Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 #=============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Santiago Garcia-Granda Departamento de Qu\'imica Fisica y Analitica Facultad de Quimica Universidad de Oviedo C/ Julian Claveria, 8 33071 Oviedo Spain ; _publ_contact_author_phone '0034 98 5103477' _publ_contact_author_fax '0034 98 5103125' _publ_contact_author_email sgg@sauron.quimica.uniovi.es _publ_requested_journal test _publ_contact_letter ; Oviedo 6/02/2003 Please receive the CIF for compounds, 3,4,5,6 and 7 submitted to be published in Thank you very much. S. Garcia-Granda. ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Crystal structure of compounds 3, 4, 5, 6, and 7 ; # The loop structure below should contain the names and addresses of all #authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Santiago Garcia-Granda' ; Departamento de Quimica Fisica y Analitica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; #========================================================================== data_3 _database_code_CSD 196132 #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 Cl 2 Mo 2 O4 P2' _chemical_formula_sum 'C15 H24 Cl 2 Mo 2 O4 P2' _chemical_formula_weight 593.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z+1/2' 'x, -y+1/2, z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z-1/2' '-x, y-1/2, -z' 'x-1/2, y, -z-1/2' _cell_length_a 11.896(2) _cell_length_b 19.191(6) _cell_length_c 9.294(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2121.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.601 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.582 _exptl_absorpt_correction_T_max 0.657 _exptl_absorpt_process_details 'XABS (Parkin, Moezzi & Hope, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius CAD-4 diffractometer' _diffrn_measurement_method '\w-2\q scan technique' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1.93 _diffrn_reflns_number 2142 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.97 _reflns_number_total 2142 _reflns_number_gt 1780 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 EXPRESS (Enraf-Nonius, 1994)' _computing_cell_refinement 'CRYSDA (Beurskens et al., 1992)' _computing_data_reduction "REFLEX (Garc\'ia-Granda et al., 1999)" _computing_structure_solution 'DIRDIF (Beurskens et al., 1992)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_molecular_graphics 'PLATON (Spek, 1982)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+9.5619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2142 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.72867(3) 0.145078(18) 0.56041(4) 0.02179(13) Uani 1 1 d . . . Cl1 Cl 0.84881(12) 0.2500 0.65685(16) 0.0267(3) Uani 1 2 d S . . Cl2 Cl 0.61086(12) 0.2500 0.46886(17) 0.0284(3) Uani 1 2 d S . . C1 C 0.8290(4) 0.0651(3) 0.5781(6) 0.0355(11) Uani 1 1 d . . . O1 O 0.8830(4) 0.0167(2) 0.5792(5) 0.0598(12) Uani 1 1 d . . . C2 C 0.6446(4) 0.0741(3) 0.4590(5) 0.0352(11) Uani 1 1 d . . . O2 O 0.5994(4) 0.0298(2) 0.3987(5) 0.0615(12) Uani 1 1 d . . . C3 C 0.5602(4) 0.1197(3) 0.6824(6) 0.0494(15) Uani 1 1 d . . . H3A H 0.4952 0.1481 0.6588 0.059 Uiso 1 1 calc R . . H3B H 0.5428 0.0709 0.6980 0.059 Uiso 1 1 calc R . . C4 C 0.6405(5) 0.1494(3) 0.7717(5) 0.0434(14) Uani 1 1 d . . . H4 H 0.6296 0.1932 0.8122 0.052 Uiso 1 1 calc R . . C5 C 0.7365(5) 0.1118(4) 0.7984(5) 0.0534(16) Uani 1 1 d . . . H5A H 0.7271 0.0626 0.8184 0.064 Uiso 1 1 calc R . . H5B H 0.7933 0.1342 0.8575 0.064 Uiso 1 1 calc R . . P1 P 0.84826(9) 0.16759(6) 0.34006(11) 0.0245(3) Uani 1 1 d . . . C6 C 0.8282(5) 0.1059(3) 0.1931(6) 0.0441(13) Uani 1 1 d . . . H6A H 0.7506 0.1057 0.1648 0.066 Uiso 1 1 calc R . . H6B H 0.8495 0.0601 0.2244 0.066 Uiso 1 1 calc R . . H6C H 0.8741 0.1194 0.1128 0.066 Uiso 1 1 calc R . . C7 C 0.9977(4) 0.1588(3) 0.3744(6) 0.0375(11) Uani 1 1 d . . . H7A H 1.0191 0.1895 0.4513 0.056 Uiso 1 1 calc R . . H7B H 1.0390 0.1708 0.2891 