C61 121.3(8) . . ? C76 C71 C72 118.2(9) . . ? C76 C71 Sb4 116.2(7) . . ? C72 C71 Sb4 125.5(7) . . ? C73 C72 C71 120.3(10) . . ? C74 C73 C72 121.2(10) . . ? C73 C74 C75 118.9(10) . . ? C74 C75 C76 120.4(10) . . ? C71 C76 C75 121.0(10) . . ? C86 C81 C82 117.0(9) . . ? C86 C81 Sb4 118.6(7) . . ? C82 C81 Sb4 124.1(6) . . ? C83 C82 C81 121.7(9) . . ? C84 C83 C82 120.0(10) . . ? C83 C84 C85 120.8(10) . . ? C86 C85 C84 118.2(9) . . ? C81 C86 C85 122.3(9) . . ? C96 C91 C92 116.8(9) . . ? C96 C91 Sb5 120.9(7) . . ? C92 C91 Sb5 122.2(6) . . ? C93 C92 C91 120.3(9) . . ? C94 C93 C92 120.5(9) . . ? C93 C94 C95 120.2(9) . . ? C96 C95 C94 118.6(9) . . ? C95 C96 C91 123.5(9) . . ? C102 C101 C106 119.3(7) . . ? C102 C101 Sb5 119.7(6) . . ? C106 C101 Sb5 121.0(6) . . ? C101 C102 C103 121.3(8) . . ? C104 C103 C102 118.3(8) . . ? C105 C104 C103 122.2(8) . . ? C104 C105 C106 119.3(8) . . ? C105 C106 C101 119.7(8) . . ? C116 C111 C112 118.1(9) . . ? C116 C111 Sb6 120.2(8) . . ? C112 C111 Sb6 121.7(7) . . ? C111 C112 C113 119.9(11) . . ? C114 C113 C112 122.2(12) . . ? C113 C114 C115 118.0(11) . . ? C114 C115 C116 121.6(12) . . ? C111 C116 C115 119.9(12) . . ? C122 C121 C126 117.2(9) . . ? C122 C121 Sb6 119.5(8) . . ? C126 C121 Sb6 123.2(7) . . ? C121 C122 C123 119.9(11) . . ? C124 C123 C122 121.6(11) . . ? C123 C124 C125 120.6(10) . . ? C124 C125 C126 118.6(10) . . ? C121 C126 C125 122.0(10) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.208 _refine_diff_density_min -1.616 _refine_diff_density_rms 0.333 # --------------------------------------------------------------- #===END ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 7 October 1991 ### ############################################################################## #============================================================================== data_global2 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof W Levason' _publ_contact_author_address ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; _publ_contact_author_phone '023 80 593792' _publ_contact_author_fax ? _publ_contact_author_email 'wxl@soton.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; J. Chem. Soc., Dalton Trans., Paper ref. 9/08296D ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, properties and structures of complexes of platinum metal halides and Group 11 metals with two distibinomethane ligands, R~2~SbCH~2~SbR~2~ (R = Me or Ph) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Even, Tina' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Genge, Anthony R. J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Hill, Angela M.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Holmes, Nicholas J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Levason, William' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Webster, Michael' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; #============================================================================== # 4. TEXT _publ_section_references ; Molecular Structure Corporation (1988) MSC/AFC Diffractometer Control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1997) SHELXL97, Program for the Refinement of Crystal Structures, University of G\"ottingen, Germany. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W.P., Garcia-Granda, S., Gould, R.O., Smits, J.M.M. and Smykalla, C. (1992). The DIRDIF program system, Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. ; #============================================================================== data_tepdbr #============================================================================== # 5. CHEMICAL DATA _audit_creation_method 'teXsan v. 1.8' _chemical_name_systematic ; Tetrabromodi(\m-bisdiphenylstibinomethane)dipalladium(II).2dichloromethane ; _chemical_name_common ? _chemical_formula_moiety 'C50 H44 Br4 Pd2 Sb4, 2(C1 H2 Cl2)' _chemical_formula_sum 'C52 H48 Br4 Cl4 Pd2 Sb4' # _chemical_formula_weight ? #============================================================================== # 6. CRYSTAL DATA #------------------------------------------------------------------------------ _audit_creation_date '1999-09-21' _audit_update_record ; ? ; #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; DIRDIF92 PATTY (Beurskens, 1992) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 15.953(5) _cell_length_b 17.000(4) _cell_length_c 11.943(3) _cell_angle_alpha 109.18(2) _cell_angle_beta 109.95(2) _cell_angle_gamma 79.65(2) _cell_volume 2867(1) _cell_formula_units_Z 2 _cell_measurement_temperature 150 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 7.0 _cell_measurement_theta_max 8.1 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ; _exptl_crystal_description 'block' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1834.18 # _chemical_formula_analytical ? # _chemical_formula_sum 'C52 H48 Br4 Cl4 Pd2 Sb4 ' # _chemical_formula_moiety '?' # _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 1728.00 _exptl_absorpt_coefficient_mu 5.485 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.491 _exptl_special_details ; The scan width was (1.47+0.35tan\q)\% with an \w scan speed of 0\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.69 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -4 -2 -2 2 -3 3 5 -4 _diffrn_reflns_number 10476 _reflns_number_total 10080 _reflns_number_gt 5415 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05148 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00681 _diffrn_orient_matrix_UB_12 -0.01876 _diffrn_orient_matrix_UB_13 -0.09105 _diffrn_orient_matrix_UB_21 -0.01218 _diffrn_orient_matrix_UB_22 -0.05697 _diffrn_orient_matrix_UB_23 -0.00515 _diffrn_orient_matrix_UB_31 -0.06541 _diffrn_orient_matrix_UB_32 0.01743 _diffrn_orient_matrix_UB_33 -0.01846 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 104 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 96 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; Br 0 8 -0.374 2.456 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pd 0 4 -1.177 1.007 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb 0 8 -0.816 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 8 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Sb(1) 0.0719(1) 0.3208(1) 0.3473(1) 0.0250(4) 1.000 . Uani d ? Sb(2) 0.2384(1) 0.4216(1) 0.3135(1) 0.0272(5) 1.000 . Uani d ? Sb(3) 0.4144(1) 0.1500(1) 0.3773(1) 0.0267(5) 1.000 . Uani d ? Sb(4) 0.1963(1) 0.1103(1) 0.3726(1) 0.0253(4) 1.000 . Uani d ? Pd(1) 0.3296(1) 0.2822(1) 0.3245(2) 0.0269(5) 1.000 . Uani d ? Pd(2) 0.1486(1) 0.1979(1) 0.2252(1) 0.0242(5) 1.000 . Uani d ? Br(1) 0.2993(2) 0.3122(2) 0.5218(2) 0.0332(7) 1.000 . Uani d ? Br(2) 0.3778(2) 0.2608(2) 0.1447(2) 0.0450(9) 1.000 . Uani d ? Br(3) 0.1014(2) 0.2833(2) 0.0772(2) 0.0311(7) 1.000 . Uani d ? Br(4) 0.2173(2) 0.0768(2) 0.0946(2) 0.0353(7) 1.000 . Uani d ? Cl(1) 0.439(2) 0.335(2) 0.934(2) 0.111(8) 0.417 . Uiso d ? Cl(2) 0.428(1) 0.463(1) 0.838(2) 0.087(7) 0.417 . Uiso d ? Cl(3) 0.6922(7) 0.1208(6) 0.1619(9) 0.047(3) 0.655 . Uiso d ? Cl(4) 0.8529(8) 0.1166(7) 0.362(1) 0.062(3) 0.655 . Uiso d ? C(1) 0.113(1) 0.439(1) 0.361(2) 0.027(5) 1.000 . Uiso d ? C(2) 0.339(1) 0.076(1) 0.419(2) 0.031(6) 1.000 . Uiso d ? C(3) 0.064(1) 0.341(1) 0.530(2) 0.024(5) 1.000 . Uiso d ? C(4) 0.120(2) 0.392(2) 0.634(2) 0.042(7) 1.000 . Uiso d ? C(5) 0.114(2) 0.401(2) 0.753(2) 0.045(7) 1.000 . Uiso d ? C(6) 0.055(2) 0.358(2) 0.762(2) 0.048(7) 1.000 . Uiso d ? C(7) -0.003(2) 0.312(2) 0.663(2) 0.042(7) 1.000 . Uiso d ? C(8) 0.001(1) 0.304(1) 0.543(2) 0.030(6) 1.000 . Uiso d ? C(9) -0.069(1) 0.317(1) 0.251(2) 0.025(5) 1.000 . Uiso d ? C(10) -0.097(2) 0.250(2) 0.153(2) 0.037(6) 1.000 . Uiso d ? C(11) -0.194(2) 0.245(2) 0.095(2) 0.046(7) 1.000 . Uiso d ? C(12) -0.252(2) 0.310(2) 0.142(2) 0.047(7) 1.000 . Uiso d ? C(13) -0.220(2) 0.377(2) 0.241(2) 0.049(7) 1.000 . Uiso d ? C(14) -0.125(2) 0.383(2) 0.301(2) 0.037(6) 1.000 . Uiso d ? C(15) 0.206(1) 0.481(1) 0.170(2) 0.028(5) 1.000 . Uiso d ? C(16) 0.120(2) 0.518(2) 0.133(2) 0.045(7) 1.000 . Uiso d ? C(17) 0.103(2) 0.570(2) 0.054(2) 0.049(7) 1.000 . Uiso d ? C(18) 0.176(2) 0.582(2) 0.020(2) 0.048(7) 1.000 . Uiso d ? C(19) 0.259(2) 0.543(2) 0.053(3) 0.068(9) 1.000 . Uiso d ? C(20) 0.272(2) 0.489(2) 0.132(2) 0.044(7) 1.000 . Uiso d ? C(21) 0.301(1) 0.521(1) 0.459(2) 0.029(6) 1.000 . Uiso d ? C(22) 0.257(2) 0.605(2) 0.467(2) 0.042(7) 1.000 . Uiso d ? C(23) 0.304(2) 0.674(2) 0.560(2) 0.056(8) 1.000 . Uiso d ? C(24) 0.385(2) 0.663(2) 0.641(2) 0.057(8) 1.000 . Uiso d ? C(25) 0.429(2) 0.580(2) 0.630(2) 0.057(8) 1.000 . Uiso d ? C(26) 0.388(2) 0.512(2) 0.541(2) 0.047(7) 1.000 . Uiso d ? C(27) 0.515(1) 0.191(1) 0.555(2) 0.029(5) 1.000 . Uiso d ? C(28) 0.555(2) 0.260(2) 0.573(2) 0.037(6) 1.000 . Uiso d ? C(29) 0.624(2) 0.288(2) 0.683(2) 0.053(8) 1.000 . Uiso d ? C(30) 0.645(2) 0.247(2) 0.775(2) 0.045(7) 1.000 . Uiso d ? C(31) 0.606(2) 0.178(2) 0.756(2) 0.048(7) 1.000 . Uiso d ? C(32) 0.536(2) 0.148(2) 0.641(2) 0.038(6) 1.000 . Uiso d ? C(33) 0.495(2) 0.058(1) 0.280(2) 0.034(6) 1.000 . Uiso d ? C(34) 0.587(2) 0.047(2) 0.340(2) 0.039(6) 1.000 . Uiso d ? C(35) 0.638(2) -0.018(2) 0.276(2) 0.049(7) 1.000 . Uiso d ? C(36) 0.598(2) -0.070(2) 0.157(2) 0.045(7) 1.000 . Uiso d ? C(37) 0.511(2) -0.054(2) 0.097(3) 0.08(1) 1.000 . Uiso d ? C(38) 0.455(2) 0.010(2) 0.163(2) 0.053(7) 1.000 . Uiso d ? C(39) 0.147(1) -0.009(1) 0.289(2) 0.028(5) 1.000 . Uiso d ? C(40) 0.189(2) -0.076(2) 0.339(2) 0.035(6) 1.000 . Uiso d ? C(41) 0.157(2) -0.155(1) 0.284(2) 0.034(6) 1.000 . Uiso d ? C(42) 0.082(2) -0.171(2) 0.174(2) 0.039(6) 1.000 . Uiso d ? C(43) 0.038(2) -0.103(2) 0.130(2) 0.036(6) 1.000 . Uiso d ? C(44) 0.071(2) -0.020(1) 0.183(2) 0.034(6) 1.000 . Uiso d ? C(45) 0.175(1) 0.134(1) 0.547(2) 0.025(5) 1.000 . Uiso d ? C(46) 0.220(2) 0.182(2) 0.657(2) 0.040(6) 1.000 . Uiso d ? C(47) 0.204(2) 0.193(1) 0.772(2) 0.035(6) 1.000 . Uiso d ? C(48) 0.145(2) 0.153(2) 0.776(2) 0.052(7) 1.000 . Uiso d ? C(49) 0.089(2) 0.104(2) 0.665(2) 0.050(7) 1.000 . Uiso d ? C(50) 0.105(2) 0.090(2) 0.544(2) 0.044(7) 1.000 . Uiso d ? C(51) 0.460(3) 0.373(3) 0.846(4) 0.02(1) 0.417 . Uiso d ? C(52) 0.801(2) 0.076(2) 0.207(3) 0.036(9) 0.655 . Uiso 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Sb(1) 0.0289(9) 0.0248(9) 0.0217(8) 0.0002(8) 0.0097(7) 0.0063(7) Sb(2) 0.0293(9) 0.028(1) 0.0271(8) 0.0002(8) 0.0101(7) 0.0102(7) Sb(3) 0.0252(9) 0.027(1) 0.0291(8) 0.0012(8) 0.0099(7) 0.0095(7) Sb(4) 0.0270(9) 0.0249(9) 0.0232(8) -0.0035(7) 0.0061(7) 0.0064(7) Pd(1) 0.028(1) 0.026(1) 0.027(1) -0.0014(8) 0.0081(8) 0.0076(8) Pd(2) 0.026(1) 0.027(1) 0.0188(8) -0.0012(8) 0.0069(7) 0.0053(7) Br(1) 0.035(1) 0.038(2) 0.028(1) -0.001(1) 0.012(1) 0.010(1) Br(2) 0.046(2) 0.056(2) 0.037(1) -0.007(1) 0.019(1) 0.011(1) Br(3) 0.037(1) 0.033(2) 0.023(1) -0.002(1) 0.007(1) 0.011(1) Br(4) 0.041(2) 0.035(2) 0.028(1) 0.004(1) 0.015(1) 0.005(1) #------------------------------------------------------------------------------ _refine_special_details ; The sof of the two CH2Cl2 molecules were lowered because of the high isotropic displacement parameters. This affects: C51, Cl1, Cl2 (sof 0.417) and C52, Cl3, Cl4 (sof 0.655). The sofs were not refined during least squares. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5415 _refine_ls_number_parameters 315 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_all 0.0762 _refine_ls_wR_factor_ref 0.0762 _refine_ls_goodness_of_fit_all 2.469 _refine_ls_goodness_of_fit_ref 2.469 _refine_ls_shift/su_max 0.0620 _refine_ls_shift/su_mean 0.0036 _refine_diff_density_min -1.32 _refine_diff_density_max 2.29 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb(1) Pd(2) 2.507(2) . . yes Sb(1) C(1) 2.16(2) . . yes Sb(1) C(3) 2.14(2) . . yes Sb(1) C(9) 2.14(2) . . yes Sb(2) Pd(1) 2.567(2) . . yes Sb(2) C(1) 2.20(2) . . yes Sb(2) C(15) 2.14(2) . . yes Sb(2) C(21) 2.09(2) . . yes Sb(3) Pd(1) 2.556(2) . . yes Sb(3) C(2) 2.15(2) . . yes Sb(3) C(27) 2.16(2) . . yes Sb(3) C(33) 2.13(2) . . yes Sb(4) Pd(2) 2.510(2) . . yes Sb(4) C(2) 2.17(2) . . yes Sb(4) C(39) 2.10(2) . . yes Sb(4) C(45) 2.12(2) . . yes Pd(1) Br(1) 2.439(3) . . yes Pd(1) Br(2) 2.418(3) . . yes Pd(2) Br(3) 2.487(3) . . yes Pd(2) Br(4) 2.474(3) . . yes Cl(1) C(51) 1.56(5) . . yes Cl(2) C(51) 1.54(5) . . yes Cl(3) C(52) 1.75(4) . . yes Cl(4) C(52) 1.71(3) . . yes C(3) C(4) 1.38(3) . . yes C(3) C(8) 1.36(3) . . yes C(4) C(5) 1.42(3) . . yes C(5) C(6) 1.34(3) . . yes C(6) C(7) 1.34(3) . . yes C(7) C(8) 1.41(3) . . yes C(9) C(10) 1.34(3) . . yes C(9) C(14) 1.41(3) . . yes C(10) C(11) 1.48(3) . . yes C(11) C(12) 1.40(3) . . yes C(12) C(13) 1.37(3) . . yes C(13) C(14) 1.45(3) . . yes C(15) C(16) 1.38(3) . . yes C(15) C(20) 1.33(3) . . yes C(16) C(17) 1.42(3) . . yes C(17) C(18) 1.43(3) . . yes C(18) C(19) 1.35(4) . . yes C(19) C(20) 1.46(4) . . yes C(21) C(22) 1.46(3) . . yes C(21) C(26) 1.41(3) . . yes C(22) C(23) 1.43(3) . . yes C(23) C(24) 1.35(3) . . yes C(24) C(25) 1.45(4) . . yes C(25) C(26) 1.37(4) . . yes C(27) C(28) 1.37(3) . . yes C(27) C(32) 1.37(3) . . yes C(28) C(29) 1.40(3) . . yes C(29) C(30) 1.40(3) . . yes C(30) C(31) 1.34(3) . . yes C(31) C(32) 1.45(3) . . yes C(33) C(34) 1.41(3) . . yes C(33) C(38) 1.37(3) . . yes C(34) C(35) 1.42(3) . . yes C(35) C(36) 1.40(3) . . yes C(36) C(37) 1.36(4) . . yes C(37) C(38) 1.46(4) . . yes C(39) C(40) 1.42(3) . . yes C(39) C(44) 1.40(3) . . yes C(40) C(41) 1.39(3) . . yes C(41) C(42) 1.43(3) . . yes C(42) C(43) 1.39(3) . . yes C(43) C(44) 1.47(3) . . yes C(45) C(46) 1.34(3) . . yes C(45) C(50) 1.43(3) . . yes C(46) C(47) 1.43(3) . . yes C(47) C(48) 1.27(3) . . yes C(48) C(49) 1.41(3) . . yes C(49) C(50) 1.49(3) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Pd(2) Sb(1) C(1) 112.8(6) . . . yes Pd(2) Sb(1) C(3) 127.4(6) . . . yes Pd(2) Sb(1) C(9) 106.9(6) . . . yes C(1) Sb(1) C(3) 102.0(8) . . . yes C(1) Sb(1) C(9) 108.6(8) . . . yes C(3) Sb(1) C(9) 97.2(8) . . . yes Pd(1) Sb(2) C(1) 114.6(6) . . . yes Pd(1) Sb(2) C(15) 128.2(6) . . . yes Pd(1) Sb(2) C(21) 111.2(6) . . . yes C(1) Sb(2) C(15) 103.9(8) . . . yes C(1) Sb(2) C(21) 97.1(8) . . . yes C(15) Sb(2) C(21) 96.1(8) . . . yes Pd(1) Sb(3) C(2) 115.4(6) . . . yes Pd(1) Sb(3) C(27) 106.6(6) . . . yes Pd(1) Sb(3) C(33) 127.8(6) . . . yes C(2) Sb(3) C(27) 101.0(8) . . . yes C(2) Sb(3) C(33) 102.8(9) . . . yes C(27) Sb(3) C(33) 99.0(8) . . . yes Pd(2) Sb(4) C(2) 111.2(6) . . . yes Pd(2) Sb(4) C(39) 112.2(6) . . . yes Pd(2) Sb(4) C(45) 129.9(6) . . . yes C(2) Sb(4) C(39) 100.4(8) . . . yes C(2) Sb(4) C(45) 101.1(8) . . . yes