data_global _journal_name_full 'Dalton Trans.' #============================================================================== # SUBMISSION DETAILS # ================== _journal_coden_Cambridge 0222 _publ_contact_author_name 'Professor Gillian Reid' _publ_contact_author_address ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; _publ_contact_author_email gr@soton.ac.uk _publ_contact_author_fax '023 8059 3781' _publ_contact_author_phone '023 8059 3609' _publ_contact_letter ; Dear Sirs, This file contains information in CIF format for four structures and is offered as supplementary data for manuscript B610808C. Sincerely, Gillian Reid ; _publ_requested_category ? #============================================================================ # TITLE AND AUTHOR LIST # ===================== _publ_section_title ; Preparation and coordinating properties of {CH2(o-C6H4CH2SbMe2)}2, a novel wide-angle cis-chelating distibine ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. # Note order: Family_name, first name(s) or initials (or mixture). loop_ _publ_author_name _publ_author_address M.D.Brown ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; W.Levason ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; G.Reid ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; M.Webster ; School of Chemistry University of Southampton Southampton SO17 1BJ, UK ; #============================================================================ # If more than one structure is reported, the remaining sections should be # completed per structure. For each data set, replace the '?' in the # data_? line below by a unique (to this file) identifier. #============================================================================ # 05mdb010 data_05mdb010 _database_code_depnum_ccdc_archive 'CCDC 285687' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2005-07-03 _chemical_name_systematic ; Iodotrimethyl(1,2-bis(2-dimethylstibinomethylphenyl)ethane)platinum(IV) ; _chemical_name_common ;Iodotrimethyl(1,2-bis(2- dimethylstibinomethylphenyl)ethane)platinum(IV) ; _chemical_melting_point ? _chemical_formula_moiety 'C23 H37 I Pt Sb2' _chemical_formula_sum 'C23 H37 I Pt Sb2' _chemical_formula_weight 879.02 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' Sb Sb -0.5866 1.5461 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2870(15) _cell_length_b 12.7061(10) _cell_length_c 16.623(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.307(6) _cell_angle_gamma 90.00 _cell_volume 2594.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6118 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 8.643 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6784 # shelxl 0.2522 _exptl_absorpt_correction_T_max 1.0000 # 0.3053 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29152 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5928 _reflns_number_gt 5300 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+7.7700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5928 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.215470(15) 0.152155(13) 0.061602(11) 0.02080(6) Uani 1 1 d . . . Sb1 Sb 0.26655(2) 0.34137(2) 0.114861(18) 0.01804(8) Uani 1 1 d . . . Sb2 Sb 0.14656(2) 0.21341(2) -0.081707(19) 0.01903(8) Uani 1 1 d . . . I1 I 0.01084(3) 0.18176(3) 0.12247(2) 0.02696(12) Uani 0.8939(13) 1 d P . . I1A I 0.3946(2) 0.1212(2) 0.01601(16) 0.0522(9) Uani 0.1061(13) 1 d P . . C21A C 0.01084(3) 0.18176(3) 0.12247(2) 0.02696(12) Uani 0.1061(13) 1 d P . . C21 C 0.3946(2) 0.1212(2) 0.01601(16) 0.0522(9) Uani 0.8939(13) 1 d P . . C1 C 0.3378(5) 0.3395(4) 0.2328(3) 0.0325(12) Uani 1 1 d . . . H1A H 0.3962 0.2870 0.2354 0.049 Uiso 1 1 calc R . . H1B H 0.2821 0.3215 0.2718 0.049 Uiso 1 1 calc R . . H1C H 0.3678 0.4091 0.2455 0.049 Uiso 1 1 calc R . . C2 C 0.1465(4) 0.4595(4) 0.1297(3) 0.0283(11) Uani 1 1 d . . . H2A H 0.1059 0.4695 0.0788 0.042 Uiso 1 1 calc R . . H2B H 0.1819 0.5257 0.1455 0.042 Uiso 1 1 calc R . . H2C H 0.0964 0.4378 0.1716 0.042 Uiso 1 1 calc R . . C3 C 0.3942(4) 0.4288(4) 0.0560(3) 0.0245(10) Uani 1 1 d . . . H3A H 0.4655 0.4072 0.0796 0.029 Uiso 1 1 calc R . . H3B H 0.3937 0.4096 -0.0017 0.029 Uiso 1 1 calc R . . C4 C 0.3836(3) 0.5465(4) 0.0631(3) 0.0213(10) Uani 1 1 d . . . C5 C 0.4187(4) 0.5951(4) 0.1341(3) 0.0254(10) Uani 1 1 d . . . H5 H 0.4503 0.5536 0.1761 0.031 Uiso 1 1 calc R . . C6 C 0.4082(4) 0.7034(4) 0.1449(3) 0.0309(11) Uani 1 1 d . . . H6 H 0.4334 0.7352 0.1936 0.037 Uiso 1 1 calc R . . C7 C 0.3615(4) 0.7640(4) 0.0852(3) 0.0340(12) Uani 1 1 d . . . H7 H 0.3528 0.8376 0.0927 0.041 Uiso 1 1 calc R . . C8 C 0.3273(4) 0.7171(4) 0.0142(3) 0.0291(11) Uani 1 1 d . . . H8 H 0.2948 0.7596 -0.0268 0.035 Uiso 1 1 calc R . . C9 C 0.3387(4) 0.6094(4) 0.0007(3) 0.0246(10) Uani 1 1 d . . . C10 C 0.3085(4) 0.5657(4) -0.0819(3) 0.0240(10) Uani 1 1 d . . . H10A H 0.3627 0.5115 -0.0961 0.029 Uiso 1 1 calc R . . H10B H 0.3136 0.6232 -0.1219 0.029 Uiso 1 1 calc R . . C11 C 0.1943(4) 0.5168(4) -0.0891(3) 0.0242(10) Uani 1 1 d . . . H11A H 0.1901 0.4553 -0.0527 0.029 Uiso 1 1 calc R . . H11B H 0.1396 0.5690 -0.0721 0.029 Uiso 1 1 calc R . . C12 C 0.1682(4) 0.4823(3) -0.1744(3) 0.0211(9) Uani 1 1 d . . . C13 C 0.1112(4) 0.5502(4) -0.2262(3) 0.0243(10) Uani 1 1 d . . . H13 H 0.0885 0.6167 -0.2066 0.029 Uiso 1 1 calc R . . C14 C 0.0869(4) 0.5237(4) -0.3050(3) 0.0282(11) Uani 1 1 d . . . H14 H 0.0471 0.5710 -0.3388 0.034 Uiso 1 1 calc R . . C15 C 0.1210(4) 0.4270(4) -0.3346(3) 0.0288(11) Uani 1 1 d . . . H15 H 0.1044 0.4077 -0.3887 0.035 Uiso 1 1 calc R . . C16 C 0.1790(4) 0.3594(4) -0.2847(3) 0.0280(11) Uani 1 1 d . . . H16 H 0.2030 0.2940 -0.3055 0.034 Uiso 1 1 calc R . . C17 C 0.2036(4) 0.3846(3) -0.2047(3) 0.0214(9) Uani 1 1 d . . . C18 C 0.2601(4) 0.3061(4) -0.1517(3) 0.0230(10) Uani 1 1 d . . . H18A H 0.3110 0.3434 -0.1145 0.028 Uiso 1 1 calc R . . H18B H 0.3034 0.2581 -0.1853 0.028 Uiso 1 1 calc R . . C19 C -0.0002(4) 0.3016(4) -0.0934(3) 0.0282(11) Uani 1 1 d . . . H19A H 0.0022 0.3609 -0.0557 0.042 Uiso 1 1 calc R . . H19B H -0.0622 0.2563 -0.0813 0.042 Uiso 1 1 calc R . . H19C H -0.0082 0.3282 -0.1485 0.042 Uiso 1 1 calc R . . C20 C 0.1132(4) 0.0959(4) -0.1696(3) 0.0269(10) Uani 1 1 d . . . H20A H 0.1748 0.0471 -0.1718 0.040 Uiso 1 1 calc R . . H20B H 0.1018 0.1292 -0.2223 0.040 Uiso 1 1 calc R . . H20C H 0.0474 0.0571 -0.1552 0.040 Uiso 1 1 calc R . . C22 C 0.1748(5) -0.0033(4) 0.0294(3) 0.0350(12) Uani 1 1 d . . . H22A H 0.1406 -0.0038 -0.0245 0.052 Uiso 1 1 calc R . . H22B H 0.1238 -0.0320 0.0682 0.052 Uiso 1 1 calc R . . H22C H 0.2408 -0.0464 0.0294 0.052 Uiso 1 1 calc R . . C23 C 0.2768(5) 0.0904(4) 0.1713(3) 0.0366(13) Uani 1 1 d . . . H23A H 0.3055 0.1479 0.2049 0.055 Uiso 1 1 calc R . . H23B H 0.3352 0.0402 0.1605 0.055 Uiso 1 1 calc R . . H23C H 0.2182 0.0545 0.1994 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02886(10) 0.01609(9) 0.01741(10) 0.00067(6) -0.00052(7) 0.00113(7) Sb1 0.01864(14) 0.01828(15) 0.01723(16) -0.00068(11) 0.00090(12) -0.00041(11) Sb2 0.02101(14) 0.01663(14) 0.01937(16) 0.00076(11) -0.00137(12) 0.00140(11) I1 0.02800(19) 0.02476(19) 0.0284(2) -0.00368(14) 0.00695(15) -0.00704(14) I1A 0.0740(19) 0.0481(15) 0.0339(15) -0.0021(11) -0.0110(13) 0.0011(13) C21A 0.02800(19) 0.02476(19) 0.0284(2) -0.00368(14) 0.00695(15) -0.00704(14) C21 0.0740(19) 0.0481(15) 0.0339(15) -0.0021(11) -0.0110(13) 0.0011(13) C1 0.045(3) 0.038(3) 0.014(3) 0.001(2) -0.006(2) -0.007(2) C2 0.022(2) 0.026(2) 0.037(3) -0.003(2) 0.010(2) 0.0014(19) C3 0.020(2) 0.022(2) 0.032(3) -0.001(2) 0.003(2) 0.0013(18) C4 0.016(2) 0.023(2) 0.025(3) -0.0027(19) 0.0075(19) -0.0052(17) C5 0.023(2) 0.033(3) 0.020(3) -0.001(2) 0.0022(19) -0.006(2) C6 0.035(3) 0.031(3) 0.027(3) -0.007(2) 0.004(2) -0.011(2) C7 0.045(3) 0.025(3) 0.032(3) -0.008(2) 0.009(3) -0.006(2) C8 0.031(3) 0.025(2) 0.031(3) 0.002(2) 0.001(2) -0.003(2) C9 0.024(2) 0.027(2) 0.022(3) -0.004(2) 0.0026(19) -0.0078(19) C10 0.027(2) 0.024(2) 0.021(3) -0.0003(19) 0.004(2) -0.0068(19) C11 0.024(2) 0.025(2) 0.024(3) 0.0002(19) 0.0015(19) 0.0003(19) C12 0.024(2) 