0.056 Uiso 1 1 calc R . . H7C H 1.0143 0.1116 0.4008 0.056 Uiso 1 1 calc R . . C8 C 0.8325(6) 0.2500 0.2427(7) 0.0288(14) Uani 1 2 d S . . H8A H 0.8868 0.2500 0.1648 0.035 Uiso 1 2 calc SR . . H8B H 0.7584 0.2500 0.1989 0.035 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0226(2) 0.0219(2) 0.0208(2) 0.00082(14) 0.00255(14) -0.00063(14) Cl1 0.0247(7) 0.0301(7) 0.0252(7) 0.000 -0.0056(6) 0.000 Cl2 0.0231(7) 0.0316(8) 0.0306(8) 0.000 -0.0064(6) 0.000 C1 0.033(2) 0.032(3) 0.042(3) 0.008(2) 0.006(2) 0.004(2) O1 0.055(2) 0.047(2) 0.076(3) 0.018(2) 0.016(2) 0.025(2) C2 0.038(3) 0.032(2) 0.036(3) -0.001(2) 0.002(2) -0.003(2) O2 0.070(3) 0.055(3) 0.060(3) -0.022(2) -0.002(2) -0.024(2) C3 0.034(3) 0.049(3) 0.066(4) 0.015(3) 0.019(3) -0.006(2) C4 0.062(4) 0.034(3) 0.034(3) -0.001(2) 0.031(3) -0.007(3) C5 0.063(4) 0.071(4) 0.026(3) 0.020(3) -0.002(3) -0.018(3) P1 0.0261(5) 0.0271(6) 0.0202(5) -0.0022(4) 0.0039(4) 0.0006(4) C6 0.058(3) 0.037(3) 0.037(3) -0.016(2) 0.007(3) -0.004(3) C7 0.027(2) 0.046(3) 0.040(3) 0.004(2) 0.005(2) 0.006(2) C8 0.030(3) 0.041(3) 0.015(3) 0.000 0.002(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.935(5) . ? Mo1 C1 1.951(5) . ? Mo1 C4 2.228(5) . ? Mo1 C5 2.304(5) . ? Mo1 C3 2.354(5) . ? Mo1 P1 2.5307(12) . ? Mo1 Cl2 2.5966(11) . ? Mo1 Cl1 2.6269(11) . ? Cl1 Mo1 2.6269(11) 3 ? Cl2 Mo1 2.5966(11) 3 ? C1 O1 1.130(6) . ? C2 O2 1.152(6) . ? C3 C4 1.388(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.374(8) . ? C4 H4 0.9300 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? P1 C7 1.814(5) . ? P1 C6 1.824(5) . ? P1 C8 1.832(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 P1 1.832(3) 3 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 78.7(2) . . ? C2 Mo1 C4 102.3(2) . . ? C1 Mo1 C4 104.1(2) . . ? C2 Mo1 C5 107.1(2) . . ? C1 Mo1 C5 71.1(2) . . ? C4 Mo1 C5 35.2(2) . . ? C2 Mo1 C3 69.5(2) . . ? C1 Mo1 C3 108.5(2) . . ? C4 Mo1 C3 35.1(2) . . ? C5 Mo1 C3 61.0(2) . . ? C2 Mo1 P1 90.93(15) . . ? C1 Mo1 P1 81.87(15) . . ? C4 Mo1 P1 166.32(14) . . ? C5 Mo1 P1 143.26(16) . . ? C3 Mo1 P1 154.66(16) . . ? C2 Mo1 Cl2 96.17(15) . . ? C1 Mo1 Cl2 165.41(15) . . ? C4 Mo1 Cl2 90.34(15) . . ? C5 Mo1 Cl2 123.45(18) . . ? C3 Mo1 Cl2 81.87(15) . . ? P1 Mo1 Cl2 84.59(5) . . ? C2 Mo1 Cl1 170.75(15) . . ? C1 Mo1 Cl1 103.95(16) . . ? C4 Mo1 Cl1 85.81(15) . . ? C5 Mo1 Cl1 82.10(16) . . ? C3 Mo1 Cl1 117.22(16) . . ? P1 Mo1 Cl1 80.76(4) . . ? Cl2 Mo1 Cl1 79.11(4) . . ? Mo1 Cl1 Mo1 100.09(5) . 3 ? Mo1 Cl2 Mo1 101.70(5) 3 . ? O1 C1 Mo1 174.6(5) . . ? O2 C2 Mo1 176.5(5) . . ? C4 C3 Mo1 67.5(3) . . ? C4 C3 H3A 116.9 . . ? Mo1 C3 H3A 116.9 . . ? C4 C3 H3B 116.9 . . ? Mo1 C3 H3B 116.9 . . ? H3A C3 H3B 114.0 . . ? C5 C4 C3 117.7(5) . . ? C5 C4 Mo1 75.4(3) . . ? C3 C4 Mo1 77.4(3) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? Mo1 C4 H4 117.1 . . ? C4 C5 Mo1 69.4(3) . . ? C4 C5 H5A 116.7 . . ? Mo1 C5 H5A 116.7 . . ? C4 C5 H5B 116.7 . . ? Mo1 C5 H5B 116.7 . . ? H5A C5 H5B 113.7 . . ? C7 P1 C6 101.5(3) . . ? C7 P1 C8 105.5(3) . . ? C6 P1 C8 100.2(3) . . ? C7 P1 Mo1 113.13(17) . . ? C6 P1 Mo1 114.95(18) . . ? C8 P1 Mo1 119.3(2) . . ? P1 C6 H6A 109.5 . . ? P1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? P1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P1 C7 H7A 109.5 . . ? P1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? P1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 P1 119.4(3) 3 . ? P1 C8 H8A 107.5 3 . ? P1 C8 H8A 107.5 . . ? P1 C8 H8B 107.5 3 . ? P1 C8 H8B 107.5 . . ? H8A C8 H8B 107.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Mo1 Cl1 Mo1 59.4(10) . . . 3 ? C1 Mo1 Cl1 Mo1 164.85(15) . . . 3 ? C4 Mo1 Cl1 Mo1 -91.69(16) . . . 3 ? C5 Mo1 Cl1 Mo1 -126.94(17) . . . 3 ? C3 Mo1 Cl1 Mo1 -75.41(17) . . . 3 ? P1 Mo1 Cl1 Mo1 85.69(5) . . . 3 ? Cl2 Mo1 Cl1 Mo1 -0.54(5) . . . 3 ? C2 Mo1 Cl2 Mo1 -171.42(15) . . . 3 ? C1 Mo1 Cl2 Mo1 -103.1(6) . . . 3 ? C4 Mo1 Cl2 Mo1 86.21(15) . . . 3 ? C5 Mo1 Cl2 Mo1 73.39(19) . . . 