C(39) Sb(4) C(45) 97.7(8) . . . yes Sb(2) Pd(1) Sb(3) 168.46(8) . . . yes Sb(2) Pd(1) Br(1) 84.53(8) . . . yes Sb(2) Pd(1) Br(2) 96.0(1) . . . yes Sb(3) Pd(1) Br(1) 83.94(8) . . . yes Sb(3) Pd(1) Br(2) 95.4(1) . . . yes Br(1) Pd(1) Br(2) 172.6(1) . . . yes Sb(1) Pd(2) Sb(4) 99.16(7) . . . yes Sb(1) Pd(2) Br(3) 81.41(8) . . . yes Sb(1) Pd(2) Br(4) 176.9(1) . . . yes Sb(4) Pd(2) Br(3) 179.4(1) . . . yes Sb(4) Pd(2) Br(4) 83.02(9) . . . yes Br(3) Pd(2) Br(4) 96.4(1) . . . yes Sb(1) C(1) Sb(2) 111.3(9) . . . yes Sb(3) C(2) Sb(4) 115(1) . . . yes Sb(1) C(3) C(4) 122(2) . . . yes Sb(1) C(3) C(8) 119(2) . . . yes C(4) C(3) C(8) 119(2) . . . yes C(3) C(4) C(5) 119(2) . . . yes C(4) C(5) C(6) 119(2) . . . yes C(5) C(6) C(7) 123(3) . . . yes C(6) C(7) C(8) 118(2) . . . yes C(3) C(8) C(7) 121(2) . . . yes Sb(1) C(9) C(10) 118(2) . . . yes Sb(1) C(9) C(14) 117(2) . . . yes C(10) C(9) C(14) 125(2) . . . yes C(9) C(10) C(11) 117(2) . . . yes C(10) C(11) C(12) 119(2) . . . yes C(11) C(12) C(13) 122(3) . . . yes C(12) C(13) C(14) 121(2) . . . yes C(9) C(14) C(13) 116(2) . . . yes Sb(2) C(15) C(16) 118(2) . . . yes Sb(2) C(15) C(20) 118(2) . . . yes C(16) C(15) C(20) 123(2) . . . yes C(15) C(16) C(17) 118(2) . . . yes C(16) C(17) C(18) 117(2) . . . yes C(17) C(18) C(19) 124(3) . . . yes C(18) C(19) C(20) 116(3) . . . yes C(15) C(20) C(19) 121(3) . . . yes Sb(2) C(21) C(22) 118(2) . . . yes Sb(2) C(21) C(26) 123(2) . . . yes C(22) C(21) C(26) 119(2) . . . yes C(21) C(22) C(23) 117(2) . . . yes C(22) C(23) C(24) 123(3) . . . yes C(23) C(24) C(25) 119(3) . . . yes C(24) C(25) C(26) 121(3) . . . yes C(21) C(26) C(25) 121(3) . . . yes Sb(3) C(27) C(28) 115(2) . . . yes Sb(3) C(27) C(32) 121(2) . . . yes C(28) C(27) C(32) 124(2) . . . yes C(27) C(28) C(29) 119(2) . . . yes C(28) C(29) C(30) 119(3) . . . yes C(29) C(30) C(31) 121(3) . . . yes C(30) C(31) C(32) 120(2) . . . yes C(27) C(32) C(31) 117(2) . . . yes Sb(3) C(33) C(34) 119(2) . . . yes Sb(3) C(33) C(38) 120(2) . . . yes C(34) C(33) C(38) 121(2) . . . yes C(33) C(34) C(35) 118(2) . . . yes C(34) C(35) C(36) 121(2) . . . yes C(35) C(36) C(37) 120(3) . . . yes C(36) C(37) C(38) 120(3) . . . yes C(33) C(38) C(37) 119(3) . . . yes Sb(4) C(39) C(40) 120(2) . . . yes Sb(4) C(39) C(44) 119(2) . . . yes C(40) C(39) C(44) 121(2) . . . yes C(39) C(40) C(41) 121(2) . . . yes C(40) C(41) C(42) 121(2) . . . yes C(41) C(42) C(43) 118(2) . . . yes C(42) C(43) C(44) 123(2) . . . yes C(39) C(44) C(43) 117(2) . . . yes Sb(4) C(45) C(46) 128(2) . . . yes Sb(4) C(45) C(50) 115(2) . . . yes C(46) C(45) C(50) 117(2) . . . yes C(45) C(46) C(47) 124(2) . . . yes C(46) C(47) C(48) 121(2) . . . yes C(47) C(48) C(49) 120(3) . . . yes C(48) C(49) C(50) 120(2) . . . yes C(45) C(50) C(49) 117(2) . . . yes Cl(1) C(51) Cl(2) 124(3) . . . yes Cl(3) C(52) Cl(4) 112(2) . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(3) C(11) 3.43(3) . 1_655 no Cl(3) C(35) 3.44(3) . . no Cl(3) C(12) 3.59(3) . 1_655 no C(6) C(16) 3.52(4) . 2_566 no C(11) C(52) 3.56(4) . 1_455 no C(13) C(23) 3.47(4) . 2_566 no C(30) C(41) 3.46(3) . 2_656 no C(30) C(51) 3.51(5) . . no C(35) C(46) 3.39(4) . 2_656 no C(35) C(47) 3.57(3) . 2_656 no C(36) C(47) 3.47(3) . 2_656 no C(37) C(37) 3.29(6) . 2_655 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Sb(1) Pd(2) Sb(4) C(2) . . . . -125.5(6) no Sb(1) Pd(2) Sb(4) C(39) . . . . 122.9(6) no Sb(1) Pd(2) Sb(4) C(45) . . . . 0.9(8) no Sb(1) C(1) Sb(2) Pd(1) . . . . -19(1) no Sb(1) C(1) Sb(2) C(15) . . . . 125.5(9) no Sb(1) C(1) Sb(2) C(21) . . . . -136(1) no Sb(1) C(3) C(4) C(5) . . . . -178(2) no Sb(1) C(3) C(8) C(7) . . . . 176(2) no Sb(1) C(9) C(10) C(11) . . . . 175(2) no Sb(1) C(9) C(14) C(13) . . . . -176(2) no Sb(2) Pd(1) Sb(3) C(2) . . . . 54.1(8) no Sb(2) Pd(1) Sb(3) C(27) . . . . -57.1(8) no Sb(2) Pd(1) Sb(3) C(33) . . . . -173.0(9) no Sb(2) C(1) Sb(1) Pd(2) . . . . -17(1) no Sb(2) C(1) Sb(1) C(3) . . . . 123.2(9) no Sb(2) C(1) Sb(1) C(9) . . . . -134.9(9) no Sb(2) C(15) C(16) C(17) . . . . 169(2) no Sb(2) C(15) C(20) C(19) . . . . -168(2) no Sb(2) C(21) C(22) C(23) . . . . -175(2) no Sb(2) C(21) C(26) C(25) . . . . 175(2) no Sb(3) Pd(1) Sb(2) C(1) . . . . -46.0(8) no Sb(3) Pd(1) Sb(2) C(15) . . . . 179.7(9) no Sb(3) Pd(1) Sb(2) C(21) . . . . 62.9(8) no Sb(3) C(2) Sb(4) Pd(2) . . . . 17(1) no Sb(3) C(2) Sb(4) C(39) . . . . 136(1) no Sb(3) C(2) Sb(4) C(45) . . . . -124(1) no Sb(3) C(27) C(28) C(29) . . . . -177(2) no Sb(3) C(27) C(32) C(31) . . . . 178(2) no Sb(3) C(33) C(34) C(35) . . . . 177(2) no Sb(3) C(33) C(38) C(37) . . . . -180(2) no Sb(4) Pd(2) Sb(1) C(1) . . . . 131.6(6) no Sb(4) Pd(2) Sb(1) C(3) . . . . 4.4(7) no Sb(4) Pd(2) Sb(1) C(9) . . . . -109.1(6) no Sb(4) C(2) Sb(3) Pd(1) . . . . 12(1) no Sb(4) C(2) Sb(3) C(27) . . . . 127(1) no Sb(4) C(2) Sb(3) C(33) . . . . -131(1) no Sb(4) C(39) C(40) C(41) . . . . -180(2) no Sb(4) C(39) C(44) C(43) . . . . -179(2) no Sb(4) C(45) C(46) C(47) . . . . -178(2) no Sb(4) C(45) C(50) C(49) . . . . 180(2) no Pd(1) Sb(2) C(15) C(16) . . . . 138(2) no Pd(1) Sb(2) C(15) C(20) . . . . -49(2) no Pd(1) Sb(2) C(21) C(22) . . . . -179(2) no Pd(1) Sb(2) C(21) C(26) . . . . 7(2) no Pd(1) Sb(3) C(27) C(28) . . . . -38(2) no Pd(1) Sb(3) C(27) C(32) . . . . 142(2) no Pd(1) Sb(3) C(33) C(34) . . . . 116(2) no Pd(1) Sb(3) C(33) C(38) . . . . -67(2) no Pd(2) Sb(1) C(3) C(4) . . . . 99(2) no Pd(2) Sb(1) C(3) C(8) . . . . -82(2) no Pd(2) Sb(1) C(9) C(10) . . . . 6(2) no Pd(2) Sb(1) C(9) C(14) . . . . -177(2) no Pd(2) Sb(4) C(39) C(40) . . . . 159(2) no Pd(2) Sb(4) C(39) C(44) . . . . -22(2) no Pd(2) Sb(4) C(45) C(46) . . . . -80(2) no Pd(2) Sb(4) C(45) C(50) . . . . 102(2) no Br(1) Pd(1) Sb(2) C(1) . . . . -45.3(6) no Br(1) Pd(1) Sb(2) C(15) . . . . -179.7(8) no Br(1) Pd(1) Sb(2) C(21) . . . . 63.6(6) no Br(1) Pd(1) Sb(3) C(2) . . . . 53.4(6) no Br(1) Pd(1) Sb(3) C(27) . . . . -57.8(6) no Br(1) Pd(1) Sb(3) C(33) . . . . -173.7(8) no Br(2) Pd(1) Sb(2) C(1) . . . . 142.1(6) no Br(2) Pd(1) Sb(2) C(15) . . . . 7.8(8) no Br(2) Pd(1) Sb(2) C(21) . . . . -109.0(6) no Br(2) Pd(1) Sb(3) C(2) . . . . -134.0(6) no Br(2) Pd(1) Sb(3) C(27) . . . . 114.8(6) no Br(2) Pd(1) Sb(3) C(33) . . . . -1.1(8) no Br(3) Pd(2) Sb(1) C(1) . . . . -48.6(6) no Br(3) Pd(2) Sb(1) C(3) . . . . -175.9(7) no Br(3) Pd(2) Sb(1) C(9) . . . . 70.7(6) no Br(3) Pd(2) Sb(4) C(2) . . . . 79(10) no Br(3) Pd(2) Sb(4) C(39) . . . . -32(10) no Br(3) Pd(2) Sb(4) C(45) . . . . -155(10) no Br(4) Pd(2) Sb(1) C(1) . . . . -94(2) no Br(4) Pd(2) Sb(1) C(3) . . . . 139(2) no Br(4) Pd(2) Sb(1) C(9) . . . . 25(2) no Br(4) Pd(2) Sb(4) C(2) . . . . 56.7(6) no Br(4) Pd(2) Sb(4) C(39) . . . . -54.8(6) no Br(4) Pd(2) Sb(4) C(45) . . . . -176.9(8) no C(1) Sb(1) C(3) C(4) . . . . -33(2) no C(1) Sb(1) C(3) C(8) . . . . 147(2) no C(1) Sb(1) C(9) C(10) . . . . 128(2) no C(1) Sb(1) C(9) C(14) . . . . -55(2) no C(1) Sb(2) C(15) C(16) . . . . 0(2) no C(1) Sb(2) C(15) C(20) . . . . 173(2) no C(1) Sb(2) C(21) C(22) . . . . -59(2) no C(1) Sb(2) C(21) C(26) . . . . 127(2) no C(2) Sb(3) C(27) C(28) . . . . -159(2) no C(2) Sb(3) C(27) C(32) . . . . 21(2) no C(2) Sb(3) C(33) C(34) . . . . -107(2) no C(2) Sb(3) C(33) C(38) . . . . 70(2) no C(2) Sb(4) C(39) C(40) . . . . 40(2) no C(2) Sb(4) C(39) C(44) . . . . -140(2) no C(2) Sb(4) C(45) C(46) . . . . 