0.021(2) 0.018(2) -0.0010(18) 0.0028(19) -0.0025(18) C13 0.022(2) 0.021(2) 0.030(3) 0.003(2) 0.005(2) 0.0028(18) C14 0.027(2) 0.034(3) 0.024(3) 0.011(2) 0.000(2) 0.003(2) C15 0.032(3) 0.037(3) 0.017(3) 0.001(2) -0.003(2) -0.007(2) C16 0.032(3) 0.027(2) 0.025(3) -0.004(2) 0.007(2) -0.002(2) C17 0.024(2) 0.019(2) 0.022(2) -0.0017(18) 0.0035(19) -0.0045(18) C18 0.022(2) 0.020(2) 0.027(3) -0.0013(19) 0.0035(19) -0.0028(18) C19 0.023(2) 0.025(2) 0.036(3) 0.003(2) -0.003(2) 0.0035(19) C20 0.033(3) 0.021(2) 0.027(3) -0.001(2) -0.006(2) -0.001(2) C22 0.052(3) 0.020(2) 0.033(3) 0.002(2) -0.003(3) -0.001(2) C23 0.065(4) 0.022(2) 0.023(3) 0.006(2) -0.007(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C22 2.103(5) . ? Pt1 C23 2.108(5) . ? Pt1 I1A 2.377(3) . ? Pt1 Sb2 2.6279(4) . ? Pt1 Sb1 2.6329(4) . ? Pt1 I1 2.7573(5) . ? Sb1 C2 2.122(4) . ? Sb1 C1 2.128(5) . ? Sb1 C3 2.173(4) . ? Sb2 C20 2.122(5) . ? Sb2 C19 2.128(5) . ? Sb2 C18 2.182(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.506(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.392(7) . ? C4 C9 1.411(7) . ? C5 C6 1.394(7) . ? C5 H5 0.9500 . ? C6 C7 1.371(8) . ? C6 H6 0.9500 . ? C7 C8 1.380(7) . ? C7 H7 0.9500 . ? C8 C9 1.394(7) . ? C8 H8 0.9500 . ? C9 C10 1.520(7) . ? C10 C11 1.537(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.511(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.396(7) . ? C12 C17 1.411(6) . ? C13 C14 1.378(7) . ? C13 H13 0.9500 . ? C14 C15 1.391(7) . ? C14 H14 0.9500 . ? C15 C16 1.381(7) . ? C15 H15 0.9500 . ? C16 C17 1.394(7) . ? C16 H16 0.9500 . ? C17 C18 1.491(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 C22 Pt1 C23 87.1(2) . . ? C22 Pt1 I1A 88.86(17) . . ? C23 Pt1 I1A 84.20(18) . . ? C22 Pt1 Sb2 88.71(15) . . ? C23 Pt1 Sb2 174.63(15) . . ? I1A Pt1 Sb2 92.38(6) . . ? C22 Pt1 Sb1 175.09(15) . . ? C23 Pt1 Sb1 88.34(15) . . ? I1A Pt1 Sb1 92.45(6) . . ? Sb2 Pt1 Sb1 95.957(12) . . ? C22 Pt1 I1 90.45(16) . . ? C23 Pt1 I1 92.54(17) . . ? I1A Pt1 I1 176.70(6) . . ? Sb2 Pt1 I1 90.834(14) . . ? Sb1 Pt1 I1 87.961(11) . . ? C2 Sb1 C1 100.0(2) . . ? C2 Sb1 C3 101.61(18) . . ? C1 Sb1 C3 97.7(2) . . ? C2 Sb1 Pt1 121.59(14) . . ? C1 Sb1 Pt1 112.91(14) . . ? C3 Sb1 Pt1 118.97(13) . . ? C20 Sb2 C19 99.07(19) . . ? C20 Sb2 C18 97.39(19) . . ? C19 Sb2 C18 102.58(18) . . ? C20 Sb2 Pt1 117.95(13) . . ? C19 Sb2 Pt1 119.57(15) . . ? C18 Sb2 Pt1 116.53(13) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 114.1(3) . . ? C4 C3 H3A 108.7 . . ? Sb1 C3 H3A 108.7 . . ? C4 C3 H3B 108.7 . . ? Sb1 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C9 118.7(4) . . ? C5 C4 C3 118.7(4) . . ? C9 C4 C3 122.6(4) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 120.0(5) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 119.4(5) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 122.1(5) . . ? C7 C8 H8 119.0 . . ? C9 C8 H8 119.0 . . ? C8 C9 C4 118.5(4) . . ? C8 C9 C10 118.7(4) . . ? C4 C9 C10 122.7(4) . . ? C9 C10 C11 114.9(4) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C12 C11 C10 111.3(4) . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C17 118.5(4) . . ? C13 C12 C11 119.5(4) . . ? C17 C12 C11 122.0(4) . . ? C14 C13 C12 122.0(4) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.4(4) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 121.8(5) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? C16 C17 C12 118.7(4) . . ? C16 C17 C18 119.8(4) . . ? C12 C17 C18 121.4(4) . . ? C17 C18 Sb2 112.4(3) . . ? C17 C18 H18A 109.1 . . ? Sb2 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? Sb2 C18 H18B 109.1 . . ? H18A C18 H18B 107.9 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Sb2 C20 H20A 109.5 . . ? Sb2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Sb2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Pt1 C22 H22A 109.5 . . ? Pt1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Pt1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Pt1 C23 H23A 109.5 . . ? Pt1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Pt1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C10 C11 C12 176.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.866 _refine_diff_density_min -1.844 _refine_diff_density_rms 0.164 #===END OF CIF ============================================================== # 06mdb001 data_06mdb001 _database_code_depnum_ccdc_archive 'CCDC 616260' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-06-18 _chemical_name_systematic ; tetracarbonyl(1,2-bis((2-dimethylstibinomethyl)phenyl)ethane)tungsten(0) ; _chemical_name_common ;tetracarbonyl(1,2-bis((2- dimethylstibinomethyl)phenyl)ethane)tungsten(0) ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 O4 Sb2 W' _chemical_formula_sum 'C24 H28 O4 Sb2 W' _chemical_formula_structural 'W (C O)4 (C20 H28 Sb2)' _chemical_formula_weight 807.81 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 # Superceded ** _symmetry_space_group_name_Hall '-P 2yn' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9641(15) _cell_length_b 23.323(3) _cell_length_c 17.0599(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.210(5) _cell_angle_gamma 90.00 _cell_volume 5128.0(9) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11801 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 6.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5443 # 0.1554 _exptl_absorpt_correction_T_max 1.0000 # 0.3832 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 58518 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.59 _reflns_number_total 11741 _reflns_number_gt 9437 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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. There are two molecules in the asymmetric unit. Molecule 1 (W1) is not disordered but molecule 2 (W2) is. Atoms that are disordered are labelled with a final 'A'. Thus C34 and C34A are two positions of a methylene group. Five atoms were clearly idendified from the diff. Fourier as disordered (C28A,C29A,C30A,C33A,C34A). In addition C26 and C27 which appear as single peaks in the maps are disordered in the sense of being either methylene or methyl C atoms. Because of the good quality of the data, it was felt desirable to add H atoms to the disordered C atoms where needed. In order to generate the correct connectivity table needed to position H atoms, it was necessary to introduce C26A,C27A,C31A,C32A,C35A with the same coordinates and Uij as the atom without the 'A' and use the PART command. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+9.7320P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11741 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.812698(14) 0.105795(8) 0.746409(10) 0.02033(5) Uani 1 1 d . . . W2 W 0.331527(13) 0.142476(7) 0.769598(10) 0.01840(5) Uani 1 1 d . A . Sb1 Sb 0.71403(2) 0.027341(12) 0.835114(16) 0.01941(7) Uani 1 1 d . . . Sb2 Sb 0.84066(2) 0.024683(13) 0.632898(17) 0.02328(7) Uani 1 1 d . . . Sb3 Sb 0.34789(2) 0.229624(13) 0.661032(16) 0.02409(7) Uani 1 1 d . . . Sb4 Sb 0.22480(2) 0.210329(13) 0.865931(16) 0.02266(7) Uani 1 1 d . . . O1 O 1.0266(3) 0.07231(15) 0.84291(18) 0.0345(8) Uani 1 1 d . . . O2 O 0.9290(3) 0.18250(14) 0.6341(2) 0.0374(9) Uani 1 1 d . . . O3 O 0.8136(3) 0.20568(17) 0.8685(2) 0.0560(11) Uani 1 1 d . . . O4 O 0.6025(3) 0.16333(16) 0.67525(18) 0.0373(9) Uani 1 1 d . . . O5 O 0.5480(3) 0.18553(14) 0.85429(19) 0.0340(8) Uani 1 1 d . A . O6 O 0.4379(3) 0.06392(14) 0.65312(19) 0.0347(8) Uani 1 1 d . A . O7 O 0.3439(3) 0.04451(15) 0.8956(2) 0.0417(9) Uani 1 1 d . A . O8 O 0.1178(3) 0.09349(15) 0.68830(18) 0.0349(8) Uani 1 1 d . A . C1 C 0.6462(4) 0.0587(2) 0.9352(3) 0.0309(11) Uani 1 1 d . . . H1A H 0.5988 0.0903 0.9190 0.046 Uiso 1 1 calc R . . H1B H 0.7010 0.0725 0.9748 0.046 Uiso 1 1 calc R . . H1C H 0.6077 0.0278 0.9577 0.046 Uiso 1 1 calc R . . C2 C 0.8089(4) -0.0389(2) 0.8912(3) 0.0310(11) Uani 1 1 d . . . H2A H 0.8466 -0.0582 0.8520 0.046 Uiso 1 1 calc R . . H2B H 0.7650 -0.0667 0.9151 0.046 Uiso 1 1 calc R . . H2C H 0.8586 -0.0221 0.9322 0.046 Uiso 1 1 calc R . . C3 C 0.5809(3) -0.02247(19) 0.7830(2) 0.0234(10) Uani 1 