3 ? C3 Mo1 Cl2 Mo1 120.42(16) . . . 3 ? P1 Mo1 Cl2 Mo1 -81.06(5) . . . 3 ? Cl1 Mo1 Cl2 Mo1 0.54(5) . . . 3 ? C2 Mo1 C1 O1 22(5) . . . . ? C4 Mo1 C1 O1 122(5) . . . . ? C5 Mo1 C1 O1 135(5) . . . . ? C3 Mo1 C1 O1 86(5) . . . . ? P1 Mo1 C1 O1 -70(5) . . . . ? Cl2 Mo1 C1 O1 -48(5) . . . . ? Cl1 Mo1 C1 O1 -149(5) . . . . ? C1 Mo1 C2 O2 -12(8) . . . . ? C4 Mo1 C2 O2 -114(8) . . . . ? C5 Mo1 C2 O2 -78(8) . . . . ? C3 Mo1 C2 O2 -127(8) . . . . ? P1 Mo1 C2 O2 69(8) . . . . ? Cl2 Mo1 C2 O2 154(8) . . . . ? Cl1 Mo1 C2 O2 95(8) . . . . ? C2 Mo1 C3 C4 157.9(4) . . . . ? C1 Mo1 C3 C4 88.2(4) . . . . ? C5 Mo1 C3 C4 33.4(3) . . . . ? P1 Mo1 C3 C4 -160.7(3) . . . . ? Cl2 Mo1 C3 C4 -102.3(3) . . . . ? Cl1 Mo1 C3 C4 -29.1(4) . . . . ? Mo1 C3 C4 C5 -65.8(4) . . . . ? C2 Mo1 C4 C5 102.3(4) . . . . ? C1 Mo1 C4 C5 21.1(4) . . . . ? C3 Mo1 C4 C5 123.4(5) . . . . ? P1 Mo1 C4 C5 -93.2(7) . . . . ? Cl2 Mo1 C4 C5 -161.3(3) . . . . ? Cl1 Mo1 C4 C5 -82.2(3) . . . . ? C2 Mo1 C4 C3 -21.1(4) . . . . ? C1 Mo1 C4 C3 -102.3(4) . . . . ? C5 Mo1 C4 C3 -123.4(5) . . . . ? P1 Mo1 C4 C3 143.3(6) . . . . ? Cl2 Mo1 C4 C3 75.3(3) . . . . ? Cl1 Mo1 C4 C3 154.3(3) . . . . ? C3 C4 C5 Mo1 66.9(4) . . . . ? C2 Mo1 C5 C4 -87.1(4) . . . . ? C1 Mo1 C5 C4 -158.3(4) . . . . ? C3 Mo1 C5 C4 -33.3(3) . . . . ? P1 Mo1 C5 C4 156.7(3) . . . . ? Cl2 Mo1 C5 C4 22.6(4) . . . . ? Cl1 Mo1 C5 C4 93.9(3) . . . . ? C2 Mo1 P1 C7 -124.5(3) . . . . ? C1 Mo1 P1 C7 -46.1(3) . . . . ? C4 Mo1 P1 C7 70.7(7) . . . . ? C5 Mo1 P1 C7 -3.6(4) . . . . ? C3 Mo1 P1 C7 -162.7(4) . . . . ? Cl2 Mo1 P1 C7 139.4(2) . . . . ? Cl1 Mo1 P1 C7 59.6(2) . . . . ? C2 Mo1 P1 C6 -8.5(3) . . . . ? C1 Mo1 P1 C6 69.9(3) . . . . ? C4 Mo1 P1 C6 -173.3(7) . . . . ? C5 Mo1 P1 C6 112.4(4) . . . . ? C3 Mo1 P1 C6 -46.7(4) . . . . ? Cl2 Mo1 P1 C6 -104.6(2) . . . . ? Cl1 Mo1 P1 C6 175.6(2) . . . . ? C2 Mo1 P1 C8 110.6(3) . . . . ? C1 Mo1 P1 C8 -171.0(3) . . . . ? C4 Mo1 P1 C8 -54.2(7) . . . . ? C5 Mo1 P1 C8 -128.6(4) . . . . ? C3 Mo1 P1 C8 72.3(4) . . . . ? Cl2 Mo1 P1 C8 14.4(2) . . . . ? Cl1 Mo1 P1 C8 -65.4(2) . . . . ? C7 P1 C8 P1 -73.5(4) . . . 3 ? C6 P1 C8 P1 -178.6(4) . . . 3 ? Mo1 P1 C8 P1 55.1(4) . . . 3 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.654 _refine_diff_density_min -0.776 _refine_diff_density_rms 0.150 #==END #========================================================================== data_4 _database_code_CSD 196133 #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H22 Mo N O2 P2, C10 H10 Cl3 Mo2 O4' _chemical_formula_sum 'C22 H32 Cl3 Mo3 N O6 P2' _chemical_formula_weight 862.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6225(4) _cell_length_b 16.2346(7) _cell_length_c 21.4232(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.951(2) _cell_angle_gamma 90.00 _cell_volume 3338.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 12.493 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.128 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details 'XABS (Parkin, Moezzi & Hope, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.01 _diffrn_orient_matrix_UB_12 0 _diffrn_orient_matrix_UB_13 0 _diffrn_orient_matrix_UB_21 0 _diffrn_orient_matrix_UB_22 0.01 _diffrn_orient_matrix_UB_23 0 _diffrn_orient_matrix_UB_31 0 _diffrn_orient_matrix_UB_32 0 _diffrn_orient_matrix_UB_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5465 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 68.18 _reflns_number_total 5465 _reflns_number_gt 3526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5465 _refine_ls_number_parameters 319 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.1844 _refine_ls_wR_factor_gt 0.1745 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo2 Mo 0.07006(8) 0.62340(5) 0.87795(3) 0.0740(3) Uani 1 1 d . . . C21 C 0.1918(11) 0.5568(6) 0.9327(4) 0.085(3) Uani 1 1 d . . . O21 O 0.2716(8) 0.5180(5) 0.9627(3) 0.110(2) Uani 1 1 d . . . C22 C 0.2043(11) 0.5885(6) 0.8189(4) 0.097(3) Uani 1 1 d . . . O22 O 0.2888(9) 0.5678(5) 0.7876(4) 0.132(3) Uani 1 1 d . . . C18 C -0.1098(13) 0.5447(7) 0.8544(6) 0.109(3) Uani 1 1 d . . . H18 H -0.1962 0.5704 0.8534 0.131 Uiso 1 1 calc R . . C19 C -0.0484(11) 0.5085(7) 0.9088(6) 0.106(3) Uani 1 1 d . . . H19A H -0.0034 0.4556 0.9043 0.127 Uiso 1 1 calc R . . H19B H -0.0983 0.5134 0.9465 0.127 Uiso 1 1 calc R . . C20 C -0.0322(11) 0.5396(7) 0.8014(5) 0.108(3) Uani 1 1 d . . . H20A H -0.0710 0.5662 0.7636 0.129 Uiso 1 1 calc R . . H20B H 0.0135 0.4876 0.7942 0.129 Uiso 1 1 calc R . . Cl1 Cl 0.2174(2) 0.74825(14) 0.90580(11) 0.0810(6) Uani 1 1 d . . . Cl2 Cl -0.0713(2) 0.69458(14) 0.96148(10) 0.0806(6) Uani 1 1 d . . . Cl3 Cl -0.0600(3) 0.73703(17) 0.81297(10) 0.0976(8) Uani 1 1 d . . . Mo3 Mo -0.01084(8) 0.82943(5) 0.90987(3) 0.0756(3) Uani 1 1 d . . . C23 C -0.1952(16) 0.8686(9) 0.9220(10) 0.171(8) Uani 1 1 d . . . O23 O -0.2874(15) 0.8904(8) 0.9420(6) 0.198(5) Uani 1 1 d . . . C24 C 0.0341(13) 0.8820(6) 0.9892(5) 0.104(3) Uani 1 1 d . . . O24 O 0.0554(11) 0.9129(5) 1.0372(4) 0.147(4) Uani 1 1 d . . . C25 C -0.0827(16) 0.9309(8) 0.8424(6) 0.214(11) Uani 1 1 d D . . H25A H -0.1328 0.9142 0.8036 0.257 Uiso 1 1 calc R . . H25B H -0.1175 0.9810 0.8604 0.257 Uiso 1 1 calc R . . C26 C 0.0669(16) 0.9185(10) 0.8474(6) 0.159(7) Uani 1 1 d D . . H26 H 0.1120 0.8967 0.8141 0.191 Uiso 1 1 calc R . . C27 C 0.1402(13) 0.9395(10) 0.9020(8) 0.178(7) Uani 1 1 d D . . H27A H 0.1155 0.9908 0.9216 0.214 Uiso 1 1 calc R . . H27B H 0.2392 0.9274 0.9053 0.214 Uiso 1 1 calc R . . Mo1 Mo 0.57499(8) 0.76813(6) 0.64482(3) 0.0853(3) Uani 1 1 d . . . C2 C 0.5805(12) 0.7392(11) 0.7318(5) 0.151(6) Uani 1 1 d . . . O2 O 0.5775(10) 0.7193(11) 0.7841(4) 0.235(8) Uani 1 1 d . . . C4 C 0.818(2) 0.7613(10) 0.6584(9) 0.230(10) Uiso 1 1 d D . . H4 H 0.8828 0.7530 0.6922 0.276 Uiso 1 1 calc R . . C3 C 0.7771(14) 0.6929(9) 0.6247(8) 0.168(7) Uani 1 1 d D . . H3A H 0.7893 0.6404 0.6459 0.201 Uiso 1 1 calc R . . H3B H 0.8014 0.6914 0.5815 0.201 Uiso 1 1 calc R . . C5 C 0.7738(12) 0.8418(9) 0.6475(7) 0.158(6) Uani 1 1 d D . . H5A H 0.7970 0.8657 0.6080 0.190 Uiso 1 1 calc R . . H5B H 0.7889 0.8796 0.6824 0.190 Uiso 1 1 calc R . . P1 P 0.3193(3) 0.76664(17) 0.64643(10) 0.0811(7) Uani 1 1 d . . . C10 C 0.2323(12) 0.8053(8) 0.7125(5) 0.123(4) Uani 1 1 d . . . H10A H 0.2409 0.8642 0.7143 0.185 Uiso 1 1 calc R . . H10B H 0.2742 0.7818 0.7504 0.185 Uiso 1 1 calc R . . H10C H 0.1355 0.7905 0.7080 0.185 Uiso 1 1 calc R . . C14 C 0.2111(12) 0.8017(7) 0.5792(5) 0.107(3) Uani 1 1 d . . . H14A H 0.2176 0.8605 0.5760 0.160 Uiso 1 1 calc R . . H14B H 0.1160 0.7864 0.5841 0.160 Uiso 1 1 calc R . . H14C H 0.2421 0.7768 0.5420 0.160 Uiso 1 1 calc R . . C7 C 0.3020(10) 0.6563(6) 0.6473(5) 0.094(3) Uani 1 1 d . . . H7A H 0.2893 0.6352 0.6889 0.113 Uiso 1 1 calc R . . H7B H 0.2271 0.6371 0.6183 0.113 Uiso 1 1 calc R . . P2 P 0.4707(3) 0.63200(17) 0.62145(13) 0.0940(8) Uani 1 1 d . . . C8 C 0.5288(13) 0.5402(8) 0.6631(8) 0.160(6) Uani 1 1 d . . . H8A H 0.6197 0.5253 0.6510 0.240 Uiso 1 1 calc R . . H8B H 0.4647 0.4961 0.6530 0.240 Uiso 1 1 calc R . . H8C H 0.5328 0.5506 0.7073 0.240 Uiso 1 1 calc R . . C9 C 0.4377(13) 0.5997(7) 0.5386(5) 0.127(4) Uani 1 1 d . . . H9A H 0.5245 0.5863 0.5214 0.190 Uiso 1 1 calc R . . H9B H 0.3936 0.6440 0.5149 0.190 Uiso 1 1 calc R . . H9C H 0.3780 0.5523 0.5365 0.190 Uiso 1 1 calc R . . N1 N 0.5626(8) 0.8010(5) 0.5438(4) 0.089(2) Uani 1 1 d . . . C11 C 0.5586(10) 0.8212(7) 0.4932(5) 0.094(3) Uani 1 1 d . . . C12 C 0.5566(11) 0.8493(10) 0.4280(5) 0.135(5) Uani 1 1 d . . . H12A H 0.5480 0.8026 0.4005 0.202 Uiso 1 1 calc R . . H12B H 0.6417 0.8780 0.4215 0.202 Uiso 1 1 calc R . . H12C H 0.4790 0.8856 0.4194 0.202 Uiso 1 1 calc R . . O1 O 0.4923(18) 0.9330(12) 0.6659(9) 0.257(7) Uiso 1 1 d . . . C1 C 0.581(3) 0.879(2) 0.6826(16) 0.332(17) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo2 0.1066(5) 0.0601(5) 0.0556(4) -0.0050(3) 0.0086(3) 