50(2) no C(2) Sb(4) C(45) C(50) . . . . -128(2) no C(3) Sb(1) C(9) C(10) . . . . -127(2) no C(3) Sb(1) C(9) C(14) . . . . 50(2) no C(3) C(4) C(5) C(6) . . . . 2(4) no C(3) C(8) C(7) C(6) . . . . 2(4) no C(4) C(3) Sb(1) C(9) . . . . -144(2) no C(4) C(3) C(8) C(7) . . . . -4(4) no C(4) C(5) C(6) C(7) . . . . -5(4) no C(5) C(4) C(3) C(8) . . . . 3(4) no C(5) C(6) C(7) C(8) . . . . 3(4) no C(8) C(3) Sb(1) C(9) . . . . 36(2) no C(9) C(10) C(11) C(12) . . . . 2(4) no C(9) C(14) C(13) C(12) . . . . 0(4) no C(10) C(9) C(14) C(13) . . . . 1(4) no C(10) C(11) C(12) C(13) . . . . -2(4) no C(11) C(10) C(9) C(14) . . . . -2(4) no C(11) C(12) C(13) C(14) . . . . 1(4) no C(15) Sb(2) C(21) C(22) . . . . 46(2) no C(15) Sb(2) C(21) C(26) . . . . -128(2) no C(15) C(16) C(17) C(18) . . . . 0(4) no C(15) C(20) C(19) C(18) . . . . -2(4) no C(16) C(15) Sb(2) C(21) . . . . -99(2) no C(16) C(15) C(20) C(19) . . . . 4(4) no C(16) C(17) C(18) C(19) . . . . 3(4) no C(17) C(16) C(15) C(20) . . . . -3(4) no C(17) C(18) C(19) C(20) . . . . -2(4) no C(20) C(15) Sb(2) C(21) . . . . 74(2) no C(21) C(22) C(23) C(24) . . . . -2(4) no C(21) C(26) C(25) C(24) . . . . 1(4) no C(22) C(21) C(26) C(25) . . . . 1(4) no C(22) C(23) C(24) C(25) . . . . 3(4) no C(23) C(22) C(21) C(26) . . . . -1(3) no C(23) C(24) C(25) C(26) . . . . -3(4) no C(27) Sb(3) C(33) C(34) . . . . -3(2) no C(27) Sb(3) C(33) C(38) . . . . 174(2) no C(27) C(28) C(29) C(30) . . . . -5(4) no C(27) C(32) C(31) C(30) . . . . 3(4) no C(28) C(27) Sb(3) C(33) . . . . 96(2) no C(28) C(27) C(32) C(31) . . . . -2(4) no C(28) C(29) C(30) C(31) . . . . 5(4) no C(29) C(28) C(27) C(32) . . . . 3(4) no C(29) C(30) C(31) C(32) . . . . -4(4) no C(32) C(27) Sb(3) C(33) . . . . -84(2) no C(33) C(34) C(35) C(36) . . . . -1(4) no C(33) C(38) C(37) C(36) . . . . 8(5) no C(34) C(33) C(38) C(37) . . . . -3(4) no C(34) C(35) C(36) C(37) . . . . 7(4) no C(35) C(34) C(33) C(38) . . . . -1(4) no C(35) C(36) C(37) C(38) . . . . -10(5) no C(39) Sb(4) C(45) C(46) . . . . 153(2) no C(39) Sb(4) C(45) C(50) . . . . -25(2) no C(39) C(40) C(41) C(42) . . . . 1(4) no C(39) C(44) C(43) C(42) . . . . -5(3) no C(40) C(39) Sb(4) C(45) . . . . -62(2) no C(40) C(39) C(44) C(43) . . . . 1(3) no C(40) C(41) C(42) C(43) . . . . -5(4) no C(41) C(40) C(39) C(44) . . . . 1(4) no C(41) C(42) C(43) C(44) . . . . 7(4) no C(44) C(39) Sb(4) C(45) . . . . 117(2) no C(45) C(46) C(47) C(48) . . . . 2(4) no C(45) C(50) C(49) C(48) . . . . -5(4) no C(46) C(45) C(50) C(49) . . . . 1(3) no C(46) C(47) C(48) C(49) . . . . -6(4) no C(47) C(46) C(45) C(50) . . . . 0(4) no C(47) C(48) C(49) C(50) . . . . 7(4) no #------------------------------------------------------------------------------ #===END ############################################################################## ### CIF submission form for molecular structure report ### ### Version: 7 October 1991 ### ############################################################################## #============================================================================== data_global3 #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof W Levason' _publ_contact_author_address ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; _publ_contact_author_phone '023 80 593792' _publ_contact_author_fax ? _publ_contact_author_email 'wxl@soton.ac.uk' _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; J. Chem. Soc., Dalton Trans. Paper ref. 9/08296D ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, properties and structures of complexes of platinum metal halides and Group 11 metals with two distibinomethane ligands, R~2~SbCH~2~SbR~2~ (R = Me or Ph) ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Even, Tina' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Genge, Anthony R. J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Hill, Angela M.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Holmes, Nicholas J.' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Levason, William' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; 'Webster, Michael' ; Department of Chemistry, University of Southampton, Southampton SO17 1BJ, England ; #============================================================================== # 4. TEXT _publ_section_references ; Molecular Structure Corporation (1988) MSC/AFC Diffractometer Control Software. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Molecular Structure Corporation. (1992-1997). teXsan. Single Crystal Structure Analysis Software. Version 1.8. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; #============================================================================== data_tina1 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; Tetrachlorobis(\m-bisdiphenylstibinomethane)diplatinum(II).acetone ; _chemical_name_common ? _chemical_formula_moiety 'C50 H44 Cl4 Pt2 Sb4, C3 H6 O1' _chemical_formula_sum 'C53 H50 Cl4 O Pt2 Sb4 ' # _chemical_formula_weight ? #=========================================================================== # 6. CRYSTAL DATA #---------------------------------------------------------------------------- _audit_creation_date '1999-10-11' _audit_creation_method 'by teXsan v1.8' _audit_update_record ; ? ; #---------------------------------------------------------------------------- #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan (MSC, 1992-1997)' _computing_structure_solution ; SHELXS86 (Sheldrick, 1985) ; _computing_structure_refinement 'teXsan (MSC, 1992-1997)' _computing_publication_material 'teXsan (MSC, 1992-1997)' #------------------------------------------------------------------------------ _cell_length_a 18.964(6) _cell_length_b 12.729(4) _cell_length_c 23.090(4) _cell_angle_alpha 90 _cell_angle_beta 107.50(2) _cell_angle_gamma 90 _cell_volume 5316(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 18.3 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _publ_section_exptl_prep ; ; _exptl_crystal_description 'prism' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_meas 'not measured' _chemical_formula_weight 1721.97 _chemical_formula_analytical ? # _chemical_formula_sum 'C53 H50 Cl4 O Pt2 Sb4 ' # _chemical_formula_moiety '?' # _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 3216.00 _exptl_absorpt_coefficient_mu 7.460 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; (North,Phillips & Matthews, 1968) ; _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.455 _exptl_special_details ; The scan width was (1.00+0.35tan\q)\% with an \w scan speed of 16\% per minute (up to 5 scans to achieve I/\s(I) > 15). Stationary background counts were recorded at each end of the scan, and the scan time:background time ratio was 2:1. ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.58 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 -2 2 -3 2 7 2 -1 7 _diffrn_reflns_number 10166 _reflns_number_total 9850 _reflns_number_gt 6448 _reflns_threshold_expression I>2.00\s(I) _diffrn_reflns_av_R_equivalents 0.05907 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.00775 _diffrn_orient_matrix_UB_12 0.00402 _diffrn_orient_matrix_UB_13 0.04091 _diffrn_orient_matrix_UB_21 -0.03769 _diffrn_orient_matrix_UB_22 0.05650 _diffrn_orient_matrix_UB_23 -0.01511 _diffrn_orient_matrix_UB_31 -0.03970 _diffrn_orient_matrix_UB_32 -0.05443 _diffrn_orient_matrix_UB_33 -0.01266 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 212 0.002 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 8 -2.352 8.388 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Sb 0 16 -0.816 1.546 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 16 0.132 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 4 0.008 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 200 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_refinement_flags _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom Pt(1) 0.07881(4) -0.00230(5) 0.75333(3) 0.0156(2) 1.000 . Uani d ? Pt(2) -0.04499(4) -0.17621(5) 0.73888(3) 0.0168(2) 1.000 . Uani d ? Sb(1) 0.00397(6) 0.14119(9) 0.77768(5) 0.0187(3) 1.000 . Uani d ? Sb(2) -0.09873(6) -0.07274(9) 0.81152(5) 0.0191(3) 1.000 . Uani d ? Sb(3) 0.00215(6) -0.25116(9) 0.65478(5) 0.0173(3) 1.000 . Uani d ? Sb(4) 0.04844(6) 0.01827(9) 0.64106(5) 0.0188(3) 1.000 . Uani d ? Cl(1) 0.1224(2) -0.0264(3) 0.8597(2) 0.026(1) 1.000 . Uani d ? Cl(2) 0.1540(2) -0.1371(3) 0.7346(2) 0.023(1) 1.000 . Uani d ? Cl(3) -0.1153(3) -0.0714(4) 0.6604(2) 0.029(1) 1.000 . Uani d ? Cl(4) 0.0205(3) -0.2943(3) 0.8113(2) 0.029(1) 1.000 . Uani d ? O(1) 0.858(1) 0.234(1) 0.9128(7) 0.077(7) 1.000 . Uani d ? C(1) -0.0510(8) 0.080(1) 0.8364(7) 0.019(4) 1.000 . Uani d ? C(2) 0.0312(9) -0.134(1) 0.5987(7) 0.020(5) 1.000 . Uani d ? C(3) 0.862(2) 0.279(2) 0.959(1) 0.059(9) 1.000 . Uani d ? C(4) 0.903(2) 0.226(2) 1.017(1) 0.08(1) 1.000 . Uani d ? C(5) 0.822(2) 0.379(2) 0.959(1) 0.10(1) 1.000 . Uani d ? C(11) -0.082(1) 0.229(1) 0.7154(7) 0.026(5) 1.000 . Uani d ? C(12) -0.065(1) 0.333(2) 0.7008(9) 0.043(6) 1.000 . Uani d ? C(13) -0.121(1) 0.388(2) 0.6597(9) 0.043(7) 1.000 . Uani d ? C(14) -0.190(1) 0.345(2) 0.6354(9) 0.045(7) 1.000 . Uani d ? C(15) -0.205(1) 0.244(2) 0.6477(9) 0.044(7) 1.000 . Uani d ? C(16) -0.148(1) 0.186(2) 0.6887(8) 0.039(6) 1.000 . Uani d ? C(21) 0.0721(9) 0.267(1) 0.8243(7) 0.022(5) 1.000 . Uani d ? C(22) 0.145(1) 0.271(1) 0.8281(8) 0.033(6) 1.000 . Uani d ? C(23) 0.190(1) 0.355(2) 0.855(1) 0.055(8) 1.000 . Uani d ? C(24) 0.159(1) 0.434(2) 0.8808(9) 0.053(8) 1.000 . Uani d ? C(25) 0.085(2) 0.431(2) 0.8782(9) 0.058(8) 1.000 . Uani d ? C(26) 0.040(1) 0.345(2) 0.8518(9) 0.043(6) 1.000 . Uani d ? C(31) -0.2108(9) -0.033(1) 0.7717(7) 0.019(5) 1.000 . Uani d ? C(32) -0.2414(9) 0.061(1) 0.7846(8) 0.026(5) 1.000 . Uani d ? C(33) -0.316(1) 0.085(2) 0.7566(9) 0.034(6) 1.000 . Uani d ? C(34) -0.358(1) 0.020(2) 0.7133(8) 0.040(6) 1.000 . Uani d ? C(35) -0.329(1) -0.073(2) 0.6993(8) 0.036(6) 1.000 . Uani d ? C(36) -0.256(1) -0.099(1) 0.7278(7) 0.025(5) 1.000 . Uani d ? C(41) -0.100(1) -0.130(2) 0.8975(7) 0.029(5) 1.000 . Uani d ? C(42) -0.107(1) -0.059(2) 0.9408(8) 0.035(6) 1.000 . Uani d ? C(43) -0.115(1) -0.092(2) 0.9961(9) 0.048(7) 1.000 . Uani d ? C(44) -0.113(1) -0.199(2) 1.0064(9) 0.056(8) 1.000 . Uani d ? C(45) -0.107(1) -0.273(2) 0.965(1) 0.057(8) 1.000 . Uani d ? C(46) -0.100(1) -0.234(2) 0.9092(8) 0.037(6) 1.000 . Uani d ? C(51) -0.0855(9) -0.331(1) 0.5871(7) 0.020(4) 1.000 . Uani d ? C(52) -0.155(1) -0.337(2) 0.5923(8) 0.031(5) 1.000 . Uani d ? C(53) -0.210(1) -0.395(2) 0.5498(9) 0.035(6) 1.000 . Uani d ? C(54) -0.192(1) -0.442(2) 0.5027(9) 0.041(6) 1.000 . Uani d ? C(55) -0.123(1) -0.436(2) 0.4962(9) 0.044(7) 1.000 . Uani d ? C(56) -0.067(1) -0.380(2) 0.5395(8) 0.036(6) 1.000 . Uani d ? C(61) 0.0859(9) -0.367(1) 0.6641(7) 0.022(5) 1.000 . Uani d ? C(62) 0.071(1) -0.463(2) 0.686(1) 0.049(7) 1.000 . Uani d ? C(63) 0.123(1) -0.544(2) 0.691(1) 0.054(8) 1.000 . Uani d ? C(64) 0.181(1) -0.532(2) 0.6718(8) 0.044(7) 1.000 . Uani d ? C(65) 0.195(1) -0.438(2) 0.6497(9) 0.045(7) 1.000 . Uani d ? C(66) 0.145(1) -0.356(2) 0.6464(8) 0.039(6) 1.000 . Uani d ? C(71) -0.037(1) 0.113(1) 0.5809(7) 0.025(5) 1.000 . Uani d ? C(72) -0.101(1) 0.072(2) 0.5457(8) 0.033(6) 1.000 . Uani d ? C(73) -0.154(1) 0.136(2) 0.5066(9) 0.052(8) 1.000 . Uani d ? C(74) -0.141(1) 0.239(2) 0.5061(9) 0.050(8) 1.000 . Uani d ? C(75) -0.075(2) 0.285(2) 0.541(1) 0.056(8) 1.000 . Uani d ? C(76) -0.020(1) 0.222(2) 0.5794(8) 0.034(6) 1.000 . Uani d ? C(81) 0.144(1) 0.086(1) 0.6267(7) 0.021(5) 1.000 . Uani d ? C(82) 0.141(1) 0.131(2) 0.5702(7) 0.031(5) 1.000 . Uani d ? C(83) 0.201(1) 0.187(2) 0.5651(9) 0.040(7) 1.000 . Uani d ? C(84) 0.264(1) 0.201(2) 0.615(1) 0.040(7) 1.000 . Uani d ? C(85) 0.265(1) 0.155(2) 0.6688(9) 0.036(6) 1.000 . Uani d ? C(86) 0.206(1) 0.101(1) 0.6751(7) 0.025(5) 1.000 . Uani d ? H(1b) -0.0895 0.1275 0.8371 0.022 1.000 . Uiso c ? H(1a) -0.0166 0.0757 0.8759 0.022 1.000 . Uiso c ? H(2b) -0.0077 -0.1293 0.5616 0.023 1.000 . Uiso c ? H(2a) 0.0754 -0.1554 0.5907 0.023 1.000 . Uiso c ? H(4b) 0.9529 0.2148 1.0174 0.094 1.000 . Uiso c ? H(4c) 0.9025 0.2698 1.0501 0.094 1.000 . Uiso c ? H(4a) 0.8806 0.1607 1.0201 0.094 1.000 . Uiso c ? H(5b) 0.8387 0.4298 0.9361 0.125 1.000 . Uiso c ? H(5c) 0.7702 0.3678 0.9408 0.125 1.000 . Uiso c ? H(5a) 0.8308 0.4026 0.9993 0.125 1.000 . Uiso c ? H(12) -0.0178 0.3629 0.7185 0.051 1.000 . Uiso c ? H(13) -0.1117 0.4573 0.6482 0.052 1.000 . Uiso c ? H(14) -0.2281 0.3860 0.6092 0.054 1.000 . Uiso c ? H(15) -0.2523 0.2136 0.6293 0.053 1.000 . Uiso c ? H(16) -0.1571 0.1155 0.6975 0.047 1.000 . Uiso c ? H(22) 0.1663 0.2152 0.8117 0.039 1.000 . Uiso c ? H(23) 0.2401 0.3581 0.8564 0.066 1.000 . Uiso c ? H(24) 0.1885 0.4914 0.9003 0.064 1.000 . Uiso c ? H(25) 0.0642 0.4873 0.8946 0.069 1.000 . Uiso c ? H(26) -0.0093 0.3404 0.8524 0.051 1.000 . Uiso c ? H(32) -0.2111 0.1085 0.8129 0.032 1.000 . Uiso c ? H(33) -0.3367 0.1472 0.7678 0.041 1.000 . Uiso c ? H(34) -0.4080 0.0379 0.6926 0.048 1.000 . Uiso c ? H(35) -0.3592 -0.1200 0.6702 0.043 1.000 . Uiso c ? H(36) -0.2356 -0.1616 0.7171 0.030 1.000 . Uiso c ? H(42) -0.1054 0.0142 0.9329 0.041 1.000 . Uiso c ? H(43) -0.1209 -0.0435 1.0253 0.058 1.000 . Uiso c ? H(44) -0.1172 -0.2230 1.0444 0.067 1.000 . Uiso c ? H(45) -0.1076 -0.3458 0.9726 0.069 1.000 . Uiso c ? H(46) -0.0942 -0.2830 0.8796 0.044 1.000 . Uiso c ? H(52) -0.1665 -0.3030 0.6249 0.037 1.000 . Uiso c ? H(53) -0.2580 -0.4014 0.5537 0.042 1.000 . Uiso c ? H(54) -0.2291 -0.4807 0.4736 0.049 1.000 . Uiso c ? H(55) -0.1128 -0.4684 0.4627 0.052 1.000 . Uiso c ? H(56) -0.0187 -0.3771 0.5366 0.044 1.000 . Uiso c ? H(62) 0.0277 -0.4738 0.6972 0.059 1.000 . Uiso c ? H(63) 0.1154 -0.6091 0.7089 0.065 1.000 . Uiso c ? H(64) 0.2138 -0.5899 0.6732 0.052 1.000 . Uiso c ? H(65) 0.2375 -0.4276 0.6369 0.054 1.000 . Uiso c ? H(66) 0.1543 -0.2898 0.6308 0.046 1.000 . Uiso c ? H(67) -0.1101 -0.0013 0.5476 0.040 1.000 . Uiso c ? H(68) -0.1981 0.1064 0.4807 0.062 1.000 . Uiso c ? H(69) -0.1781 0.2832 0.4809 0.059 1.000 . Uiso c ? H(70) -0.0668 0.3589 0.5390 0.067 1.000 . Uiso c ? H(71) 0.0256 0.2504 0.6035 0.040 1.000 . Uiso c ? H(72) 0.0981 0.1229 0.5361 0.037 1.000 . Uiso c ? H(73) 0.1992 0.2176 0.5271 0.048 1.000 . Uiso c ? H(74) 0.3054 0.2397 0.6109 0.048 1.000 . Uiso c ? H(75) 0.3082 0.1610 0.7027 0.043 1.000 . Uiso c ? H(76) 0.2070 0.0737 0.7137 0.030 1.000 . Uiso c ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0198(3) 0.0112(3) 0.0132(3) -0.0004(3) 0.0013(2) 