# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Yasushi Mizobe' _publ_contact_author_email YMIZOBE@IIS.U-TOKYO.AC.JP _publ_section_title ; Preparation of bis(hydrosulfido) complex of Mo having tetraphosphine coligand and its transformation into MoRh2 and MoIr2 mixed-metal sulfido clusters ; loop_ _publ_author_name 'Yasushi Mizobe' 'Kentaro Iwasa' 'Fumiya Niikura' 'Hidetake Seino' # Attachment 'mizobe-cif-rev.txt' data___[Mo(SH)2(P4)]_(1) _database_code_depnum_ccdc_archive 'CCDC 719133' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C46 H44 Mo P4 S2 ' _chemical_formula_moiety 'C46 H44 Mo P4 S2 ' _chemical_formula_weight 880.81 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 14.054(3) _cell_length_b 12.073(2) _cell_length_c 25.259(5) _cell_angle_alpha 90.0000 _cell_angle_beta 103.7494(10) _cell_angle_gamma 90.0000 _cell_volume 4163.1(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10141 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.9 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816.00 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.617 _exptl_absorpt_correction_T_max 0.959 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 33293 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_theta_max 27.87 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9892 _reflns_number_gt 5700 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.1300 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 9892 _refine_ls_number_parameters 528 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.2300\s(Fo^2^) + 0.0500]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.92 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Mo(1) Mo 0.18555(2) 0.27480(2) 0.177120(10) 0.02638(6) Uani 1.00 1 d . . . S(1) S 0.22884(10) 0.07746(8) 0.18470(4) 0.0504(2) Uani 1.00 1 d . . . S(2) S 0.10004(7) 0.20984(8) 0.24225(4) 0.0435(2) Uani 1.00 1 d . . . P(1) P 0.17543(6) 0.25290(7) 0.07866(3) 0.0314(2) Uani 1.00 1 d . . . P(2) P 0.04748(6) 0.39037(7) 0.13316(3) 0.03076(19) Uani 1.00 1 d . . . P(3) P 0.21351(6) 0.45380(7) 0.22205(3) 0.03036(19) Uani 1.00 1 d . . . P(4) P 0.36139(6) 0.31255(8) 0.18718(4) 0.0355(2) Uani 1.00 1 d . . . C(1) C 0.0447(2) 0.2666(3) 0.04172(14) 0.0408(9) Uani 1.00 1 d . . . C(2) C 0.0094(2) 0.3770(3) 0.05759(13) 0.0405(9) Uani 1.00 1 d . . . C(3) C 0.0646(2) 0.5398(2) 0.14306(14) 0.0363(8) Uani 1.00 1 d . . . C(4) C 0.0065(3) 0.6212(3) 0.11179(16) 0.0494(10) Uani 1.00 1 d . . . C(5) C 0.0260(3) 0.7303(3) 0.12375(19) 0.0573(12) Uani 1.00 1 d . . . C(6) C 0.1002(3) 0.7615(3) 0.16732(18) 0.0548(12) Uani 1.00 1 d . . . C(7) C 0.1586(3) 0.6814(3) 0.19894(16) 0.0465(10) Uani 1.00 1 d . . . C(8) C 0.1409(2) 0.5700(2) 0.18639(13) 0.0343(8) Uani 1.00 1 d . . . C(9) C 0.3402(2) 0.5088(3) 0.23450(15) 0.0417(9) Uani 1.00 1 d . . . C(10) C 0.3883(2) 0.4630(3) 0.19107(16) 0.0442(10) Uani 1.00 1 d . . . C(11) C 0.2240(2) 0.3514(3) 0.03532(13) 0.0370(8) Uani 1.00 1 d . . . C(12) C 0.2372(2) 0.4607(3) 0.05234(16) 0.0465(10) Uani 1.00 1 d . . . C(13) C 0.2633(3) 0.5412(3) 0.0186(2) 0.0658(14) Uani 1.00 1 d . . . C(14) C 0.2752(3) 0.5122(4) -0.0322(2) 0.0722(16) Uani 1.00 1 d . . . C(15) C 0.2617(3) 0.4045(4) -0.04960(19) 0.0657(14) Uani 1.00 1 d . . . C(16) C 0.2348(2) 0.3236(3) -0.01722(15) 0.0471(10) Uani 1.00 1 d . . . C(17) C 0.2044(2) 0.1157(2) 0.05374(13) 0.0382(8) Uani 1.00 1 d . . . C(18) C 0.2953(3) 0.0940(3) 0.04358(15) 0.0463(10) Uani 1.00 1 d . . . C(19) C 0.3187(4) -0.0125(3) 0.02959(19) 0.0650(14) Uani 1.00 1 d . . . C(20) C 0.2526(4) -0.0972(4) 0.0257(2) 0.0738(16) Uani 1.00 1 d . . . C(21) C 0.1640(4) -0.0774(3) 0.03635(18) 0.0698(15) Uani 1.00 1 d . . . C(22) C 0.1386(3) 0.0286(3) 0.05073(17) 0.0531(11) Uani 1.00 1 d . . . C(23) C -0.0723(2) 0.3688(2) 0.14989(13) 0.0353(8) Uani 1.00 1 d . . . C(24) C -0.1207(2) 0.2688(3) 0.13473(18) 0.0468(10) Uani 1.00 1 d . . . C(25) C -0.2121(3) 0.2492(3) 0.14387(19) 0.0523(11) Uani 1.00 1 d . . . C(26) C -0.2567(2) 0.3279(4) 0.16866(17) 0.0536(11) Uani 1.00 1 d . . . C(27) C -0.2102(3) 0.4256(4) 0.18469(17) 0.0576(12) Uani 1.00 1 d . . . C(28) C -0.1176(2) 0.4468(3) 0.17539(16) 0.0487(10) Uani 1.00 1 d . . . C(29) C 0.1892(2) 0.4629(2) 0.29023(13) 0.0362(8) Uani 1.00 1 d . . . C(30) C 0.0992(2) 0.5001(3) 0.29702(15) 0.0431(9) Uani 1.00 1 d . . . C(31) C 0.0775(3) 0.4972(3) 0.34798(17) 0.0515(11) Uani 1.00 1 d . . . C(32) C 0.1466(3) 0.4592(3) 0.39271(16) 0.0561(12) Uani 1.00 1 d . . . C(33) C 0.2355(3) 0.4222(3) 0.38637(16) 0.0560(12) Uani 1.00 1 d . . . C(34) C 0.2565(3) 0.4218(3) 0.33543(15) 0.0461(10) Uani 1.00 1 d . . . C(35) C 0.4393(2) 0.2605(3) 0.14367(16) 0.0491(10) Uani 1.00 1 d . . . C(36) C 0.4739(3) 0.1526(4) 0.15082(19) 0.0672(14) Uani 1.00 1 d . . . C(37) C 0.5297(3) 0.1088(6) 0.1171(2) 0.095(2) Uani 1.00 1 d . . . C(38) C 0.5496(3) 0.1715(7) 0.0759(2) 0.105(2) Uani 1.00 1 d . . . C(39) C 0.5158(3) 0.2782(6) 0.0682(2) 0.089(2) Uani 1.00 1 d . . . C(40) C 0.4613(3) 0.3241(4) 0.10232(18) 0.0636(14) Uani 1.00 1 d . . . C(41) C 0.4370(2) 0.2714(3) 0.25539(15) 0.0442(9) Uani 1.00 1 d . . . C(42) C 0.3986(3) 0.2127(3) 0.29227(16) 0.0548(11) Uani 1.00 1 d . . . C(43) C 0.4549(4) 0.1918(4) 0.34479(19) 0.0748(16) Uani 1.00 1 d . . . C(44) C 0.5485(4) 0.2325(5) 0.3608(2) 0.0822(17) Uani 1.00 1 d P . . C(45) C 0.5886(4) 0.2897(5) 0.3244(2) 0.0840(18) Uani 1.00 1 d . . . C(46) C 0.5343(3) 0.3090(4) 0.27207(19) 0.0636(13) Uani 1.00 1 d . . . H(1) H 0.0391 0.2637 0.0035 0.047 Uiso 1.00 1 c R . . H(2) H 0.0072 0.2086 0.0520 0.047 Uiso 1.00 1 c R . . H(3) H -0.0599 0.3812 0.0459 0.047 Uiso 1.00 1 c R . . H(4) H 0.0380 0.4349 0.0411 0.047 Uiso 1.00 1 c R . . H(5) H -0.0464 0.6004 0.0824 0.057 Uiso 1.00 1 c R . . H(6) H -0.0127 0.7855 0.1019 0.068 Uiso 1.00 1 c R . . H(7) H 0.1123 0.8378 0.1755 0.065 Uiso 1.00 1 c R . . H(8) H 0.2098 0.7018 0.2292 0.055 Uiso 1.00 1 c R . . H(9) H 0.3385 0.5874 0.2330 0.048 Uiso 1.00 1 c R . . H(10) H 0.3765 0.4857 0.2694 0.048 Uiso 1.00 1 c R . . H(11) H 0.4571 0.4752 0.2009 0.053 Uiso 1.00 1 c R . . H(12) H 0.3613 0.4974 0.1570 0.053 Uiso 1.00 1 c R . . H(13) H 0.2282 0.4804 0.0872 0.054 Uiso 1.00 1 c R . . H(14) H 0.2726 0.6158 0.0306 0.075 Uiso 1.00 1 c R . . H(15) H 0.2938 0.5664 -0.0551 0.086 Uiso 1.00 1 c R . . H(16) H 0.2696 0.3845 -0.0847 0.080 Uiso 1.00 1 c R . . H(17) H 0.2240 0.2495 -0.0298 0.057 Uiso 1.00 1 c R . . H(18) H 0.3411 0.1528 0.0462 0.055 Uiso 1.00 1 c R . . H(19) H 0.3812 -0.0265 0.0227 0.076 Uiso 1.00 1 c R . . H(20) H 0.2685 -0.1696 0.0158 0.086 Uiso 1.00 1 c R . . H(21) H 0.1185 -0.1365 0.0340 0.080 Uiso 1.00 1 c R . . H(22) H 0.0766 0.0418 0.0583 0.064 Uiso 1.00 1 c R . . H(23) H -0.0902 0.2136 0.1177 0.057 Uiso 1.00 1 c R . . H(24) H -0.2441 0.1806 0.1332 0.063 Uiso 1.00 1 c R . . H(25) H -0.3199 0.3145 0.1747 0.065 Uiso 1.00 1 c R . . H(26) H -0.2411 0.4801 0.2020 0.071 Uiso 1.00 1 c R . . H(27) H -0.0855 0.5150 0.1868 0.058 Uiso 1.00 1 c R . . H(28) H 0.0522 0.5277 0.2664 0.052 Uiso 1.00 1 c R . . H(29) H 0.0153 0.5215 0.3520 0.065 Uiso 1.00 1 c R . . H(30) H 0.1323 0.4588 0.4276 0.069 Uiso 1.00 1 c R . . H(31) H 0.2831 0.3964 0.4172 0.065 Uiso 1.00 1 c R . . H(32) H 0.3174 0.3938 0.3311 0.054 Uiso 1.00 1 c R . . H(33) H 0.4589 0.1084 0.1789 0.078 Uiso 1.00 1 c R . . H(34) H 0.5550 0.0357 0.1227 0.110 Uiso 1.00 1 c R . . H(35) H 0.5857 0.1404 0.0522 0.126 Uiso 1.00 1 c R . . H(36) H 0.5303 0.3212 0.0396 0.110 Uiso 1.00 1 c R . . H(37) H 0.4396 0.3988 0.0978 0.077 Uiso 1.00 1 c R . . H(38) H 0.3334 0.1857 0.2814 0.063 Uiso 1.00 1 c R . . H(39) H 0.4279 0.1502 0.3696 0.086 Uiso 1.00 1 c R . . H(40) H 0.5858 0.2199 0.3969 0.091 Uiso 1.00 1 c R . . H(41) H 0.6535 0.3174 0.3355 0.094 Uiso 1.00 1 c R . . H(42) H 0.5625 0.3471 0.2466 0.074 Uiso 1.00 1 c R . . H(43) H 0.300(7) 0.079(9) 0.193(4) 0.25(5) Uiso 1.00 1 c . . . H(44) H 0.055(4) 0.286(5) 0.259(2) 0.12(2) Uiso 1.00 1 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 Mo(1) 0.02666(14) 0.02802(14) 0.02356(13) -0.00105(10) 0.00420(9) 0.00100(10) S(1) 0.0752(7) 0.0331(4) 0.0434(5) 0.0090(4) 0.0152(4) 0.0035(3) S(2) 0.0489(5) 0.0431(4) 0.0433(4) -0.0056(4) 0.0206(4) 0.0063(3) P(1) 0.0316(4) 0.0359(4) 0.0260(3) -0.0037(3) 0.0055(3) -0.0016(3) P(2) 0.0268(3) 0.0339(4) 0.0297(4) 0.0000(3) 0.0029(3) 0.0013(3) P(3) 0.0319(4) 0.0303(3) 0.0270(3) -0.0009(3) 0.0032(3) -0.0020(3) P(4) 0.0289(4) 0.0446(4) 0.0318(4) 0.0016(3) 0.0047(3) -0.0029(3) C(1) 0.0350(17) 0.055(2) 0.0287(15) -0.0064(16) 0.0009(13) -0.0065(15) C(2) 0.0332(17) 0.053(2) 0.0313(16) 0.0026(15) 0.0006(13) 0.0028(15) C(3) 0.0386(18) 0.0323(15) 0.0375(17) 0.0022(14) 0.0080(14) 0.0033(13) C(4) 0.052(2) 0.044(2) 0.045(2) 0.0101(17) -0.0008(17) 0.0089(16) C(5) 0.066(2) 0.042(2) 0.061(2) 0.0177(19) 0.010(2) 0.0150(19) C(6) 0.074(2) 0.0297(17) 0.059(2) 0.0046(18) 0.013(2) -0.0001(17) C(7) 0.058(2) 0.0349(17) 0.044(2) -0.0021(17) 0.0054(17) -0.0069(15) C(8) 0.0407(18) 0.0322(15) 0.0302(15) 0.0018(13) 0.0089(13) 0.0029(12) C(9) 0.0356(18) 0.0384(17) 0.047(2) -0.0064(14) 0.0008(15) -0.0084(15) C(10) 0.0343(18) 0.053(2) 0.045(2) -0.0112(16) 0.0097(15) 0.0013(16) C(11) 0.0325(16) 0.0437(18) 0.0332(16) -0.0005(14) 0.0049(13) 0.0050(14) C(12) 0.045(2) 0.0458(19) 0.044(2) -0.0081(16) 0.0019(16) 0.0067(16) C(13) 0.060(2) 0.055(2) 0.072(3) -0.015(2) -0.004(2) 0.021(2) C(14) 0.059(2) 0.087(3) 0.069(3) -0.013(2) 0.011(2) 0.040(2) C(15) 0.056(2) 0.097(3) 0.048(2) 0.005(2) 0.020(2) 0.028(2) C(16) 0.050(2) 0.058(2) 0.0357(18) 0.0081(18) 0.0133(16) 0.0076(16) C(17) 0.049(2) 0.0364(16) 0.0265(15) -0.0025(15) 0.0048(14) -0.0032(13) C(18) 0.058(2) 0.0427(19) 0.0363(18) 0.0042(17) 0.0078(16) -0.0051(15) C(19) 0.073(3) 0.060(2) 0.057(2) 0.018(2) 0.006(2) -0.012(2) C(20) 0.104(4) 0.050(2) 0.061(2) 0.016(2) 0.008(2) -0.009(2) C(21) 0.112(4) 0.040(2) 0.049(2) -0.023(2) 0.002(2) -0.0056(18) C(22) 0.066(2) 0.046(2) 0.048(2) -0.0101(19) 0.0143(19) -0.0078(17) C(23) 0.0289(15) 0.0396(17) 0.0345(16) 0.0027(13) 0.0018(12) 0.0054(13) C(24) 0.0345(18) 0.0422(19) 0.067(2) 0.0007(15) 0.0182(17) 0.0008(18) C(25) 0.0360(19) 0.054(2) 0.068(2) -0.0065(17) 0.0136(18) 0.008(2) C(26) 0.0328(19) 0.081(2) 0.049(2) -0.001(2) 0.0142(16) 0.008(2) C(27) 0.044(2) 0.085(3) 0.047(2) 0.008(2) 0.0192(18) -0.015(2) C(28) 0.045(2) 0.059(2) 0.041(2) -0.0008(18) 0.0079(16) -0.0117(17) C(29) 0.0451(19) 0.0308(15) 0.0307(16) -0.0015(14) 0.0050(13) -0.0011(12) C(30) 0.051(2) 0.0427(18) 0.0360(18) 0.0030(16) 0.0102(15) -0.0029(15) C(31) 0.058(2) 0.050(2) 0.054(2) -0.0091(19) 0.0272(19) -0.0059(18) C(32) 0.082(3) 0.055(2) 0.0344(19) -0.019(2) 0.0201(19) -0.0013(17) C(33) 0.075(3) 0.054(2) 0.0335(19) -0.007(2) 0.0019(18) 0.0070(17) C(34) 0.052(2) 0.0445(19) 0.0376(18) -0.0008(17) 0.0031(16) 0.0009(15) C(35) 0.0242(16) 0.079(2) 0.0417(19) 0.0051(17) 0.0028(14) -0.0142(19) C(36) 0.050(2) 0.094(3) 0.050(2) 0.027(2) -0.0017(19) -0.022(2) C(37) 0.060(3) 0.145(5) 0.069(3) 0.051(3) -0.006(2) -0.041(3) C(38) 0.043(2) 0.198(8) 0.074(3) 0.022(3) 0.013(2) -0.057(4) C(39) 0.050(2) 0.163(6) 0.063(3) -0.025(3) 0.028(2) -0.027(3) C(40) 0.041(2) 0.103(3) 0.049(2) -0.015(2) 0.0158(18) -0.009(2) C(41) 0.0359(18) 0.055(2) 0.0365(18) 0.0126(16) -0.0013(14) -0.0113(16) C(42) 0.056(2) 0.063(2) 0.039(2) 0.013(2) -0.0018(17) 0.0025(18) C(43) 0.082(3) 0.091(3) 0.042(2) 0.030(3) -0.001(2) 0.012(2) C(44) 0.084(3) 0.096(4) 0.048(2) 0.036(3) -0.022(2) -0.008(2) C(45) 0.052(2) 0.117(4) 0.067(3) 0.018(3) -0.019(2) -0.025(3) C(46) 0.039(2) 0.090(3) 0.055(2) 0.011(2) -0.0025(18) -0.009(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) S(1) 2.4552(10) yes . . Mo(1) S(2) 2.3886(11) yes . . Mo(1) P(1) 2.4713(8) yes . . Mo(1) P(2) 2.4333(8) yes . . Mo(1) P(3) 2.4292(8) yes . . Mo(1) P(4) 2.4659(8) yes . . P(1) C(1) 1.859(3) yes . . P(1) C(11) 1.854(3) yes . . P(1) C(17) 1.851(3) yes . . P(2) C(2) 1.863(3) yes . . P(2) C(3) 1.829(3) yes . . P(2) C(23) 1.849(3) yes . . P(3) C(8) 1.840(3) yes . . P(3) C(9) 1.856(3) yes . . P(3) C(29) 1.837(3) yes . . P(4) C(10) 1.854(3) yes . . P(4) C(35) 1.837(4) yes . . P(4) C(41) 1.864(3) yes . . C(1) C(2) 1.509(5) yes . . C(3) C(4) 1.396(4) yes . . C(3) C(8) 1.387(4) yes . . C(4) C(5) 1.365(5) yes . . C(5) C(6) 1.377(5) yes . . C(6) C(7) 1.391(5) yes . . C(7) C(8) 1.391(4) yes . . C(9) C(10) 1.523(5) yes . . C(11) C(12) 1.386(5) yes . . C(11) C(16) 1.412(5) yes . . C(12) C(13) 1.398(6) yes . . C(13) C(14) 1.377(7) yes . . C(14) C(15) 1.372(7) yes . . C(15) C(16) 1.383(6) yes . . C(17) C(18) 1.386(6) yes . . C(17) C(22) 1.390(5) yes . . C(18) C(19) 1.393(6) yes . . C(19) C(20) 1.369(7) yes . . C(20) C(21) 1.357(9) yes . . C(21) C(22) 1.399(6) yes . . C(23) C(24) 1.393(5) yes . . C(23) C(28) 1.379(5) yes . . C(24) C(25) 1.378(6) yes . . C(25) C(26) 1.370(6) yes . . C(26) C(27) 1.362(6) yes . . C(27) C(28) 1.401(6) yes . . C(29) C(30) 1.391(5) yes . . C(29) C(34) 1.389(4) yes . . C(30) C(31) 1.392(6) yes . . C(31) C(32) 1.381(5) yes . . C(32) C(33) 1.372(7) yes . . C(33) C(34) 1.387(6) yes . . C(35) C(36) 1.386(7) yes . . C(35) C(40) 1.389(6) yes . . C(36) C(37) 1.392(8) yes . . C(37) C(38) 1.367(10) yes . . C(38) C(39) 1.371(11) yes . . C(39) C(40) 1.397(8) yes . . C(41) C(42) 1.378(6) yes . . C(41) C(46) 1.407(5) yes . . C(42) C(43) 1.397(5) yes . . C(43) C(44) 1.373(8) yes . . C(44) C(45) 1.372(8) yes . . C(45) C(46) 1.380(6) yes . . S(1) H(43) 0.97(10) no . . S(2) H(44) 1.25(6) no . . C(1) H(1) 0.950 no . . C(1) H(2) 0.950 no . . C(2) H(3) 0.950 no . . C(2) H(4) 0.950 no . . C(4) H(5) 0.950 no . . C(5) H(6) 0.950 no . . C(6) H(7) 0.950 no . . C(7) H(8) 0.950 no . . C(9) H(9) 0.950 no . . C(9) H(10) 0.950 no . . C(10) H(11) 0.950 no . . C(10) H(12) 0.950 no . . C(12) H(13) 0.950 no . . C(13) H(14) 0.950 no . . C(14) H(15) 0.950 no . . C(15) H(16) 0.950 no . . C(16) H(17) 0.950 no . . C(18) H(18) 0.950 no . . C(19) H(19) 0.950 no . . C(20) H(20) 0.950 no . . C(21) H(21) 0.950 no . . C(22) H(22) 0.950 no . . C(24) H(23) 0.950 no . . C(25) H(24) 0.950 no . . C(26) H(25) 0.950 no . . C(27) H(26) 0.950 no . . C(28) H(27) 0.950 no . . C(30) H(28) 0.950 no . . C(31) H(29) 0.950 no . . C(32) H(30) 0.950 no . . C(33) H(31) 0.950 no . . C(34) H(32) 0.950 no . . C(36) H(33) 0.950 no . . C(37) H(34) 0.950 no . . C(38) H(35) 0.950 no . . C(39) H(36) 0.950 no . . C(40) H(37) 0.950 no . . C(42) H(38) 0.950 no . . C(43) H(39) 0.950 no . . C(44) H(40) 0.950 no . . C(45) H(41) 0.950 no . . C(46) H(42) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(1) Mo(1) S(2) 77.50(3) yes . . . S(1) Mo(1) P(1) 85.90(3) yes . . . S(1) Mo(1) P(2) 138.42(3) yes . . . S(1) Mo(1) P(3) 144.82(3) yes . . . S(1) Mo(1) P(4) 87.00(4) yes . . . S(2) Mo(1) P(1) 137.73(3) yes . . . S(2) Mo(1) P(2) 91.45(3) yes . . . S(2) Mo(1) P(3) 91.28(3) yes . . . S(2) Mo(1) P(4) 130.21(3) yes . . . P(1) Mo(1) P(2) 75.71(2) yes . . . P(1) Mo(1) P(3) 121.98(2) yes . . . P(1) Mo(1) P(4) 86.56(3) yes . . . P(2) Mo(1) P(3) 74.09(2) yes . . . P(2) Mo(1) P(4) 127.73(3) yes . . . P(3) Mo(1) P(4) 74.96(3) yes . . . Mo(1) P(1) C(1) 108.01(12) yes . . . Mo(1) P(1) C(11) 125.77(10) yes . . . Mo(1) P(1) C(17) 118.24(10) yes . . . C(1) P(1) C(11) 96.03(15) yes . . . C(1) P(1) C(17) 100.37(16) yes . . . C(11) P(1) C(17) 103.40(16) yes . . . Mo(1) P(2) C(2) 114.92(12) yes . . . Mo(1) P(2) C(3) 116.00(10) yes . . . Mo(1) P(2) C(23) 119.04(10) yes . . . C(2) P(2) C(3) 102.84(16) yes . . . C(2) P(2) C(23) 99.59(15) yes . . . C(3) P(2) C(23) 101.84(16) yes . . . Mo(1) P(3) C(8) 116.13(10) yes . . . Mo(1) P(3) C(9) 116.07(12) yes . . . Mo(1) P(3) C(29) 116.45(11) yes . . . C(8) P(3) C(9) 102.03(15) yes . . . C(8) P(3) C(29) 102.02(15) yes . . . C(9) P(3) C(29) 101.82(16) yes . . . Mo(1) P(4) C(10) 111.94(12) yes . . . Mo(1) P(4) C(35) 126.90(12) yes . . . Mo(1) P(4) C(41) 112.53(13) yes . . . C(10) P(4) C(35) 102.9(2) yes . . . C(10) P(4) C(41) 98.51(16) yes . . . C(35) P(4) C(41) 99.88(17) yes . . . P(1) C(1) C(2) 107.1(2) yes . . . P(2) C(2) C(1) 108.4(2) yes . . . P(2) C(3) C(4) 125.2(2) yes . . . P(2) C(3) C(8) 114.8(2) yes . . . C(4) C(3) C(8) 120.0(3) yes . . . C(3) C(4) C(5) 119.7(3) yes . . . C(4) C(5) C(6) 121.0(3) yes . . . C(5) C(6) C(7) 120.0(3) yes . . . C(6) C(7) C(8) 119.5(3) yes . . . P(3) C(8) C(3) 114.9(2) yes . . . P(3) C(8) C(7) 125.3(2) yes . . . C(3) C(8) C(7) 119.8(3) yes . . . P(3) C(9) C(10) 108.7(2) yes . . . P(4) C(10) C(9) 105.9(2) yes . . . P(1) C(11) C(12) 117.9(2) yes . . . P(1) C(11) C(16) 122.6(2) yes . . . C(12) C(11) C(16) 118.8(3) yes . . . C(11) C(12) C(13) 120.5(3) yes . . . C(12) C(13) C(14) 119.9(4) yes . . . C(13) C(14) C(15) 120.1(5) yes . . . C(14) C(15) C(16) 121.1(4) yes . . . C(11) C(16) C(15) 119.6(3) yes . . . P(1) C(17) C(18) 121.3(2) yes . . . P(1) C(17) C(22) 119.9(3) yes . . . C(18) C(17) C(22) 118.5(3) yes . . . C(17) C(18) C(19) 120.4(4) yes . . . C(18) C(19) C(20) 120.6(5) yes . . . C(19) C(20) C(21) 119.6(4) yes . . . C(20) C(21) C(22) 121.0(4) yes . . . C(17) C(22) C(21) 119.9(4) yes . . . P(2) C(23) C(24) 118.1(2) yes . . . P(2) C(23) C(28) 123.8(2) yes . . . C(24) C(23) C(28) 118.1(3) yes . . . C(23) C(24) C(25) 121.1(3) yes . . . C(24) C(25) C(26) 120.2(3) yes . . . C(25) C(26) C(27) 119.9(4) yes . . . C(26) C(27) C(28) 120.5(4) yes . . . C(23) C(28) C(27) 120.3(3) yes . . . P(3) C(29) C(30) 120.8(2) yes . . . P(3) C(29) C(34) 120.5(3) yes . . . C(30) C(29) C(34) 118.4(3) yes . . . C(29) C(30) C(31) 120.7(3) yes . . . C(30) C(31) C(32) 120.0(4) yes . . . C(31) C(32) C(33) 119.7(4) yes . . . C(32) C(33) C(34) 120.7(3) yes . . . C(29) C(34) C(33) 120.5(4) yes . . . P(4) C(35) C(36) 119.0(3) yes . . . P(4) C(35) C(40) 122.1(3) yes . . . C(36) C(35) C(40) 118.9(4) yes . . . C(35) C(36) C(37) 120.5(5) yes . . . C(36) C(37) C(38) 120.1(6) yes . . . C(37) C(38) C(39) 120.1(6) yes . . . C(38) C(39) C(40) 120.4(6) yes . . . C(35) C(40) C(39) 119.8(5) yes . . . P(4) C(41) C(42) 122.2(2) yes . . . P(4) C(41) C(46) 119.4(3) yes . . . C(42) C(41) C(46) 118.2(3) yes . . . C(41) C(42) C(43) 120.7(4) yes . . . C(42) C(43) C(44) 120.1(5) yes . . . C(43) C(44) C(45) 120.0(4) yes . . . C(44) C(45) C(46) 120.4(4) yes . . . C(41) C(46) C(45) 120.6(4) yes . . . Mo(1) S(1) H(43) 103(6) no . . . Mo(1) S(2) H(44) 112(3) no . . . P(1) C(1) H(1) 109.9 no . . . P(1) C(1) H(2) 110.1 no . . . C(2) C(1) H(1) 110.5 no . . . C(2) C(1) H(2) 109.8 no . . . H(1) C(1) H(2) 109.5 no . . . P(2) C(2) H(3) 109.7 no . . . P(2) C(2) H(4) 109.6 no . . . C(1) C(2) H(3) 110.1 no . . . C(1) C(2) H(4) 109.5 no . . . H(3) C(2) H(4) 109.5 no . . . C(3) C(4) H(5) 120.0 no . . . C(5) C(4) H(5) 120.4 no . . . C(4) C(5) H(6) 119.4 no . . . C(6) C(5) H(6) 119.5 no . . . C(5) C(6) H(7) 120.1 no . . . C(7) C(6) H(7) 119.9 no . . . C(6) C(7) H(8) 120.8 no . . . C(8) C(7) H(8) 119.7 no . . . P(3) C(9) H(9) 109.7 no . . . P(3) C(9) H(10) 109.5 no . . . C(10) C(9) H(9) 110.1 no . . . C(10) C(9) H(10) 109.3 no . . . H(9) C(9) H(10) 109.5 no . . . P(4) C(10) H(11) 110.3 no . . . P(4) C(10) H(12) 110.4 no . . . C(9) C(10) H(11) 110.7 no . . . C(9) C(10) H(12) 110.1 no . . . H(11) C(10) H(12) 109.5 no . . . C(11) C(12) H(13) 119.3 no . . . C(13) C(12) H(13) 120.2 no . . . C(12) C(13) H(14) 120.1 no . . . C(14) C(13) H(14) 120.0 no . . . C(13) C(14) H(15) 120.3 no . . . C(15) C(14) H(15) 119.6 no . . . C(14) C(15) H(16) 120.1 no . . . C(16) C(15) H(16) 118.8 no . . . C(11) C(16) H(17) 119.6 no . . . C(15) C(16) H(17) 120.8 no . . . C(17) C(18) H(18) 119.0 no . . . C(19) C(18) H(18) 120.6 no . . . C(18) C(19) H(19) 119.7 no . . . C(20) C(19) H(19) 119.6 no . . . C(19) C(20) H(20) 120.5 no . . . C(21) C(20) H(20) 119.9 no . . . C(20) C(21) H(21) 119.4 no . . . C(22) C(21) H(21) 119.6 no . . . C(17) C(22) H(22) 119.6 no . . . C(21) C(22) H(22) 120.5 no . . . C(23) C(24) H(23) 119.2 no . . . C(25) C(24) H(23) 119.6 no . . . C(24) C(25) H(24) 120.0 no . . . C(26) C(25) H(24) 119.8 no . . . C(25) C(26) H(25) 120.1 no . . . C(27) C(26) H(25) 120.0 no . . . C(26) C(27) H(26) 119.8 no . . . C(28) C(27) H(26) 119.7 no . . . C(23) C(28) H(27) 119.7 no . . . C(27) C(28) H(27) 120.0 no . . . C(29) C(30) H(28) 119.3 no . . . C(31) C(30) H(28) 120.0 no . . . C(30) C(31) H(29) 120.0 no . . . C(32) C(31) H(29) 120.0 no . . . C(31) C(32) H(30) 120.0 no . . . C(33) C(32) H(30) 120.4 no . . . C(32) C(33) H(31) 119.7 no . . . C(34) C(33) H(31) 119.6 no . . . C(29) C(34) H(32) 119.3 no . . . C(33) C(34) H(32) 120.2 no . . . C(35) C(36) H(33) 119.5 no . . . C(37) C(36) H(33) 120.0 no . . . C(36) C(37) H(34) 120.4 no . . . C(38) C(37) H(34) 119.5 no . . . C(37) C(38) H(35) 119.8 no . . . C(39) C(38) H(35) 120.1 no . . . C(38) C(39) H(36) 119.5 no . . . C(40) C(39) H(36) 120.1 no . . . C(35) C(40) H(37) 119.6 no . . . C(39) C(40) H(37) 120.6 no . . . C(41) C(42) H(38) 119.1 no . . . C(43) C(42) H(38) 120.1 no . . . C(42) C(43) H(39) 119.9 no . . . C(44) C(43) H(39) 120.0 no . . . C(43) C(44) H(40) 119.7 no . . . C(45) C(44) H(40) 120.2 no . . . C(44) C(45) H(41) 119.9 no . . . C(46) C(45) H(41) 119.7 no . . . C(41) C(46) H(42) 119.0 no . . . C(45) C(46) H(42) 120.4 no . . . #===end #============================================================================== data___[Mo(P4)(mu3-S)2{Rh(CO)2}2]-1.3(CH2Cl2)_(4a) _database_code_depnum_ccdc_archive 'CCDC 719134' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C51.30 H44.60 Cl2.60 Mo O4 P4 Rh2 S2 ' _chemical_formula_moiety 'C50 H42 Mo O4 P4 Rh2 S2, 1.3(C H2 Cl2)' _chemical_formula_weight 1307.06 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 41.2344(14) _cell_length_b 11.9799(4) _cell_length_c 21.7291(9) _cell_angle_alpha 90.0000 _cell_angle_beta 96.1025(7) _cell_angle_gamma 90.0000 _cell_volume 10673.0(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 13829 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5220.80 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 0.834 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 41536 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12020 _reflns_number_gt 8735 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.1131 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12020 _refine_ls_number_parameters 638 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.6000\s(Fo^2^) + 0.1500]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.47 _refine_diff_density_min -0.66 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Rh(1) Rh 0.139950(10) -0.04562(3) -0.015410(10) 0.04544(8) Uani 1.00 1 d . . . Rh(2) Rh 0.111720(10) 0.17860(2) -0.042790(10) 0.04106(8) Uani 1.00 1 d . . . Mo(1) Mo 0.133620(10) 0.12653(2) 0.097240(10) 0.02466(6) Uani 1.00 1 d . . . Cl(1) Cl 0.0000 0.9113(17) 0.2500 0.402(8) Uiso 0.60 2 d SP . . Cl(2) Cl 0.0000 0.6970(19) 0.2500 0.443(10) Uiso 0.60 2 d SP . . Cl(3) Cl 0.0732(4) -0.5210(14) 0.3501(7) 0.390(7) Uiso 0.50 1 d P . . Cl(5) Cl 0.0145(3) -0.5292(11) 0.3270(6) 0.417(6) Uiso 0.65 1 d P . . Cl(6) Cl 0.0076(6) -0.501(2) 0.3918(12) 0.319(11) Uiso 0.25 1 d P . . Cl(7) Cl 0.0478(3) -0.5101(12) 0.4540(6) 0.395(6) Uiso 0.60 1 d P . . S(1) S 0.16335(2) 0.13024(9) 0.00443(4) 0.0415(2) Uani 1.00 1 d . . . S(2) S 0.09444(2) 0.03816(7) 0.02014(4) 0.0341(2) Uani 1.00 1 d . . . P(1) P 0.18932(2) 0.09062(7) 0.15000(4) 0.02793(19) Uani 1.00 1 d . . . P(2) P 0.12573(2) 0.01421(7) 0.18901(4) 0.0307(2) Uani 1.00 1 d . . . P(3) P 0.08466(2) 0.20147(7) 0.13697(4) 0.0305(2) Uani 1.00 1 d . . . P(4) P 0.14565(2) 0.32704(7) 0.11148(4) 0.02923(19) Uani 1.00 1 d . . . O(1) O 0.19812(13) -0.1302(5) -0.0715(3) 0.164(2) Uani 1.00 1 d . . . O(2) O 0.10490(13) -0.2647(3) -0.0308(2) 0.134(2) Uani 1.00 1 d . . . O(3) O 0.13884(13) 0.3392(4) -0.12894(18) 0.1226(18) Uani 1.00 1 d . . . O(4) O 0.04452(10) 0.2154(4) -0.1057(2) 