0.0044(4) C21 0.120(7) 0.067(6) 0.067(5) 0.005(5) 0.004(5) 0.001(5) O21 0.142(6) 0.098(6) 0.089(5) 0.023(4) 0.002(4) 0.021(5) C22 0.146(8) 0.078(7) 0.071(6) 0.025(5) 0.028(6) 0.030(6) O22 0.191(7) 0.117(7) 0.096(5) 0.026(5) 0.071(5) 0.060(6) C18 0.134(8) 0.091(9) 0.101(8) -0.036(7) 0.002(7) -0.017(7) C19 0.138(8) 0.063(7) 0.121(9) -0.018(6) 0.035(7) -0.013(6) C20 0.146(9) 0.096(9) 0.079(7) -0.026(6) -0.009(6) -0.002(7) Cl1 0.0987(13) 0.0638(14) 0.0804(14) 0.0041(11) 0.0061(11) 0.0002(11) Cl2 0.1131(15) 0.0659(14) 0.0640(12) -0.0056(10) 0.0149(10) -0.0003(11) Cl3 0.1358(18) 0.0943(19) 0.0598(12) -0.0099(12) -0.0141(12) 0.0197(15) Mo3 0.1089(5) 0.0602(5) 0.0575(4) -0.0021(3) 0.0034(3) 0.0117(4) C23 0.149(11) 0.070(9) 0.31(2) 0.009(11) 0.113(13) 0.038(8) O23 0.256(14) 0.147(11) 0.195(13) 0.001(9) 0.046(11) 0.035(10) C24 0.165(10) 0.063(7) 0.082(7) -0.003(6) -0.007(7) 0.044(7) O24 0.234(9) 0.106(7) 0.094(6) -0.042(5) -0.045(6) 0.056(6) C25 0.46(3) 0.105(11) 0.071(8) 0.012(7) -0.033(13) 0.135(16) C26 0.229(17) 0.165(16) 0.083(8) 0.017(9) 0.011(9) 0.127(14) C27 0.159(12) 0.126(14) 0.26(2) 0.031(15) 0.074(14) 0.038(10) Mo1 0.1093(5) 0.0969(7) 0.0496(4) -0.0062(4) 0.0048(3) -0.0220(4) C2 0.111(8) 0.28(2) 0.063(7) 0.022(9) -0.007(6) -0.040(10) O2 0.150(7) 0.50(2) 0.056(5) 0.059(9) -0.009(5) -0.061(11) C3 0.169(13) 0.194(17) 0.143(13) -0.017(12) 0.029(10) -0.075(12) C5 0.122(9) 0.213(19) 0.138(12) 0.012(12) 0.002(8) -0.082(11) P1 0.1099(15) 0.0810(18) 0.0527(12) -0.0005(11) 0.0074(11) -0.0017(13) C10 0.147(10) 0.142(11) 0.083(7) -0.020(7) 0.036(7) 0.001(8) C14 0.143(8) 0.098(8) 0.078(7) 0.008(6) -0.008(6) 0.013(7) C7 0.120(7) 0.087(8) 0.074(6) 0.009(5) -0.001(5) -0.019(6) P2 0.1272(19) 0.0636(17) 0.0931(18) 0.0110(14) 0.0216(15) -0.0017(14) C8 0.144(10) 0.102(10) 0.238(17) 0.101(11) 0.037(10) 0.027(8) C9 0.184(11) 0.090(9) 0.110(9) -0.040(7) 0.039(8) -0.025(8) N1 0.125(6) 0.073(5) 0.069(5) 0.007(4) 0.013(4) -0.012(4) C11 0.109(7) 0.101(9) 0.071(6) 0.015(6) 0.005(5) -0.016(6) C12 0.119(8) 0.214(15) 0.070(6) 0.050(8) -0.002(6) -0.029(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo2 C21 1.931(11) . ? Mo2 C22 1.953(10) . ? Mo2 C18 2.182(11) . ? Mo2 C20 2.298(10) . ? Mo2 C19 2.307(10) . ? Mo2 Cl1 2.521(2) . ? Mo2 Cl3 2.582(3) . ? Mo2 Cl2 2.593(2) . ? C21 O21 1.155(10) . ? C22 O22 1.140(10) . ? C18 C19 1.400(15) . ? C18 C20 1.403(14) . ? C18 H18 0.9300 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? Cl1 Mo3 2.568(2) . ? Cl2 Mo3 2.538(2) . ? Cl3 Mo3 2.578(2) . ? Mo3 C23 1.920(13) . ? Mo3 C24 1.924(11) . ? Mo3 C26 2.140(16) . ? Mo3 C25 2.267(11) . ? Mo3 C27 2.316(15) . ? C23 O23 1.070(15) . ? C24 O24 1.151(12) . ? C25 C26 1.450(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.367(9) . ? C26 H26 0.9300 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? Mo1 C2 1.919(12) . ? Mo1 C1 1.97(4) . ? Mo1 N1 2.224(8) . ? Mo1 C5 2.254(11) . ? Mo1 C4 2.34(2) . ? Mo1 C3 2.361(15) . ? Mo1 P1 2.463(3) . ? Mo1 P2 2.464(3) . ? C2 O2 1.168(13) . ? C4 C3 1.368(10) . ? C4 C5 1.390(10) . ? C4 H4 0.9300 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? P1 C7 1.799(11) . ? P1 C10 1.806(10) . ? P1 C14 1.810(10) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C7 P2 1.795(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? P2 C8 1.805(11) . ? P2 C9 1.858(11) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N1 C11 1.131(11) . ? C11 C12 1.467(13) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? O1 C1 1.26(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Mo2 C22 80.3(4) . . ? C21 Mo2 C18 104.5(5) . . ? C22 Mo2 C18 103.3(5) . . ? C21 Mo2 C20 108.3(4) . . ? C22 Mo2 C20 68.6(4) . . ? C18 Mo2 C20 36.4(4) . . ? C21 Mo2 C19 70.4(4) . . ? C22 Mo2 C19 108.2(4) . . ? C18 Mo2 C19 36.2(4) . . ? C20 Mo2 C19 62.0(4) . . ? C21 Mo2 Cl1 89.9(3) . . ? C22 Mo2 Cl1 90.0(4) . . ? C18 Mo2 Cl1 161.7(3) . . ? C20 Mo2 Cl1 148.3(3) . . ? C19 Mo2 Cl1 149.7(3) . . ? C21 