1 d . . . H3A H 0.5167 0.0000 0.7864 0.028 Uiso 1 1 calc R . . H3B H 0.5879 -0.0290 0.7265 0.028 Uiso 1 1 calc R . . C4 C 0.5705(3) -0.07949(19) 0.8229(2) 0.0201(9) Uani 1 1 d . . . C5 C 0.5318(3) -0.0806(2) 0.8964(3) 0.0250(10) Uani 1 1 d . . . H5 H 0.5112 -0.0456 0.9185 0.030 Uiso 1 1 calc R . . C6 C 0.5227(4) -0.1311(2) 0.9378(3) 0.0269(10) Uani 1 1 d . . . H6 H 0.4964 -0.1306 0.9877 0.032 Uiso 1 1 calc R . . C7 C 0.5522(3) -0.1819(2) 0.9058(2) 0.0249(10) Uani 1 1 d . . . H7 H 0.5478 -0.2167 0.9341 0.030 Uiso 1 1 calc R . . C8 C 0.5885(3) -0.18224(19) 0.8323(2) 0.0231(10) Uani 1 1 d . . . H8 H 0.6078 -0.2176 0.8105 0.028 Uiso 1 1 calc R . . C9 C 0.5972(3) -0.13162(19) 0.7895(2) 0.0212(9) Uani 1 1 d . . . C10 C 0.6348(3) -0.13697(19) 0.7088(2) 0.0229(10) Uani 1 1 d . . . H10A H 0.5927 -0.1115 0.6716 0.028 Uiso 1 1 calc R . . H10B H 0.6237 -0.1769 0.6899 0.028 Uiso 1 1 calc R . . C11 C 0.7503(3) -0.12159(19) 0.7079(2) 0.0226(10) Uani 1 1 d . . . H11A H 0.7603 -0.0805 0.7215 0.027 Uiso 1 1 calc R . . H11B H 0.7920 -0.1443 0.7490 0.027 Uiso 1 1 calc R . . C12 C 0.7899(3) -0.13272(18) 0.6290(2) 0.0185(9) Uani 1 1 d . . . C13 C 0.8436(3) -0.1826(2) 0.6172(2) 0.0233(10) Uani 1 1 d . . . H13 H 0.8521 -0.2103 0.6583 0.028 Uiso 1 1 calc R . . C14 C 0.8854(3) -0.1934(2) 0.5476(3) 0.0283(11) Uani 1 1 d . . . H14 H 0.9233 -0.2276 0.5413 0.034 Uiso 1 1 calc R . . C15 C 0.8712(4) -0.1537(2) 0.4871(2) 0.0284(11) Uani 1 1 d . . . H15 H 0.8996 -0.1605 0.4389 0.034 Uiso 1 1 calc R . . C16 C 0.8155(3) -0.1041(2) 0.4970(2) 0.0248(10) Uani 1 1 d . . . H16 H 0.8046 -0.0776 0.4546 0.030 Uiso 1 1 calc R . . C17 C 0.7751(3) -0.09224(19) 0.5674(2) 0.0207(9) Uani 1 1 d . . . C18 C 0.7261(3) -0.03549(18) 0.5788(3) 0.0242(10) Uani 1 1 d . . . H18A H 0.6695 -0.0400 0.6129 0.029 Uiso 1 1 calc R . . H18B H 0.6956 -0.0203 0.5272 0.029 Uiso 1 1 calc R . . C19 C 0.9663(4) -0.0320(2) 0.6674(3) 0.0314(11) Uani 1 1 d . . . H19A H 0.9554 -0.0502 0.7176 0.047 Uiso 1 1 calc R . . H19B H 1.0314 -0.0103 0.6735 0.047 Uiso 1 1 calc R . . H19C H 0.9697 -0.0616 0.6269 0.047 Uiso 1 1 calc R . . C20 C 0.8928(4) 0.0535(2) 0.5256(3) 0.0315(11) Uani 1 1 d . . . H20A H 0.8430 0.0812 0.5002 0.047 Uiso 1 1 calc R . . H20B H 0.8988 0.0208 0.4904 0.047 Uiso 1 1 calc R . . H20C H 0.9607 0.0720 0.5368 0.047 Uiso 1 1 calc R . . C21 C 0.9493(4) 0.08212(19) 0.8066(2) 0.0235(10) Uani 1 1 d . . . C22 C 0.8859(4) 0.1551(2) 0.6769(3) 0.0276(10) Uani 1 1 d . . . C23 C 0.8108(4) 0.1680(2) 0.8248(3) 0.0313(11) Uani 1 1 d . . . C24 C 0.6762(4) 0.1388(2) 0.6985(2) 0.0273(11) Uani 1 1 d . . . C25 C 0.3993(4) 0.2057(2) 0.5508(2) 0.0279(11) Uani 1 1 d . A . H25A H 0.4021 0.2398 0.5174 0.042 Uiso 1 1 calc R . . H25B H 0.3509 0.1778 0.5243 0.042 Uiso 1 1 calc R . . H25C H 0.4686 0.1886 0.5600 0.042 Uiso 1 1 calc R . . C26 C 0.4680(5) 0.2904(2) 0.7001(3) 0.0517(17) Uani 0.576(5) 1 d P A 1 H26A H 0.4554 0.3058 0.7516 0.078 Uiso 0.576(5) 1 calc PR A 1 H26B H 0.4677 0.3218 0.6619 0.078 Uiso 0.576(5) 1 calc PR A 1 H26C H 0.5357 0.2712 0.7046 0.078 Uiso 0.576(5) 1 calc PR A 1 C27 C 0.2280(5) 0.2886(3) 0.6156(3) 0.0534(18) Uani 0.576(5) 1 d P A 1 H27A H 0.1901 0.2738 0.5662 0.064 Uiso 0.576(5) 1 calc PR A 1 H27B H 0.1779 0.2951 0.6545 0.064 Uiso 0.576(5) 1 calc PR A 1 C28 C 0.2912(6) 0.3486(3) 0.5990(4) 0.0199(17) Uani 0.576(5) 1 d P A 1 C29 C 0.3474(6) 0.3514(4) 0.5343(4) 0.0266(19) Uani 0.576(5) 1 d P A 1 H29 H 0.3476 0.3189 0.5006 0.032 Uiso 0.576(5) 1 calc PR A 1 C30 C 0.4022(10) 0.3985(6) 0.5171(7) 0.032(3) Uani 0.576(5) 1 d P A 1 H30 H 0.4418 0.3993 0.4734 0.039 Uiso 0.576(5) 1 calc PR A 1 C31 C 0.3969(5) 0.4498(3) 0.5709(3) 0.0460(15) Uani 0.576(5) 1 d P A 1 H31 H 0.4284 0.4848 0.5576 0.055 Uiso 0.576(5) 1 calc PR A 1 C32 C 0.3478(4) 0.4474(2) 0.6383(4) 0.0470(15) Uani 0.576(5) 1 d P A 1 H32 H 0.3544 0.4770 0.6768 0.056 Uiso 0.576(5) 1 calc PR A 1 C26A C 0.4680(5) 0.2904(2) 0.7001(3) 0.0517(17) Uani 0.424(5) 1 d P A 2 H26X H 0.4781 0.2927 0.7584 0.062 Uiso 0.424(5) 1 calc PR A 2 H26Y H 0.5347 0.2797 0.6807 0.062 Uiso 0.424(5) 1 calc PR A 2 C27A C 0.2280(5) 0.2886(3) 0.6156(3) 0.0534(18) Uani 0.424(5) 1 d P A 2 H27X H 0.1929 0.3038 0.6592 0.080 Uiso 0.424(5) 1 calc PR A 2 H27Y H 0.1775 0.2685 0.5783 0.080 Uiso 0.424(5) 1 calc PR A 2 H27Z H 0.2590 0.3203 0.5885 0.080 Uiso 0.424(5) 1 calc PR A 2 C28A C 0.4249(8) 0.3515(4) 0.6616(6) 0.023(2) Uani 0.424(5) 1 d P A 2 C29A C 0.4553(9) 0.3596(5) 0.5866(6) 0.032(3) Uani 0.424(5) 1 d P A 2 H29A H 0.4914 0.3298 0.5632 0.038 Uiso 0.424(5) 1 calc PR A 2 C30A C 0.4335(15) 0.4117(8) 0.5442(9) 0.032(4) Uani 0.424(5) 1 d P A 2 H30A H 0.4504 0.4143 0.4915 0.039 Uiso 0.424(5) 1 calc PR A 2 C31A C 0.3969(5) 0.4498(3) 0.5709(3) 0.0460(15) Uani 0.424(5) 1 d P A 2 H31A H 0.4001 0.4858 0.5452 0.055 Uiso 0.424(5) 1 calc PR A 2 C32A C 0.3478(4) 0.4474(2) 0.6383(4) 0.0470(15) Uani 0.424(5) 1 d P A 2 H32A H 0.2989 0.4759 0.6492 0.056 Uiso 0.424(5) 1 calc PR A 2 C33 C 0.2873(6) 0.3982(3) 0.6465(4) 0.0197(17) Uani 0.576(5) 1 d P A 1 C34 C 0.2214(6) 0.4016(3) 0.7152(4) 0.0242(18) Uani 0.576(5) 1 d P A 1 H34A H 0.2171 0.4423 0.7310 0.029 Uiso 0.576(5) 1 calc PR A 1 H34B H 0.1502 0.3890 0.6959 0.029 Uiso 0.576(5) 1 calc PR A 1 C35 C 0.2566(5) 0.3679(3) 0.7862(3) 0.0497(17) Uani 0.576(5) 1 d P A 1 H35A H 0.3310 0.3766 0.8003 0.060 Uiso 0.576(5) 1 calc PR A 1 H35B H 0.2520 0.3269 0.7711 0.060 Uiso 0.576(5) 1 calc PR A 1 C33A C 0.3745(8) 0.3965(4) 0.6968(6) 0.023(2) Uani 0.424(5) 1 d P A 2 C34A C 0.3394(9) 0.3928(5) 0.7782(6) 0.024(2) Uani 0.424(5) 1 d P A 2 H34X H 0.3950 0.3736 0.8130 0.028 Uiso 0.424(5) 1 calc PR A 2 H34Y H 0.3339 0.4325 0.7982 0.028 Uiso 0.424(5) 1 calc PR A 2 C35A C 0.2566(5) 0.3679(3) 0.7862(3) 0.0497(17) Uani 0.424(5) 1 d P A 2 H35X H 0.2691 0.3264 0.7796 0.060 Uiso 0.424(5) 1 calc PR A 2 H35Y H 0.2061 0.3797 0.7414 0.060 Uiso 0.424(5) 1 calc PR A 2 C36 C 0.2035(4) 0.3746(2) 0.8599(2) 0.0295(11) Uani 1 1 d . . . C37 C 0.1361(4) 0.4206(2) 0.8671(3) 0.0302(11) Uani 1 1 d . A . H37 H 0.1227 0.4466 0.8243 0.036 Uiso 1 1 calc R . . C38 C 0.0885(3) 0.4293(2) 0.9346(3) 0.0252(10) Uani 1 1 d . . . H38 H 0.0433 0.4610 0.9381 0.030 Uiso 1 1 calc R A . C39 C 0.1070(3) 0.3916(2) 0.9970(3) 0.0273(11) Uani 1 1 d . A . H39 H 0.0742 0.3971 1.0436 0.033 Uiso 1 1 calc R . . C40 C 0.1738(3) 0.3455(2) 0.9914(2) 0.0259(10) Uani 1 1 d . . . H40 H 0.1862 0.3197 1.0344 0.031 Uiso 1 1 calc R A . C41 C 0.2229(3) 0.33656(19) 0.9235(2) 0.0229(10) Uani 1 1 d . A . C42 C 0.2968(4) 0.2873(2) 0.9206(2) 0.0267(10) Uani 1 1 d . A . H42A H 0.3266 0.2780 0.9750 0.032 Uiso 1 1 calc R . . H42B H 0.3546 0.2993 0.8907 0.032 Uiso 1 1 calc R . . C43 C 0.0774(4) 0.2421(2) 0.8196(3) 0.0401(13) Uani 1 1 d . A . H43A H 0.0835 0.2616 0.7694 0.060 Uiso 1 1 calc R . . H43B H 0.0521 0.2692 0.8570 0.060 Uiso 1 1 calc R . . H43C H 0.0284 0.2101 0.8108 0.060 Uiso 1 1 calc R . . C44 C 0.1806(4) 0.1722(2) 0.9710(3) 0.0352(12) Uani 1 1 d . A . H44A H 0.2416 0.1549 1.0008 0.053 Uiso 1 1 calc R . . H44B H 0.1282 0.1426 0.9572 0.053 Uiso 1 1 calc R . . H44C H 0.1517 0.2017 1.0033 0.053 Uiso 1 1 calc R . . C45 C 0.4694(4) 0.17054(19) 0.8237(2) 0.0240(10) Uani 1 1 d . . . C46 C 0.3998(4) 0.09294(19) 0.6966(3) 0.0248(10) Uani 1 1 d . . . C47 C 0.3370(4) 0.08042(19) 0.8492(3) 0.0262(10) Uani 1 1 d . . . C48 C 0.1933(4) 0.1128(2) 0.7170(2) 0.0244(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02263(10) 0.01687(9) 0.02316(9) -0.00081(7) 0.01012(7) -0.00257(7) W2 0.02039(9) 0.01592(9) 0.01947(9) 0.00163(7) 0.00489(7) 0.00062(7) Sb1 0.02131(15) 0.01824(15) 0.01987(14) 0.00056(11) 0.00763(11) -0.00158(12) Sb2 0.02919(17) 0.01868(16) 0.02403(15) -0.00117(12) 0.01231(12) -0.00336(13) Sb3 0.03672(18) 0.01729(15) 0.01922(14) 0.00195(12) 0.00745(13) 0.00375(13) Sb4 0.02466(16) 0.02522(17) 0.01884(14) 0.00177(12) 0.00570(12) 0.00543(13) O1 0.033(2) 0.041(2) 0.0302(18) -0.0021(15) 0.0058(16) 0.0019(17) O2 0.043(2) 0.0223(19) 0.051(2) 0.0048(16) 0.0249(17) -0.0041(16) O3 0.052(3) 0.043(2) 0.074(3) -0.037(2) 0.008(2) 0.002(2) O4 0.030(2) 0.054(2) 0.0278(18) 0.0059(16) 0.0054(15) 0.0046(18) O5 0.034(2) 