0.1118(16) Uani 1.00 1 d . . . C(1) C 0.17661(15) -0.1000(5) -0.0481(2) 0.089(2) Uani 1.00 1 d . . . C(2) C 0.11810(14) -0.1821(4) -0.0255(2) 0.0770(17) Uani 1.00 1 d . . . C(3) C 0.12904(14) 0.2811(4) -0.0948(2) 0.0693(15) Uani 1.00 1 d . . . C(4) C 0.07004(13) 0.2016(4) -0.0809(2) 0.0665(14) Uani 1.00 1 d . . . C(5) C 0.22580(8) 0.1753(2) 0.14406(15) 0.0330(8) Uani 1.00 1 d . . . C(6) C 0.23811(9) 0.2446(3) 0.19234(16) 0.0415(9) Uani 1.00 1 d . . . C(7) C 0.26589(10) 0.3074(3) 0.18683(19) 0.0530(11) Uani 1.00 1 d . . . C(8) C 0.28181(10) 0.3019(3) 0.1345(2) 0.0556(12) Uani 1.00 1 d . . . C(9) C 0.27011(9) 0.2325(3) 0.08655(19) 0.0479(10) Uani 1.00 1 d . . . C(10) C 0.24212(9) 0.1689(2) 0.09149(16) 0.0397(9) Uani 1.00 1 d . . . C(11) C 0.20576(8) -0.0500(2) 0.13479(14) 0.0319(7) Uani 1.00 1 d . . . C(12) C 0.23856(8) -0.0746(3) 0.15046(16) 0.0395(9) Uani 1.00 1 d . . . C(13) C 0.25022(10) -0.1820(3) 0.14399(18) 0.0462(10) Uani 1.00 1 d . . . C(14) C 0.22938(11) -0.2661(3) 0.12152(19) 0.0513(11) Uani 1.00 1 d . . . C(15) C 0.19689(11) -0.2429(3) 0.10623(19) 0.0542(11) Uani 1.00 1 d . . . C(16) C 0.18520(9) -0.1360(3) 0.11292(17) 0.0418(9) Uani 1.00 1 d . . . C(17) C 0.18887(8) 0.0759(2) 0.23412(14) 0.0347(8) Uani 1.00 1 d . . . C(18) C 0.16291(8) -0.0109(3) 0.24356(16) 0.0401(9) Uani 1.00 1 d . . . C(19) C 0.10877(9) -0.1289(2) 0.18174(16) 0.0383(9) Uani 1.00 1 d . . . C(20) C 0.11785(12) -0.2132(4) 0.2237(2) 0.0710(14) Uani 1.00 1 d . . . C(21) C 0.10231(14) -0.3167(4) 0.2198(2) 0.0815(17) Uani 1.00 1 d . . . C(22) C 0.07830(14) -0.3363(3) 0.1732(2) 0.0733(16) Uani 1.00 1 d . . . C(23) C 0.06924(16) -0.2553(4) 0.1309(2) 0.0898(19) Uani 1.00 1 d . . . C(24) C 0.08459(12) -0.1513(3) 0.1355(2) 0.0635(13) Uani 1.00 1 d . . . C(25) C 0.09741(8) 0.0732(3) 0.24025(15) 0.0362(8) Uani 1.00 1 d . . . C(26) C 0.09403(10) 0.0361(3) 0.30030(17) 0.0504(11) Uani 1.00 1 d . . . C(27) C 0.07140(11) 0.0854(4) 0.33329(19) 0.0616(13) Uani 1.00 1 d . . . C(28) C 0.05105(12) 0.1678(4) 0.3079(2) 0.0664(14) Uani 1.00 1 d . . . C(29) C 0.05404(11) 0.2059(3) 0.24823(19) 0.0563(12) Uani 1.00 1 d . . . C(30) C 0.07754(9) 0.1578(3) 0.21476(16) 0.0384(9) Uani 1.00 1 d . . . C(31) C 0.04424(8) 0.1752(3) 0.09528(17) 0.0411(9) Uani 1.00 1 d . . . C(32) C 0.02620(10) 0.0821(3) 0.1083(2) 0.0591(13) Uani 1.00 1 d . . . C(33) C -0.00411(12) 0.0619(4) 0.0759(2) 0.0787(17) Uani 1.00 1 d . . . C(34) C -0.01657(12) 0.1346(6) 0.0302(2) 0.091(2) Uani 1.00 1 d . . . C(35) C 0.00119(13) 0.2249(6) 0.0167(2) 0.094(2) Uani 1.00 1 d . . . C(36) C 0.03146(10) 0.2443(4) 0.0488(2) 0.0659(14) Uani 1.00 1 d . . . C(37) C 0.08407(8) 0.3554(2) 0.14436(16) 0.0378(8) Uani 1.00 1 d . . . C(38) C 0.10647(8) 0.4041(2) 0.10036(16) 0.0373(8) Uani 1.00 1 d . . . C(39) C 0.16103(8) 0.3891(2) 0.18708(14) 0.0323(8) Uani 1.00 1 d . . . C(40) C 0.17744(10) 0.4900(3) 0.19262(18) 0.0450(10) Uani 1.00 1 d . . . C(41) C 0.18601(10) 0.5379(3) 0.2500(2) 0.0553(12) Uani 1.00 1 d . . . C(42) C 0.17776(10) 0.4860(3) 0.30263(18) 0.0543(12) Uani 1.00 1 d . . . C(43) C 0.16130(10) 0.3865(3) 0.29814(17) 0.0509(11) Uani 1.00 1 d . . . C(44) C 0.15297(9) 0.3376(3) 0.24040(15) 0.0390(9) Uani 1.00 1 d . . . C(45) C 0.16889(9) 0.4064(2) 0.05828(15) 0.0370(8) Uani 1.00 1 d . . . C(46) C 0.15352(11) 0.4711(3) 0.01043(17) 0.0550(12) Uani 1.00 1 d . . . C(47) C 0.17160(14) 0.5368(4) -0.02566(19) 0.0674(15) Uani 1.00 1 d . . . C(48) C 0.20446(13) 0.5406(3) -0.01638(19) 0.0574(13) Uani 1.00 1 d . . . C(49) C 0.22006(12) 0.4762(3) 0.0299(2) 0.0579(12) Uani 1.00 1 d . . . C(50) C 0.20265(10) 0.4108(3) 0.06697(18) 0.0477(10) Uani 1.00 1 d . . . C(51) C 0.0268(9) 0.808(2) 0.2373(18) 0.202(16) Uiso 0.30 1 d P . . C(52) C 0.0477(6) -0.529(3) 0.3836(18) 0.56(2) Uiso 1.00 1 d . . . H(1) H 0.2277 0.2496 0.2292 0.049 Uiso 1.00 1 c R . . H(2) H 0.2743 0.3558 0.2193 0.063 Uiso 1.00 1 c R . . H(3) H 0.3012 0.3437 0.1321 0.067 Uiso 1.00 1 c R . . H(4) H 0.2809 0.2293 0.0501 0.058 Uiso 1.00 1 c R . . H(5) H 0.2343 0.1201 0.0587 0.048 Uiso 1.00 1 c R . . H(6) H 0.2532 -0.0171 0.1654 0.047 Uiso 1.00 1 c R . . H(7) H 0.2727 -0.1982 0.1547 0.056 Uiso 1.00 1 c R . . H(8) H 0.2377 -0.3388 0.1152 0.062 Uiso 1.00 1 c R . . H(9) H 0.1824 -0.3020 0.0932 0.064 Uiso 1.00 1 c R . . H(10) H 0.1627 -0.1210 0.1021 0.050 Uiso 1.00 1 c R . . H(11) H 0.2096 0.0517 0.2527 0.041 Uiso 1.00 1 c R . . H(12) H 0.1835 0.1451 0.2519 0.042 Uiso 1.00 1 c R . . H(13) H 0.1571 -0.0057 0.2846 0.048 Uiso 1.00 1 c R . . H(14) H 0.1713 -0.0833 0.2369 0.048 Uiso 1.00 1 c R . . H(15) H 0.1354 -0.2015 0.2551 0.083 Uiso 1.00 1 c R . . H(16) H 0.1092 -0.3750 0.2478 0.097 Uiso 1.00 1 c R . . H(17) H 0.0663 -0.4041 0.1723 0.089 Uiso 1.00 1 c R . . H(18) H 0.0534 -0.2716 0.0970 0.105 Uiso 1.00 1 c R . . H(19) H 0.0785 -0.0967 0.1047 0.075 Uiso 1.00 1 c R . . H(20) H 0.1074 -0.0227 0.3178 0.061 Uiso 1.00 1 c R . . H(21) H 0.0694 0.0608 0.3743 0.076 Uiso 1.00 1 c R . . H(22) H 0.0348 0.1979 0.3310 0.082 Uiso 1.00 1 c R . . H(23) H 0.0406 0.2650 0.2310 0.069 Uiso 1.00 1 c R . . H(24) H 0.0347 0.0309 0.1393 0.072 Uiso 1.00 1 c R . . H(25) H -0.0157 -0.0027 0.0864 0.097 Uiso 1.00 1 c R . . H(26) H -0.0376 0.1194 0.0098 0.108 Uiso 1.00 1 c R . . H(27) H -0.0081 0.2701 -0.0164 0.110 Uiso 1.00 1 c R . . H(28) H 0.0428 0.3081 0.0364 0.077 Uiso 1.00 1 c R . . H(29) H 0.0625 0.3823 0.1339 0.045 Uiso 1.00 1 c R . . H(30) H 0.0914 0.3761 0.1857 0.045 Uiso 1.00 1 c R . . H(31) H 0.1102 0.4808 0.1095 0.044 Uiso 1.00 1 c R . . H(32) H 0.0970 0.3966 0.0588 0.044 Uiso 1.00 1 c R . . H(33) H 0.1825 0.5272 0.1562 0.054 Uiso 1.00 1 c R . . H(34) H 0.1975 0.6068 0.2529 0.065 Uiso 1.00 1 c R . . H(35) H 0.1838 0.5189 0.3420 0.064 Uiso 1.00 1 c R . . H(36) H 0.1556 0.3518 0.3348 0.061 Uiso 1.00 1 c R . . H(37) H 0.1417 0.2683 0.2376 0.047 Uiso 1.00 1 c R . . H(38) H 0.1304 0.4706 0.0028 0.066 Uiso 1.00 1 c R . . H(39) H 0.1605 0.5798 -0.0581 0.081 Uiso 1.00 1 c R . . H(40) H 0.2164 0.5849 -0.0424 0.071 Uiso 1.00 1 c R . . H(41) H 0.2432 0.4774 0.0366 0.072 Uiso 1.00 1 c R . . H(42) H 0.2140 0.3692 0.0998 0.059 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.04521(17) 0.04570(18) 0.04482(17) 0.00365(13) 0.00205(13) -0.01484(13) Rh(2) 0.05008(18) 0.04181(17) 0.03015(15) -0.00743(13) -0.00103(12) 0.00179(11) Mo(1) 0.02443(13) 0.02545(14) 0.02393(13) -0.00247(9) 0.00174(9) -0.00101(9) S(1) 0.0372(4) 0.0577(5) 0.0307(4) -0.0113(4) 0.0085(3) -0.0075(3) S(2) 0.0324(4) 0.0357(4) 0.0335(4) -0.0066(3) -0.0002(3) -0.0035(3) P(1) 0.0261(3) 0.0279(3) 0.0295(3) -0.0023(3) 0.0017(3) -0.0016(3) P(2) 0.0292(3) 0.0317(4) 0.0315(4) -0.0012(3) 0.0045(3) 0.0049(3) P(3) 0.0281(3) 0.0312(4) 0.0326(4) 0.0004(3) 0.0041(3) 0.0003(3) P(4) 0.0334(4) 0.0268(4) 0.0273(3) -0.0036(3) 0.0025(3) -0.0004(3) O(1) 0.102(3) 0.168(5) 0.236(6) 0.023(3) 0.086(4) -0.071(4) O(2) 0.130(4) 0.054(2) 0.213(5) -0.019(2) -0.007(3) -0.041(3) O(3) 0.169(4) 0.127(3) 0.071(2) -0.070(3) 0.010(2) 0.038(2) O(4) 0.078(2) 0.139(4) 0.108(3) 0.010(2) -0.036(2) 0.030(2) C(1) 0.083(3) 0.089(4) 0.100(4) 0.013(3) 0.027(3) -0.030(3) C(2) 0.075(3) 0.054(3) 0.099(3) 0.004(2) -0.001(2) -0.028(2) C(3) 0.093(3) 0.071(3) 0.043(2) -0.023(2) 0.002(2) 0.004(2) C(4) 0.071(3) 0.068(3) 0.056(2) -0.005(2) -0.015(2) 0.019(2) C(5) 0.0282(15) 0.0306(16) 0.0396(17) -0.0023(12) 0.0012(12) 0.0009(13) C(6) 0.0396(18) 0.0417(19) 0.0427(19) -0.0110(15) 0.0023(14) -0.0063(15) C(7) 0.046(2) 0.049(2) 0.063(2) -0.0153(17) -0.0042(18) -0.0115(18) C(8) 0.038(2) 0.053(2) 0.076(2) -0.0175(17) 0.0071(19) -0.004(2) C(9) 0.0411(19) 0.048(2) 0.057(2) -0.0091(16) 0.0172(16) 0.0034(17) C(10) 0.0436(19) 0.0354(18) 0.0408(18) -0.0073(14) 0.0080(14) -0.0050(14) C(11) 0.0312(15) 0.0318(16) 0.0329(15) 0.0003(12) 0.0045(12) 0.0002(12) C(12) 0.0347(17) 0.0353(18) 0.0480(19) 0.0009(14) 0.0026(14) -0.0021(15) C(13) 0.042(2) 0.042(2) 0.055(2) 0.0090(16) 0.0084(16) 0.0055(16) C(14) 0.063(2) 0.0299(18) 0.061(2) 0.0103(17) 0.0097(19) -0.0025(16) C(15) 0.064(2) 0.0306(19) 0.066(2) -0.0037(17) -0.002(2) -0.0070(17) C(16) 0.0399(18) 0.0360(18) 0.048(2) -0.0010(14) -0.0002(15) -0.0015(15) C(17) 0.0338(16) 0.0386(18) 0.0314(16) 0.0050(13) 0.0020(12) -0.0010(13) C(18) 0.0334(16) 0.048(2) 0.0392(18) 0.0027(15) 0.0034(13) 0.0131(15) C(19) 0.0418(18) 0.0308(17) 0.0432(18) -0.0013(14) 0.0087(15) 0.0049(14) C(20) 0.064(2) 0.051(2) 0.093(3) -0.012(2) -0.017(2) 0.028(2) C(21) 0.078(3) 0.044(2) 0.119(4) -0.010(2) -0.005(3) 0.035(2) C(22) 0.091(3) 0.034(2) 0.097(3) -0.018(2) 0.016(3) 0.001(2) C(23) 0.119(4) 0.066(3) 0.077(3) -0.050(3) -0.022(3) 0.008(2) C(24) 0.078(3) 0.050(2) 0.058(2) -0.021(2) -0.010(2) 0.014(2) C(25) 0.0345(16) 0.0418(19) 0.0333(16) -0.0018(14) 0.0082(13) 0.0023(14) C(26) 0.049(2) 0.065(2) 0.0387(19) 0.0084(19) 0.0110(16) 0.0142(17) C(27) 0.066(2) 0.082(3) 0.041(2) 0.008(2) 0.0245(19) 0.009(2) C(28) 0.073(3) 0.079(3) 0.053(2) 0.019(2) 0.034(2) 0.006(2) C(29) 0.061(2) 0.061(2) 0.051(2) 0.017(2) 0.0253(19) 0.0074(19) C(30) 0.0407(18) 0.0383(18) 0.0371(17) 0.0007(14) 0.0078(14) 0.0019(14) C(31) 0.0264(15) 0.048(2) 0.050(2) -0.0010(14) 0.0068(14) -0.0107(16) C(32) 0.044(2) 0.058(2) 0.078(3) -0.0100(19) 0.019(2) -0.013(2) C(33) 0.043(2) 0.084(3) 0.115(4) -0.028(2) 0.035(2) -0.047(3) C(34) 0.035(2) 0.140(6) 0.096(4) -0.010(3) -0.001(2) -0.053(4) C(35) 0.051(2) 0.132(5) 0.091(4) -0.004(3) -0.028(2) -0.008(3) C(36) 0.043(2) 0.082(3) 0.068(2) -0.003(2) -0.016(2) 0.005(2) C(37) 0.0325(16) 0.0372(18) 0.0438(18) 0.0039(14) 0.0046(14) -0.0008(14) C(38) 0.0404(18) 0.0290(16) 0.0411(18) 0.0015(13) -0.0011(14) 0.0036(13) C(39) 0.0323(15) 0.0314(16) 0.0336(16) 0.0019(12) 0.0049(12) -0.0064(12) C(40) 0.050(2) 0.0389(19) 0.047(2) -0.0033(16) 0.0070(16) -0.0090(16) C(41) 0.051(2) 0.048(2) 0.065(2) -0.0027(18) -0.0053(19) -0.0246(19) C(42) 0.050(2) 0.068(2) 0.043(2) 0.011(2) -0.0051(17) -0.0254(19) C(43) 0.053(2) 0.069(2) 0.0302(17) 0.009(2) 0.0039(15) -0.0072(17) C(44) 0.0393(18) 0.045(2) 0.0325(16) 0.0024(15) 0.0036(13) -0.0038(14) C(45) 0.0498(19) 0.0260(15) 0.0360(17) -0.0060(14) 0.0080(14) -0.0029(12) C(46) 0.063(2) 0.065(2) 0.0366(19) -0.008(2) 0.0036(17) 0.0120(18) C(47) 0.095(3) 0.068(3) 0.041(2) 0.001(2) 0.014(2) 0.022(2) C(48) 0.085(3) 0.045(2) 0.047(2) -0.011(2) 0.032(2) -0.0004(17) C(49) 0.065(2) 0.047(2) 0.068(2) -0.010(2) 0.037(2) -0.004(2) C(50) 0.053(2) 0.0374(19) 0.056(2) -0.0004(17) 0.0184(18) 0.0064(16) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Disordered CH2Cl2 molecules were modelled as following. Cl(1)-C(51)-Cl(2) 30% occ. Cl(1)-C(51*)-Cl(2) 30% occ. Cl(3)-C(52)-Cl(5) 15% occ. Cl(3)-C(52)-Cl(6) 25% occ. Cl(3)-C(52)-Cl(7) 10% occ. Cl(5)-C(52)-Cl(7) 50% occ. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.9626(4) yes . . Rh(1) S(1) 2.3382(10) yes . . Rh(1) S(2) 2.3311(9) yes . . Rh(1) C(1) 1.856(6) yes . . Rh(1) C(2) 1.869(5) yes . . Rh(2) S(1) 2.3359(8) yes . . Rh(2) S(2) 2.3271(9) yes . . Rh(2) C(3) 1.862(5) yes . . Rh(2) C(4) 1.847(5) yes . . Mo(1) S(1) 2.4693(9) yes . . Mo(1) S(2) 2.4417(8) yes . . Mo(1) P(1) 2.4929(8) yes . . Mo(1) P(2) 2.4558(9) yes . . Mo(1) P(3) 2.4490(9) yes . . Mo(1) P(4) 2.4656(8) yes . . Cl(1) C(51) 1.71(4) yes . . Cl(1) C(51) 1.71(4) yes . 2_555 Cl(2) C(51) 1.77(4) yes . . Cl(2) C(51) 1.77(4) yes . 