0.0008(2) Pt(2) 0.0199(4) 0.0126(3) 0.0165(3) -0.0008(3) 0.0032(3) -0.0004(3) Sb(1) 0.0217(6) 0.0116(6) 0.0202(6) 0.0004(5) 0.0025(5) -0.0004(4) Sb(2) 0.0227(6) 0.0175(6) 0.0164(5) 0.0006(5) 0.0049(5) -0.0007(5) Sb(3) 0.0210(6) 0.0119(6) 0.0170(5) 0.0002(5) 0.0028(5) -0.0010(4) Sb(4) 0.0257(6) 0.0139(6) 0.0139(5) -0.0013(5) 0.0012(5) 0.0017(4) Cl(1) 0.036(3) 0.026(3) 0.013(2) 0.004(2) 0.003(2) 0.002(2) Cl(2) 0.029(2) 0.013(2) 0.022(2) 0.007(2) 0.002(2) 0.000(2) Cl(3) 0.033(3) 0.029(3) 0.024(2) 0.015(2) 0.007(2) 0.008(2) Cl(4) 0.032(3) 0.020(2) 0.027(2) 0.007(2) -0.001(2) 0.009(2) O(1) 0.15(2) 0.05(1) 0.04(1) 0.01(1) 0.04(1) 0.003(9) C(1) 0.008(8) 0.012(9) 0.031(9) 0.003(7) -0.002(7) -0.013(7) C(2) 0.02(1) 0.005(8) 0.03(1) -0.003(7) 0.006(8) 0.001(7) C(3) 0.10(2) 0.05(2) 0.04(1) -0.02(1) 0.03(1) -0.01(1) C(4) 0.08(2) 0.09(2) 0.05(2) 0.00(2) 0.01(1) -0.02(2) C(5) 0.21(4) 0.04(2) 0.08(2) 0.01(2) 0.08(2) 0.00(2) C(11) 0.03(1) 0.02(1) 0.024(9) 0.008(8) 0.001(8) -0.003(8) C(12) 0.05(1) 0.01(1) 0.05(1) 0.01(1) 0.00(1) 0.004(9) C(13) 0.07(2) 0.02(1) 0.05(1) 0.01(1) 0.02(1) 0.010(9) C(14) 0.03(1) 0.06(2) 0.04(1) 0.03(1) 0.00(1) 0.00(1) C(15) 0.03(1) 0.05(2) 0.04(1) 0.00(1) 0.00(1) 0.01(1) C(16) 0.03(1) 0.05(1) 0.03(1) 0.01(1) -0.007(9) 0.01(1) C(21) 0.015(9) 0.02(1) 0.026(9) -0.010(7) -0.006(7) 0.006(7) C(22) 0.04(1) 0.02(1) 0.03(1) -0.008(9) -0.006(9) 0.000(8) C(23) 0.05(2) 0.06(2) 0.05(1) -0.03(1) 0.01(1) -0.02(1) C(24) 0.08(2) 0.03(1) 0.04(1) -0.02(1) -0.01(1) 0.01(1) C(25) 0.10(2) 0.02(1) 0.04(1) 0.00(1) 0.00(1) -0.01(1) C(26) 0.05(1) 0.02(1) 0.05(1) 0.016(9) -0.01(1) -0.004(9) C(31) 0.019(9) 0.03(1) 0.009(7) 0.000(8) 0.004(7) 0.011(7) C(32) 0.02(1) 0.02(1) 0.04(1) -0.013(8) 0.000(8) 0.002(8) C(33) 0.03(1) 0.03(1) 0.04(1) -0.001(9) 0.012(9) -0.003(9) C(34) 0.04(1) 0.05(1) 0.03(1) 0.00(1) 0.001(9) 0.01(1) C(35) 0.04(1) 0.03(1) 0.03(1) -0.01(1) -0.001(9) -0.002(9) C(36) 0.03(1) 0.03(1) 0.024(9) -0.008(8) 0.009(8) -0.011(8) C(41) 0.02(1) 0.05(1) 0.012(8) -0.021(9) 0.000(7) 0.001(8) C(42) 0.04(1) 0.04(1) 0.03(1) 0.00(1) 0.017(9) 0.003(9) C(43) 0.06(2) 0.06(2) 0.02(1) 0.00(1) 0.01(1) 0.00(1) C(44) 0.05(2) 0.09(2) 0.02(1) 0.01(1) 0.01(1) 0.01(1) C(45) 0.07(2) 0.05(2) 0.05(1) 0.00(1) 0.02(1) 0.03(1) C(46) 0.04(1) 0.04(1) 0.03(1) -0.01(1) -0.001(9) 0.009(9) C(51) 0.011(9) 0.012(9) 0.028(9) -0.002(7) -0.006(7) 0.005(7) C(52) 0.03(1) 0.04(1) 0.021(9) -0.006(9) 0.002(8) -0.002(8) C(53) 0.02(1) 0.05(1) 0.04(1) 0.002(9) 0.007(9) 0.01(1) C(54) 0.04(1) 0.03(1) 0.04(1) -0.01(1) -0.02(1) 0.002(9) C(55) 0.07(2) 0.02(1) 0.03(1) 0.00(1) 0.00(1) -0.006(9) C(56) 0.04(1) 0.04(1) 0.03(1) -0.01(1) 0.004(9) -0.004(9) C(61) 0.02(1) 0.03(1) 0.012(8) 0.012(8) 0.000(7) -0.009(7) C(62) 0.05(1) 0.03(1) 0.06(2) 0.01(1) 0.01(1) 0.01(1) C(63) 0.06(2) 0.03(1) 0.06(2) 0.02(1) 0.01(1) 0.02(1) C(64) 0.05(2) 0.04(1) 0.03(1) 0.03(1) 0.00(1) -0.005(9) C(65) 0.03(1) 0.06(2) 0.04(1) 0.00(1) 0.000(9) -0.03(1) C(66) 0.04(1) 0.05(1) 0.03(1) 0.01(1) 0.01(1) 0.00(1) C(71) 0.03(1) 0.03(1) 0.016(9) 0.016(8) 0.003(8) 0.001(8) C(72) 0.04(1) 0.04(1) 0.019(9) 0.01(1) 0.004(8) 0.007(9) C(73) 0.04(1) 0.07(2) 0.04(1) 0.02(1) 0.01(1) 0.02(1) C(74) 0.06(2) 0.07(2) 0.03(1) 0.03(1) 0.02(1) 0.02(1) C(75) 0.10(2) 0.03(1) 0.05(1) 0.03(1) 0.03(1) 0.02(1) C(76) 0.05(1) 0.03(1) 0.03(1) 0.01(1) 0.016(9) 0.003(8) C(81) 0.04(1) 0.011(9) 0.016(8) -0.002(8) 0.007(8) -0.001(7) C(82) 0.04(1) 0.03(1) 0.016(9) 0.010(9) 0.003(8) 0.011(8) C(83) 0.05(1) 0.05(1) 0.03(1) 0.00(1) 0.02(1) 0.01(1) C(84) 0.05(1) 0.02(1) 0.06(1) 0.01(1) 0.03(1) 0.01(1) C(85) 0.04(1) 0.02(1) 0.06(1) -0.007(9) 0.02(1) -0.008(9) C(86) 0.05(1) 0.012(9) 0.014(8) 0.014(8) 0.002(8) 0.000(7) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00002|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 6448 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_all 0.0615 _refine_ls_wR_factor_ref 0.0615 _refine_ls_goodness_of_fit_all 2.325 _refine_ls_goodness_of_fit_ref 2.325 _refine_ls_shift/su_max 0.0180 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -4.25 _refine_diff_density_max 4.55 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) Sb(1) 2.479(1) . . yes Pt(1) Sb(4) 2.494(1) . . yes Pt(1) Cl(1) 2.365(4) . . yes Pt(1) Cl(2) 2.353(4) . . yes Pt(2) Sb(2) 2.572(1) . . yes Pt(2) Sb(3) 2.554(1) . . yes Pt(2) Cl(3) 2.321(4) . . yes Pt(2) Cl(4) 2.312(4) . . yes Sb(1) C(1) 2.09(2) . . yes Sb(1) C(11) 2.14(2) . . yes Sb(1) C(21) 2.13(2) . . yes Sb(2) C(1) 2.15(2) . . yes Sb(2) C(31) 2.11(2) . . yes Sb(2) C(41) 2.12(2) . . yes Sb(3) C(2) 2.15(2) . . yes Sb(3) C(51) 2.16(2) . . yes Sb(3) C(61) 2.13(2) . . yes Sb(4) C(2) 2.15(2) . . yes Sb(4) C(71) 2.15(2) . . yes Sb(4) C(81) 2.12(2) . . yes O(1) C(3) 1.19(2) . . yes C(1) H(1b) 0.95 . . no C(1) H(1a) 0.95 . . no C(2) H(2b) 0.95 . . no C(2) H(2a) 0.95 . . no C(3) C(4) 1.49(3) . . yes C(3) C(5) 1.48(4) . . yes C(4) H(4b) 0.95 . . no C(4) H(4c) 0.95 . . no C(4) H(4a) 0.95 . . no C(5) H(5b) 0.95 . . no C(5) H(5c) 0.95 . . no C(5) H(5a) 0.95 . . no C(11) C(12) 1.42(3) . . yes C(11) C(16) 1.34(3) . . yes C(12) C(13) 1.38(3) . . yes C(12) H(12) 0.95 . . no C(13) C(14) 1.37(3) . . yes C(13) H(13) 0.95 . . no C(14) C(15) 1.36(3) . . yes C(14) H(14) 0.95 . . no C(15) C(16) 1.41(3) . . yes C(15) H(15) 0.95 . . no C(16) H(16) 0.95 . . no C(21) C(22) 1.36(2) . . yes C(21) C(26) 1.41(3) . . yes C(22) C(23) 1.39(3) . . yes C(22) H(22) 0.95 . . no C(23) C(24) 1.38(3) . . yes C(23) H(23) 0.95 . . no C(24) C(25) 1.38(3) . . yes C(24) H(24) 0.95 . . no C(25) C(26) 1.40(3) . . yes C(25) H(25) 0.95 . . no C(26) H(26) 0.95 . . no C(31) C(32) 1.40(2) . . yes C(31) C(36) 1.39(2) . . yes C(32) C(33) 1.40(3) . . yes C(32) H(32) 0.95 . . no C(33) C(34) 1.36(3) . . yes C(33) H(33) 0.95 . . no C(34) C(35) 1.39(3) . . yes C(34) H(34) 0.95 . . no C(35) C(36) 1.39(3) . . yes C(35) H(35) 0.95 . . no C(36) H(36) 0.95 . . no C(41) C(42) 1.38(3) . . yes C(41) C(46) 1.36(3) . . yes C(42) C(43) 1.40(3) . . yes C(42) H(42) 0.95 . . no C(43) C(44) 1.38(3) . . yes C(43) H(43) 0.95 . . no C(44) C(45) 1.38(3) . . yes C(44) H(44) 0.95 . . no C(45) C(46) 1.41(3) . . yes C(45) H(45) 0.95 . . no C(46) H(46) 0.95 . . no C(51) C(52) 1.36(2) . . yes C(51) C(56) 1.40(2) . . yes C(52) C(53) 1.40(3) . . yes C(52) H(52) 0.95 . . no C(53) C(54) 1.37(3) . . yes C(53) H(53) 0.95 . . no C(54) C(55) 1.36(3) . . yes C(54) H(54) 0.95 . . no C(55) C(56) 1.41(3) . . yes C(55) H(55) 0.95 . . no C(56) H(56) 0.95 . . no C(61) C(62) 1.38(3) . . yes C(61) C(66) 1.32(3) . . yes C(62) C(63) 1.40(3) . . yes C(62) H(62) 0.95 . . no C(63) C(64) 1.33(3) . . yes C(63) H(63) 0.95 . . no C(64) C(65) 1.36(3) . . yes C(64) H(64) 0.95 . . no C(65) C(66) 1.39(3) . . yes C(65) H(65) 0.95 . . no C(66) H(66) 0.95 . . no C(71) C(72) 1.35(3) . . yes C(71) C(76) 1.43(3) . . yes C(72) C(73) 1.39(3) . . yes C(72) H(67) 0.95 . . no C(73) C(74) 1.34(3) . . yes C(73) H(68) 0.95 . . no C(74) C(75) 1.40(3) . . yes C(74) H(69) 0.95 . . no C(75) C(76) 1.39(3) . . yes C(75) H(70) 0.95 . . no C(76) H(71) 0.95 . . no C(81) C(82) 1.41(2) . . yes C(81) C(86) 1.37(2) . . yes C(82) C(83) 1.38(3) . . yes C(82) H(72) 0.95 . . no C(83) C(84) 1.40(3) . . yes C(83) H(73) 0.95 . . no C(84) C(85) 1.37(3) . . yes C(84) H(74) 0.95 . . no C(85) C(86) 1.37(3) . . yes C(85) H(75) 