0.032(2) 0.0349(19) -0.0016(15) -0.0019(15) -0.0098(16) O6 0.042(2) 0.0272(19) 0.0364(19) -0.0060(15) 0.0087(16) 0.0066(16) O7 0.054(2) 0.030(2) 0.041(2) 0.0166(17) 0.0001(17) -0.0088(18) O8 0.0285(19) 0.051(2) 0.0252(17) -0.0004(16) 0.0021(14) -0.0152(17) C1 0.035(3) 0.032(3) 0.029(2) -0.002(2) 0.017(2) -0.003(2) C2 0.027(3) 0.029(3) 0.036(3) 0.004(2) -0.002(2) 0.001(2) C3 0.019(2) 0.025(3) 0.027(2) -0.0014(19) 0.0034(18) -0.0012(19) C4 0.015(2) 0.022(2) 0.022(2) 0.0013(18) 0.0008(17) -0.0022(18) C5 0.024(2) 0.021(2) 0.031(2) -0.0014(19) 0.0075(19) -0.002(2) C6 0.030(3) 0.029(3) 0.023(2) -0.0013(19) 0.0095(19) -0.005(2) C7 0.029(3) 0.022(2) 0.023(2) 0.0037(19) 0.0027(19) -0.005(2) C8 0.025(2) 0.021(2) 0.024(2) 0.0008(18) 0.0037(18) -0.0057(19) C9 0.018(2) 0.025(2) 0.021(2) 0.0007(18) 0.0036(17) -0.0032(19) C10 0.024(2) 0.024(2) 0.021(2) 0.0009(18) 0.0022(18) -0.005(2) C11 0.028(2) 0.022(2) 0.019(2) 0.0014(18) 0.0037(18) -0.003(2) C12 0.019(2) 0.018(2) 0.019(2) 0.0033(17) 0.0012(16) -0.0050(18) C13 0.021(2) 0.027(3) 0.021(2) 0.0029(18) -0.0007(18) -0.0012(19) C14 0.023(2) 0.030(3) 0.032(3) -0.003(2) 0.0037(19) 0.003(2) C15 0.032(3) 0.036(3) 0.018(2) -0.003(2) 0.0095(19) -0.003(2) C16 0.027(2) 0.028(3) 0.020(2) 0.0035(19) 0.0046(18) 0.000(2) C17 0.019(2) 0.023(2) 0.021(2) 0.0004(18) 0.0034(17) -0.0029(18) C18 0.027(2) 0.020(2) 0.026(2) 0.0006(18) 0.0071(19) -0.004(2) C19 0.029(3) 0.030(3) 0.036(3) -0.006(2) 0.005(2) -0.003(2) C20 0.037(3) 0.029(3) 0.033(3) 0.005(2) 0.019(2) -0.001(2) C21 0.027(3) 0.021(2) 0.024(2) 0.0006(19) 0.012(2) -0.008(2) C22 0.030(3) 0.020(2) 0.034(3) -0.004(2) 0.012(2) -0.001(2) C23 0.026(3) 0.029(3) 0.040(3) -0.004(2) 0.007(2) -0.003(2) C24 0.031(3) 0.035(3) 0.018(2) 0.000(2) 0.011(2) -0.004(2) C25 0.029(3) 0.036(3) 0.020(2) 0.000(2) 0.0072(19) 0.001(2) C26 0.093(5) 0.032(3) 0.027(3) 0.005(2) -0.010(3) -0.031(3) C27 0.071(4) 0.062(4) 0.028(3) 0.011(3) 0.008(3) 0.049(3) C28 0.024(4) 0.016(4) 0.018(4) 0.004(3) -0.006(3) 0.001(3) C29 0.035(5) 0.027(5) 0.018(4) 0.007(3) 0.005(3) 0.011(4) C30 0.043(8) 0.030(7) 0.026(7) 0.001(5) 0.013(5) 0.002(5) C31 0.044(3) 0.038(4) 0.052(4) 0.025(3) -0.013(3) -0.020(3) C32 0.031(3) 0.026(3) 0.087(4) 0.009(3) 0.017(3) 0.003(2) C26A 0.093(5) 0.032(3) 0.027(3) 0.005(2) -0.010(3) -0.031(3) C27A 0.071(4) 0.062(4) 0.028(3) 0.011(3) 0.008(3) 0.049(3) C28A 0.024(6) 0.021(6) 0.025(5) 0.005(4) 0.008(4) -0.010(5) C29A 0.034(7) 0.035(7) 0.027(6) -0.005(5) 0.008(5) -0.006(5) C30A 0.057(12) 0.018(9) 0.021(9) 0.004(6) 0.002(7) -0.009(7) C31A 0.044(3) 0.038(4) 0.052(4) 0.025(3) -0.013(3) -0.020(3) C32A 0.031(3) 0.026(3) 0.087(4) 0.009(3) 0.017(3) 0.003(2) C33 0.018(4) 0.023(4) 0.017(4) 0.002(3) 0.000(3) 0.002(3) C34 0.028(4) 0.024(4) 0.022(4) 0.001(3) 0.005(3) 0.001(3) C35 0.086(5) 0.044(4) 0.023(3) 0.014(2) 0.023(3) 0.036(3) C33A 0.032(6) 0.015(5) 0.023(5) 0.001(4) 0.003(5) -0.010(5) C34A 0.034(7) 0.019(6) 0.019(5) 0.006(4) 0.009(5) -0.005(5) C35A 0.086(5) 0.044(4) 0.023(3) 0.014(2) 0.023(3) 0.036(3) C36 0.042(3) 0.028(3) 0.019(2) -0.0002(19) 0.004(2) 0.011(2) C37 0.037(3) 0.032(3) 0.021(2) -0.001(2) 0.000(2) 0.009(2) C38 0.022(2) 0.024(3) 0.029(2) -0.009(2) 0.0026(19) -0.001(2) C39 0.025(2) 0.033(3) 0.025(2) -0.010(2) 0.0082(19) -0.007(2) C40 0.029(3) 0.028(3) 0.021(2) -0.0016(19) 0.0053(19) -0.005(2) C41 0.026(2) 0.020(2) 0.022(2) -0.0031(18) 0.0029(18) 0.0026(19) C42 0.034(3) 0.029(3) 0.018(2) 0.0022(19) 0.0060(19) 0.003(2) C43 0.031(3) 0.047(4) 0.040(3) -0.006(3) -0.003(2) 0.012(3) C44 0.040(3) 0.041(3) 0.026(2) 0.007(2) 0.009(2) -0.009(2) C45 0.031(3) 0.019(2) 0.023(2) -0.0011(18) 0.007(2) -0.001(2) C46 0.030(3) 0.019(2) 0.025(2) 0.0040(19) 0.002(2) 0.002(2) C47 0.026(3) 0.019(2) 0.034(3) 0.001(2) 0.002(2) -0.007(2) C48 0.029(3) 0.027(3) 0.019(2) 0.0041(19) 0.0092(19) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C22 1.968(5) . ? W1 C23 1.975(5) . ? W1 C24 2.019(5) . ? W1 C21 2.025(5) . ? W1 Sb2 2.7590(4) . ? W1 Sb1 2.7736(4) . ? W2 C46 1.977(5) . ? W2 C47 1.980(5) . ? W2 C45 2.029(5) . ? W2 C48 2.036(5) . ? W2 Sb4 2.7589(4) . ? W2 Sb3 2.7734(4) . ? Sb1 C1 2.133(4) . ? Sb1 C2 2.135(4) . ? Sb1 C3 2.188(4) . ? Sb2 C20 2.128(4) . ? Sb2 C19 2.131(5) . ? Sb2 C18 2.175(4) . ? Sb3 C25 2.137(4) . ? Sb3 C27 2.156(5) . ? Sb3 C26 2.158(5) . ? Sb4 C43 2.121(5) . ? Sb4 C44 2.134(4) . ? Sb4 C42 2.186(5) . ? O1 C21 1.143(5) . ? O2 C22 1.159(5) . ? O3 C23 1.151(6) . ? O4 C24 1.148(6) . ? O5 C45 1.149(5) . ? O6 C46 1.154(5) . ? O7 C47 1.150(5) . ? O8 C48 1.140(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.506(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.400(6) . ? C4 C9 1.402(6) . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? C6 C7 1.376(6) . ? C6 H6 0.9500 . ? C7 C8 1.386(6) . ? C7 H7 0.9500 . ? C8 C9 1.399(6) . ? C8 H8 0.9500 . ? C9 C10 1.515(5) . ? C10 C11 1.541(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.514(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.382(6) . ? C12 C17 1.411(6) . ? C13 C14 1.381(6) . ? C13 H13 0.9500 . ? C14 C15 1.384(6) . ? C14 H14 0.9500 . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 C17 1.390(6) . ? C16 H16 0.9500 . ? C17 C18 1.490(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.661(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.388(10) . ? C28 C33 1.418(10) . ? C29 C30 1.358(15) . ? C29 H29 0.9500 . ? C30 C31 1.514(13) . ? C30 H30 0.9500 . ? C31 C32 1.375(8) . ? C31 H31 0.9500 . ? C32 C33 1.404(9) . ? C32 H32 0.9500 . ? C28A C29A 1.392(14) . ? C28A C33A 1.404(14) . ? C29A C30A 1.43(2) . ? C29A H29A 0.9500 . ? C30A H30A 0.9500 . ? C33 C34 1.525(9) . ? C34 C35 1.474(8) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.506(6) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C33A C34A 1.511(13) . ? C34A H34X 0.9900 . ? C34A H34Y 0.9900 . ? C36 C37 1.396(6) . ? C36 C41 1.404(6) . ? C37 C38 1.379(6) . ? C37 H37 0.9500 . ? C38 C39 1.382(6) . ? C38 H38 0.9500 . ? C39 C40 1.390(6) . ? C39 H39 0.9500 . ? C40 C41 1.395(6) . ? C40 H40 0.9500 . ? C41 C42 1.500(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? 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 C22 W1 C23 91.22(19) . . ? C22 W1 C24 89.57(19) . . ? C23 W1 C24 85.39(19) . . ? C22 W1 C21 90.72(18) . . ? C23 W1 C21 86.07(19) . . ? C24 W1 C21 171.45(18) . . ? C22 W1 Sb2 82.45(13) . . ? C23 W1 Sb2 172.35(14) . . ? C24 W1 Sb2 98.80(13) . . ? C21 W1 Sb2 89.70(12) . . ? C22 W1 Sb1 174.34(13) . . ? C23 W1 Sb1 94.31(14) . . ? C24 W1 Sb1 92.08(12) . . ? C21 W1 Sb1 88.46(11) . . ? Sb2 W1 Sb1 91.947(12) . . ? C46 W2 C47 91.12(18) . . ? C46 W2 C45 92.46(18) . . ? C47 W2 C45 87.65(18) . . ? C46 W2 C48 87.53(18) . . ? C47 W2 C48 91.07(18) . . ? C45 W2 C48 178.73(18) . . ? C46 W2 Sb4 176.48(13) . . ? C47 W2 Sb4 89.66(13) . . ? C45 W2 Sb4 91.01(12) . . ? C48 W2 Sb4 89.02(12) . . ? C46 W2 Sb3 86.31(12) . . ? C47 W2 Sb3 173.58(13) . . ? C45 W2 Sb3 86.58(12) . . ? C48 W2 Sb3 94.69(12) . . ? Sb4 W2 Sb3 93.265(12) . . ? C1 Sb1 C2 99.04(19) . . ? C1 Sb1 C3 97.57(18) . . ? C2 Sb1 C3 100.88(18) . . ? C1 Sb1 W1 117.69(13) . . ? C2 Sb1 W1 116.39(13) . . ? C3 Sb1 W1 121.25(11) . . ? C20 Sb2 C19 97.44(18) . . ? C20 Sb2 C18 96.03(18) . . ? C19 Sb2 C18 100.56(18) . . ? C20 Sb2 W1 117.71(13) . . ? C19 Sb2 W1 112.72(13) . . ? C18 Sb2 W1 127.20(11) . . ? C25 Sb3 C27 97.56(18) . . ? C25 Sb3 C26 99.2(2) . . ? C27 Sb3 C26 99.2(3) . . ? C25 Sb3 W2 116.75(13) . . ? C27 Sb3 W2 127.12(17) . . ? C26 Sb3 W2 112.34(14) . . ? C43 Sb4 C44 98.4(2) . . ? C43 Sb4 C42 101.43(19) . . ? C44 Sb4 C42 97.19(18) . . ? C43 Sb4 W2 117.89(14) . . ? C44 Sb4 W2 117.32(15) . . ? C42 Sb4 W2 120.44(12) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 113.0(3) . . ? C4 C3 H3A 109.0 . . ? Sb1 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? Sb1 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C9 118.4(4) . . ? C5 C4 C3 118.6(4) . . ? C9 C4 C3 123.0(4) . . ? C6 C5 C4 122.1(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C7 C6 C5 119.1(4) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 121.4(4) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 