2_555 Cl(3) C(52) 1.34(3) yes . . Cl(5) Cl(6) 1.50(3) yes . . Cl(5) C(52) 1.74(3) yes . . Cl(6) Cl(7) 2.03(2) yes . . Cl(6) C(52) 1.72(4) yes . . Cl(7) C(52) 1.55(4) yes . . P(1) C(5) 1.830(3) yes . . P(1) C(11) 1.858(3) yes . . P(1) C(17) 1.838(3) yes . . P(2) C(18) 1.860(3) yes . . P(2) C(19) 1.852(3) yes . . P(2) C(25) 1.838(3) yes . . P(3) C(30) 1.823(3) yes . . P(3) C(31) 1.838(3) yes . . P(3) C(37) 1.852(3) yes . . P(4) C(38) 1.854(3) yes . . P(4) C(39) 1.852(3) yes . . P(4) C(45) 1.842(3) yes . . O(1) C(1) 1.128(8) yes . . O(2) C(2) 1.129(7) yes . . O(3) C(3) 1.123(6) yes . . O(4) C(4) 1.142(6) yes . . C(5) C(6) 1.391(4) yes . . C(5) C(10) 1.388(5) yes . . C(6) C(7) 1.386(5) yes . . C(7) C(8) 1.373(6) yes . . C(8) C(9) 1.380(5) yes . . C(9) C(10) 1.397(5) yes . . C(11) C(12) 1.391(4) yes . . C(11) C(16) 1.386(4) yes . . C(12) C(13) 1.386(5) yes . . C(13) C(14) 1.379(5) yes . . C(14) C(15) 1.374(6) yes . . C(15) C(16) 1.382(5) yes . . C(17) C(18) 1.522(4) yes . . C(19) C(20) 1.384(5) yes . . C(19) C(24) 1.365(5) yes . . C(20) C(21) 1.395(6) yes . . C(21) C(22) 1.360(7) yes . . C(22) C(23) 1.361(7) yes . . C(23) C(24) 1.397(7) yes . . C(25) C(26) 1.399(5) yes . . C(25) C(30) 1.382(4) yes . . C(26) C(27) 1.369(6) yes . . C(27) C(28) 1.373(6) yes . . C(28) C(29) 1.392(6) yes . . C(29) C(30) 1.396(5) yes . . C(31) C(32) 1.386(5) yes . . C(31) C(36) 1.367(5) yes . . C(32) C(33) 1.389(6) yes . . C(33) C(34) 1.378(8) yes . . C(34) C(35) 1.355(9) yes . . C(35) C(36) 1.383(6) yes . . C(37) C(38) 1.515(5) yes . . C(39) C(40) 1.385(5) yes . . C(39) C(44) 1.384(4) yes . . C(40) C(41) 1.385(5) yes . . C(41) C(42) 1.375(6) yes . . C(42) C(43) 1.370(6) yes . . C(43) C(44) 1.394(5) yes . . C(45) C(46) 1.394(5) yes . . C(45) C(50) 1.386(5) yes . . C(46) C(47) 1.383(6) yes . . C(47) C(48) 1.349(7) yes . . C(48) C(49) 1.372(6) yes . . C(49) C(50) 1.379(6) yes . . C(6) H(1) 0.950 no . . C(7) H(2) 0.950 no . . C(8) H(3) 0.950 no . . C(9) H(4) 0.950 no . . C(10) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(15) H(9) 0.950 no . . C(16) H(10) 0.950 no . . C(17) H(11) 0.950 no . . C(17) H(12) 0.950 no . . C(18) H(13) 0.950 no . . C(18) H(14) 0.950 no . . C(20) H(15) 0.950 no . . C(21) H(16) 0.950 no . . C(22) H(17) 0.950 no . . C(23) H(18) 0.950 no . . C(24) H(19) 0.950 no . . C(26) H(20) 0.950 no . . C(27) H(21) 0.950 no . . C(28) H(22) 0.950 no . . C(29) H(23) 0.950 no . . C(32) H(24) 0.950 no . . C(33) H(25) 0.950 no . . C(34) H(26) 0.950 no . . C(35) H(27) 0.950 no . . C(36) H(28) 0.950 no . . C(37) H(29) 0.950 no . . C(37) H(30) 0.950 no . . C(38) H(31) 0.950 no . . C(38) H(32) 0.950 no . . C(40) H(33) 0.950 no . . C(41) H(34) 0.950 no . . C(42) H(35) 0.950 no . . C(43) H(36) 0.950 no . . C(44) H(37) 0.950 no . . C(46) H(38) 0.950 no . . C(47) H(39) 0.950 no . . C(48) H(40) 0.950 no . . C(49) H(41) 0.950 no . . C(50) H(42) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 50.63(2) yes . . . Rh(2) Rh(1) S(2) 50.45(2) yes . . . Rh(2) Rh(1) C(1) 124.1(2) yes . . . Rh(2) Rh(1) C(2) 126.56(17) yes . . . S(1) Rh(1) S(2) 83.22(3) yes . . . S(1) Rh(1) C(1) 92.86(19) yes . . . S(1) Rh(1) C(2) 174.01(18) yes . . . S(2) Rh(1) C(1) 174.5(2) yes . . . S(2) Rh(1) C(2) 91.19(18) yes . . . C(1) Rh(1) C(2) 92.9(2) yes . . . Rh(1) Rh(2) S(1) 50.70(2) yes . . . Rh(1) Rh(2) S(2) 50.56(2) yes . . . Rh(1) Rh(2) C(3) 123.50(17) yes . . . Rh(1) Rh(2) C(4) 123.51(16) yes . . . S(1) Rh(2) S(2) 83.35(3) yes . . . S(1) Rh(2) C(3) 92.28(16) yes . . . S(1) Rh(2) C(4) 174.21(16) yes . . . S(2) Rh(2) C(3) 174.07(17) yes . . . S(2) Rh(2) C(4) 92.45(16) yes . . . C(3) Rh(2) C(4) 91.6(2) yes . . . S(1) Mo(1) S(2) 78.30(2) yes . . . S(1) Mo(1) P(1) 82.27(3) yes . . . S(1) Mo(1) P(2) 142.48(3) yes . . . S(1) Mo(1) P(3) 141.33(3) yes . . . S(1) Mo(1) P(4) 88.52(3) yes . . . S(2) Mo(1) P(1) 138.65(3) yes . . . S(2) Mo(1) P(2) 100.63(3) yes . . . S(2) Mo(1) P(3) 83.73(3) yes . . . S(2) Mo(1) P(4) 128.18(2) yes . . . P(1) Mo(1) P(2) 74.17(2) yes . . . P(1) Mo(1) P(3) 130.91(2) yes . . . P(1) Mo(1) P(4) 86.97(2) yes . . . P(2) Mo(1) P(3) 74.29(2) yes . . . P(2) Mo(1) P(4) 118.31(2) yes . . . P(3) Mo(1) P(4) 76.17(2) yes . . . Rh(1) S(1) Rh(2) 78.67(2) yes . . . Rh(1) S(1) Mo(1) 84.46(3) yes . . . Rh(2) S(1) Mo(1) 81.65(2) yes . . . Rh(1) S(2) Rh(2) 78.99(3) yes . . . Rh(1) S(2) Mo(1) 85.23(2) yes . . . Rh(2) S(2) Mo(1) 82.42(2) yes . . . Mo(1) P(1) C(5) 126.57(10) yes . . . Mo(1) P(1) C(11) 114.23(10) yes . . . Mo(1) P(1) C(17) 111.57(10) yes . . . C(5) P(1) C(11) 99.89(15) yes . . . C(5) P(1) C(17) 102.62(14) yes . . . C(11) P(1) C(17) 97.62(14) yes . . . Mo(1) P(2) C(18) 115.76(11) yes . . . Mo(1) P(2) C(19) 121.29(11) yes . . . Mo(1) P(2) C(25) 115.39(11) yes . . . C(18) P(2) C(19) 100.55(16) yes . . . C(18) P(2) C(25) 102.11(15) yes . . . C(19) P(2) C(25) 98.57(16) yes . . . Mo(1) P(3) C(30) 116.22(12) yes . . . Mo(1) P(3) C(31) 120.12(12) yes . . . Mo(1) P(3) C(37) 114.50(11) yes . . . C(30) P(3) C(31) 100.42(16) yes . . . C(30) P(3) C(37) 101.57(16) yes . . . C(31) P(3) C(37) 101.19(15) yes . . . Mo(1) P(4) C(38) 107.92(10) yes . . . Mo(1) P(4) C(39) 123.19(10) yes . . . Mo(1) P(4) C(45) 122.34(11) yes . . . C(38) P(4) C(39) 97.32(15) yes . . . C(38) P(4) C(45) 99.54(15) yes . . . C(39) P(4) C(45) 101.40(14) yes . . . Rh(1) C(1) O(1) 175.6(5) yes . . . Rh(1) C(2) O(2) 179.0(5) yes . . . Rh(2) C(3) O(3) 176.1(4) yes . . . Rh(2) C(4) O(4) 178.5(4) yes . . . P(1) C(5) C(6) 121.0(2) yes . . . P(1) C(5) C(10) 120.1(2) yes . . . C(6) C(5) C(10) 118.9(3) yes . . . C(5) C(6) C(7) 119.8(3) yes . . . C(6) C(7) C(8) 121.2(3) yes . . . C(7) C(8) C(9) 119.6(3) yes . . . C(8) C(9) C(10) 119.8(3) yes . . . C(5) C(10) C(9) 120.6(3) yes . . . P(1) C(11) C(12) 120.8(2) yes . . . P(1) C(11) C(16) 120.9(2) yes . . . C(12) C(11) C(16) 118.0(3) yes . . . C(11) C(12) C(13) 120.7(3) yes . . . C(12) C(13) C(14) 120.3(3) yes . . . C(13) C(14) C(15) 119.5(3) yes . . . C(14) C(15) C(16) 120.3(3) yes . . . C(11) C(16) C(15) 121.2(3) yes . . . P(1) C(17) C(18) 106.3(2) yes . . . P(2) C(18) C(17) 110.4(2) yes . . . P(2) C(19) C(20) 123.1(2) yes . . . P(2) C(19) C(24) 119.0(2) yes . . . C(20) C(19) C(24) 117.8(3) yes . . . C(19) C(20) C(21) 121.2(4) yes . . . C(20) C(21) C(22) 119.5(4) yes . . . C(21) C(22) C(23) 120.4(4) yes . . . C(22) C(23) C(24) 119.9(4) yes . . . C(19) C(24) C(23) 121.2(4) yes . . . P(2) C(25) C(26) 125.1(2) yes . . . P(2) C(25) C(30) 115.3(2) yes . . . C(26) C(25) C(30) 119.5(3) yes . . . C(25) C(26) C(27) 119.5(3) yes . . . C(26) C(27) C(28) 121.3(4) yes . . . C(27) C(28) C(29) 120.0(4) yes . . . C(28) C(29) C(30) 119.0(4) yes . . . P(3) C(30) C(25) 115.8(2) yes . . . P(3) C(30) C(29) 123.6(2) yes . . . C(25) C(30) C(29) 120.6(3) yes . . . P(3) C(31) C(32) 121.1(2) yes . . . P(3) C(31) C(36) 121.2(3) yes . . . C(32) C(31) C(36) 117.7(3) yes . . . C(31) C(32) C(33) 120.7(4) yes . . . C(32) C(33) C(34) 120.1(5) yes . . . C(33) C(34) C(35) 119.4(4) yes . . . C(34) C(35) C(36) 120.3(5) yes . . . C(31) C(36) C(35) 121.8(4) yes . . . P(3) C(37) C(38) 108.3(2) yes . . . P(4) C(38) C(37) 107.9(2) yes . . . P(4) C(39) C(40) 123.1(2) yes . . . P(4) C(39) C(44) 118.3(2) yes . . . C(40) C(39) C(44) 118.4(3) yes . . . C(39) C(40) C(41) 121.0(3) yes . . . C(40) C(41) C(42) 120.0(3) yes . . . C(41) C(42) C(43) 119.9(3) yes . . . C(42) C(43) C(44) 120.2(3) yes . . . C(39) C(44) C(43) 120.5(3) yes . . . P(4) C(45) C(46) 122.0(3) yes . . . P(4) C(45) C(50) 121.1(2) yes . . . C(46) C(45) C(50) 116.8(3) yes . . . C(45) C(46) C(47) 120.6(4) yes . . . C(46) C(47) C(48) 121.9(4) yes . . . C(47) C(48) C(49) 118.4(4) yes . . . C(48) C(49) C(50) 121.0(4) yes . . . C(45) C(50) C(49) 121.3(3) yes . . . Cl(1) C(51) Cl(2) 95(2) yes . . . Cl(3) C(52) Cl(5) 103(2) yes . . . Cl(3) C(52) Cl(6) 149(3) yes . . . Cl(3) C(52) Cl(7) 127(2) yes . . . Cl(5) C(52) Cl(7) 128(2) yes . . . C(5) C(6) H(1) 120.9 no . . . C(7) C(6) H(1) 119.3 no . . . C(6) C(7) H(2) 120.4 no . . . C(8) C(7) H(2) 118.4 no . . . C(7) C(8) H(3) 120.0 no . . . C(9) C(8) H(3) 120.3 no . . . C(8) C(9) H(4) 119.9 no . . . C(10) C(9) H(4) 120.4 no . . . C(5) C(10) H(5) 119.7 no . . . C(9) C(10) H(5) 119.6 no . . . C(11) C(12) H(6) 119.7 no . . . C(13) C(12) H(6) 119.5 no . . . C(12) C(13) H(7) 120.2 no . . . C(14) C(13) H(7) 119.5 no . . . C(13) C(14) H(8) 120.0 no . . . C(15) C(14) H(8) 120.4 no . . . C(14) C(15) H(9) 119.2 no . . . C(16) C(15) H(9) 120.4 no . . . C(11) C(16) H(10) 119.3 no . . . C(15) C(16) H(10) 119.5 no . . . P(1) C(17) H(11) 110.4 no . . . P(1) C(17) H(12) 110.3 no . . . C(18) C(17) H(11) 110.3 no . . . C(18) C(17) H(12) 110.0 no . . . H(11) C(17) H(12) 109.5 no . . . P(2) C(18) H(13) 108.4 no . . . P(2) C(18) H(14) 109.8 no . . . C(17) C(18) H(13) 109.4 no . . . C(17) C(18) H(14) 109.4 no . . . H(13) C(18) H(14) 109.5 no . . . C(19) C(20) H(15) 119.8 no . . . C(21) C(20) H(15) 118.9 no . . . C(20) C(21) H(16) 120.8 no . . . C(22) C(21) H(16) 119.6 no . . . C(21) C(22) H(17) 120.0 no . . . C(23) C(22) H(17) 119.4 no . . . C(22) C(23) H(18) 119.6 no . . . C(24) C(23) H(18) 120.4 no . . . C(19) C(24) H(19) 120.1 no . . . C(23) C(24) H(19) 118.7 no . . . C(25) C(26) H(20) 119.9 no . . . C(27) C(26) H(20) 120.6 no . . . C(26) C(27) H(21) 119.3 no . . . C(28) C(27) H(21) 119.3 no . . . C(27) C(28) H(22) 119.7 no . . . C(29) C(28) H(22) 120.3 no . . . C(28) C(29) H(23) 120.4 no . . . C(30) C(29) H(23) 120.6 no . . . C(31) C(32) H(24) 119.9 no . . . C(33) C(32) H(24) 119.5 no . . . C(32) C(33) H(25) 117.9 no . . . C(34) C(33) H(25) 122.0 no . . . C(33) C(34) H(26) 117.8 no . . . C(35) C(34) H(26) 122.7 no . . . C(34) C(35) H(27) 115.8 no . . . C(36) C(35) H(27) 123.9 no . . . C(31) C(36) H(28) 122.3 no . . . C(35) C(36) H(28) 115.9 no . . . P(3) C(37) H(29) 109.8 no . . . P(3) C(37) H(30) 109.7 no . . . C(38) C(37) H(29) 109.6 no . . . C(38) C(37) H(30) 110.1 no . . . H(29) C(37) H(30) 109.5 no . . . P(4) C(38) H(31) 109.5 no . . . P(4) C(38) H(32) 110.0 no . . . C(37) C(38) H(31) 109.7 no . . . C(37) C(38) H(32) 110.2 no . . . H(31) C(38) H(32) 109.5 no . . . C(39) C(40) H(33) 119.0 no . . . C(41) C(40) H(33) 120.0 no . . . C(40) C(41) H(34) 119.7 no . . . C(42) C(41) H(34) 120.3 no . . . C(41) C(42) H(35) 119.8 no . . . C(43) C(42) H(35) 120.3 no . . . C(42) C(43) H(36) 119.0 no . . . C(44) C(43) H(36) 120.8 no . . . C(39) C(44) H(37) 119.7 no . . . C(43) C(44) H(37) 119.8 no . . . C(45) C(46) H(38) 119.6 no . . . C(47) C(46) H(38) 119.8 no . . . C(46) C(47) H(39) 118.9 no . . . C(48) C(47) H(39) 119.2 no . . . C(47) C(48) H(40) 120.4 no . . . C(49) C(48) H(40) 121.2 no . . . C(48) C(49) H(41) 119.2 no . . . C(50) C(49) H(41) 119.8 no . . . C(45) C(50) H(42) 119.2 no . . . C(49) C(50) H(42) 119.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Rh(1) Mo(1) 3.2325(3) ? . . Rh(2) Mo(1) 3.1430(3) ? . . #===end #============================================================================== data___[Mo(P4)(mu3-S)2{Rh(CO)2}2]-0.5(CH2Cl2)_(4b) _database_code_depnum_ccdc_archive 'CCDC 719135' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C50.50 H43 Cl Mo O4 P4 Rh2 S2 ' _chemical_formula_moiety 'C50 H42 Mo O4 P4 Rh2 S2, 0.5(C H2 Cl2)' _chemical_formula_weight 1239.11 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.709(4) _cell_length_b 17.143(4) _cell_length_c 20.980(5) _cell_angle_alpha 90.0000 _cell_angle_beta 101.0700(13) _cell_angle_gamma 90.0000 _cell_volume 4839(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7120 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour black _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2476.00 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.661 _exptl_absorpt_correction_T_max 0.883 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 36280 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11062 _reflns_number_gt 5033 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.2010 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 11062 _refine_ls_number_parameters 624 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 1.