0.95 . . no C(86) H(76) 0.95 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Sb(1) Pt(1) Sb(4) 100.91(4) . . . yes Sb(1) Pt(1) Cl(1) 84.5(1) . . . yes Sb(1) Pt(1) Cl(2) 177.4(1) . . . yes Sb(4) Pt(1) Cl(1) 173.0(1) . . . yes Sb(4) Pt(1) Cl(2) 81.3(1) . . . yes Cl(1) Pt(1) Cl(2) 93.1(1) . . . yes Sb(2) Pt(2) Sb(3) 170.06(4) . . . yes Sb(2) Pt(2) Cl(3) 88.1(1) . . . yes Sb(2) Pt(2) Cl(4) 95.4(1) . . . yes Sb(3) Pt(2) Cl(3) 82.6(1) . . . yes Sb(3) Pt(2) Cl(4) 94.1(1) . . . yes Cl(3) Pt(2) Cl(4) 174.5(2) . . . yes Pt(1) Sb(1) C(1) 107.8(4) . . . yes Pt(1) Sb(1) C(11) 127.3(4) . . . yes Pt(1) Sb(1) C(21) 111.5(5) . . . yes C(1) Sb(1) C(11) 101.6(6) . . . yes C(1) Sb(1) C(21) 107.1(6) . . . yes C(11) Sb(1) C(21) 99.8(6) . . . yes Pt(2) Sb(2) C(1) 114.8(4) . . . yes Pt(2) Sb(2) C(31) 112.6(4) . . . yes Pt(2) Sb(2) C(41) 123.7(6) . . . yes C(1) Sb(2) C(31) 100.8(6) . . . yes C(1) Sb(2) C(41) 100.6(7) . . . yes C(31) Sb(2) C(41) 101.2(6) . . . yes Pt(2) Sb(3) C(2) 114.2(4) . . . yes Pt(2) Sb(3) C(51) 110.9(5) . . . yes Pt(2) Sb(3) C(61) 127.0(4) . . . yes C(2) Sb(3) C(51) 99.7(6) . . . yes C(2) Sb(3) C(61) 102.9(6) . . . yes C(51) Sb(3) C(61) 97.8(6) . . . yes Pt(1) Sb(4) C(2) 109.5(4) . . . yes Pt(1) Sb(4) C(71) 128.6(4) . . . yes Pt(1) Sb(4) C(81) 105.3(4) . . . yes C(2) Sb(4) C(71) 103.2(6) . . . yes C(2) Sb(4) C(81) 108.4(6) . . . yes C(71) Sb(4) C(81) 100.5(7) . . . yes Sb(1) C(1) Sb(2) 114.5(7) . . . yes Sb(1) C(1) H(1b) 108.2 . . . no Sb(1) C(1) H(1a) 108.2 . . . no Sb(2) C(1) H(1b) 108.2 . . . no Sb(2) C(1) H(1a) 108.2 . . . no H(1b) C(1) H(1a) 109.5 . . . no Sb(3) C(2) Sb(4) 112.5(7) . . . yes Sb(3) C(2) H(2b) 108.7 . . . no Sb(3) C(2) H(2a) 108.7 . . . no Sb(4) C(2) H(2b) 108.7 . . . no Sb(4) C(2) H(2a) 108.7 . . . no H(2b) C(2) H(2a) 109.5 . . . no O(1) C(3) C(4) 117(3) . . . yes O(1) C(3) C(5) 121(3) . . . yes C(4) C(3) C(5) 121(2) . . . yes C(3) C(4) H(4b) 109.5 . . . no C(3) C(4) H(4c) 109.5 . . . no C(3) C(4) H(4a) 109.5 . . . no H(4b) C(4) H(4c) 109.5 . . . no H(4b) C(4) H(4a) 109.4 . . . no H(4c) C(4) H(4a) 109.4 . . . no C(3) C(5) H(5b) 109.5 . . . no C(3) C(5) H(5c) 109.5 . . . no C(3) C(5) H(5a) 109.5 . . . no H(5b) C(5) H(5c) 109.4 . . . no H(5b) C(5) H(5a) 109.5 . . . no H(5c) C(5) H(5a) 109.4 . . . no Sb(1) C(11) C(12) 118(1) . . . yes Sb(1) C(11) C(16) 121(1) . . . yes C(12) C(11) C(16) 121(2) . . . yes C(11) C(12) C(13) 117(2) . . . yes C(11) C(12) H(12) 121.5 . . . no C(13) C(12) H(12) 121.5 . . . no C(12) C(13) C(14) 121(2) . . . yes C(12) C(13) H(13) 119.6 . . . no C(14) C(13) H(13) 119.6 . . . no C(13) C(14) C(15) 122(2) . . . yes C(13) C(14) H(14) 119.1 . . . no C(15) C(14) H(14) 119.1 . . . no C(14) C(15) C(16) 118(2) . . . yes C(14) C(15) H(15) 121.1 . . . no C(16) C(15) H(15) 121.1 . . . no C(11) C(16) C(15) 121(2) . . . yes C(11) C(16) H(16) 119.4 . . . no C(15) C(16) H(16) 119.4 . . . no Sb(1) C(21) C(22) 121(1) . . . yes Sb(1) C(21) C(26) 119(1) . . . yes C(22) C(21) C(26) 120(2) . . . yes C(21) C(22) C(23) 122(2) . . . yes C(21) C(22) H(22) 119.1 . . . no C(23) C(22) H(22) 119.1 . . . no C(22) C(23) C(24) 118(2) . . . yes C(22) C(23) H(23) 120.8 . . . no C(24) C(23) H(23) 120.9 . . . no C(23) C(24) C(25) 121(2) . . . yes C(23) C(24) H(24) 119.6 . . . no C(25) C(24) H(24) 119.4 . . . no C(24) C(25) C(26) 121(2) . . . yes C(24) C(25) H(25) 119.7 . . . no C(26) C(25) H(25) 119.7 . . . no C(21) C(26) C(25) 118(2) . . . yes C(21) C(26) H(26) 121.1 . . . no C(25) C(26) H(26) 121.2 . . . no Sb(2) C(31) C(32) 123(1) . . . yes Sb(2) C(31) C(36) 119(1) . . . yes C(32) C(31) C(36) 118(2) . . . yes C(31) C(32) C(33) 121(2) . . . yes C(31) C(32) H(32) 119.3 . . . no C(33) C(32) H(32) 119.4 . . . no C(32) C(33) C(34) 119(2) . . . yes C(32) C(33) H(33) 120.3 . . . no C(34) C(33) H(33) 120.3 . . . no C(33) C(34) C(35) 120(2) . . . yes C(33) C(34) H(34) 119.9 . . . no C(35) C(34) H(34) 119.8 . . . no C(34) C(35) C(36) 120(2) . . . yes C(34) C(35) H(35) 119.9 . . . no C(36) C(35) H(35) 119.9 . . . no C(31) C(36) C(35) 121(2) . . . yes C(31) C(36) H(36) 119.6 . . . no C(35) C(36) H(36) 119.6 . . . no Sb(2) C(41) C(42) 119(2) . . . yes Sb(2) C(41) C(46) 121(1) . . . yes C(42) C(41) C(46) 120(2) . . . yes C(41) C(42) C(43) 121(2) . . . yes C(41) C(42) H(42) 119.4 . . . no C(43) C(42) H(42) 119.4 . . . no C(42) C(43) C(44) 117(2) . . . yes C(42) C(43) H(43) 121.4 . . . no C(44) C(43) H(43) 121.4 . . . no C(43) C(44) C(45) 123(2) . . . yes C(43) C(44) H(44) 118.3 . . . no C(45) C(44) H(44) 118.3 . . . no C(44) C(45) C(46) 117(2) . . . yes C(44) C(45) H(45) 121.5 . . . no C(46) C(45) H(45) 121.5 . . . no C(41) C(46) C(45) 121(2) . . . yes C(41) C(46) H(46) 119.4 . . . no C(45) C(46) H(46) 119.4 . . . no Sb(3) C(51) C(52) 121(1) . . . yes Sb(3) C(51) C(56) 118(1) . . . yes C(52) C(51) C(56) 121(2) . . . yes C(51) C(52) C(53) 120(2) . . . yes C(51) C(52) H(52) 119.9 . . . no C(53) C(52) H(52) 119.9 . . . no C(52) C(53) C(54) 119(2) . . . yes C(52) C(53) H(53) 120.7 . . . no C(54) C(53) H(53) 120.7 . . . no C(53) C(54) C(55) 122(2) . . . yes C(53) C(54) H(54) 118.8 . . . no C(55) C(54) H(54) 118.9 . . . no C(54) C(55) C(56) 119(2) . . . yes C(54) C(55) H(55) 120.3 . . . no C(56) C(55) H(55) 120.3 . . . no C(51) C(56) C(55) 119(2) . . . yes C(51) C(56) H(56) 120.7 . . . no C(55) C(56) H(56) 120.7 . . . no Sb(3) C(61) C(62) 115(1) . . . yes Sb(3) C(61) C(66) 125(2) . . . yes C(62) C(61) C(66) 120(2) . . . yes C(61) C(62) C(63) 118(2) . . . yes C(61) C(62) H(62) 120.8 . . . no C(63) C(62) H(62) 120.8 . . . no C(62) C(63) C(64) 121(2) . . . yes C(62) C(63) H(63) 119.4 . . . no C(64) C(63) H(63) 119.4 . . . no C(63) C(64) C(65) 120(2) . . . yes C(63) C(64) H(64) 120.1 . . . no C(65) C(64) H(64) 120.1 . . . no C(64) C(65) C(66) 119(2) . . . yes C(64) C(65) H(65) 120.6 . . . no C(66) C(65) H(65) 120.5 . . . no C(61) C(66) C(65) 122(2) . . . yes C(61) C(66) H(66) 119.1 . . . no C(65) C(66) H(66) 119.1 . . . no Sb(4) C(71) C(72) 123(1) . . . yes Sb(4) C(71) C(76) 116(1) . . . yes C(72) C(71) C(76) 122(2) . . . yes C(71) C(72) C(73) 121(2) . . . yes C(71) C(72) H(67) 119.7 . . . no C(73) C(72) H(67) 119.6 . . . no C(72) C(73) C(74) 119(2) . . . yes C(72) C(73) H(68) 120.6 . . . no C(74) C(73) H(68) 120.5 . . . no C(73) C(74) C(75) 123(2) . . . yes C(73) C(74) H(69) 118.7 . . . no C(75) C(74) H(69) 118.6 . . . no C(74) C(75) C(76) 119(2) . . . yes C(74) C(75) H(70) 120.5 . . . no C(76) C(75) H(70) 120.4 . . . no C(71) C(76) C(75) 117(2) . . . yes C(71) C(76) H(71) 121.5 . . . no C(75) C(76) H(71) 121.5 . . . no Sb(4) C(81) C(82) 121(1) . . . yes Sb(4) C(81) C(86) 119(1) . . . yes C(82) C(81) C(86) 119(2) . . . yes C(81) C(82) C(83) 119(2) . . . yes C(81) C(82) H(72) 120.6 . . . no C(83) C(82) H(72) 120.6 . . . no C(82) C(83) C(84) 122(2) . . . yes C(82) C(83) H(73) 119.2 . . . no C(84) C(83) H(73) 119.3 . . . no C(83) C(84) C(85) 118(2) . . . yes C(83) C(84) H(74) 121.1 . . . no C(85) C(84) H(74) 121.1 . . . no C(84) C(85) C(86) 122(2) . . . yes C(84) C(85) H(75) 119.2 . . . no C(86) C(85) H(75) 119.2 . . . no C(81) C(86) C(85) 121(2) . . . yes C(81) C(86) H(76) 119.5 . . . no C(85) C(86) H(76) 119.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl(2) C(64) 3.49(2) . 2_556 no Cl(2) C(85) 3.51(2) . 