118.9(4) . . ? C8 C9 C10 117.2(4) . . ? C4 C9 C10 123.9(4) . . ? C9 C10 C11 113.5(3) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C11 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 113.1(3) . . ? C12 C11 H11A 109.0 . . ? C10 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? C10 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C17 119.0(4) . . ? C13 C12 C11 119.9(4) . . ? C17 C12 C11 121.1(4) . . ? C14 C13 C12 122.0(4) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 119.8(4) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 121.5(4) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C12 118.5(4) . . ? C16 C17 C18 119.8(4) . . ? C12 C17 C18 121.5(4) . . ? C17 C18 Sb2 110.3(3) . . ? C17 C18 H18A 109.6 . . ? Sb2 C18 H18A 109.6 . . ? C17 C18 H18B 109.6 . . ? Sb2 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Sb2 C20 H20A 109.5 . . ? Sb2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Sb2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 W1 175.4(4) . . ? O2 C22 W1 177.6(4) . . ? O3 C23 W1 176.4(4) . . ? O4 C24 W1 172.1(4) . . ? Sb3 C25 H25A 109.5 . . ? Sb3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Sb3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Sb3 C26 H26A 109.5 . . ? Sb3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Sb3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 Sb3 104.4(4) . . ? C28 C27 H27A 110.9 . . ? Sb3 C27 H27A 110.9 . . ? C28 C27 H27B 110.9 . . ? Sb3 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C29 C28 C33 118.1(7) . . ? C29 C28 C27 119.1(6) . . ? C33 C28 C27 122.8(6) . . ? C30 C29 C28 122.8(8) . . ? C30 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C29 C30 C31 116.8(9) . . ? C29 C30 H30 121.6 . . ? C31 C30 H30 121.6 . . ? C32 C31 C30 122.0(7) . . ? C32 C31 H31 119.0 . . ? C30 C31 H31 119.0 . . ? C31 C32 C33 115.5(6) . . ? C31 C32 H32 122.2 . . ? C33 C32 H32 122.2 . . ? C29A C28A C33A 118.8(10) . . ? C28A C29A C30A 121.5(12) . . ? C28A C29A H29A 119.3 . . ? C30A C29A H29A 119.3 . . ? C29A C30A H30A 118.8 . . ? C32 C33 C28 123.7(6) . . ? C32 C33 C34 113.6(6) . . ? C28 C33 C34 122.6(7) . . ? C35 C34 C33 117.0(6) . . ? C35 C34 H34A 108.0 . . ? C33 C34 H34A 108.0 . . ? C35 C34 H34B 108.0 . . ? C33 C34 H34B 108.0 . . ? H34A C34 H34B 107.3 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H35A 107.3 . . ? C36 C35 H35A 107.3 . . ? C34 C35 H35B 107.3 . . ? C36 C35 H35B 107.3 . . ? H35A C35 H35B 106.9 . . ? C28A C33A C34A 123.4(9) . . ? C33A C34A H34X 107.7 . . ? C33A C34A H34Y 107.7 . . ? H34X C34A H34Y 107.1 . . ? C37 C36 C41 118.7(4) . . ? C37 C36 C35 120.0(4) . . ? C41 C36 C35 121.3(4) . . ? C38 C37 C36 121.7(4) . . ? C38 C37 H37 119.1 . . ? C36 C37 H37 119.1 . . ? C37 C38 C39 119.6(4) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C38 C39 C40 119.7(4) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C41 121.1(4) . . ? C39 C40 H40 119.4 . . ? C41 C40 H40 119.4 . . ? C40 C41 C36 119.1(4) . . ? C40 C41 C42 119.5(4) . . ? C36 C41 C42 121.3(4) . . ? C41 C42 Sb4 113.5(3) . . ? C41 C42 H42A 108.9 . . ? Sb4 C42 H42A 108.9 . . ? C41 C42 H42B 108.9 . . ? Sb4 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? Sb4 C43 H43A 109.5 . . ? Sb4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Sb4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Sb4 C44 H44A 109.5 . . ? Sb4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Sb4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O5 C45 W2 178.9(4) . . ? O6 C46 W2 178.7(4) . . ? O7 C47 W2 177.6(4) . . ? O8 C48 W2 176.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag # C22 W1 Sb1 C1 179(20) . . . . ? # C22 W1 Sb1 C2 61.8(14) . . . . ? # C22 W1 Sb1 C3 -61.4(14) . . . . ? # C23 W1 Sb2 C20 -45.5(11) . . . . ? # C23 W1 Sb2 C19 66.7(11) . . . . ? # C23 W1 Sb2 C18 -168.7(11) . . . . ? # C47 W2 Sb3 C25 74.8(12) . . . . ? # C47 W2 Sb3 C27 -160.8(12) . . . . ? # C47 W2 Sb3 C26 -38.9(12) . . . . ? # C46 W2 Sb4 C43 -20(2) . . . . ? # C46 W2 Sb4 C44 97(2) . . . . ? # C46 W2 Sb4 C42 -145(2) . . . . ? # C22 W1 C21 O1 75(4) . . . . ? # C23 W1 C21 O1 -16(4) . . . . ? # C24 W1 C21 O1 -17(5) . . . . ? # Sb2 W1 C21 O1 158(4) . . . . ? # Sb1 W1 C21 O1 -110(4) . . . . ? # C23 W1 C22 O2 180(100) . . . . ? # C24 W1 C22 O2 -95(11) . . . . ? # C21 W1 C22 O2 93(11) . . . . ? # Sb2 W1 C22 O2 4(11) . . . . ? # Sb1 W1 C22 O2 12(12) . . . . ? # C22 W1 C23 O3 -16(8) . . . . ? # C24 W1 C23 O3 -106(8) . . . . ? # C21 W1 C23 O3 74(8) . . . . ? # Sb2 W1 C23 O3 18(9) . . . . ? # Sb1 W1 C23 O3 162(8) . . . . ? # C22 W1 C24 O4 -66(3) . . . . ? # C23 W1 C24 O4 25(3) . . . . ? # C21 W1 C24 O4 25(3) . . . . ? # Sb2 W1 C24 O4 -149(3) . . . . ? # Sb1 W1 C24 O4 119(3) . . . . ? C23 W1 Sb1 C1 11.5(2) . . . . ? C24 W1 Sb1 C1 -74.1(2) . . . . ? C21 W1 Sb1 C1 97.4(2) . . . . ? Sb2 W1 Sb1 C1 -172.95(16) . . . . ? C23 W1 Sb1 C2 -105.8(2) . . . . ? C24 W1 Sb1 C2 168.65(19) . . . . ? C21 W1 Sb1 C2 -19.88(19) . . . . ? Sb2 W1 Sb1 C2 69.76(15) . . . . ? C23 W1 Sb1 C3 131.0(2) . . . . ? C24 W1 Sb1 C3 45.44(19) . . . . ? C21 W1 Sb1 C3 -143.09(18) . . . . ? Sb2 W1 Sb1 C3 -53.44(14) . . . . ? C22 W1 Sb2 C20 -11.2(2) . . . . ? C24 W1 Sb2 C20 77.2(2) . . . . ? C21 W1 Sb2 C20 -101.92(19) . . . . ? Sb1 W1 Sb2 C20 169.63(16) . . . . ? C22 W1 Sb2 C19 101.1(2) . . . . ? C24 W1 Sb2 C19 -170.54(19) . . . . ? C21 W1 Sb2 C19 10.32(18) . . . . ? Sb1 W1 Sb2 C19 -78.13(14) . . . . ? C22 W1 Sb2 C18 -134.4(2) . . . . ? C24 W1 Sb2 C18 -45.98(19) . . . . ? C21 W1 Sb2 C18 134.88(19) . . . . ? Sb1 W1 Sb2 C18 46.43(15) . . . . ? C46 W2 Sb3 C25 8.20(19) . . . . ? C45 W2 Sb3 C25 100.89(19) . . . . ? C48 W2 Sb3 C25 -79.01(19) . . . . ? Sb4 W2 Sb3 C25 -168.29(14) . . . . ? C46 W2 Sb3 C27 132.7(2) . . . . ? C45 W2 Sb3 C27 -134.6(2) . . . . ? C48 W2 Sb3 C27 45.5(2) . . . . ? Sb4 W2 Sb3 C27 -43.8(2) . . . . ? C46 W2 Sb3 C26 -105.4(2) . . . . ? C45 W2 Sb3 C26 -12.7(2) . . . . ? C48 W2 Sb3 C26 167.4(2) . . . . ? Sb4 W2 Sb3 C26 78.1(2) . . . . ? C47 W2 Sb4 C43 -122.7(2) . . . . ? C45 W2 Sb4 C43 149.6(2) . . . . ? C48 W2 Sb4 C43 -31.7(2) . . . . ? Sb3 W2 Sb4 C43 62.99(18) . . . . ? C47 W2 Sb4 C44 -5.4(2) . . . . ? C45 W2 Sb4 C44 -93.1(2) . . . . ? C48 W2 Sb4 C44 85.7(2) . . . . ? Sb3 W2 Sb4 C44 -179.68(16) . . . . ? C47 W2 Sb4 C42 112.43(19) . . . . ? C45 W2 Sb4 C42 24.79(18) . . . . ? C48 W2 Sb4 C42 -156.49(18) . . . . ? Sb3 W2 Sb4 C42 -61.84(13) . . . . ? C1 Sb1 C3 C4 -79.0(3) . . . . ? C2 Sb1 C3 C4 21.8(3) . . . . ? W1 Sb1 C3 C4 152.0(2) . . . . ? Sb1 C3 C4 C5 75.8(4) . . . . ? Sb1 C3 C4 C9 -104.6(4) . . . . ? C9 C4 C5 C6 2.2(7) . . . . ? C3 C4 C5 C6 -178.2(4) . . . . ? C4 C5 C6 C7 -0.2(7) . . . . ? C5 C6 C7 C8 -1.4(7) . . . . ? C6 C7 C8 C9 0.8(7) . . . . ? C7 C8 C9 C4 1.3(6) . . . . ? C7 C8 C9 C10 -178.4(4) . . . . ? C5 C4 C9 C8 -2.7(6) . . . . ? C3 C4 C9 C8 177.7(4) . . . . ? C5 C4 C9 C10 176.9(4) . . . . ? C3 C4 C9 C10 -2.7(6) . . . . ? C8 C9 C10 C11 -100.8(5) . . . . ? C4 C9 C10 C11 79.6(5) . . . . ? C9 C10 C11 C12 174.3(4) . . . . ? C10 C11 C12 C13 -98.3(5) . . . . ? C10 C11 C12 C17 83.2(5) . . . . ? C17 C12 C13 C14 1.6(7) . . . . ? C11 C12 C13 C14 -176.9(4) . . . . ? C12 C13 C14 C15 -1.4(7) . . . . ? C13 C14 C15 C16 -0.2(7) . . . . ? C14 C15 C16 C17 1.6(7) . . . . ? C15 C16 C17 C12 -1.4(7) . . . . ? C15 C16 C17 C18 173.1(4) . . . . ? C13 C12 C17 C16 -0.1(6) . . . . ? C11 C12 C17 C16 178.4(4) . . . . ? C13 C12 C17 C18 -174.6(4) . . . . ? C11 C12 C17 C18 3.9(6) . . . . ? C16 C17 C18 Sb2 -91.4(4) . . . . ? C12 C17 C18 Sb2 83.0(4) . . . . ? C20 Sb2 C18 C17 87.1(3) . . . . ? C19 Sb2 C18 C17 -11.7(3) . . . . ? W1 Sb2 C18 C17 -141.1(2) . . . . ? C25 Sb3 C27 C28 -79.8(4) . . . . ? C26 Sb3 C27 C28 20.8(4) . . . . ? W2 Sb3 C27 C28 148.1(3) . . . . ? Sb3 C27 C28 C29 74.6(7) . . . . ? Sb3 C27 C28 C33 -107.8(6) . . . . ? C33 C28 C29 C30 3.1(13) . . . . ? C27 C28 C29 C30 -179.2(8) . . . . ? C28 C29 C30 C31 -1.9(15) . . . . ? C29 C30 C31 C32 6.3(14) . . . . ? C30 C31 C32 C33 -11.2(10) . . . . ? C33A C28A C29A C30A -2.0(17) . . . . ? C31 C32 C33 C28 12.6(10) . . . . ? C31 C32 C33 C34 -171.0(6) . . . . ? C29 C28 C33 C32 -8.8(11) . . . . ? C27 