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.14 _refine_diff_density_min -1.90 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Rh Rh -1.118 0.919 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Rh(1) Rh 0.11757(8) 0.25452(6) 0.28609(5) 0.0358(2) Uani 1.00 1 d . . . Rh(2) Rh 0.32730(9) 0.21315(7) 0.28408(5) 0.0427(3) Uani 1.00 1 d . . . Mo(1) Mo 0.16985(8) 0.22565(6) 0.14532(5) 0.0286(2) Uani 1.00 1 d . . . Cl(1) Cl 0.492(2) -0.0530(15) -0.0099(15) 0.239(13) Uiso 0.50 1 d P . . Cl(2) Cl 0.536(2) 0.1056(14) 0.0218(14) 0.242(12) Uiso 0.50 1 d P . . S(1) S 0.2328(2) 0.31860(19) 0.23481(16) 0.0402(9) Uani 1.00 1 d . . . S(2) S 0.1816(2) 0.14462(18) 0.24429(15) 0.0363(8) Uani 1.00 1 d . . . P(1) P 0.1113(2) 0.35360(19) 0.09564(16) 0.0324(8) Uani 1.00 1 d . . . P(2) P 0.2501(2) 0.24363(19) 0.05348(16) 0.0311(8) Uani 1.00 1 d . . . P(3) P 0.2095(2) 0.09263(19) 0.11561(16) 0.0351(9) Uani 1.00 1 d . . . P(4) P 0.0078(2) 0.17020(19) 0.10047(16) 0.0345(9) Uani 1.00 1 d . . . O(1) O 0.0414(10) 0.4020(6) 0.3360(6) 0.082(4) Uani 1.00 1 d . . . O(2) O -0.0042(8) 0.1486(6) 0.3547(5) 0.057(3) Uani 1.00 1 d . . . O(3) O 0.5156(13) 0.2939(11) 0.3403(11) 0.183(9) Uani 1.00 1 d . . . O(4) O 0.4117(10) 0.0731(8) 0.3598(7) 0.094(5) Uani 1.00 1 d . . . C(1) C 0.0715(11) 0.3457(8) 0.3173(7) 0.048(4) Uani 1.00 1 d . . . C(2) C 0.0391(10) 0.1889(8) 0.3280(6) 0.041(3) Uani 1.00 1 d . . . C(3) C 0.4424(15) 0.2686(13) 0.3159(10) 0.095(7) Uani 1.00 1 d . . . C(4) C 0.3831(13) 0.1250(10) 0.3294(8) 0.061(5) Uani 1.00 1 d . . . C(5) C -0.0038(9) 0.3973(7) 0.1084(6) 0.034(3) Uani 1.00 1 d . . . C(6) C -0.0065(12) 0.4312(7) 0.1687(6) 0.048(4) Uani 1.00 1 d . . . C(7) C -0.0949(12) 0.4651(8) 0.1812(8) 0.055(5) Uani 1.00 1 d . . . C(8) C -0.1786(14) 0.4642(10) 0.1334(9) 0.071(6) Uani 1.00 1 d . . . C(9) C -0.1747(11) 0.4312(10) 0.0740(8) 0.062(5) Uani 1.00 1 d . . . C(10) C -0.0897(10) 0.3971(8) 0.0621(7) 0.045(4) Uani 1.00 1 d . . . C(11) C 0.1936(10) 0.4409(7) 0.1105(5) 0.034(3) Uani 1.00 1 d . . . C(12) C 0.2948(11) 0.4339(8) 0.1238(7) 0.048(4) Uani 1.00 1 d . . . C(13) C 0.3581(11) 0.4973(8) 0.1249(7) 0.053(4) Uani 1.00 1 d . . . C(14) C 0.3179(13) 0.5715(8) 0.1131(7) 0.057(5) Uani 1.00 1 d . . . C(15) C 0.2149(12) 0.5799(7) 0.1011(6) 0.048(4) Uani 1.00 1 d . . . C(16) C 0.1547(11) 0.5154(7) 0.0986(6) 0.046(4) Uani 1.00 1 d . . . C(17) C 0.0997(10) 0.3498(7) 0.0072(6) 0.043(3) Uani 1.00 1 d . . . C(18) C 0.1974(10) 0.3201(7) -0.0068(6) 0.040(3) Uani 1.00 1 d . . . C(19) C 0.3861(10) 0.2680(7) 0.0670(6) 0.041(3) Uani 1.00 1 d . . . C(20) C 0.4311(14) 0.3003(10) 0.0195(8) 0.066(5) Uani 1.00 1 d . . . C(21) C 0.5304(15) 0.3178(11) 0.0314(10) 0.080(7) Uani 1.00 1 d . . . C(22) C 0.5871(14) 0.3006(10) 0.0916(10) 0.072(6) Uani 1.00 1 d . . . C(23) C 0.5436(12) 0.2701(10) 0.1391(9) 0.066(5) Uani 1.00 1 d . . . C(24) C 0.4432(10) 0.2538(9) 0.1267(7) 0.048(4) Uani 1.00 1 d . . . C(25) C 0.2532(10) 0.1548(7) 0.0040(6) 0.040(3) Uani 1.00 1 d . . . C(26) C 0.2752(12) 0.1534(9) -0.0589(6) 0.053(4) Uani 1.00 1 d . . . C(27) C 0.2756(13) 0.0829(9) -0.0897(7) 0.062(5) Uani 1.00 1 d . . . C(28) C 0.2604(12) 0.0141(9) -0.0605(7) 0.058(5) Uani 1.00 1 d . . . C(29) C 0.2404(11) 0.0147(8) 0.0019(6) 0.048(4) Uani 1.00 1 d . . . C(30) C 0.2358(9) 0.0857(7) 0.0337(6) 0.037(3) Uani 1.00 1 d . . . C(31) C 0.3163(12) 0.0384(8) 0.1613(7) 0.049(4) Uani 1.00 1 d . . . C(32) C 0.4115(13) 0.0557(10) 0.1518(8) 0.065(5) Uani 1.00 1 d . . . C(33) C 0.4918(17) 0.0173(13) 0.1852(12) 0.099(8) Uani 1.00 1 d . . . C(34) C 0.4864(19) -0.0377(16) 0.2271(11) 0.104(9) Uani 1.00 1 d . . . C(35) C 0.395(2) -0.0590(12) 0.2388(10) 0.103(8) Uani 1.00 1 d . . . C(36) C 0.3044(14) -0.0201(9) 0.2047(7) 0.067(5) Uani 1.00 1 d . . . C(37) C 0.1069(10) 0.0266(7) 0.1144(6) 0.042(3) Uani 1.00 1 d . . . C(38) C 0.0153(10) 0.0660(7) 0.0757(6) 0.041(3) Uani 1.00 1 d . . . C(39) C -0.0863(9) 0.1943(7) 0.0250(6) 0.033(3) Uani 1.00 1 d . . . C(40) C -0.0582(11) 0.1924(7) -0.0352(6) 0.044(4) Uani 1.00 1 d . . . C(41) C -0.1263(11) 0.1962(8) -0.0921(6) 0.046(4) Uani 1.00 1 d . . . C(42) C -0.2266(11) 0.2049(8) -0.0918(7) 0.048(4) Uani 1.00 1 d . . . C(43) C -0.2562(11) 0.2101(8) -0.0325(7) 0.050(4) Uani 1.00 1 d . . . C(44) C -0.1869(10) 0.2057(8) 0.0260(7) 0.045(4) Uani 1.00 1 d . . . C(45) C -0.0759(10) 0.1678(7) 0.1593(6) 0.038(3) Uani 1.00 1 d . . . C(46) C -0.1047(11) 0.0969(8) 0.1838(6) 0.048(4) Uani 1.00 1 d . . . C(47) C -0.1730(12) 0.0994(10) 0.2254(7) 0.058(5) Uani 1.00 1 d . . . C(48) C -0.2097(12) 0.1687(11) 0.2435(7) 0.061(5) Uani 1.00 1 d . . . C(49) C -0.1818(12) 0.2378(10) 0.2198(7) 0.056(5) Uani 1.00 1 d . . . C(50) C -0.1122(10) 0.2372(8) 0.1792(6) 0.041(3) Uani 1.00 1 d . . . C(51) C 0.515(4) 0.039(2) -0.0410(13) 0.14(2) Uiso 0.50 1 d P . . H(1) H 0.0517 0.4315 0.2016 0.059 Uiso 1.00 1 c R . . H(2) H -0.0962 0.4882 0.2222 0.068 Uiso 1.00 1 c R . . H(3) H -0.2389 0.4860 0.1413 0.088 Uiso 1.00 1 c R . . H(4) H -0.2321 0.4324 0.0405 0.073 Uiso 1.00 1 c R . . H(5) H -0.0900 0.3727 0.0213 0.054 Uiso 1.00 1 c R . . H(6) H 0.3231 0.3835 0.1324 0.057 Uiso 1.00 1 c R . . H(7) H 0.4281 0.4901 0.1338 0.062 Uiso 1.00 1 c R . . H(8) H 0.3598 0.6156 0.1132 0.069 Uiso 1.00 1 c R . . H(9) H 0.1861 0.6304 0.0946 0.057 Uiso 1.00 1 c R . . H(10) H 0.0847 0.5220 0.0885 0.055 Uiso 1.00 1 c R . . H(11) H 0.0472 0.3156 -0.0110 0.050 Uiso 1.00 1 c R . . H(12) H 0.0864 0.4005 -0.0107 0.050 Uiso 1.00 1 c R . . H(13) H 0.2430 0.3622 -0.0043 0.049 Uiso 1.00 1 c R . . H(14) H 0.1865 0.2983 -0.0492 0.049 Uiso 1.00 1 c R . . H(15) H 0.3923 0.3106 -0.0222 0.081 Uiso 1.00 1 c R . . H(16) H 0.5600 0.3412 -0.0013 0.101 Uiso 1.00 1 c R . . H(17) H 0.6566 0.3103 0.0999 0.087 Uiso 1.00 1 c R . . H(18) H 0.5824 0.2599 0.1809 0.078 Uiso 1.00 1 c R . . H(19) H 0.4134 0.2324 0.1601 0.059 Uiso 1.00 1 c R . . H(20) H 0.2897 0.2002 -0.0794 0.065 Uiso 1.00 1 c R . . H(21) H 0.2866 0.0819 -0.1331 0.076 Uiso 1.00 1 c R . . H(22) H 0.2637 -0.0338 -0.0827 0.070 Uiso 1.00 1 c R . . H(23) H 0.2299 -0.0329 0.0228 0.056 Uiso 1.00 1 c R . . H(24) H 0.4206 0.0948 0.1215 0.075 Uiso 1.00 1 c R . . H(25) H 0.5557 0.0315 0.1778 0.114 Uiso 1.00 1 c R . . H(26) H 0.5448 -0.0630 0.2493 0.116 Uiso 1.00 1 c R . . H(27) H 0.3895 -0.0993 0.2691 0.119 Uiso 1.00 1 c R . . H(28) H 0.2405 -0.0343 0.2120 0.079 Uiso 1.00 1 c R . . H(29) H 0.1191 -0.0211 0.0943 0.051 Uiso 1.00 1 c R . . H(30) H 0.0978 0.0166 0.1575 0.051 Uiso 1.00 1 c R . . H(31) H -0.0423 0.0392 0.0829 0.050 Uiso 1.00 1 c R . . H(32) H 0.0181 0.0639 0.0308 0.050 Uiso 1.00 1 c R . . H(33) H 0.0104 0.1882 -0.0369 0.052 Uiso 1.00 1 c R . . H(34) H -0.1045 0.1928 -0.1323 0.055 Uiso 1.00 1 c R . . H(35) H -0.2739 0.2074 -0.1313 0.056 Uiso 1.00 1 c R . . H(36) H -0.3246 0.2167 -0.0314 0.060 Uiso 1.00 1 c R . . H(37) H -0.2084 0.2105 0.0662 0.054 Uiso 1.00 1 c R . . H(38) H -0.0785 0.0487 0.1724 0.058 Uiso 1.00 1 c R . . H(39) H -0.1946 0.0520 0.2416 0.070 Uiso 1.00 1 c R . . H(40) H -0.2548 0.1688 0.2727 0.076 Uiso 1.00 1 c R . . H(41) H -0.2095 0.2856 0.2308 0.068 Uiso 1.00 1 c R . . H(42) H -0.0893 0.2853 0.1650 0.049 Uiso 1.00 1 c R . . H(43) H 0.5754 0.0333 -0.0563 0.171 Uiso 0.50 1 c R . . H(44) H 0.4634 0.0538 -0.0760 0.171 Uiso 0.50 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Rh(1) 0.0474(6) 0.0298(5) 0.0301(5) 0.0024(4) 0.0074(4) -0.0020(19) Rh(2) 0.0436(6) 0.0435(6) 0.0388(6) 0.0008(5) 0.0023(5) 0.002(2) Mo(1) 0.0371(6) 0.0223(5) 0.0257(5) -0.0004(4) 0.0040(4) -0.0007(7) S(1) 0.061(2) 0.0261(16) 0.0325(17) -0.0043(15) 0.0053(15) -0.002(2) S(2) 0.053(2) 0.0257(15) 0.0298(16) 0.0011(14) 0.0068(14) 0.0005(5) P(1) 0.0401(19) 0.0239(15) 0.0314(17) -0.0003(14) 0.0026(14) -0.0003(2) P(2) 0.0377(18) 0.0275(16) 0.0280(16) 0.0018(14) 0.0063(13) 0.0011(11) P(3) 0.049(2) 0.0248(16) 0.0316(17) 0.0036(15) 0.0068(15) -0.0016(15) P(4) 0.043(2) 0.0271(16) 0.0332(17) -0.0031(14) 0.0055(15) -0.003(2) O(1) 0.105(10) 0.040(6) 0.113(10) 0.017(6) 0.053(8) -0.011(10) O(2) 0.062(7) 0.055(6) 0.054(6) -0.010(5) 0.014(5) 0.004(4) O(3) 0.102(14) 0.149(17) 0.25(2) -0.060(12) -0.083(15) 0.10(9) O(4) 0.102(11) 0.072(9) 0.101(11) 0.043(8) -0.001(8) 0.03(2) C(1) 0.060(10) 0.040(8) 0.042(8) -0.002(7) 0.007(7) 0.002(2) C(2) 0.045(8) 0.046(8) 0.031(7) -0.003(6) 0.000(6) -0.010(9) C(3) 0.062(13) 0.114(18) 0.091(15) -0.021(12) -0.037(11) 0.05(4) C(4) 0.063(11) 0.061(11) 0.057(10) 0.013(9) 0.007(8) -0.013(12) C(5) 0.036(7) 0.027(6) 0.037(6) 0.008(5) 0.004(5) 0.010(9) C(6) 0.073(11) 0.036(7) 0.039(7) 0.015(7) 0.015(7) -0.0014(14) C(7) 0.062(10) 0.044(8) 0.062(10) 0.009(8) 0.023(8) -0.008(7) C(8) 0.067(12) 0.066(11) 0.086(14) 0.016(9) 0.034(10) 0.0012(12) C(9) 0.045(9) 0.074(12) 0.063(11) 0.016(8) -0.004(8) 0.009(8) C(10) 0.046(8) 0.038(7) 0.052(8) 0.003(6) 0.011(6) -0.005(4) C(11) 0.042(7) 0.033(6) 0.024(6) 0.000(5) -0.000(5) -0.004(4) C(12) 0.055(9) 0.028(7) 0.059(9) -0.012(6) 0.010(7) -0.010(9) C(13) 0.039(8) 0.042(8) 0.074(11) -0.009(6) -0.002(7) 0.008(7) C(14) 0.073(12) 0.037(8) 0.063(10) -0.025(8) 0.016(8) 0.003(2) C(15) 0.069(10) 0.025(6) 0.047(8) -0.002(6) 0.007(7) -0.004(3) C(16) 0.060(10) 0.027(7) 0.050(8) 0.008(6) 0.008(7) 0.007(7) C(17) 0.058(9) 0.029(6) 0.038(7) -0.005(6) 0.001(6) -0.0004(4) C(18) 0.048(8) 0.031(7) 0.044(7) 0.001(6) 0.013(6) -0.002(2) C(19) 0.042(8) 0.035(7) 0.044(7) 0.001(6) 0.008(6) -0.005(5) C(20) 0.081(13) 0.075(12) 0.046(9) 0.003(10) 0.023(9) 0.007(6) C(21) 0.069(13) 0.079(13) 0.105(16) -0.011(10) 0.048(12) 0.03(2) C(22) 0.054(11) 0.066(12) 0.099(15) -0.009(9) 0.022(10) -0.009(8) C(23) 0.043(9) 0.082(13) 0.069(11) -0.011(9) 0.005(8) -0.015(15) C(24) 0.031(7) 0.071(10) 0.046(8) -0.007(7) 0.015(6) -0.0010(10) C(25) 0.048(8) 0.035(7) 0.038(7) 0.006(6) 0.008(6) 0.0004(4) C(26) 0.088(12) 0.049(9) 0.026(6) 0.006(8) 0.020(7) -0.004(4) C(27) 0.098(13) 0.055(10) 0.038(8) 0.021(9) 0.020(8) -0.013(12) C(28) 0.079(12) 0.041(8) 0.055(9) 0.009(8) 0.013(8) -0.017(16) C(29) 0.065(10) 0.035(7) 0.040(7) -0.003(7) 0.005(7) -0.010(9) C(30) 0.036(7) 0.031(7) 0.044(7) -0.004(5) 0.008(5) -0.007(6) C(31) 0.064(10) 0.035(7) 0.044(8) 0.018(7) 0.004(7) -0.009(9) C(32) 0.061(11) 0.064(11) 0.062(11) 0.012(9) -0.009(8) 0.003(2) C(33) 0.075(15) 0.086(16) 0.12(2) 0.013(12) -0.017(13) 0.006(6) C(34) 0.100(18) 0.12(2) 0.071(15) 0.051(17) -0.040(14) -0.015(14) C(35) 0.17(2) 0.061(13) 0.068(13) 0.059(15) -0.005(15) 0.020(19) C(36) 0.088(14) 0.052(10) 0.057(10) 0.026(9) 0.005(9) 0.014(13) C(37) 0.060(9) 0.022(6) 0.044(8) -0.006(6) 0.009(6) 0.0005(4) C(38) 0.047(8) 0.031(7) 0.048(8) -0.005(6) 0.018(6) -0.006(6) C(39) 0.037(7) 0.026(6) 0.035(6) 0.003(5) 0.006(5) -0.0013(12) C(40) 0.049(8) 0.033(7) 0.049(8) -0.006(6) 0.008(6) -0.0004(4) C(41) 0.064(10) 0.045(8) 0.028(7) 0.002(7) 0.006(6) -0.004(4) C(42) 0.052(9) 0.048(8) 0.041(8) 0.002(7) 0.002(6) 0.0003(3) C(43) 0.048(9) 0.048(8) 0.053(9) 0.012(7) 0.012(7) 0.009(8) C(44) 0.047(8) 0.047(8) 0.043(8) 0.004(6) 0.011(6) -0.004(3) C(45) 0.047(8) 0.036(7) 0.032(6) 0.007(6) 0.011(5) 0.003(3) C(46) 0.054(9) 0.043(8) 0.048(8) 0.005(7) 0.015(7) 0.004(4) C(47) 0.060(10) 0.060(10) 0.056(10) -0.015(8) 0.014(8) 0.009(9) C(48) 0.062(11) 0.084(13) 0.043(8) -0.006(9) 0.023(7) 0.004(4) C(49) 0.071(11) 0.062(10) 0.037(8) -0.002(8) 0.020(7) 0.003(2) C(50) 0.038(7) 0.041(7) 0.044(7) -0.001(6) 0.010(6) 0.0017(16) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Rh(1) Rh(2) 2.9695(16) yes . . Rh(1) S(1) 2.347(4) yes . . Rh(1) S(2) 2.320(3) yes . . Rh(1) C(1) 1.852(15) yes . . Rh(1) C(2) 1.886(15) yes . . Rh(2) S(1) 2.346(3) yes . . Rh(2) S(2) 2.330(3) yes . . Rh(2) C(3) 1.85(2) yes . . Rh(2) C(4) 1.868(17) yes . . Mo(1) S(1) 2.487(3) yes . . Mo(1) S(2) 2.478(3) yes . . Mo(1) P(1) 2.494(3) yes . . Mo(1) P(2) 2.415(3) yes . . Mo(1) P(3) 2.452(3) yes . . Mo(1) P(4) 2.433(3) yes . . Cl(1) C(51) 1.76(4) yes . . Cl(2) C(51) 1.72(4) yes . . P(1) C(5) 1.813(13) yes . . P(1) C(11) 1.864(13) yes . . P(1) C(17) 1.832(13) yes . . P(2) C(18) 1.868(13) yes . . P(2) C(19) 1.878(14) yes . . P(2) C(25) 1.848(14) yes . . P(3) C(30) 1.827(14) yes . . P(3) C(31) 1.840(15) yes . . P(3) C(37) 1.803(14) yes . . P(4) C(38) 1.869(13) yes . . P(4) C(39) 1.887(12) yes . . P(4) C(45) 1.841(15) yes . . O(1) C(1) 