2_546 no O(1) C(1) 3.42(2) . 1_655 no O(1) C(35) 3.49(2) . 2_556 no O(1) C(53) 3.58(3) . 2_556 no C(3) C(53) 3.59(3) . 2_556 no C(13) C(34) 3.50(3) . 2_456 no C(13) C(33) 3.58(3) . 2_456 no C(15) C(46) 3.55(3) . 2_456 no C(24) C(85) 3.51(3) . 2_556 no C(54) C(83) 3.59(3) . 3_556 no C(55) C(83) 3.60(3) . 3_556 no #------------------------------------------------------------------------------ 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Pt(1) Sb(1) C(1) Sb(2) . . . . -43.4(7) no Pt(1) Sb(1) C(11) C(12) . . . . -103(1) no Pt(1) Sb(1) C(11) C(16) . . . . 73(2) no Pt(1) Sb(1) C(21) C(22) . . . . 11(2) no Pt(1) Sb(1) C(21) C(26) . . . . -168(1) no Pt(1) Sb(4) C(2) Sb(3) . . . . 22.5(8) no Pt(1) Sb(4) C(71) C(72) . . . . -102(1) no Pt(1) Sb(4) C(71) C(76) . . . . 80(1) no Pt(1) Sb(4) C(81) C(82) . . . . -165(1) no Pt(1) Sb(4) C(81) C(86) . . . . 4(1) no Pt(2) Sb(2) C(1) Sb(1) . . . . 19.3(8) no Pt(2) Sb(2) C(31) C(32) . . . . -146(1) no Pt(2) Sb(2) C(31) C(36) . . . . 30(1) no Pt(2) Sb(2) C(41) C(42) . . . . 159(1) no Pt(2) Sb(2) C(41) C(46) . . . . -25(2) no Pt(2) Sb(3) C(2) Sb(4) . . . . 18.6(8) no Pt(2) Sb(3) C(51) C(52) . . . . -1(2) no Pt(2) Sb(3) C(51) C(56) . . . . -177(1) no Pt(2) Sb(3) C(61) C(62) . . . . 60(2) no Pt(2) Sb(3) C(61) C(66) . . . . -125(1) no Sb(1) Pt(1) Sb(4) C(2) . . . . -137.7(5) no Sb(1) Pt(1) Sb(4) C(71) . . . . -11.5(7) no Sb(1) Pt(1) Sb(4) C(81) . . . . 105.9(5) no Sb(1) C(1) Sb(2) C(31) . . . . -101.9(7) no Sb(1) C(1) Sb(2) C(41) . . . . 154.4(8) no Sb(1) C(11) C(12) C(13) . . . . 179(2) no Sb(1) C(11) C(16) C(15) . . . . 180(2) no Sb(1) C(21) C(22) C(23) . . . . 176(2) no Sb(1) C(21) C(26) C(25) . . . . -175(2) no Sb(2) Pt(2) Sb(3) C(2) . . . . 24.7(6) no Sb(2) Pt(2) Sb(3) C(51) . . . . -87.0(5) no Sb(2) Pt(2) Sb(3) C(61) . . . . 155.0(7) no Sb(2) C(1) Sb(1) C(11) . . . . 92.4(8) no Sb(2) C(1) Sb(1) C(21) . . . . -163.5(7) no Sb(2) C(31) C(32) C(33) . . . . 179(1) no Sb(2) C(31) C(36) C(35) . . . . -178(1) no Sb(2) C(41) C(42) C(43) . . . . 174(2) no Sb(2) C(41) C(46) C(45) . . . . -175(2) no Sb(3) Pt(2) Sb(2) C(1) . . . . -55.7(5) no Sb(3) Pt(2) Sb(2) C(31) . . . . 58.8(5) no Sb(3) Pt(2) Sb(2) C(41) . . . . -179.2(6) no Sb(3) C(2) Sb(4) C(71) . . . . -117.1(8) no Sb(3) C(2) Sb(4) C(81) . . . . 136.9(7) no Sb(3) C(51) C(52) C(53) . . . . -176(1) no Sb(3) C(51) C(56) C(55) . . . . 178(1) no Sb(3) C(61) C(62) C(63) . . . . 178(2) no Sb(3) C(61) C(66) C(65) . . . . -175(1) no Sb(4) Pt(1) Sb(1) C(1) . . . . 134.1(4) no Sb(4) Pt(1) Sb(1) C(11) . . . . 13.4(6) no Sb(4) Pt(1) Sb(1) C(21) . . . . -108.6(5) no Sb(4) C(2) Sb(3) C(51) . . . . 136.9(8) no Sb(4) C(2) Sb(3) C(61) . . . . -122.7(7) no Sb(4) C(71) C(72) C(73) . . . . -179(1) no Sb(4) C(71) C(76) C(75) . . . . -180(1) no Sb(4) C(81) C(82) C(83) . . . . 171(2) no Sb(4) C(81) C(86) C(85) . . . . -173(1) no Cl(1) Pt(1) Sb(1) C(1) . . . . -50.3(4) no Cl(1) Pt(1) Sb(1) C(11) . . . . -171.0(6) no Cl(1) Pt(1) Sb(1) C(21) . . . . 67.0(5) no Cl(1) Pt(1) Sb(4) C(2) . . . . 81(1) no Cl(1) Pt(1) Sb(4) C(71) . . . . -153(1) no Cl(1) Pt(1) Sb(4) C(81) . . . . -35(1) no Cl(2) Pt(1) Sb(1) C(1) . . . . -80(2) no Cl(2) Pt(1) Sb(1) C(11) . . . . 159(3) no Cl(2) Pt(1) Sb(1) C(21) . . . . 37(2) no Cl(2) Pt(1) Sb(4) C(2) . . . . 43.8(5) no Cl(2) Pt(1) Sb(4) C(71) . . . . 170.0(7) no Cl(2) Pt(1) Sb(4) C(81) . . . . -72.6(5) no Cl(3) Pt(2) Sb(2) C(1) . . . . -77.2(5) no Cl(3) Pt(2) Sb(2) C(31) . . . . 37.4(5) no Cl(3) Pt(2) Sb(2) C(41) . . . . 159.3(5) no Cl(3) Pt(2) Sb(3) C(2) . . . . 46.4(5) no Cl(3) Pt(2) Sb(3) C(51) . . . . -65.4(5) no Cl(3) Pt(2) Sb(3) C(61) . . . . 176.7(6) no Cl(4) Pt(2) Sb(2) C(1) . . . . 107.1(5) no Cl(4) Pt(2) Sb(2) C(31) . . . . -138.4(5) no Cl(4) Pt(2) Sb(2) C(41) . . . . -16.5(5) no Cl(4) Pt(2) Sb(3) C(2) . . . . -138.1(5) no Cl(4) Pt(2) Sb(3) C(51) . . . . 110.2(5) no Cl(4) Pt(2) Sb(3) C(61) . . . . -7.8(6) no C(1) Sb(1) C(11) C(12) . . . . 133(2) no C(1) Sb(1) C(11) C(16) . . . . -50(2) no C(1) Sb(1) C(21) C(22) . . . . 129(1) no C(1) Sb(1) C(21) C(26) . . . . -50(2) no C(1) Sb(2) C(31) C(32) . . . . -23(1) no C(1) Sb(2) C(31) C(36) . . . . 153(1) no C(1) Sb(2) C(41) C(42) . . . . 29(2) no C(1) Sb(2) C(41) C(46) . . . . -155(2) no C(2) Sb(3) C(51) C(52) . . . . -121(2) no C(2) Sb(3) C(51) C(56) . . . . 62(2) no C(2) Sb(3) C(61) C(62) . . . . -165(1) no C(2) Sb(3) C(61) C(66) . . . . 9(2) no C(2) Sb(4) C(71) C(72) . . . . 27(2) no C(2) Sb(4) C(71) C(76) . . . . -152(1) no C(2) Sb(4) C(81) C(82) . . . . 78(2) no C(2) Sb(4) C(81) C(86) . . . . -113(1) no C(11) Sb(1) C(21) C(22) . . . . -125(1) no C(11) Sb(1) C(21) C(26) . . . . 55(2) no C(11) C(12) C(13) C(14) . . . . 1(3) no C(11) C(16) C(15) C(14) . . . . 1(3) no C(12) C(11) Sb(1) C(21) . . . . 23(2) no C(12) C(11) C(16) C(15) . . . . -4(3) no C(12) C(13) C(14) C(15) . . . . -4(3) no C(13) C(12) C(11) C(16) . . . . 2(3) no C(13) C(14) C(15) C(16) . . . . 3(3) no C(16) C(11) Sb(1) C(21) . . . . -160(2) no C(21) C(22) C(23) C(24) . . . . 2(3) no C(21) C(26) C(25) C(24) . . . . -4(3) no C(22) C(21) C(26) C(25) . . . . 5(3) no C(22) C(23) C(24) C(25) . . . . -1(4) no C(23) C(22) C(21) C(26) . . . . -4(3) no C(23) C(24) C(25) C(26) . . . . 2(4) no C(31) Sb(2) C(41) C(42) . . . . -74(2) no C(31) Sb(2) C(41) C(46) . . . . 102(2) no C(31) C(32) C(33) C(34) . . . . -4(3) no C(31) C(36) C(35) C(34) . . . . 2(3) no C(32) C(31) Sb(2) C(41) . . . . 81(1) no C(32) C(31) C(36) C(35) . . . . -2(3) no C(32) C(33) C(34) C(35) . . . . 3(3) no C(33) C(32) C(31) C(36) . . . . 3(3) no C(33) C(34) C(35) C(36) . . . . -2(3) no C(36) C(31) Sb(2) C(41) . . . . -104(1) no C(41) C(42) C(43) C(44) . . . . 2(3) no C(41) C(46) C(45) C(44) . . . . -1(3) no C(42) C(41) C(46) C(45) . . . . 2(3) no C(42) C(43) C(44) C(45) . . . . -2(4) no C(43) C(42) C(41) C(46) . . . . -2(3) no C(43) C(44) C(45) C(46) . . . . 2(4) no C(51) Sb(3) C(61) C(62) . . . . -63(2) no C(51) Sb(3) C(61) C(66) . . . . 111(2) no C(51) C(52) C(53) C(54) . . . . -1(3) no C(51) C(56) C(55) C(54) . . . . -2(3) no C(52) C(51) Sb(3) C(61) . . . . 134(2) no C(52) C(51) C(56) C(55) . . . . 2(3) no C(52) C(53) C(54) C(55) . . . . 1(3) no C(53) C(52) C(51) C(56) . . . . 0(3) no C(53) C(54) C(55) C(56) . . . . 1(3) no C(56) C(51) Sb(3) C(61) . . . . -42(2) no C(61) C(62) C(63) C(64) . . . . -5(4) no C(61) C(66) C(65) C(64) . . . . 0(3) no C(62) C(61) C(66) C(65) . . . . -1(3) no C(62) C(63) C(64) C(65) . . . . 4(4) no C(63) C(62) C(61) C(66) . . . . 3(3) no C(63) C(64) C(65) C(66) . . . . -2(3) no C(71) Sb(4) C(81) C(82) . . . . -30(2) no C(71) Sb(4) C(81) C(86) . . . . 140(1) no C(71) C(72) C(73) C(74) . . . . -2(3) no C(71) C(76) C(75) C(74) . . . . -1(3) no C(72) C(71) Sb(4) C(81) . . . . 139(2) no C(72) C(71) C(76) C(75) . . . . 2(3) no C(72) C(73) C(74) C(75) . . . . 3(3) no C(73) C(72) C(71) C(76) . . . . 0(3) no C(73) C(74) C(75) C(76) . . . . -2(3) no C(76) C(71) Sb(4) C(81) . . . . -40(1) no C(81) C(82) C(83) C(84) . . . . 0(3) no C(81) C(86) C(85) C(84) . . . . 3(3) no C(82) C(81) C(86) C(85) . . . . -3(3) no C(82) C(83) C(84) C(85) . . . . 0(3) no C(83) C(82) C(81) C(86) . . . . 1(3) no C(83) C(84) C(85) C(86) . . . . -2(3) no #------------------------------------------------------------------------------ # _eof