C28 C33 C32 173.6(6) . . . . ? C29 C28 C33 C34 175.2(7) . . . . ? C27 C28 C33 C34 -2.4(10) . . . . ? C32 C33 C34 C35 -104.8(8) . . . . ? C28 C33 C34 C35 71.6(9) . . . . ? C33 C34 C35 C36 172.4(6) . . . . ? C29A C28A C33A C34A -179.1(10) . . . . ? C34 C35 C36 C37 -13.3(9) . . . . ? C34 C35 C36 C41 169.0(6) . . . . ? C41 C36 C37 C38 -0.1(8) . . . . ? C35 C36 C37 C38 -178.0(5) . . . . ? C36 C37 C38 C39 -0.3(7) . . . . ? C37 C38 C39 C40 0.4(7) . . . . ? C38 C39 C40 C41 0.1(7) . . . . ? C39 C40 C41 C36 -0.5(7) . . . . ? C39 C40 C41 C42 178.2(4) . . . . ? C37 C36 C41 C40 0.6(7) . . . . ? C35 C36 C41 C40 178.4(5) . . . . ? C37 C36 C41 C42 -178.2(4) . . . . ? C35 C36 C41 C42 -0.4(8) . . . . ? C40 C41 C42 Sb4 94.9(4) . . . . ? C36 C41 C42 Sb4 -86.4(5) . . . . ? C43 Sb4 C42 C41 9.5(3) . . . . ? C44 Sb4 C42 C41 -90.6(3) . . . . ? W2 Sb4 C42 C41 141.7(2) . . . . ? # C46 W2 C45 O5 -39(19) . . . . ? # C47 W2 C45 O5 52(19) . . . . ? # C48 W2 C45 O5 50(23) . . . . ? # Sb4 W2 C45 O5 141(19) . . . . ? # Sb3 W2 C45 O5 -125(19) . . . . ? # C47 W2 C46 O6 106(18) . . . . ? # C45 W2 C46 O6 -166(100) . . . . ? # C48 W2 C46 O6 15(18) . . . . ? # Sb4 W2 C46 O6 3(20) . . . . ? # Sb3 W2 C46 O6 -80(18) . . . . ? # C46 W2 C47 O7 65(10) . . . . ? # C45 W2 C47 O7 -27(10) . . . . ? # C48 W2 C47 O7 152(10) . . . . ? # Sb4 W2 C47 O7 -119(10) . . . . ? # Sb3 W2 C47 O7 -1(11) . . . . ? # C46 W2 C48 O8 53(6) . . . . ? # C47 W2 C48 O8 -38(6) . . . . ? # C45 W2 C48 O8 -36(12) . . . . ? # Sb4 W2 C48 O8 -128(6) . . . . ? # Sb3 W2 C48 O8 139(6) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.845 _refine_diff_density_min -1.277 _refine_diff_density_rms 0.159 #===END OF CIF ============================================================== # 06mdb003 data_06mdb003 _database_code_depnum_ccdc_archive 'CCDC 616261' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-07-18 _chemical_name_systematic ; tetracarbonyl(1,2-bis((2-dimethylstibinomethyl)phenyl)ethane)tungsten(0) ; _chemical_name_common ;tetracarbonyl(1,2-bis((2- dimethylstibinomethyl)phenyl)ethane)tungsten(0) ; _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 O4 Sb2 W' _chemical_formula_sum 'C24 H28 O4 Sb2 W' _chemical_formula_weight 807.81 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' O O 0.0106 0.0060 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc _symmetry_Int_Tables_number 9 # Superceded ** _symmetry_space_group_name_Hall 'C -2yc' # Superceded ** loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 17.705(3) _cell_length_b 11.6869(15) _cell_length_c 12.4991(10) _cell_angle_alpha 90.00 _cell_angle_beta 94.506(10) _cell_angle_gamma 90.00 _cell_volume 2578.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2908 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 6.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7500 # 0.3538 _exptl_absorpt_correction_T_max 1.0000 # 0.5601 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17199 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5633 _reflns_number_gt 5428 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.208(4) _refine_ls_number_reflns 5633 _refine_ls_number_parameters 281 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0235 _refine_ls_wR_factor_ref 0.0495 _refine_ls_wR_factor_gt 0.0489 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.980999(11) 0.961247(14) 0.552447(13) 0.01959(5) Uani 1 1 d . . . Sb1 Sb 0.874861(17) 0.78825(3) 0.55926(2) 0.02388(8) Uani 1 1 d . . . Sb2 Sb 1.068267(18) 0.82487(3) 0.43084(2) 0.02490(8) Uani 1 1 d . . . O1 O 1.0702(2) 0.8608(3) 0.7618(3) 0.0367(9) Uani 1 1 d . . . O2 O 0.9006(2) 1.1051(3) 0.3597(3) 0.0345(8) Uani 1 1 d . . . O3 O 0.8775(2) 1.0933(3) 0.7036(3) 0.0330(9) Uani 1 1 d . . . O4 O 1.1059(3) 1.1531(4) 0.5545(4) 0.0488(11) Uani 1 1 d . . . C1 C 0.7703(3) 0.8309(4) 0.6241(4) 0.0322(12) Uani 1 1 d . . . H1A H 0.7805 0.8774 0.6889 0.048 Uiso 1 1 calc R . . H1B H 0.7440 0.7606 0.6423 0.048 Uiso 1 1 calc R . . H1C H 0.7384 0.8744 0.5708 0.048 Uiso 1 1 calc R . . C2 C 0.8293(3) 0.6894(5) 0.4232(5) 0.0407(14) Uani 1 1 d . . . H2A H 0.8709 0.6619 0.3827 0.061 Uiso 1 1 calc R . . H2B H 0.7953 0.7376 0.3768 0.061 Uiso 1 1 calc R . . H2C H 0.8010 0.6240 0.4484 0.061 Uiso 1 1 calc R . . C3 C 0.9144(3) 0.6559(5) 0.6713(4) 0.0305(12) Uani 1 1 d . . . H3A H 0.9699 0.6474 0.6684 0.037 Uiso 1 1 calc R . . H3B H 0.9050 0.6809 0.7447 0.037 Uiso 1 1 calc R . . C4 C 0.8777(3) 0.5406(4) 0.6508(5) 0.0281(13) Uani 1 1 d . . . C5 C 0.8063(3) 0.5223(5) 0.6807(5) 0.0372(14) Uani 1 1 d . . . H5 H 0.7812 0.5835 0.7132 0.045 Uiso 1 1 calc R . . C6 C 0.7685(4) 0.4189(6) 0.6659(5) 0.0463(16) Uani 1 1 d . . . H6 H 0.7180 0.4109 0.6854 0.056 Uiso 1 1 calc R . . C7 C 0.8048(3) 0.3292(5) 0.6233(5) 0.0361(13) Uani 1 1 d . . . H7 H 0.7808 0.2566 0.6158 0.043 Uiso 1 1 calc R . . C8 C 0.8769(4) 0.3448(5) 0.5910(5) 0.0441(15) Uani 1 1 d . . . H8 H 0.9004 0.2833 0.5566 0.053 Uiso 1 1 calc R . . C9 C 0.9172(3) 0.4489(5) 0.6073(5) 0.0326(13) Uani 1 1 d . . . C10 C 0.9996(3) 0.4541(5) 0.5737(5) 0.0358(14) Uani 1 1 d . . . H10A H 1.0312 0.4989 0.6275 0.043 Uiso 1 1 calc R . . H10B H 1.0206 0.3757 0.5724 0.043 Uiso 1 1 calc R . . C11 C 1.0032(3) 0.5066(5) 0.4679(5) 0.0339(12) Uani 1 1 d . . . H11A H 0.9882 0.5880 0.4715 0.041 Uiso 1 1 calc R . . H11B H 0.9669 0.4677 0.4157 0.041 Uiso 1 1 calc R . . C12 C 1.0819(3) 0.4985(5) 0.4299(4) 0.0280(11) Uani 1 1 d . . . C13 C 1.1008(3) 0.4053(5) 0.3678(4) 0.0317(12) Uani 1 1 d . . . H13 H 1.0639 0.3477 0.3516 0.038 Uiso 1 1 calc R . . C14 C 1.1713(3) 0.3935(5) 0.3291(4) 0.0313(12) Uani 1 1 d . . . H14 H 1.1824 0.3288 0.2872 0.038 Uiso 1 1 calc R . . C15 C 1.2256(3) 0.4771(4) 0.3519(4) 0.0297(12) Uani 1 1 d . . . H15 H 1.2741 0.4712 0.3246 0.036 Uiso 1 1 calc R . . C16 C 1.2081(3) 0.5703(4) 0.4156(4) 0.0253(11) Uani 1 1 d . . . H16 H 1.2454 0.6276 0.4311 0.030 Uiso 1 1 calc R . . C17 C 1.1379(2) 0.5817(4) 0.4567(3) 0.0182(9) Uani 1 1 d . . . C18 C 1.1204(3) 0.6838(4) 0.5223(4) 0.0228(10) Uani 1 1 d . . . H18A H 1.1680 0.7113 0.5607 0.027 Uiso 1 1 calc R . . H18B H 1.0861 0.6600 0.5771 0.027 Uiso 1 1 calc R . . C19 C 1.0270(3) 0.7385(6) 0.2891(4) 0.0423(15) Uani 1 1 d . . . H19A H 0.9793 0.6999 0.3013 0.064 Uiso 1 1 calc R . . H19B H 1.0643 0.6816 0.2698 0.064 Uiso 1 1 calc R . . H19C H 1.0183 0.7938 0.2305 0.064 Uiso 1 1 calc R . . C20 C 1.1683(3) 0.8946(6) 0.3712(5) 0.0481(17) Uani 1 1 d . . . H20A H 1.1960 0.9394 0.4278 0.072 Uiso 1 1 calc R . . H20B H 1.1542 0.9442 0.3096 0.072 Uiso 1 1 calc R . . H20C H 1.2006 0.8322 0.3489 0.072 Uiso 1 1 calc R . . C21 C 1.0372(3) 0.8932(4) 0.6844(4) 0.0234(11) Uani 1 1 d . . . C22 C 0.9284(3) 1.0470(4) 0.4253(5) 0.0272(12) Uani 1 1 d . . . C23 C 0.9161(3) 1.0446(4) 0.6467(4) 0.0240(11) Uani 1 1 d . . . C24 C 1.0590(3) 1.0813(5) 0.5540(4) 0.0316(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.02029(9) 0.01396(9) 0.02578(9) -0.00150(8) 0.00980(6) -0.00127(8) Sb1 0.02201(16) 0.01530(16) 0.03529(18) -0.00291(13) 0.00837(13) -0.00257(13) Sb2 0.02648(18) 0.02146(18) 0.02841(17) 0.00051(13) 0.01251(13) 0.00481(14) O1 0.036(2) 0.032(2) 0.042(2) 0.0083(17) 0.0038(17) 0.0002(17) O2 0.038(2) 0.034(2) 0.0318(19) 0.0059(17) 0.0062(16) 0.0075(18) O3 0.038(2) 0.023(2) 0.040(2) 0.0021(16) 0.0217(17) 0.0049(16) O4 0.049(3) 0.042(3) 0.057(3) -0.004(2) 0.017(2) -0.026(2) C1 0.029(3) 0.025(3) 0.044(3) 0.002(2) 0.013(2) -0.002(2) C2 0.043(4) 0.037(3) 0.043(3) -0.015(3) 0.007(3) -0.004(3) C3 0.030(3) 0.023(3) 0.039(3) 0.005(2) 0.003(2) 0.001(2) C4 0.032(3) 0.023(3) 0.029(3) 0.005(2) 0.005(2) 0.001(2) C5 0.031(3) 0.035(4) 0.046(4) 0.003(3) 0.007(3) -0.003(2) C6 0.033(3) 0.037(4) 0.071(5) 0.013(3) 0.023(3) -0.002(3) C7 0.029(3) 0.022(3) 0.057(4) 0.002(2) 0.000(3) -0.010(2) C8 0.055(4) 0.023(3) 0.056(4) -0.002(3) 0.015(3) -0.008(3) C9 0.033(3) 0.029(3) 0.036(3) -0.003(2) 0.004(2) -0.005(2) C10 0.036(4) 0.028(3) 0.043(4) 0.000(2) 0.004(3) -0.005(2) C11 0.031(3) 0.025(3) 0.046(3) -0.007(3) 0.001(2) -0.001(2) C12 0.025(3) 0.027(3) 0.033(3) -0.008(2) 0.004(2) -0.001(2) C13 0.037(3) 0.024(3) 0.035(3) -0.005(2) 0.005(2) -0.002(2) C14 