1.148(19) yes . . O(2) C(2) 1.128(19) yes . . O(3) C(3) 1.12(2) yes . . O(4) C(4) 1.12(2) yes . . C(5) C(6) 1.399(19) yes . . C(5) C(10) 1.376(17) yes . . C(6) C(7) 1.41(2) yes . . C(7) C(8) 1.37(2) yes . . C(8) C(9) 1.38(2) yes . . C(9) C(10) 1.37(2) yes . . C(11) C(12) 1.37(2) yes . . C(11) C(16) 1.388(18) yes . . C(12) C(13) 1.39(2) yes . . C(13) C(14) 1.39(2) yes . . C(14) C(15) 1.39(2) yes . . C(15) C(16) 1.37(2) yes . . C(17) C(18) 1.51(2) yes . . C(19) C(20) 1.38(2) yes . . C(19) C(24) 1.365(19) yes . . C(20) C(21) 1.37(2) yes . . C(21) C(22) 1.38(2) yes . . C(22) C(23) 1.36(2) yes . . C(23) C(24) 1.38(2) yes . . C(25) C(26) 1.41(2) yes . . C(25) C(30) 1.381(19) yes . . C(26) C(27) 1.37(2) yes . . C(27) C(28) 1.36(2) yes . . C(28) C(29) 1.39(2) yes . . C(29) C(30) 1.394(19) yes . . C(31) C(32) 1.39(2) yes . . C(31) C(36) 1.39(2) yes . . C(32) C(33) 1.36(2) yes . . C(33) C(34) 1.30(3) yes . . C(34) C(35) 1.38(4) yes . . C(35) C(36) 1.46(3) yes . . C(37) C(38) 1.517(18) yes . . C(39) C(40) 1.39(2) yes . . C(39) C(44) 1.40(2) yes . . C(40) C(41) 1.369(18) yes . . C(41) C(42) 1.38(2) yes . . C(42) C(43) 1.38(2) yes . . C(43) C(44) 1.401(19) yes . . C(45) C(46) 1.40(2) yes . . C(45) C(50) 1.386(19) yes . . C(46) C(47) 1.40(2) yes . . C(47) C(48) 1.37(2) yes . . C(48) C(49) 1.37(2) yes . . C(49) C(50) 1.40(2) yes . . C(6) H(1) 0.950 no . . C(7) H(2) 0.950 no . . C(8) H(3) 0.950 no . . C(9) H(4) 0.950 no . . C(10) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(15) H(9) 0.950 no . . C(16) H(10) 0.950 no . . C(17) H(11) 0.950 no . . C(17) H(12) 0.950 no . . C(18) H(13) 0.950 no . . C(18) H(14) 0.950 no . . C(20) H(15) 0.950 no . . C(21) H(16) 0.950 no . . C(22) H(17) 0.950 no . . C(23) H(18) 0.950 no . . C(24) H(19) 0.950 no . . C(26) H(20) 0.950 no . . C(27) H(21) 0.950 no . . C(28) H(22) 0.950 no . . C(29) H(23) 0.950 no . . C(32) H(24) 0.950 no . . C(33) H(25) 0.950 no . . C(34) H(26) 0.950 no . . C(35) H(27) 0.950 no . . C(36) H(28) 0.950 no . . C(37) H(29) 0.950 no . . C(37) H(30) 0.950 no . . C(38) H(31) 0.950 no . . C(38) H(32) 0.950 no . . C(40) H(33) 0.950 no . . C(41) H(34) 0.950 no . . C(42) H(35) 0.950 no . . C(43) H(36) 0.950 no . . C(44) H(37) 0.950 no . . C(46) H(38) 0.950 no . . C(47) H(39) 0.950 no . . C(48) H(40) 0.950 no . . C(49) H(41) 0.950 no . . C(50) H(42) 0.950 no . . C(51) H(43) 0.950 no . . C(51) H(44) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Rh(2) Rh(1) S(1) 50.72(8) yes . . . Rh(2) Rh(1) S(2) 50.45(9) yes . . . Rh(2) Rh(1) C(1) 127.1(4) yes . . . Rh(2) Rh(1) C(2) 120.3(4) yes . . . S(1) Rh(1) S(2) 82.55(12) yes . . . S(1) Rh(1) C(1) 94.1(5) yes . . . S(1) Rh(1) C(2) 170.6(4) yes . . . S(2) Rh(1) C(1) 176.7(5) yes . . . S(2) Rh(1) C(2) 89.0(4) yes . . . C(1) Rh(1) C(2) 94.3(6) yes . . . Rh(1) Rh(2) S(1) 50.77(10) yes . . . Rh(1) Rh(2) S(2) 50.17(9) yes . . . Rh(1) Rh(2) C(3) 129.2(7) yes . . . Rh(1) Rh(2) C(4) 119.2(5) yes . . . S(1) Rh(2) S(2) 82.39(12) yes . . . S(1) Rh(2) C(3) 97.1(6) yes . . . S(1) Rh(2) C(4) 170.0(5) yes . . . S(2) Rh(2) C(3) 179.4(7) yes . . . S(2) Rh(2) C(4) 90.8(5) yes . . . C(3) Rh(2) C(4) 89.7(8) yes . . . S(1) Mo(1) S(2) 76.66(10) yes . . . S(1) Mo(1) P(1) 77.83(10) yes . . . S(1) Mo(1) P(2) 112.05(12) yes . . . S(1) Mo(1) P(3) 136.54(11) yes . . . S(1) Mo(1) P(4) 134.49(13) yes . . . S(2) Mo(1) P(1) 143.82(12) yes . . . S(2) Mo(1) P(2) 140.71(12) yes . . . S(2) Mo(1) P(3) 73.13(11) yes . . . S(2) Mo(1) P(4) 90.72(11) yes . . . P(1) Mo(1) P(2) 73.37(11) yes . . . P(1) Mo(1) P(3) 141.33(11) yes . . . P(1) Mo(1) P(4) 89.16(11) yes . . . P(2) Mo(1) P(3) 76.03(12) yes . . . P(2) Mo(1) P(4) 105.27(11) yes . . . P(3) Mo(1) P(4) 76.64(12) yes . . . Rh(1) S(1) Rh(2) 78.51(11) yes . . . Rh(1) S(1) Mo(1) 83.10(11) yes . . . Rh(2) S(1) Mo(1) 85.47(11) yes . . . Rh(1) S(2) Rh(2) 79.37(10) yes . . . Rh(1) S(2) Mo(1) 83.86(10) yes . . . Rh(2) S(2) Mo(1) 86.03(11) yes . . . Mo(1) P(1) C(5) 121.4(4) yes . . . Mo(1) P(1) C(11) 120.0(4) yes . . . Mo(1) P(1) C(17) 110.5(4) yes . . . C(5) P(1) C(11) 99.2(5) yes . . . C(5) P(1) C(17) 104.8(6) yes . . . C(11) P(1) C(17) 97.5(5) yes . . . Mo(1) P(2) C(18) 116.9(4) yes . . . Mo(1) P(2) C(19) 119.9(4) yes . . . Mo(1) P(2) C(25) 114.0(4) yes . . . C(18) P(2) C(19) 101.0(6) yes . . . C(18) P(2) C(25) 104.2(5) yes . . . C(19) P(2) C(25) 98.0(6) yes . . . Mo(1) P(3) C(30) 113.2(4) yes . . . Mo(1) P(3) C(31) 122.0(4) yes . . . Mo(1) P(3) C(37) 112.1(4) yes . . . C(30) P(3) C(31) 100.1(6) yes . . . C(30) P(3) C(37) 103.9(6) yes . . . C(31) P(3) C(37) 103.4(6) yes . . . Mo(1) P(4) C(38) 112.7(4) yes . . . Mo(1) P(4) C(39) 131.7(4) yes . . . Mo(1) P(4) C(45) 113.0(4) yes . . . C(38) P(4) C(39) 92.3(5) yes . . . C(38) P(4) C(45) 103.9(6) yes . . . C(39) P(4) C(45) 98.9(5) yes . . . Rh(1) C(1) O(1) 178.8(14) yes . . . Rh(1) C(2) O(2) 177.0(11) yes . . . Rh(2) C(3) O(3) 171(2) yes . . . Rh(2) C(4) O(4) 174.7(17) yes . . . P(1) C(5) C(6) 118.7(9) yes . . . P(1) C(5) C(10) 123.0(10) yes . . . C(6) C(5) C(10) 118.2(13) yes . . . C(5) C(6) C(7) 120.7(13) yes . . . C(6) C(7) C(8) 119.2(16) yes . . . C(7) C(8) C(9) 119.5(17) yes . . . C(8) C(9) C(10) 121.5(14) yes . . . C(5) C(10) C(9) 120.8(14) yes . . . P(1) C(11) C(12) 121.5(10) yes . . . P(1) C(11) C(16) 120.6(10) yes . . . C(12) C(11) C(16) 117.2(12) yes . . . C(11) C(12) C(13) 122.8(12) yes . . . C(12) C(13) C(14) 119.3(14) yes . . . C(13) C(14) C(15) 118.7(14) yes . . . C(14) C(15) C(16) 120.2(13) yes . . . C(11) C(16) C(15) 121.8(14) yes . . . P(1) C(17) C(18) 107.5(8) yes . . . P(2) C(18) C(17) 110.3(9) yes . . . P(2) C(19) C(20) 123.2(10) yes . . . P(2) C(19) C(24) 118.5(11) yes . . . C(20) C(19) C(24) 118.3(13) yes . . . C(19) C(20) C(21) 121.5(16) yes . . . C(20) C(21) C(22) 119(2) yes . . . C(21) C(22) C(23) 120.3(17) yes . . . C(22) C(23) C(24) 120.0(15) yes . . . C(19) C(24) C(23) 120.9(15) yes . . . P(2) C(25) C(26) 125.0(10) yes . . . P(2) C(25) C(30) 115.4(10) yes . . . C(26) C(25) C(30) 119.6(12) yes . . . C(25) C(26) C(27) 118.7(14) yes . . . C(26) C(27) C(28) 122.3(15) yes . . . C(27) C(28) C(29) 119.5(14) yes . . . C(28) C(29) C(30) 119.5(13) yes . . . P(3) C(30) C(25) 116.8(10) yes . . . P(3) C(30) C(29) 122.8(10) yes . . . C(25) C(30) C(29) 120.4(13) yes . . . P(3) C(31) C(32) 119.6(11) yes . . . P(3) C(31) C(36) 121.7(13) yes . . . C(32) C(31) C(36) 118.7(15) yes . . . C(31) C(32) C(33) 121.0(18) yes . . . C(32) C(33) C(34) 124(2) yes . . . C(33) C(34) C(35) 119(2) yes . . . C(34) C(35) C(36) 120.5(19) yes . . . C(31) C(36) C(35) 117.1(18) yes . . . P(3) C(37) C(38) 106.9(8) yes . . . P(4) C(38) C(37) 111.1(8) yes . . . P(4) C(39) C(40) 119.5(10) yes . . . P(4) C(39) C(44) 122.4(10) yes . . . C(40) C(39) C(44) 117.6(11) yes . . . C(39) C(40) C(41) 122.0(14) yes . . . C(40) C(41) C(42) 120.8(14) yes . . . C(41) C(42) C(43) 118.3(12) yes . . . C(42) C(43) C(44) 121.1(14) yes . . . C(39) C(44) C(43) 120.0(14) yes . . . P(4) C(45) C(46) 121.3(10) yes . . . P(4) C(45) C(50) 119.2(10) yes . . . C(46) C(45) C(50) 119.4(13) yes . . . C(45) C(46) C(47) 118.1(14) yes . . . C(46) C(47) C(48) 121.6(16) yes . . . C(47) C(48) C(49) 120.5(16) yes . . . C(48) C(49) C(50) 119.2(15) yes . . . C(45) C(50) C(49) 121.1(13) yes . . . Cl(1) C(51) Cl(2) 109(2) yes . . . C(5) C(6) H(1) 119.6 no . . . C(7) C(6) H(1) 119.6 no . . . C(6) C(7) H(2) 120.3 no . . . C(8) C(7) H(2) 120.5 no . . . C(7) C(8) H(3) 120.2 no . . . C(9) C(8) H(3) 120.3 no . . . C(8) C(9) H(4) 119.3 no . . . C(10) C(9) H(4) 119.2 no . . . C(5) C(10) H(5) 119.5 no . . . C(9) C(10) H(5) 119.6 no . . . C(11) C(12) H(6) 118.6 no . . . C(13) C(12) H(6) 118.6 no . . . C(12) C(13) H(7) 120.4 no . . . C(14) C(13) H(7) 120.3 no . . . C(13) C(14) H(8) 120.7 no . . . C(15) C(14) H(8) 120.6 no . . . C(14) C(15) H(9) 119.9 no . . . C(16) C(15) H(9) 119.9 no . . . C(11) C(16) H(10) 119.1 no . . . C(15) C(16) H(10) 119.1 no . . . P(1) C(17) H(11) 110.0 no . . . P(1) C(17) H(12) 110.0 no . . . C(18) C(17) H(11) 110.0 no . . . C(18) C(17) H(12) 109.9 no . . . H(11) C(17) H(12) 109.5 no . . . P(2) C(18) H(13) 109.3 no . . . P(2) C(18) H(14) 109.2 no . . . C(17) C(18) H(13) 109.3 no . . . C(17) C(18) H(14) 109.2 no . . . H(13) C(18) H(14) 109.5 no . . . C(19) C(20) H(15) 119.3 no . . . C(21) C(20) H(15) 119.3 no . . . C(20) C(21) H(16) 120.5 no . . . C(22) C(21) H(16) 120.5 no . . . C(21) C(22) H(17) 119.9 no . . . C(23) C(22) H(17) 119.9 no . . . C(22) C(23) H(18) 120.1 no . . . C(24) C(23) H(18) 119.9 no . . . C(19) C(24) H(19) 119.5 no . . . C(23) C(24) H(19) 119.6 no . . . C(25) C(26) H(20) 120.7 no . . . C(27) C(26) H(20) 120.6 no . . . C(26) C(27) H(21) 118.9 no . . . C(28) C(27) H(21) 118.8 no . . . C(27) C(28) H(22) 120.2 no . . . C(29) C(28) H(22) 120.2 no . . . C(28) C(29) H(23) 120.2 no . . . C(30) C(29) H(23) 120.3 no . . . C(31) C(32) H(24) 119.6 no . . . C(33) C(32) H(24) 119.4 no . . . C(32) C(33) H(25) 118.4 no . . . C(34) C(33) H(25) 118.0 no . . . C(33) C(34) H(26) 120.6 no . . . C(35) C(34) H(26) 120.4 no . . . C(34) C(35) H(27) 119.8 no . . . C(36) C(35) H(27) 119.7 no . . . C(31) C(36) H(28) 121.4 no . . . C(35) C(36) H(28) 121.5 no . . . P(3) C(37) H(29) 110.1 no . . . P(3) C(37) H(30) 110.1 no . . . C(38) C(37) H(29) 110.1 no . . . C(38) C(37) H(30) 110.1 no . . . H(29) C(37) H(30) 109.5 no . . . P(4) C(38) H(31) 109.1 no . . . P(4) C(38) H(32) 109.0 no . . . C(37) C(38) H(31) 109.1 no . . . C(37) C(38) H(32) 109.1 no . . . H(31) C(38) H(32) 109.5 no . . . C(39) C(40) H(33) 119.0 no . . . C(41) C(40) H(33) 119.0 no . . . C(40) C(41) H(34) 119.6 no . . . C(42) C(41) H(34) 119.5 no . . . C(41) C(42) H(35) 120.8 no . . . C(43) C(42) H(35) 120.9 no . . . C(42) C(43) H(36) 119.4 no . . . C(44) C(43) H(36) 119.4 no . . . C(39) C(44) H(37) 120.0 no . . . C(43) C(44) H(37) 120.0 no . . . C(45) C(46) H(38) 121.0 no . . . C(47) C(46) H(38) 121.0 no . . . C(46) C(47) H(39) 119.2 no . . . C(48) C(47) H(39) 119.2 no . . . C(47) C(48) H(40) 119.8 no . . . C(49) C(48) H(40) 119.7 no . . . C(48) C(49) H(41) 120.4 no . . . C(50) C(49) H(41) 120.4 no . . . C(45) C(50) H(42) 119.5 no . . . C(49) C(50) H(42) 119.4 no . . . Cl(1) C(51) H(43) 105.2 no . . . Cl(1) C(51) H(44) 111.3 no . . . Cl(2) C(51) H(43) 107.6 no . . . Cl(2) C(51) H(44) 113.9 no . . . H(43) C(51) H(44) 109.5 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Mo(1) Rh(1) 3.2084(15) ? . . Mo(1) Rh(2) 3.2813(13) ? . . #===end #============================================================================== data___[Mo(P4)(mu3-S)2{Ir(CO)2}2]-1.375(CH2Cl2)_(6) _database_code_depnum_ccdc_archive 'CCDC 719136' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C51.38 H44.75 Cl2.75 Ir2 Mo O4 P4 S2 ' _chemical_formula_moiety 'C50 H42 Ir2 Mo O4 P4 S2, 1.375 (C H2 Cl2)' _chemical_formula_weight 1492.12 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 41.213(9) _cell_length_b 12.066(2) _cell_length_c 21.619(4) _cell_angle_alpha 90.0000 _cell_angle_beta 95.8523(10) _cell_angle_gamma 90.0000 _cell_volume 10695(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9441 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 293.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5758.24 _exptl_absorpt_coefficient_mu 5.