0.029(3) 0.033(3) 0.033(3) -0.002(2) 0.009(2) 0.014(2) C15 0.024(3) 0.031(3) 0.036(3) 0.002(2) 0.017(2) 0.010(2) C16 0.025(3) 0.021(3) 0.030(3) 0.003(2) 0.008(2) 0.006(2) C17 0.017(2) 0.019(3) 0.019(2) 0.0015(18) 0.0054(17) 0.0014(19) C18 0.020(2) 0.024(3) 0.025(3) -0.004(2) 0.0030(18) -0.006(2) C19 0.053(4) 0.045(4) 0.029(3) -0.001(3) 0.003(3) 0.020(3) C20 0.042(4) 0.046(4) 0.061(4) 0.022(3) 0.034(3) 0.013(3) C21 0.024(3) 0.017(3) 0.030(3) -0.002(2) 0.011(2) -0.007(2) C22 0.025(3) 0.024(3) 0.034(3) -0.007(2) 0.010(2) -0.003(2) C23 0.026(3) 0.015(3) 0.032(3) 0.0058(19) 0.006(2) -0.0019(19) C24 0.035(3) 0.026(3) 0.035(3) -0.002(2) 0.010(2) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C23 1.966(5) . ? W1 C24 1.968(5) . ? W1 C21 2.021(5) . ? W1 C22 2.041(6) . ? W1 Sb2 2.7580(4) . ? W1 Sb1 2.7661(4) . ? Sb1 C1 2.138(5) . ? Sb1 C2 2.159(5) . ? Sb1 C3 2.165(5) . ? Sb2 C19 2.119(6) . ? Sb2 C20 2.136(5) . ? Sb2 C18 2.171(5) . ? O1 C21 1.155(6) . ? O2 C22 1.146(6) . ? O3 C23 1.173(6) . ? O4 C24 1.179(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.509(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.363(8) . ? C4 C9 1.412(8) . ? C5 C6 1.387(9) . ? C5 H5 0.9500 . ? C6 C7 1.360(9) . ? C6 H6 0.9500 . ? C7 C8 1.381(8) . ? C7 H7 0.9500 . ? C8 C9 1.417(8) . ? C8 H8 0.9500 . ? C9 C10 1.551(8) . ? C10 C11 1.463(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.511(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.394(8) . ? C12 C17 1.410(7) . ? C13 C14 1.379(7) . ? C13 H13 0.9500 . ? C14 C15 1.385(8) . ? C14 H14 0.9500 . ? C15 C16 1.399(7) . ? C15 H15 0.9500 . ? C16 C17 1.388(6) . ? C16 H16 0.9500 . ? C17 C18 1.494(7) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 C23 W1 C24 94.8(2) . . ? C23 W1 C21 88.8(2) . . ? C24 W1 C21 88.4(2) . . ? C23 W1 C22 88.3(2) . . ? C24 W1 C22 86.3(2) . . ? C21 W1 C22 173.7(2) . . ? C23 W1 Sb2 174.31(13) . . ? C24 W1 Sb2 89.66(15) . . ? C21 W1 Sb2 87.78(14) . . ? C22 W1 Sb2 95.50(15) . . ? C23 W1 Sb1 85.04(14) . . ? C24 W1 Sb1 177.23(16) . . ? C21 W1 Sb1 88.80(13) . . ? C22 W1 Sb1 96.50(15) . . ? Sb2 W1 Sb1 90.339(14) . . ? C1 Sb1 C2 98.2(2) . . ? C1 Sb1 C3 99.6(2) . . ? C2 Sb1 C3 102.1(2) . . ? C1 Sb1 W1 116.86(14) . . ? C2 Sb1 W1 125.41(17) . . ? C3 Sb1 W1 110.85(14) . . ? C19 Sb2 C20 97.5(3) . . ? C19 Sb2 C18 100.5(2) . . ? C20 Sb2 C18 98.3(2) . . ? C19 Sb2 W1 124.41(16) . . ? C20 Sb2 W1 119.18(18) . . ? C18 Sb2 W1 112.45(13) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 114.5(3) . . ? C4 C3 H3A 108.6 . . ? Sb1 C3 H3A 108.6 . . ? C4 C3 H3B 108.6 . . ? Sb1 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C9 119.0(5) . . ? C5 C4 C3 119.3(5) . . ? C9 C4 C3 121.6(5) . . ? C4 C5 C6 123.3(6) . . ? C4 C5 H5 118.4 . . ? C6 C5 H5 118.4 . . ? C7 C6 C5 119.1(6) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 119.3(5) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C7 C8 C9 122.6(6) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C4 C9 C8 116.6(5) . . ? C4 C9 C10 125.4(5) . . ? C8 C9 C10 118.0(5) . . ? C11 C10 C9 111.7(5) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.3(5) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C13 C12 C17 118.5(5) . . ? C13 C12 C11 119.5(5) . . ? C17 C12 C11 122.1(5) . . ? C14 C13 C12 122.4(5) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 119.4(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C14 C15 C16 119.0(5) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 122.1(5) . . ? C17 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C16 C17 C12 118.6(5) . . ? C16 C17 C18 120.7(4) . . ? C12 C17 C18 120.6(4) . . ? C17 C18 Sb2 114.5(3) . . ? C17 C18 H18A 108.6 . . ? Sb2 C18 H18A 108.6 . . ? C17 C18 H18B 108.6 . . ? Sb2 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Sb2 C20 H20A 109.5 . . ? Sb2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Sb2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O1 C21 W1 176.0(4) . . ? O2 C22 W1 173.1(4) . . ? O3 C23 W1 179.3(4) . . ? O4 C24 W1 179.7(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.031 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.130 #===END OF CIF ============================================================== # 06mdb002 data_06mdb002 _database_code_depnum_ccdc_archive 'CCDC 616262' _audit_creation_method 'SHELXL-97 + hand edit' _audit_creation_date 2006-07-21 _chemical_name_systematic ; Dichloro(1,2-bis((2-dimethylstibinomethyl)phenyl)ethane)platinum(II) ; _chemical_name_common ;Dichloro(1,2-bis((2- dimethylstibinomethyl)phenyl)ethane)platinum(ii) ; _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Cl2 Pt Sb2' _chemical_formula_sum 'C20 H28 Cl2 Pt Sb2' _chemical_formula_weight 777.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 # Superceded ** _symmetry_space_group_name_Hall '-P 2ybc' # Superceded ** 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 14.243(5) _cell_length_b 13.068(3) _cell_length_c 12.380(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.302(12) _cell_angle_gamma 90.00 _cell_volume 2304.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5427 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 8.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6319 # 0.4795 _exptl_absorpt_correction_T_max 1.0000 # 0.7243 _exptl_absorpt_process_details 'G.M. Sheldrick, (2003). SADABS. Version 2.10. Bruker AXS Inc.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'area detector, Nonius Kappa ccd' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25377 _diffrn_reflns_av_R_equivalents 0.1482 _diffrn_reflns_av_sigmaI/netI 0.1564 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 27.59 _reflns_number_total 5290 _reflns_number_gt 2926 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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 _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+0.7059P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5290 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1470 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.59386(3) 0.05931(3) 0.97097(4) 0.02584(16) Uani 0.9070(13) 1 d P . . Pt1A Pt 0.4618(4) 0.0813(3) 1.0808(4) 0.0363(18) Uani 0.0930(13) 1 d P . . Sb1 Sb 0.71307(5) -0.07901(5) 0.99707(6) 0.0323(2) Uani 1 1 d . . . Sb2 Sb 0.58937(5) 0.04415(5) 0.76838(6) 0.0320(2) Uani 1 1 d . . . Cl1 Cl 0.4956(2) 0.20136(17) 0.9503(2) 0.0360(7) Uani 1 1 d . . . Cl2 Cl 0.6116(2) 0.09546(18) 1.1559(2) 0.0378(7) Uani 1 1 d . . . C1 C 0.7291(8) -0.1385(8) 1.1533(9) 0.041(3) Uani 1 1 d . . . H1A H 0.6779 -0.1865 1.1681 0.062 Uiso 1 1 calc R . . H1B H 0.7274 -0.0824 1.2059 0.062 Uiso 1 1 calc R . . H1C H 0.7894 -0.1742 1.1589 0.062 Uiso 1 1 calc R . . C2 C 0.7231(9) -0.2175(7) 0.9088(10) 0.049(3) Uani 1 1 d . . . H2A H 0.7422 -0.2729 0.9575 0.073 Uiso 1 1 calc R . . H2B H 0.7699 -0.2098 0.8516 0.073 Uiso 1 1 calc R . . H2C H 0.6620 -0.2337 0.8765 0.073 Uiso 1 1 calc R . . C3 C 0.8500(8) -0.0111(7) 0.9745(9) 0.034(3) Uani 1 1 d . . . H3A H 0.8447 0.0440 0.9199 0.041 Uiso 1 1 calc R . . H3B H 0.8704 0.0207 1.0433 0.041 Uiso 1 1 calc R . . C4 C 0.9260(9) -0.0875(8) 0.9379(9) 0.042(3) Uani 1 1 d . . . C5 C 0.9635(10) -0.1559(9) 1.0119(11) 0.059(4) Uani 1 1 d . . . H5 H 0.9426 -0.1521 1.0845 0.070 Uiso 1 1 calc R . . C6 C 1.0288(10) -0.2286(9) 0.9864(12) 0.057(4) Uani 1 1 d . . . H6 H 1.0507 -0.2763 1.0387 0.068 Uiso 1 1 calc R . . C7 C 1.0618(10) -0.2300(9) 0.8816(13) 0.065(4) Uani 1 1 d . . . H7 H 1.1083 -0.2787 0.8623 0.078 Uiso 1 1 calc R . . C8 C 1.0285(9) -0.1616(9) 0.8030(11) 0.058(4) Uani 1 1 d . . . H8 H 1.0518 -0.1639 0.7314 0.070 Uiso 1 1 calc R . . C9 C 0.9598(10) -0.0892(9) 0.8322(10) 0.053(4) Uani 1 1 d . . . C10 C 0.9286(9) -0.0146(9) 0.7450(10) 0.055(4) Uani 1 1 d . . . H10A H 0.9162 0.0534 0.7772 0.066 Uiso 1 1 calc R . . H10B H 0.9787 -0.0069 0.6904 0.066 Uiso 1 1 calc R . . C11 C 0.8401(10) -0.0555(8) 0.6920(10) 0.053(4) Uani 1 1 d . . . H11A H 0.7887 -0.0550 0.7455 0.063 Uiso 1 1 calc R . . H11B H 0.8508 -0.1274 0.6700 0.063 Uiso 1 1 calc R . . C12 C 0.8095(10) 0.0065(9) 0.5926(10) 0.052(3) Uani 1 1 d . . . C13 C 0.8397(10) -0.0187(9) 0.4911(10) 0.055(4) Uani 1 1 d . . . H13 H 0.8833 -0.0732 0.4830 0.066 Uiso 1 1 calc R . . C14 C 0.8091(11) 0.0321(11) 0.4013(10) 0.061(4) Uani 1 1 d . . . H14 H 0.8319 0.0125 0.3324 0.073 Uiso 1 1 calc R . . C15 C 0.7463(11) 0.1103(10) 0.4087(11) 0.063(4) Uani 1 1 d . . . H15 H 0.7231 0.1440 0.3460 0.075 Uiso 1 1 calc R . . C16 C 0.7183(9) 0.1385(9) 0.5092(11) 0.049(3) Uani 1 1 d . . . H16 H 0.6755 0.1940 0.5151 0.058 Uiso 1 1 calc R . . C17 C 0.7485(8) 0.0911(8) 0.6044(9) 0.036(3) Uani 1 1 d . . . C18 C 0.7117(8) 0.1272(8) 0.7126(9) 0.039(3) Uani 1 1 d . . . H18A H 0.6956 0.2007 0.7070 0.047 Uiso 1 1 calc R . . H18B H 0.7624 0.1204 0.7671 0.047 Uiso 1 1 calc R . . C19 C 0.5969(9) -0.0954(7) 0.6786(11) 0.055(4) Uani 1 1 d . . . H19A H 0.5333 -0.1179 0.6595 0.083 Uiso 1 1 calc R . . H19B H 0.6277 -0.1480 0.7226 0.083 Uiso 1 1 calc R . . H19C H 0.6331 -0.0841 0.6126 0.083 Uiso 1 1 calc R . . C20 C 0.4849(8) 0.1211(8) 0.6792(9) 0.042(3) Uani 1 1 d . . . H20A H 0.5066 0.1316 0.6050 0.063 Uiso 1 1 calc R . . H20B H 0.4721 0.1875 0.7128 0.063 Uiso 1 1 calc R . . H20C H 0.4274 0.0800 0.6782 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0291(3) 0.0240(2) 0.0244(3) -0.00032(19) -0.0011(2) -0.0005(2) Pt1A 0.055(4) 0.025(2) 0.029(3) 0.0054(19) -0.011(2) 0.003(2) Sb1 0.0328(5) 0.0326(4) 0.0314(4) 0.0026(3) -0.0014(4) 0.0035(3) Sb2 0.0362(5) 0.0319(4) 0.0279(4) 0.0039(3) 0.0006(4) 0.0041(3) Cl1 0.0411(19) 0.0281(12) 0.0387(17) -0.0016(12) -0.0045(14) 0.0040(12) Cl2 0.047(2) 0.0348(13) 0.0317(15) -0.0032(12) -0.0052(14) -0.0004(13) C1 0.033(7) 0.045(6) 0.046(8) 0.006(6) -0.014(6) 0.004(6) C2 0.058(9) 0.038(6) 0.051(8) -0.004(6) -0.007(7) 0.003(6) C3 0.032(7) 0.036(6) 0.034(7) 0.009(5) 0.003(6) -0.010(5) C4 0.040(8) 0.051(7) 0.036(7) 0.005(6) -0.002(6) 0.001(6) C5 0.068(11) 0.047(7) 0.060(9) 0.012(7) -0.006(8) 0.004(7) C6 0.063(11) 0.040(7) 0.067(11) 0.009(7) -0.006(8) 0.008(7) C7 0.058(11) 0.051(8) 0.086(12) 0.001(8) -0.010(9) 0.016(7) C8 0.048(10) 0.069(9) 0.058(9) -0.016(7) 0.015(8) -0.007(7) C9 0.053(10) 0.065(8) 0.040(8) 0.002(6) 0.002(7) 0.020(7) C10 0.055(10) 0.064(8) 0.047(8) 0.001(7) 0.022(7) 0.002(7) C11 0.071(10) 0.046(7) 0.041(8) 0.006(6) 0.004(7) 0.009(7) C12 0.059(10) 0.058(8) 0.037(8) -0.001(6) 0.000(7) -0.004(7) C13 0.059(10) 0.062(8) 0.043(9) -0.026(7) 0.009(7) -0.003(7) C14 0.070(11) 0.090(10) 0.023(7) -0.007(7) 0.013(7) -0.031(9) C15 0.082(12) 0.071(9) 0.035(9) -0.001(7) -0.007(8) -0.012(9) C16 0.042(9) 0.049(7) 0.055(9) 0.016(7) 0.005(7) -0.007(6) C17 0.033(8) 0.042(6) 0.034(7) 0.008(5) -0.001(6) -0.003(5) C18 0.029(7) 0.040(6) 0.048(8) 0.011(6) -0.010(6) 0.000(5) C19 0.058(10) 0.032(6) 0.077(10) -0.013(6) -0.002(8) 0.002(6) C20 0.053(9) 0.041(6) 0.034(7) -0.002(5) -0.004(6) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 Pt1A 2.101(4) 3_657 ? Pt1 Cl1 2.338(2) . ? Pt1 Pt1A 2.344(6) . ? Pt1 Cl2 2.350(3) . ? Pt1 Sb1 2.4998(9) . ? Pt1 Sb2 2.5163(11) . ? Pt1 Pt1 3.1761(12) 3_657 ? Pt1A Pt1 2.101(4) 3_657 ? Pt1A Cl1 2.304(5) . ? Pt1A Cl2 2.330(6) . ? Pt1A Sb2 2.593(5) 3_657 ? Pt1A Sb1 2.667(5) 3_657 ? Pt1A Pt1A 3.118(10) 3_657 ? Sb1 C1 2.095(10) . ? Sb1 C2 2.119(10) . ? Sb1 C3 2.162(10) . ? Sb1 Pt1A 2.667(5) 3_657 ? Sb2 C20 2.104(10) . ? Sb2 C19 2.138(10) . ? Sb2 C18 2.169(11) . ? Sb2 Pt1A 2.593(5) 3_657 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.542(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.385(15) . ? C4 C9 1.397(17) . ? C5 C6 1.368(17) . ? C5 H5 0.9500 . ? C6 C7 1.382(18) . ? C6 H6 0.9500 . ? C7 C8 1.402(17) . ? C7 H7 0.9500 . ? C8 C9 1.409(17) . ? C8 H8 0.9500 . ? C9 C10 1.519(16) . ? C10 C11 1.515(16) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.534(15) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.371(17) . ? C12 C17 1.415(16) . ? C13 C14 1.364(16) . ? C13 H13 0.9500 . ? C14 C15 1.361(18) . ? C14 H14 0.9500 . ? C15 C16 1.360(17) . ? C15 H15 0.9500 . ? C16 C17 1.397(15) . ? C16 H16 0.9500 . ? C17 C18 1.515(15) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 Pt1A Pt1 Cl1 115.87(15) 3_657 . ? Pt1A Pt1 Pt1A 88.94(18) 3_657 . ? Cl1 Pt1 Pt1A 58.96(12) . . ? Pt1A Pt1 Cl2 120.76(15) 3_657 . ? Cl1 Pt1 Cl2 90.48(9) . . ? Pt1A Pt1 Cl2 59.52(13) . . ? Pt1A Pt1 Sb1 70.24(14) 3_657 . ? Cl1 Pt1 Sb1 173.75(7) . . ? Pt1A Pt1 Sb1 124.08(10) . . ? Cl2 Pt1 Sb1 87.13(7) . . ? Pt1A Pt1 Sb2 67.64(13) 3_657 . ? Cl1 Pt1 Sb2 86.63(7) . . ? Pt1A Pt1 Sb2 124.86(11) . . ? Cl2 Pt1 Sb2 171.45(7) . . ? Sb1 Pt1 Sb2 94.91(3) . . ? Pt1A Pt1 Pt1 47.55(16) 3_657 3_657 ? Cl1 Pt1 Pt1 84.73(8) . 3_657 ? Pt1A Pt1 Pt1 41.40(10) . 3_657 ? Cl2 Pt1 Pt1 87.93(8) . 3_657 ? Sb1 Pt1 Pt1 100.94(3) . 3_657 ? Sb2 Pt1 Pt1 99.80(3) . 3_657 ? Pt1 Pt1A Cl1 117.5(2) 3_657 . ? Pt1 Pt1A Cl2 122.3(2) 3_657 . ? Cl1 Pt1A Cl2 91.8(2) . . ? Pt1 Pt1A Pt1 91.06(18) 3_657 . ? Cl1 Pt1A Pt1 60.40(16) . . ? Cl2 Pt1A Pt1 60.37(16) . . ? Pt1 Pt1A Sb2 63.84(12) 3_657 3_657 ? Cl1 Pt1A Sb2 174.9(3) . 3_657 ? Cl2 Pt1A Sb2 91.32(16) . 3_657 ? Pt1 Pt1A Sb2 124.72(18) . 3_657 ? Pt1 Pt1A Sb1 61.91(13) 3_657 3_657 ? Cl1 Pt1A Sb1 87.26(15) . 3_657 ? Cl2 Pt1A Sb1 175.4(2) . 3_657 ? Pt1 Pt1A Sb1 122.67(18) . 3_657 ? Sb2 Pt1A Sb1 89.27(17) 3_657 3_657 ? Pt1 Pt1A Pt1A 48.72(12) 3_657 3_657 ? Cl1 Pt1A Pt1A 86.5(2) . 3_657 ? Cl2 Pt1A Pt1A 89.3(2) . 3_657 ? Pt1 Pt1A Pt1A 42.34(15) . 3_657 ? Sb2 Pt1A Pt1A 97.53(18) 3_657 3_657 ? Sb1 Pt1A Pt1A 95.08(19) 3_657 3_657 ? C1 Sb1 C2 98.8(4) . . ? C1 Sb1 C3 100.3(4) . . ? C2 Sb1 C3 102.7(5) . . ? C1 Sb1 Pt1 117.2(3) . . ? C2 Sb1 Pt1 126.8(3) . . ? C3 Sb1 Pt1 107.4(3) . . ? C1 Sb1 Pt1A 115.2(3) . 3_657 ? C2 Sb1 Pt1A 82.5(4) . 3_657 ? C3 Sb1 Pt1A 143.1(3) . 3_657 ? Pt1 Sb1 Pt1A 47.85(9) . 3_657 ? C20 Sb2 C19 99.9(4) . . ? C20 Sb2 C18 99.2(4) . . ? C19 Sb2 C18 102.6(5) . . ? C20 Sb2 Pt1 120.0(3) . . ? C19 Sb2 Pt1 125.7(3) . . ? C18 Sb2 Pt1 105.2(3) . . ? C20 Sb2 Pt1A 118.7(4) . 3_657 ? C19 Sb2 Pt1A 81.4(4) . 3_657 ? C18 Sb2 Pt1A 140.8(3) . 3_657 ? Pt1 Sb2 Pt1A 48.52(10) . 3_657 ? Pt1A Cl1 Pt1 60.64(15) . . ? Pt1A Cl2 Pt1 60.12(15) . . ? Sb1 C1 H1A 109.5 . . ? Sb1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Sb1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Sb1 C2 H2A 109.5 . . ? Sb1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Sb1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 Sb1 114.0(7) . . ? C4 C3 H3A 108.8 . . ? Sb1 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? Sb1 C3 H3B 108.8 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C9 118.4(12) . . ? C5 C4 C3 119.5(11) . . ? C9 C4 C3 122.1(10) . . ? C6 C5 C4 123.8(14) . . ? C6 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C5 C6 C7 117.4(12) . . ? C5 C6 H6 121.3 . . ? C7 C6 H6 121.3 . . ? C6 C7 C8 121.8(13) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? C7 C8 C9 118.9(13) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C4 C9 C8 119.6(11) . . ? C4 C9 C10 123.7(11) . . ? C8 C9 C10 116.7(12) . . ? C11 C10 C9 108.7(10) . . ? C11 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? C11 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C10 C11 C12 113.2(10) . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.8 . . ? C13 C12 C17 118.6(11) . . ? C13 C12 C11 121.3(12) . . ? C17 C12 C11 120.2(11) . . ? C14 C13 C12 122.0(13) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C15 C14 C13 121.2(13) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 117.4(12) . . ? C16 C15 H15 121.3 . . ? C14 C15 H15 121.3 . . ? C15 C16 C17 124.1(13) . . ? C15 C16 H16 117.9 . . ? C17 C16 H16 117.9 . . ? C16 C17 C12 116.5(11) . . ? C16 C17 C18 120.1(10) . . ? C12 C17 C18 123.3(10) . . ? C17 C18 Sb2 114.1(7) . . ? C17 C18 H18A 108.7 . . ? Sb2 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? Sb2 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? Sb2 C19 H19A 109.5 . . ? Sb2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Sb2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Sb2 C20 H20A 109.5 . . ? Sb2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Sb2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.483 _refine_diff_density_min -1.677 _refine_diff_density_rms 0.256