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.293 _exptl_absorpt_correction_T_max 0.572 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 41685 _diffrn_reflns_av_R_equivalents 0.080 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12245 _reflns_number_gt 5474 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1770 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 12245 _refine_ls_number_parameters 673 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 0.3500\s(Fo^2^) + 0.0400]/(4Fo^2^)' _refine_ls_shift/su_max 0.0010 _refine_diff_density_max 2.70 _refine_diff_density_min -2.01 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ir Ir -1.444 7.990 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Ir(1) Ir 0.141110(10) 0.45583(4) -0.01657(2) 0.04896(13) Uani 1.00 1 d . . . Ir(2) Ir 0.111790(10) 0.67939(4) -0.04254(2) 0.04363(12) Uani 1.00 1 d . . . Mo(1) Mo 0.13401(2) 0.62432(6) 0.09751(3) 0.02798(19) Uani 1.00 1 d . . . Cl(1) Cl 0.0000 0.419(2) 0.2500 0.314(14) Uani 0.75 2 d SP . . Cl(2) Cl 0.0000 0.199(2) 0.2500 0.319(15) Uani 0.75 2 d SP . . Cl(3) Cl 0.0502(6) 0.9897(14) 0.4585(11) 0.291(11) Uani 0.60 1 d P . . Cl(4) Cl 0.0082(5) 0.956(2) 0.3439(17) 0.334(15) Uani 0.55 1 d P . . Cl(5) Cl 0.0740(8) 0.979(2) 0.353(2) 0.295(18) Uani 0.40 1 d P . . Cl(6) Cl 0.0387(13) 0.999(3) 0.3210(19) 0.26(2) Uani 0.25 1 d P . . Cl(7) Cl 0.0147(12) 1.019(4) 0.412(4) 0.33(4) Uani 0.20 1 d P . . S(1) S 0.16405(7) 0.6320(2) 0.00454(11) 0.0453(7) Uani 1.00 1 d . . . S(2) S 0.09476(6) 0.5365(2) 0.01974(11) 0.0375(6) Uani 1.00 1 d . . . P(1) P 0.18964(6) 0.5868(2) 0.15109(11) 0.0319(6) Uani 1.00 1 d . . . P(2) P 0.12562(7) 0.5121(2) 0.19012(12) 0.0346(6) Uani 1.00 1 d . . . P(3) P 0.08484(7) 0.6990(2) 0.13709(12) 0.0341(6) Uani 1.00 1 d . . . P(4) P 0.14630(6) 0.82426(19) 0.11243(11) 0.0319(6) Uani 1.00 1 d . . . O(1) O 0.1998(3) 0.3717(13) -0.0699(8) 0.171(7) Uani 1.00 1 d . . . O(2) O 0.1081(3) 0.2354(8) -0.0345(6) 0.122(5) Uani 1.00 1 d . . . O(3) O 0.0439(2) 0.7166(10) -0.1032(5) 0.110(4) Uani 1.00 1 d . . . O(4) O 0.1379(3) 0.8477(10) -0.1264(5) 0.125(5) Uani 1.00 1 d . . . C(1) C 0.1771(4) 0.3996(14) -0.0473(8) 0.103(6) Uani 1.00 1 d . . . C(2) C 0.1205(4) 0.3202(11) -0.0282(7) 0.082(5) Uani 1.00 1 d . . . C(3) C 0.0698(3) 0.7030(11) -0.0784(5) 0.065(4) Uani 1.00 1 d . . . C(4) C 0.1288(3) 0.7852(13) -0.0926(6) 0.077(4) Uani 1.00 1 d . . . C(5) C 0.2266(2) 0.6736(7) 0.1452(4) 0.035(2) Uani 1.00 1 d . . . C(6) C 0.2425(2) 0.6674(8) 0.0921(5) 0.043(2) Uani 1.00 1 d . . . C(7) C 0.2710(2) 0.7274(9) 0.0870(5) 0.051(3) Uani 1.00 1 d . . . C(8) C 0.2821(3) 0.7938(10) 0.1352(6) 0.059(3) Uani 1.00 1 d . . . C(9) C 0.2663(2) 0.8034(9) 0.1890(5) 0.055(3) Uani 1.00 1 d . . . C(10) C 0.2383(2) 0.7393(8) 0.1933(4) 0.044(2) Uani 1.00 1 d . . . C(11) C 0.2063(2) 0.4479(7) 0.1355(4) 0.036(2) Uani 1.00 1 d . . . C(12) C 0.1861(2) 0.3613(8) 0.1156(5) 0.047(3) Uani 1.00 1 d . . . C(13) C 0.1972(3) 0.2535(9) 0.1099(5) 0.057(3) Uani 1.00 1 d . . . C(14) C 0.2298(3) 0.2335(9) 0.1233(5) 0.057(3) Uani 1.00 1 d . . . C(15) C 0.2502(2) 0.3183(9) 0.1433(5) 0.050(3) Uani 1.00 1 d . . . C(16) C 0.2383(2) 0.4228(8) 0.1504(4) 0.041(2) Uani 1.00 1 d . . . C(17) C 0.1888(2) 0.5737(8) 0.2362(4) 0.042(2) Uani 1.00 1 d . . . C(18) C 0.1630(2) 0.4882(8) 0.2451(4) 0.041(2) Uani 1.00 1 d . . . C(19) C 0.1088(2) 0.3691(8) 0.1825(5) 0.047(3) Uani 1.00 1 d . . . C(20) C 0.0865(3) 0.3449(11) 0.1345(6) 0.079(4) Uani 1.00 1 d . . . C(21) C 0.0708(4) 0.2426(12) 0.1289(7) 0.091(5) Uani 1.00 1 d . . . C(22) C 0.0794(4) 0.1629(9) 0.1742(6) 0.072(4) Uani 1.00 1 d . . . C(23) C 0.1030(4) 0.1837(11) 0.2207(8) 0.083(5) Uani 1.00 1 d . . . C(24) C 0.1179(3) 0.2888(11) 0.2259(7) 0.074(4) Uani 1.00 1 d . . . C(25) C 0.0973(2) 0.5730(8) 0.2413(4) 0.036(2) Uani 1.00 1 d . . . C(26) C 0.0941(2) 0.5357(9) 0.3009(5) 0.051(3) Uani 1.00 1 d . . . C(27) C 0.0708(3) 0.5859(11) 0.3336(5) 0.061(3) Uani 1.00 1 d . . . C(28) C 0.0508(3) 0.6653(11) 0.3090(5) 0.067(4) Uani 1.00 1 d . . . C(29) C 0.0534(3) 0.7050(9) 0.2472(5) 0.054(3) Uani 1.00 1 d . . . C(30) C 0.0775(2) 0.6554(8) 0.2156(4) 0.040(2) Uani 1.00 1 d . . . C(31) C 0.0444(2) 0.6718(8) 0.0946(5) 0.042(2) Uani 1.00 1 d . . . C(32) C 0.0270(3) 0.5807(10) 0.1079(6) 0.061(3) Uani 1.00 1 d . . . C(33) C -0.0038(3) 0.5604(11) 0.0765(7) 0.074(4) Uani 1.00 1 d . . . C(34) C -0.0165(3) 0.6325(16) 0.0305(7) 0.085(5) Uani 1.00 1 d . . . C(35) C 0.0012(3) 0.7226(16) 0.0181(7) 0.096(6) Uani 1.00 1 d . . . C(36) C 0.0308(3) 0.7436(11) 0.0497(5) 0.059(3) Uani 1.00 1 d . . . C(37) C 0.0844(2) 0.8521(7) 0.1448(4) 0.038(2) Uani 1.00 1 d . . . C(38) C 0.1072(2) 0.9014(7) 0.1008(4) 0.038(2) Uani 1.00 1 d . . . C(39) C 0.1698(2) 0.9042(8) 0.0604(4) 0.043(2) Uani 1.00 1 d . . . C(40) C 0.1539(2) 0.9691(10) 0.0126(4) 0.051(3) Uani 1.00 1 d . . . C(41) C 0.1737(4) 1.0373(10) -0.0231(5) 0.066(4) Uani 1.00 1 d . . . C(42) C 0.2064(3) 1.0416(9) -0.0126(5) 0.060(4) Uani 1.00 1 d . . . C(43) C 0.2214(3) 0.9726(9) 0.0325(5) 0.054(3) Uani 1.00 1 d . . . C(44) C 0.2036(2) 0.9073(8) 0.0693(5) 0.046(3) Uani 1.00 1 d . . . C(45) C 0.1609(2) 0.8858(7) 0.1886(4) 0.034(2) Uani 1.00 1 d . . . C(46) C 0.1775(3) 0.9871(9) 0.1946(5) 0.052(3) Uani 1.00 1 d . . . C(47) C 0.1850(2) 1.0319(9) 0.2524(5) 0.054(3) Uani 1.00 1 d . . . C(48) C 0.1771(3) 0.9824(10) 0.3042(5) 0.058(3) Uani 1.00 1 d . . . C(49) C 0.1609(3) 0.8818(10) 0.3004(5) 0.059(3) Uani 1.00 1 d . . . C(50) C 0.1527(2) 0.8333(8) 0.2425(4) 0.035(2) Uani 1.00 1 d . . . C(51) C 0.0272(16) 0.324(5) 0.234(2) 0.13(2) Uiso 0.38 1 d P . . C(52) C 0.0430(7) 0.928(3) 0.3893(12) 0.34(2) Uiso 1.00 1 d . . . H(1) H 0.2338 0.6211 0.0589 0.052 Uiso 1.00 1 c R . . H(2) H 0.2822 0.7221 0.0508 0.062 Uiso 1.00 1 c R . . H(3) H 0.3014 0.8354 0.1324 0.072 Uiso 1.00 1 c R . . H(4) H 0.2742 0.8525 0.2215 0.065 Uiso 1.00 1 c R . . H(5) H 0.2275 0.7418 0.2301 0.052 Uiso 1.00 1 c R . . H(6) H 0.1636 0.3768 0.1054 0.056 Uiso 1.00 1 c R . . H(7) H 0.1826 0.1951 0.0967 0.067 Uiso 1.00 1 c R . . H(8) H 0.2381 0.1608 0.1191 0.068 Uiso 1.00 1 c R . . H(9) H 0.2729 0.3044 0.1522 0.060 Uiso 1.00 1 c R . . H(10) H 0.2526 0.4803 0.1659 0.050 Uiso 1.00 1 c R . . H(11) H 0.2095 0.5501 0.2550 0.050 Uiso 1.00 1 c R . . H(12) H 0.1833 0.6424 0.2537 0.050 Uiso 1.00 1 c R . . H(13) H 0.1572 0.4915 0.2865 0.050 Uiso 1.00 1 c R . . H(14) H 0.1715 0.4169 0.2374 0.050 Uiso 1.00 1 c R . . H(15) H 0.0810 0.4001 0.1038 0.094 Uiso 1.00 1 c R . . H(16) H 0.0549 0.2268 0.0952 0.106 Uiso 1.00 1 c R . . H(17) H 0.0687 0.0930 0.1719 0.087 Uiso 1.00 1 c R . . H(18) H 0.1093 0.1275 0.2502 0.099 Uiso 1.00 1 c R . . H(19) H 0.1341 0.3046 0.2592 0.087 Uiso 1.00 1 c R . . H(20) H 0.1077 0.4780 0.3186 0.061 Uiso 1.00 1 c R . . H(21) H 0.0687 0.5615 0.3747 0.074 Uiso 1.00 1 c R . . H(22) H 0.0348 0.6954 0.3329 0.084 Uiso 1.00 1 c R . . H(23) H 0.0397 0.7617 0.2288 0.067 Uiso 1.00 1 c R . . H(24) H 0.0364 0.5305 0.1386 0.075 Uiso 1.00 1 c R . . H(25) H -0.0159 0.4975 0.0871 0.092 Uiso 1.00 1 c R . . H(26) H -0.0372 0.6175 0.0087 0.102 Uiso 1.00 1 c R . . H(27) H -0.0075 0.7720 -0.0136 0.112 Uiso 1.00 1 c R . . H(28) H 0.0428 0.8077 0.0406 0.071 Uiso 1.00 1 c R . . H(29) H 0.0628 0.8791 0.1346 0.045 Uiso 1.00 1 c R . . H(30) H 0.0918 0.8727 0.1862 0.045 Uiso 1.00 1 c R . . H(31) H 0.1109 0.9779 0.1089 0.046 Uiso 1.00 1 c R . . H(32) H 0.0978 0.8920 0.0592 0.046 Uiso 1.00 1 c R . . H(33) H 0.1308 0.9669 0.0046 0.061 Uiso 1.00 1 c R . . H(34) H 0.1631 1.0819 -0.0553 0.081 Uiso 1.00 1 c R . . H(35) H 0.2187 1.0897 -0.0358 0.074 Uiso 1.00 1 c R . . H(36) H 0.2445 0.9700 0.0385 0.067 Uiso 1.00 1 c R . . H(37) H 0.2146 0.8637 0.1016 0.055 Uiso 1.00 1 c R . . H(38) H 0.1835 1.0238 0.1587 0.063 Uiso 1.00 1 c R . . H(39) H 0.1961 1.1010 0.2561 0.063 Uiso 1.00 1 c R . . H(40) H 0.1825 1.0160 0.3436 0.069 Uiso 1.00 1 c R . . H(41) H 0.1555 0.8457 0.3370 0.071 Uiso 1.00 1 c R . . H(42) H 0.1417 0.7642 0.2393 0.043 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ir(1) 0.0490(2) 0.0525(2) 0.0450(2) 0.0039(2) 0.0027(2) -0.0148(2) Ir(2) 0.0544(2) 0.0459(2) 0.0296(2) -0.0082(2) -0.00029(18) 0.00153(18) Mo(1) 0.0289(4) 0.0303(4) 0.0247(3) -0.0021(3) 0.0025(3) -0.0008(3) Cl(1) 0.48(4) 0.25(2) 0.22(2) 0.0000 0.08(2) 0.0000 Cl(2) 0.34(3) 0.30(2) 0.31(3) 0.0000 0.02(2) 0.0000 Cl(3) 0.30(2) 0.163(13) 0.38(2) -0.015(14) -0.08(2) -0.083(16) Cl(4) 0.167(18) 0.27(2) 0.54(4) -0.085(17) -0.06(2) 0.12(2) Cl(5) 0.22(3) 0.15(2) 0.51(6) -0.001(19) 0.06(3) 0.08(2) Cl(6) 0.17(4) 0.19(3) 0.42(8) 0.01(3) -0.01(4) -0.01(4) Cl(7) 0.30(8) 0.17(4) 0.49(11) -0.07(4) -0.07(8) -0.14(6) S(1) 0.0405(15) 0.0698(18) 0.0267(11) -0.0095(13) 0.0094(10) -0.0070(12) S(2) 0.0373(13) 0.0418(13) 0.0330(12) -0.0097(10) 0.0019(10) -0.0033(10) P(1) 0.0310(13) 0.0325(12) 0.0322(12) -0.0022(10) 0.0038(10) -0.0026(10) P(2) 0.0352(14) 0.0380(13) 0.0312(12) 0.0013(11) 0.0059(10) 0.0051(10) P(3) 0.0373(14) 0.0345(12) 0.0309(12) 0.0002(10) 0.0051(10) 0.0007(10) P(4) 0.0381(14) 0.0298(11) 0.0283(11) -0.0036(10) 0.0057(10) -0.0017(9) O(1) 0.097(10) 0.161(13) 0.27(2) -0.005(9) 0.099(12) -0.101(13) O(2) 0.127(10) 0.043(5) 0.192(13) -0.020(6) -0.009(9) -0.041(7) O(3) 0.090(8) 0.122(9) 0.106(8) 0.018(7) -0.045(7) 0.036(7) O(4) 0.167(13) 0.130(10) 0.074(7) -0.074(9) 0.001(7) 0.046(7) C(1) 0.099(13) 0.099(12) 0.116(14) 0.022(10) 0.034(11) -0.049(11) C(2) 0.088(11) 0.062(9) 0.090(11) -0.004(8) -0.012(8) -0.023(7) C(3) 0.073(9) 0.072(8) 0.046(6) -0.000(7) -0.011(6) 0.012(6) C(4) 0.080(10) 0.108(11) 0.041(7) -0.033(9) -0.005(6) -0.001(7) C(5) 0.032(5) 0.037(5) 0.037(5) 0.003(4) 0.004(4) -0.002(4) C(6) 0.037(5) 0.044(5) 0.049(6) -0.011(4) 0.010(4) -0.005(4) C(7) 0.037(6) 0.046(6) 0.071(8) -0.016(5) 0.011(5) 0.001(5) C(8) 0.049(7) 0.061(7) 0.070(8) -0.020(6) 0.021(6) -0.001(6) C(9) 0.044(6) 0.060(7) 0.058(7) -0.012(5) -0.009(5) -0.017(5) C(10) 0.051(6) 0.045(5) 0.035(5) -0.016(5) 0.004(4) 0.003(4) C(11) 0.038(5) 0.034(4) 0.036(5) 0.003(4) -0.003(4) -0.002(4) C(12) 0.049(6) 0.040(5) 0.052(6) 0.017(5) 0.003(5) 0.002(4) C(13) 0.062(8) 0.037(5) 0.068(7) -0.006(5) -0.005(6) -0.008(5) C(14) 0.057(7) 0.042(6) 0.072(8) 0.007(5) 0.006(6) -0.003(5) C(15) 0.043(6) 0.050(6) 0.057(6) 0.004(5) 0.010(5) -0.001(5) C(16) 0.037(5) 0.036(5) 0.051(6) -0.002(4) 0.009(4) 0.007(4) C(17) 0.039(5) 0.049(6) 0.038(5) 0.005(4) 0.003(4) 0.008(4) C(18) 0.045(6) 0.044(5) 0.035(5) 0.004(4) 0.005(4) 0.008(4) C(19) 0.053(7) 0.040(5) 0.051(6) 0.011(5) 0.014(5) 0.015(5) C(20) 0.100(11) 0.076(9) 0.058(8) -0.040(8) -0.009(7) 0.026(7) C(21) 0.113(13) 0.072(9) 0.080(10) -0.052(9) -0.026(9) 0.008(8) C(22) 0.110(12) 0.033(6) 0.074(9) -0.020(6) 0.020(8) -0.001(6) C(23) 0.085(11) 0.058(8) 0.106(12) -0.003(7) 0.002(9) 0.041(8) C(24) 0.067(9) 0.060(8) 0.090(10) -0.004(6) -0.013(7) 0.022(7) C(25) 0.035(5) 0.040(5) 0.035(5) -0.003(4) 0.006(4) 0.003(4) C(26) 0.055(7) 0.055(6) 0.044(6) 0.009(5) 0.015(5) 0.004(5) C(27) 0.051(7) 0.094(9) 0.040(6) 0.000(7) 0.013(5) 0.014(6) C(28) 0.085(10) 0.079(9) 0.045(6) 0.025(7) 0.041(6) 0.001(6) C(29) 0.063(8) 0.055(6) 0.049(6) 0.013(5) 0.027(5) 0.006(5) C(30) 0.048(6) 0.043(5) 0.032(4) 0.008(4) 0.015(4) 0.006(4) C(31) 0.016(4) 0.053(6) 0.057(6) -0.000(4) 0.003(4) -0.007(5) C(32) 0.051(7) 0.063(7) 0.073(8) -0.004(6) 0.029(6) -0.016(6) C(33) 0.051(8) 0.069(8) 0.110(12) -0.027(7) 0.047(8) -0.045(8) C(34) 0.033(7) 0.127(14) 0.094(11) -0.009(8) -0.005(7) -0.048(10) C(35) 0.058(9) 0.126(14) 0.096(12) 0.003(10) -0.031(8) -0.020(11) C(36) 0.049(7) 0.065(7) 0.063(7) -0.004(6) -0.002(6) -0.001(6) C(37) 0.038(5) 0.030(4) 0.046(5) 0.006(4) 0.008(4) 0.005(4) C(38) 0.040(5) 0.033(4) 0.042(5) 0.003(4) 0.001(4) -0.006(4) C(39) 0.045(6) 0.043(5) 0.043(5) 0.003(4) 0.004(4) -0.005(4) C(40) 0.037(6) 0.082(8) 0.034(5) -0.004(5) -0.001(4) 0.005(5) C(41) 0.107(12) 0.063(8) 0.033(5) -0.012(7) 0.019(6) 0.014(5) C(42) 0.086(10) 0.040(6) 0.059(7) -0.002(6) 0.030(7) 0.003(5) C(43) 0.060(8) 0.047(6) 0.061(7) -0.011(5) 0.032(6) -0.005(5) C(44) 0.048(6) 0.040(5) 0.051(6) -0.007(5) 0.012(5) 0.012(4) C(45) 0.030(5) 0.040(5) 0.031(4) 0.001(4) -0.001(3) -0.007(4) C(46) 0.070(8) 0.044(6) 0.045(6) -0.012(5) 0.013(5) -0.007(5) C(47) 0.045(6) 0.057(7) 0.056(7) -0.004(5) -0.014(5) -0.020(5) C(48) 0.056(7) 0.068(8) 0.050(7) 0.018(6) 0.000(5) -0.026(6) C(49) 0.071(8) 0.074(8) 0.032(5) 0.010(7) 0.009(5) -0.007(5) C(50) 0.030(5) 0.044(5) 0.033(4) -0.001(4) 0.008(3) -0.004(4) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; Disordered CH2Cl2 molecules were modelled as following. Cl(1)-C(51)-Cl(2) 37.5% occ. Cl(1)-C(51*)-Cl(2) 37.5% occ. Cl(3)-C(52)-Cl(4) 35% occ. Cl(3)-C(52)-Cl(6) 25% occ. Cl(4)-C(52)-Cl(5) 20% occ. Cl(5)-C(52)-Cl(7) 20% occ. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Ir(1) Ir(2) 2.9856(6) yes . . Ir(1) S(1) 2.352(3) yes . . Ir(1) S(2) 2.349(2) yes . . Ir(1) C(1) 1.815(19) yes . . Ir(1) C(2) 1.849(14) yes . . Ir(2) S(1) 2.357(2) yes . . Ir(2) S(2) 2.339(2) yes . . Ir(2) C(3) 1.844(14) yes . . Ir(2) C(4) 1.857(15) yes . . Mo(1) S(1) 2.468(2) yes . . Mo(1) S(2) 2.452(2) yes . . Mo(1) P(1) 2.502(2) yes . . Mo(1) P(2) 2.471(2) yes . . Mo(1) P(3) 2.451(2) yes . . Mo(1) P(4) 2.479(2) yes . . Cl(1) C(51) 1.66(6) yes . . Cl(2) C(51) 1.93(6) yes . . Cl(3) C(52) 1.67(3) yes . . Cl(4) C(52) 1.69(3) yes . . Cl(5) C(52) 1.68(4) yes . . Cl(6) C(52) 1.70(5) yes . . Cl(7) C(52) 1.71(6) yes . . P(1) C(5) 1.863(10) yes . . P(1) C(11) 1.855(9) yes . . P(1) C(17) 1.851(10) yes . . P(2) C(18) 1.869(10) yes . . P(2) C(19) 1.859(10) yes . . P(2) C(25) 1.842(10) yes . . P(3) C(30) 1.832(10) yes . . P(3) C(31) 1.851(9) yes . . P(3) C(37) 1.855(9) yes . . P(4) C(38) 1.857(9) yes . . P(4) C(39) 1.833(11) yes . . P(4) C(45) 1.850(9) yes . . O(1) C(1) 1.15(2) yes . . O(2) C(2) 1.146(18) yes . . O(3) C(3) 1.156(18) yes . . O(4) C(4) 1.140(19) yes . . C(5) C(6) 1.381(15) yes . . C(5) C(10) 1.357(13) yes . . C(6) C(7) 1.393(15) yes . . C(7) C(8) 1.356(17) yes . . C(8) C(9) 1.393(18) yes . . C(9) C(10) 1.401(16) yes . . C(11) C(12) 1.376(14) yes . . C(11) C(16) 1.361(14) yes . . C(12) C(13) 1.389(15) yes . . C(13) C(14) 1.366(17) yes . . C(14) C(15) 1.367(16) yes . . C(15) C(16) 1.367(15) yes . . C(17) C(18) 1.509(14) yes . . C(19) C(20) 1.348(17) yes . . C(19) C(24) 1.373(17) yes . . C(20) C(21) 1.39(2) yes . . C(21) C(22) 1.392(19) yes . . C(22) C(23) 1.35(2) yes . . C(23) C(24) 1.409(19) yes . . C(25) C(26) 1.385(14) yes . . C(25) C(30) 1.366(13) yes . . C(26) C(27) 1.386(17) yes . . C(27) C(28) 1.340(18) yes . . C(28) C(29) 1.435(17) yes . . C(29) C(30) 1.396(16) yes . . C(31) C(32) 1.357(16) yes . . C(31) C(36) 1.376(16) yes . . C(32) C(33) 1.399(18) yes . . C(33) C(34) 1.38(2) yes . . C(34) C(35) 1.35(2) yes . . C(35) C(36) 1.359(19) yes . . C(37) C(38) 1.524(14) yes . . C(39) C(40) 1.405(14) yes . . C(39) C(44) 1.388(15) yes . . C(40) C(41) 1.438(18) yes . . C(41) C(42) 1.35(2) yes . . C(42) C(43) 1.379(16) yes . . C(43) C(44) 1.382(16) yes . . C(45) C(46) 1.400(14) yes . . C(45) C(50) 1.398(13) yes . . C(46) C(47) 1.367(16) yes . . C(47) C(48) 1.337(17) yes . . C(48) C(49) 1.384(18) yes . . C(49) C(50) 1.391(14) yes . . C(6) H(1) 0.950 no . . C(7) H(2) 0.950 no . . C(8) H(3) 0.950 no . . C(9) H(4) 0.950 no . . C(10) H(5) 0.950 no . . C(12) H(6) 0.950 no . . C(13) H(7) 0.950 no . . C(14) H(8) 0.950 no . . C(15) H(9) 0.950 no . . C(16) H(10) 0.950 no . . C(17) H(11) 0.950 no . . C(17) H(12) 0.950 no . . C(18) H(13) 0.950 no . . C(18) H(14) 0.950 no . . C(20) H(15) 0.950 no . . C(21) H(16) 0.950 no . . C(22) H(17) 0.950 no . . C(23) H(18) 0.950 no . . C(24) H(19) 0.950 no . . C(26) H(20) 0.950 no . . C(27) H(21) 0.950 no . . C(28) H(22) 0.950 no . . C(29) H(23) 0.950 no . . C(32) H(24) 0.950 no . . C(33) H(25) 0.950 no . . C(34) H(26) 0.950 no . . C(35) H(27) 0.950 no . . C(36) H(28) 0.950 no . . C(37) H(29) 0.950 no . . C(37) H(30) 0.950 no . . C(38) H(31) 0.950 no . . C(38) H(32) 0.950 no . . C(40) H(33) 0.950 no . . C(41) H(34) 0.950 no . . C(42) H(35) 0.950 no . . C(43) H(36) 0.950 no . . C(44) H(37) 0.950 no . . C(46) H(38) 0.950 no . . C(47) H(39) 0.950 no . . C(48) H(40) 0.950 no . . C(49) H(41) 0.950 no . . C(50) H(42) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Ir(2) Ir(1) S(1) 50.72(6) yes . . . Ir(2) Ir(1) S(2) 50.28(6) yes . . . Ir(2) Ir(1) C(1) 126.8(5) yes . . . Ir(2) Ir(1) C(2) 127.1(4) yes . . . S(1) Ir(1) S(2) 83.39(9) yes . . . S(1) Ir(1) C(1) 94.7(5) yes . . . S(1) Ir(1) C(2) 175.0(5) yes . . . S(2) Ir(1) C(1) 177.0(5) yes . . . S(2) Ir(1) C(2) 92.0(5) yes . . . C(1) Ir(1) C(2) 90.0(7) yes . . . Ir(1) Ir(2) S(1) 50.58(7) yes . . . Ir(1) Ir(2) S(2) 50.60(6) yes . . . Ir(1) Ir(2) C(3) 124.3(4) yes . . . Ir(1) Ir(2) C(4) 124.1(4) yes . . . S(1) Ir(2) S(2) 83.52(9) yes . . . S(1) Ir(2) C(3) 174.7(4) yes . . . S(1) Ir(2) C(4) 92.0(4) yes . . . S(2) Ir(2) C(3) 91.8(4) yes . . . S(2) Ir(2) C(4) 174.6(4) yes . . . C(3) Ir(2) C(4) 92.5(6) yes . . . S(1) Mo(1) S(2) 78.95(8) yes . . . S(1) Mo(1) P(1) 82.63(8) yes . . . S(1) Mo(1) P(2) 143.51(10) yes . . . S(1) Mo(1) P(3) 140.54(9) yes . . . S(1) Mo(1) P(4) 87.52(9) yes . . . S(2) Mo(1) P(1) 138.48(8) yes . . . S(2) Mo(1) P(2) 100.48(8) yes . . . S(2) Mo(1) P(3) 83.52(8) yes . . . S(2) Mo(1) P(4) 128.41(8) yes . . . P(1) Mo(1) P(2) 73.92(8) yes . . . P(1) Mo(1) P(3) 131.01(8) yes . . . P(1) Mo(1) P(4) 87.15(8) yes . . . P(2) Mo(1) P(3) 74.32(9) yes . . . P(2) Mo(1) P(4) 118.14(8) yes . . . P(3) Mo(1) P(4) 76.22(8) yes . . . Ir(1) S(1) Ir(2) 78.70(8) yes . . . Ir(1) S(1) Mo(1) 84.21(9) yes . . . Ir(2) S(1) Mo(1) 81.29(9) yes . . . Ir(1) S(2) Ir(2) 79.12(8) yes . . . Ir(1) S(2) Mo(1) 84.61(8) yes . . . Ir(2) S(2) Mo(1) 81.99(8) yes . . . Mo(1) P(1) C(5) 125.7(3) yes . . . Mo(1) P(1) C(11) 114.7(3) yes . . . Mo(1) P(1) C(17) 111.5(3) yes . . . C(5) P(1) C(11) 100.1(4) yes . . . C(5) P(1) C(17) 102.3(4) yes . . . C(11) P(1) C(17) 98.5(4) yes . . . Mo(1) P(2) C(18) 115.2(3) yes . . . Mo(1) P(2) C(19) 121.3(3) yes . . . Mo(1) P(2) C(25) 114.7(3) yes . . . C(18) P(2) C(19) 100.9(4) yes . . . C(18) P(2) C(25) 102.2(4) yes . . . C(19) P(2) C(25) 99.8(5) yes . . . Mo(1) P(3) C(30) 116.0(3) yes . . . Mo(1) P(3) C(31) 119.8(3) yes . . . Mo(1) P(3) C(37) 114.5(3) yes . . . C(30) P(3) C(31) 100.6(4) yes . . . C(30) P(3) C(37) 101.5(4) yes . . . C(31) P(3) C(37) 101.8(4) yes . . . Mo(1) P(4) C(38) 107.9(3) yes . . . Mo(1) P(4) C(39) 123.1(3) yes . . . Mo(1) P(4) C(45) 123.4(3) yes . . . C(38) P(4) C(39) 99.2(4) yes . . . C(38) P(4) C(45) 96.8(4) yes . . . C(39) P(4) C(45) 101.0(4) yes . . . Ir(1) C(1) O(1) 174.2(16) yes . . . Ir(1) C(2) O(2) 178.8(9) yes . . . Ir(2) C(3) O(3) 177.1(12) yes . . . Ir(2) C(4) O(4) 175.5(13) yes . . . P(1) C(5) C(6) 119.1(7) yes . . . P(1) C(5) C(10) 120.4(8) yes . . . C(6) C(5) C(10) 120.5(9) yes . . . C(5) C(6) C(7) 120.9(9) yes . . . C(6) C(7) C(8) 117.8(11) yes . . . C(7) C(8) C(9) 122.8(11) yes . . . C(8) C(9) C(10) 117.8(10) yes . . . C(5) C(10) C(9) 120.2(10) yes . . . P(1) C(11) C(12) 121.4(8) yes . . . P(1) C(11) C(16) 121.7(7) yes . . . C(12) C(11) C(16) 116.4(9) yes . . . C(11) C(12) C(13) 123.1(10) yes . . . C(12) C(13) C(14) 118.1(10) yes . . . C(13) C(14) C(15) 119.7(10) yes . . . C(14) C(15) C(16) 120.6(10) yes . . . C(11) C(16) C(15) 122.0(9) yes . . . P(1) C(17) C(18) 105.7(6) yes . . . P(2) C(18) C(17) 111.1(6) yes . . . P(2) C(19) C(20) 119.2(9) yes . . . P(2) C(19) C(24) 121.4(9) yes . . . C(20) C(19) C(24) 119.3(11) yes . . . C(19) C(20) C(21) 122.2(12) yes . . . C(20) C(21) C(22) 118.0(13) yes . . . C(21) C(22) C(23) 120.5(12) yes . . . C(22) C(23) C(24) 120.1(13) yes . . . C(19) C(24) C(23) 119.7(12) yes . . . P(2) C(25) C(26) 123.8(7) yes . . . P(2) C(25) C(30) 115.8(7) yes . . . C(26) C(25) C(30) 120.3(9) yes . . . C(25) C(26) C(27) 117.9(10) yes . . . C(26) C(27) C(28) 122.9(11) yes . . . C(27) C(28) C(29) 120.3(12) yes . . . C(28) C(29) C(30) 116.0(10) yes . . . P(3) C(30) C(25) 116.0(7) yes . . . P(3) C(30) C(29) 121.5(7) yes . . . C(25) C(30) C(29) 122.5(9) yes . . . P(3) C(31) C(32) 120.4(8) yes . . . P(3) C(31) C(36) 121.2(8) yes . . . C(32) C(31) C(36) 118.4(10) yes . . . C(31) C(32) C(33) 120.6(11) yes . . . C(32) C(33) C(34) 119.8(13) yes . . . C(33) C(34) C(35) 118.4(13) yes . . . C(34) C(35) C(36) 121.6(15) yes . . . C(31) C(36) C(35) 121.1(13) yes . . . P(3) C(37) C(38) 108.6(6) yes . . . P(4) C(38) C(37) 107.6(6) yes . . . P(4) C(39) C(40) 120.5(8) yes . . . P(4) C(39) C(44) 121.0(7) yes . . . C(40) C(39) C(44) 118.4(10) yes . . . C(39) C(40) C(41) 117.7(10) yes . . . C(40) C(41) C(42) 123.0(11) yes . . . C(41) C(42) C(43) 117.8(12) yes . . . C(42) C(43) C(44) 121.7(12) yes . . . C(39) C(44) C(43) 121.2(10) yes . . . P(4) C(45) C(46) 123.0(7) yes . . . P(4) C(45) C(50) 118.4(7) yes . . . C(46) C(45) C(50) 118.3(8) yes . . . C(45) C(46) C(47) 119.5(10) yes . . . C(46) C(47) C(48) 122.5(11) yes . . . C(47) C(48) C(49) 119.9(11) yes . . . C(48) C(49) C(50) 119.5(10) yes . . . C(45) C(50) C(49) 120.2(9) yes . . . Cl(1) C(51) Cl(2) 95(3) yes . . . Cl(3) C(52) Cl(4) 120(2) yes . . . Cl(3) C(52) Cl(6) 123(2) yes . . . Cl(4) C(52) Cl(5) 107(2) yes . . . Cl(5) C(52) Cl(7) 118(3) yes . . . C(5) C(6) H(1) 119.1 no . . . C(7) C(6) H(1) 120.0 no . . . C(6) C(7) H(2) 121.0 no . . . C(8) C(7) H(2) 121.3 no . . . C(7) C(8) H(3) 118.9 no . . . C(9) C(8) H(3) 118.3 no . . . C(8) C(9) H(4) 121.1 no . . . C(10) C(9) H(4) 121.1 no . . . C(5) C(10) H(5) 119.9 no . . . C(9) C(10) H(5) 120.0 no . . . C(11) C(12) H(6) 117.8 no . . . C(13) C(12) H(6) 119.1 no . . . C(12) C(13) H(7) 121.2 no . . . C(14) C(13) H(7) 120.7 no . . . C(13) C(14) H(8) 120.0 no . . . C(15) C(14) H(8) 120.3 no . . . C(14) C(15) H(9) 119.6 no . . . C(16) C(15) H(9) 119.8 no . . . C(11) C(16) H(10) 118.3 no . . . C(15) C(16) H(10) 119.7 no . . . P(1) C(17) H(11) 110.2 no . . . P(1) C(17) H(12) 110.6 no . . . C(18) C(17) H(11) 110.8 no . . . C(18) C(17) H(12) 110.1 no . . . H(11) C(17) H(12) 109.5 no . . . P(2) C(18) H(13) 108.9 no . . . P(2) C(18) H(14) 108.8 no . . . C(17) C(18) H(13) 109.8 no . . . C(17) C(18) H(14) 108.7 no . . . H(13) C(18) H(14) 109.5 no . . . C(19) C(20) H(15) 118.6 no . . . C(21) C(20) H(15) 119.2 no . . . C(20) C(21) H(16) 121.5 no . . . C(22) C(21) H(16) 120.4 no . . . C(21) C(22) H(17) 119.6 no . . . C(23) C(22) H(17) 119.9 no . . . C(22) C(23) H(18) 119.8 no . . . C(24) C(23) H(18) 120.1 no . . . C(19) C(24) H(19) 119.8 no . . . C(23) C(24) H(19) 120.5 no . . . C(25) C(26) H(20) 120.4 no . . . C(27) C(26) H(20) 121.7 no . . . C(26) C(27) H(21) 118.5 no . . . C(28) C(27) H(21) 118.7 no . . . C(27) C(28) H(22) 119.6 no . . . C(29) C(28) H(22) 120.1 no . . . C(28) C(29) H(23) 122.2 no . . . C(30) C(29) H(23) 121.8 no . . . C(31) C(32) H(24) 118.6 no . . . C(33) C(32) H(24) 120.8 no . . . C(32) C(33) H(25) 119.8 no . . . C(34) C(33) H(25) 120.4 no . . . C(33) C(34) H(26) 119.5 no . . . C(35) C(34) H(26) 122.0 no . . . C(34) C(35) H(27) 118.3 no . . . C(36) C(35) H(27) 120.0 no . . . C(31) C(36) H(28) 118.4 no . . . C(35) C(36) H(28) 120.5 no . . . P(3) C(37) H(29) 109.8 no . . . P(3) C(37) H(30) 109.9 no . . . C(38) C(37) H(29) 110.1 no . . . C(38) C(37) H(30) 109.1 no . . . H(29) C(37) H(30) 109.5 no . . . P(4) C(38) H(31) 110.0 no . . . P(4) C(38) H(32) 109.4 no . . . C(37) C(38) H(31) 111.2 no . . . C(37) C(38) H(32) 109.1 no . . . H(31) C(38) H(32) 109.5 no . . . C(39) C(40) H(33) 120.3 no . . . C(41) C(40) H(33) 122.0 no . . . C(40) C(41) H(34) 118.4 no . . . C(42) C(41) H(34) 118.6 no . . . C(41) C(42) H(35) 121.1 no . . . C(43) C(42) H(35) 121.1 no . . . C(42) C(43) H(36) 119.3 no . . . C(44) C(43) H(36) 119.1 no . . . C(39) C(44) H(37) 118.8 no . . . C(43) C(44) H(37) 120.0 no . . . C(45) C(46) H(38) 119.8 no . . . C(47) C(46) H(38) 120.7 no . . . C(46) C(47) H(39) 119.0 no . . . C(48) C(47) H(39) 118.5 no . . . C(47) C(48) H(40) 120.4 no . . . C(49) C(48) H(40) 119.6 no . . . C(48) C(49) H(41) 120.5 no . . . C(50) C(49) H(41) 120.0 no . . . C(45) C(50) H(42) 119.5 no . . . C(49) C(50) H(42) 120.3 no . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Mo(1) Ir(1) 3.2325(8) ? . . Mo(1) Ir(2) 3.1436(7) ? . . #===end #============================================================================== # End of CIF #==============================================================================