Mo2 Cl3 168.2(3) . . ? C22 Mo2 Cl3 100.1(3) . . ? C18 Mo2 Cl3 86.9(4) . . ? C20 Mo2 Cl3 82.6(3) . . ? C19 Mo2 Cl3 120.1(3) . . ? Cl1 Mo2 Cl3 78.29(8) . . ? C21 Mo2 Cl2 98.9(3) . . ? C22 Mo2 Cl2 168.0(4) . . ? C18 Mo2 Cl2 88.6(3) . . ? C20 Mo2 Cl2 122.5(3) . . ? C19 Mo2 Cl2 82.5(3) . . ? Cl1 Mo2 Cl2 77.96(8) . . ? Cl3 Mo2 Cl2 78.22(8) . . ? O21 C21 Mo2 175.3(9) . . ? O22 C22 Mo2 175.6(10) . . ? C19 C18 C20 115.6(12) . . ? C19 C18 Mo2 76.8(6) . . ? C20 C18 Mo2 76.3(7) . . ? C19 C18 H18 122.2 . . ? C20 C18 H18 122.2 . . ? Mo2 C18 H18 115.9 . . ? C18 C19 Mo2 67.0(6) . . ? C18 C19 H19A 117.0 . . ? Mo2 C19 H19A 117.0 . . ? C18 C19 H19B 117.0 . . ? Mo2 C19 H19B 117.0 . . ? H19A C19 H19B 114.0 . . ? C18 C20 Mo2 67.3(6) . . ? C18 C20 H20A 117.0 . . ? Mo2 C20 H20A 117.0 . . ? C18 C20 H20B 117.0 . . ? Mo2 C20 H20B 117.0 . . ? H20A C20 H20B 114.0 . . ? Mo2 Cl1 Mo3 87.28(7) . . ? Mo3 Cl2 Mo2 86.38(7) . . ? Mo3 Cl3 Mo2 85.78(7) . . ? C23 Mo3 C24 83.5(7) . . ? C23 Mo3 C26 103.1(6) . . ? C24 Mo3 C26 100.7(5) . . ? C23 Mo3 C25 66.5(7) . . ? C24 Mo3 C25 106.3(4) . . ? C26 Mo3 C25 38.3(3) . . ? C23 Mo3 C27 110.2(6) . . ? C24 Mo3 C27 67.5(5) . . ? C26 Mo3 C27 35.5(3) . . ? C25 Mo3 C27 63.8(4) . . ? C23 Mo3 Cl2 89.2(5) . . ? C24 Mo3 Cl2 92.4(3) . . ? C26 Mo3 Cl2 162.9(3) . . ? C25 Mo3 Cl2 146.6(4) . . ? C27 Mo3 Cl2 149.4(4) . . ? C23 Mo3 Cl1 167.3(5) . . ? C24 Mo3 Cl1 96.7(3) . . ? C26 Mo3 Cl1 89.4(3) . . ? C25 Mo3 Cl1 125.1(4) . . ? C27 Mo3 Cl1 81.4(3) . . ? Cl2 Mo3 Cl1 78.13(7) . . ? C23 Mo3 Cl3 100.5(6) . . ? C24 Mo3 Cl3 170.7(3) . . ? C26 Mo3 Cl3 86.7(4) . . ? C25 Mo3 Cl3 83.0(3) . . ? C27 Mo3 Cl3 118.1(4) . . ? Cl2 Mo3 Cl3 79.29(8) . . ? Cl1 Mo3 Cl3 77.52(8) . . ? O23 C23 Mo3 164(2) . . ? O24 C24 Mo3 177.2(12) . . ? C26 C25 Mo3 66.1(7) . . ? C26 C25 H25A 117.1 . . ? Mo3 C25 H25A 117.1 . . ? C26 C25 H25B 117.1 . . ? Mo3 C25 H25B 117.1 . . ? H25A C25 H25B 114.1 . . ? C27 C26 C25 118.6(9) . . ? C27 C26 Mo3 79.3(10) . . ? C25 C26 Mo3 75.6(8) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? Mo3 C26 H26 115.1 . . ? C26 C27 Mo3 65.2(9) . . ? C26 C27 H27A 117.2 . . ? Mo3 C27 H27A 117.2 . . ? C26 C27 H27B 117.2 . . ? Mo3 C27 H27B 117.2 . . ? H27A C27 H27B 114.3 . . ? C2 Mo1 C1 80.0(11) . . ? C2 Mo1 N1 178.5(4) . . ? C1 Mo1 N1 100.3(11) . . ? C2 Mo1 C5 98.0(5) . . ? C1 Mo1 C5 60.3(10) . . ? N1 Mo1 C5 83.4(4) . . ? C2 Mo1 C4 84.7(6) . . ? C1 Mo1 C4 89.4(10) . . ? N1 Mo1 C4 96.8(6) . . ? C5 Mo1 C4 35.2(3) . . ? C2 Mo1 C3 94.8(6) . . ? C1 Mo1 C3 123.0(10) . . ? N1 Mo1 C3 86.3(5) . . ? C5 Mo1 C3 64.6(3) . . ? C4 Mo1 C3 33.8(3) . . ? C2 Mo1 P1 86.8(4) . . ? C1 Mo1 P1 90.3(10) . . ? N1 Mo1 P1 91.7(2) . . ? C5 Mo1 P1 148.4(4) . . ? C4 Mo1 P1 171.4(5) . . ? C3 Mo1 P1 146.5(3) . . ? C2 Mo1 P2 87.8(5) . . ? C1 Mo1 P2 154.4(10) . . ? N1 Mo1 P2 91.4(2) . . ? C5 Mo1 P2 144.5(4) . . ? C4 Mo1 P2 111.9(4) . . ? C3 Mo1 P2 80.1(3) . . ? P1 Mo1 P2 66.48(9) . . ? O2 C2 Mo1 176.5(12) . . ? C3 C4 C5 126.8(13) . . ? C3 C4 Mo1 73.8(10) . . ? C5 C4 Mo1 69.0(9) . . ? C3 C4 H4 116.6 . . ? C5 C4 H4 116.6 . . ? Mo1 C4 H4 135.4 . . ? C4 C3 Mo1 72.3(10) . . ? C4 C3 H3A 116.3 . . ? Mo1 C3 H3A 116.3 . . ? C4 C3 H3B 116.3 . . ? Mo1 C3 H3B 116.3 . . ? H3A C3 H3B 113.3 . . ? C4 C5 Mo1 75.9(10) . . ? C4 C5 H5A 115.9 . . ? Mo1 C5 H5A 115.9 . . ? C4 C5 H5B 115.9 . . ? Mo1 C5 H5B 115.9 . . ? H5A C5 H5B 112.9 . . ? C7 P1 C10 106.8(5) . . ? C7 P1 C14 105.8(5) . . ? C10 P1 C14 104.0(6) . . ? C7 P1 Mo1 95.9(3) . . ? C10 P1 Mo1 121.7(4) . . ? C14 P1 Mo1 120.4(4) . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P2 C7 P1 97.4(5) . . ? P2 C7 H7A 112.3 . . ? P1 C7 H7A 112.3 . . ? P2 C7 H7B 112.3 . . ? P1 C7 H7B 112.3 . . ? H7A C7 H7B 109.9 . . ? C7 P2 C8 106.5(5) . . ? C7 P2 C9 105.0(5) . . ? C8 P2 C9 105.4(7) . . ? C7 P2 Mo1 96.0(4) . . ? C8 P2 Mo1 122.2(5) . . ? C9 P2 Mo1 119.2(4) . . ? P2 C8 H8A 109.5 . . ? P2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? P2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 N1 Mo1 176.9(9) . . ? N1 C11 C12 178.2(12) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C1 Mo1 121(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C22 Mo2 C21 O21 24(11) . . . . ? C18 Mo2 C21 O21 125(11) . . . . ? C20 Mo2 C21 O21 87(11) . . . . ? C19 Mo2 C21 O21 137(11) . . . . ? Cl1 Mo2 C21 O21 -67(11) . . . . ? Cl3 Mo2 C21 O21 -69(12) . . . . ? Cl2 Mo2 C21 O21 -144(11) . . . . ? C21 Mo2 C22 O22 -29(13) . . . . ? C18 Mo2 C22 O22 -131(13) . . . . ? C20 Mo2 C22 O22 -143(13) . . . . ? C19 Mo2 C22 O22 -94(13) . . . . ? Cl1 Mo2 C22 O22 61(13) . . . . ? Cl3 Mo2 C22 O22 139(13) . . . . ? Cl2 Mo2 C22 O22 58(13) . . . . ? C21 Mo2 C18 C19 19.7(8) . . . . ? C22 Mo2 C18 C19 102.9(7) . . . . ? C20 Mo2 C18 C19 120.9(11) . . . . ? Cl1 Mo2 C18 C19 -121.5(11) . . . . ? Cl3 Mo2 C18 C19 -157.5(7) . . . . ? Cl2 Mo2 C18 C19 -79.2(7) . . . . ? C21 Mo2 C18 C20 -101.3(8) . . . . ? C22 Mo2 C18 C20 -18.1(8) . . . . ? C19 Mo2 C18 C20 -120.9(11) . . . . ? Cl1 Mo2 C18 C20 117.5(10) . . . . ? Cl3 Mo2 C18 C20 81.6(7) . . . . ? Cl2 Mo2 C18 C20 159.9(7) . . . . ? C20 C18 C19 Mo2 67.6(9) . . . . ? C21 Mo2 C19 C18 -159.8(8) . . . . ? C22 Mo2 C19 C18 -87.6(8) . . . . ? C20 Mo2 C19 C18 -35.2(7) . . . . ? Cl1 Mo2 C19 C18 148.0(6) . . . . ? Cl3 Mo2 C19 C18 26.3(8) . . . . ? Cl2 Mo2 C19 C18 97.9(7) . . . . ? C19 C18 C20 Mo2 -67.8(9) . . . . ? C21 Mo2 C20 C18 89.8(8) . . . . ? C22 Mo2 C20 C18 161.1(9) . . . . ? C19 Mo2 C20 C18 35.0(7) . . . . ? Cl1 Mo2 C20 C18 -148.0(7) . . . . ? Cl3 Mo2 C20 C18 -95.0(8) . . . . ? Cl2 Mo2 C20 C18 -24.0(9) . . . . ? C21 Mo2 Cl1 Mo3 -138.8(3) . . . . ? C22 Mo2 Cl1 Mo3 141.0(3) . . . . ? C18 Mo2 Cl1 Mo3 3.9(11) . . . . ? C20 Mo2 Cl1 Mo3 94.7(6) . . . . ? C19 Mo2 Cl1 Mo3 -90.6(6) . . . . ? Cl3 Mo2 Cl1 Mo3 40.66(7) . . . . ? Cl2 Mo2 Cl1 Mo3 -39.61(7) . . . . ? C21 Mo2 Cl2 Mo3 128.2(3) . . . . ? C22 Mo2 Cl2 Mo3 43.1(13) . . . . ? C18 Mo2 Cl2 Mo3 -127.3(4) . . . . ? C20 Mo2 Cl2 Mo3 -113.3(4) . . . . ? C19 Mo2 Cl2 Mo3 -163.1(3) . . . . ? Cl1 Mo2 Cl2 Mo3 40.21(7) . . . . ? Cl3 Mo2 Cl2 Mo3 -40.15(8) . . . . ? C21 Mo2 Cl3 Mo3 -37.7(14) . . . . ? C22 Mo2 Cl3 Mo3 -128.4(4) . . . . ? C18 Mo2 Cl3 Mo3 128.6(3) . . . . ? C20 Mo2 Cl3 Mo3 164.9(3) . . . . ? C19 Mo2 Cl3 Mo3 113.5(3) . . . . ? Cl1 Mo2 Cl3 Mo3 -40.53(7) . . . . ? Cl2 Mo2 Cl3 Mo3 39.43(8) . . . . ? Mo2 Cl2 Mo3 C23 140.9(7) . . . . ? Mo2 Cl2 Mo3 C24 -135.7(3) . . . . ? Mo2 Cl2 Mo3 C26 4.6(14) . . . . ? Mo2 Cl2 Mo3 C25 99.2(7) . . . . ? Mo2 Cl2 Mo3 C27 -88.5(7) . . . . ? Mo2 Cl2 Mo3 Cl1 -39.31(7) . . . . ? Mo2 Cl2 Mo3 Cl3 40.04(8) . . . . ? Mo2 Cl1 Mo3 C23 41(3) . . . . ? Mo2 Cl1 Mo3 C24 131.7(4) . . . . ? Mo2 Cl1 Mo3 C26 -127.6(4) . . . . ? Mo2 Cl1 Mo3 C25 -112.9(4) . . . . ? Mo2 Cl1 Mo3 C27 -162.3(4) . . . . ? Mo2 Cl1 Mo3 Cl2 40.62(7) . . . . ? Mo2 Cl1 Mo3 Cl3 -40.87(8) . . . . ? Mo2 Cl3 Mo3 C23 -127.4(5) . . . . ? Mo2 Cl3 Mo3 C24 -13(2) . . . . ? Mo2 Cl3 Mo3 C26 129.9(4) . . . . ? Mo2 Cl3 Mo3 C25 168.2(4) . . . . ? Mo2 Cl3 Mo3 C27 112.9(4) . . . . ? Mo2 Cl3 Mo3 Cl2 -40.28(8) . . . . ? Mo2 Cl3 Mo3 Cl1 39.79(7) . . . . ? C24 Mo3 C23 O23 -23(6) . . . . ? C26 Mo3 C23 O23 -123(6) . . . . ? C25 Mo3 C23 O23 -134(6) . . . . ? C27 Mo3 C23 O23 -87(6) . . . . ? Cl2 Mo3 C23 O23 69(6) . . . . ? Cl1 Mo3 C23 O23 68(7) . . . . ? Cl3 Mo3 C23 O23 148(6) . . . . ? C23 Mo3 C24 O24 29(19) . . . . ? C26 Mo3 C24 O24 131(19) . . . . ? C25 Mo3 C24 O24 92(19) . . . . ? C27 Mo3 C24 O24 144(19) . . . . ? Cl2 Mo3 C24 O24 -60(19) . . . . ? Cl1 Mo3 C24 O24 -139(19) . . . . ? Cl3 Mo3 C24 O24 -87(19) . . . . ? C23 Mo3 C25 C26 161.9(10) . . . . ? C24 Mo3 C25 C26 86.7(8) . . . . ? C27 Mo3 C25 C26 32.6(6) . . . . ? Cl2 Mo3 C25 C26 -151.7(6) . . . . ? Cl1 Mo3 C25 C26 -24.1(8) . . . . ? Cl3 Mo3 C25 C26 -93.5(7) . . . . ? Mo3 C25 C26 C27 -69.0(14) . . . . ? C23 Mo3 C26 C27 106.4(10) . . . . ? C24 Mo3 C26 C27 20.7(9) . . . . ? C25 Mo3 C26 C27 123.5(10) . . . . ? Cl2 Mo3 C26 C27 -118.8(13) . . . . ? Cl1 Mo3 C26 C27 -76.0(7) . . . . ? Cl3 Mo3 C26 C27 -153.6(8) . . . . ? C23 Mo3 C26 C25 -17.0(10) . . . . ? C24 Mo3 C26 C25 -102.8(8) . . . . ? C27 Mo3 C26 C25 -123.5(10) . . . . ? Cl2 Mo3 C26 C25 117.8(12) . . . . ? Cl1 Mo3 C26 C25 160.5(7) . . . . ? Cl3 Mo3 C26 C25 83.0(7) . . . . ? C25 C26 C27 Mo3 67.0(13) . . . . ? C23 Mo3 C27 C26 -84.4(11) . . . . ? C24 Mo3 C27 C26 -158.0(9) . . . . ? C25 Mo3 C27 C26 -35.2(7) . . . . ? Cl2 Mo3 C27 C26 149.5(6) . . . . ? Cl1 Mo3 C27 C26 101.1(8) . . . . ? Cl3 Mo3 C27 C26 30.2(8) . . . . ? C1 Mo1 C2 O2 124(29) . . . . ? N1 Mo1 C2 O2 22(49) . . . . ? C5 Mo1 C2 O2 -178(100) . . . . ? C4 Mo1 C2 O2 -145(29) . . . . ? C3 Mo1 C2 O2 -113(29) . . . . ? P1 Mo1 C2 O2 33(29) . . . . ? P2 Mo1 C2 O2 -33(29) . . . . ? C2 Mo1 C4 C3 106.8(12) . . . . ? C1 Mo1 C4 C3 -173.2(15) . . . . ? N1 Mo1 C4 C3 -72.9(11) . . . . ? C5 Mo1 C4 C3 -141.2(17) . . . . ? P1 Mo1 C4 C3 98(3) . . . . ? P2 Mo1 C4 C3 21.3(12) . . . . ? C2 Mo1 C4 C5 -112.0(11) . . . . ? C1 Mo1 C4 C5 -32.0(14) . . . . ? N1 Mo1 C4 C5 68.3(10) . . . . ? C3 Mo1 C4 C5 141.2(17) . . . . ? P1 Mo1 C4 C5 -120(3) . . . . ? P2 Mo1 C4 C5 162.5(8) . . . . ? C5 C4 C3 Mo1 -47(2) . . . . ? C2 Mo1 C3 C4 -73.1(12) . . . . ? C1 Mo1 C3 C4 8.1(18) . . . . ? N1 Mo1 C3 C4 108.0(11) . . . . ? C5 Mo1 C3 C4 23.5(10) . . . . ? P1 Mo1 C3 C4 -164.5(9) . . . . ? P2 Mo1 C3 C4 -160.0(11) . . . . ? C3 C4 C5 Mo1 49(2) . . . . ? C2 Mo1 C5 C4 68.8(12) . . . . ? C1 Mo1 C5 C4 142.4(17) . . . . ? N1 Mo1 C5 C4 -111.8(11) . . . . ? C3 Mo1 C5 C4 -22.7(10) . . . . ? P1 Mo1 C5 C4 165.8(9) . . . . ? P2 Mo1 C5 C4 -28.7(14) . . . . ? C2 Mo1 P1 C7 -75.3(6) . . . . ? C1 Mo1 P1 C7 -155.3(11) . . . . ? N1 Mo1 P1 C7 104.4(4) . . . . ? C5 Mo1 P1 C7 -175.4(8) . . . . ? C4 Mo1 P1 C7 -67(3) . . . . ? C3 Mo1 P1 C7 18.5(8) . . . . ? P2 Mo1 P1 C7 13.7(3) . . . . ? C2 Mo1 P1 C10 38.7(8) . . . . ? C1 Mo1 P1 C10 -41.3(12) . . . . ? N1 Mo1 P1 C10 -141.6(6) . . . . ? C5 Mo1 P1 C10 -61.5(9) . . . . ? C4 Mo1 P1 C10 47(3) . . . . ? C3 Mo1 P1 C10 132.5(9) . . . . ? P2 Mo1 P1 C10 127.6(5) . . . . ? C2 Mo1 P1 C14 172.4(7) . . . . ? C1 Mo1 P1 C14 92.5(11) . . . . ? N1 Mo1 P1 C14 -7.9(5) . . . . ? C5 Mo1 P1 C14 72.3(9) . . . . ? C4 Mo1 P1 C14 -179(83) . . . . ? C3 Mo1 P1 C14 -93.8(9) . . . . ? P2 Mo1 P1 C14 -98.6(5) . . . . ? C10 P1 C7 P2 -143.1(5) . . . . ? C14 P1 C7 P2 106.5(5) . . . . ? Mo1 P1 C7 P2 -17.4(4) . . . . ? P1 C7 P2 C8 143.5(7) . . . . ? P1 C7 P2 C9 -104.9(5) . . . . ? P1 C7 P2 Mo1 17.4(4) . . . . ? C2 Mo1 P2 C7 73.8(5) . . . . ? C1 Mo1 P2 C7 13(2) . . . . ? N1 Mo1 P2 C7 -104.9(4) . . . . ? C5 Mo1 P2 C7 174.5(7) . . . . ? C4 Mo1 P2 C7 157.2(6) . . . . ? C3 Mo1 P2 C7 169.0(5) . . . . ? P1 Mo1 P2 C7 -13.7(3) . . . . ? C2 Mo1 P2 C8 -40.0(7) . . . . ? C1 Mo1 P2 C8 -101(2) . . . . ? N1 Mo1 P2 C8 141.2(6) . . . . ? C5 Mo1 P2 C8 60.7(9) . . . . ? C4 Mo1 P2 C8 43.3(8) . . . . ? C3 Mo1 P2 C8 55.2(7) . . . . ? P1 Mo1 P2 C8 -127.5(6) . . . . ? C2 Mo1 P2 C9 -175.3(6) . . . . ? C1 Mo1 P2 C9 124(2) . . . . ? N1 Mo1 P2 C9 5.9(5) . . . . ? C5 Mo1 P2 C9 -74.7(8) . . . . ? C4 Mo1 P2 C9 -92.0(8) . . . . ? C3 Mo1 P2 C9 -80.1(6) . . . . ? P1 Mo1 P2 C9 97.2(5) . . . . ? C2 Mo1 N1 C11 121(26) . . . . ? C1 Mo1 N1 C11 19(17) . . . . ? C5 Mo1 N1 C11 -39(17) . . . . ? C4 Mo1 N1 C11 -71(17) . . . . ? C3 Mo1 N1 C11 -104(17) . . . . ? P1 Mo1 N1 C11 110(17) . . . . ? P2 Mo1 N1 C11 176(17) . . . . ? Mo1 N1 C11 C12 24(58) . . . . ? C2 Mo1 C1 O1 -127(3) . . . . ? N1 Mo1 C1 O1 51(3) . . . . ? C5 Mo1 C1 O1 128(4) . . . . ? C4 Mo1 C1 O1 148(3) . . . . ? C3 Mo1 C1 O1 144(3) . . . . ? P1 Mo1 C1 O1 -40(3) . . . . ? P2 Mo1 C1 O1 -65(4) . . . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 68.18 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 1.472 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.193 #==END #========================================================================== data_5 _database_code_CSD 196134 #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Cl2 Mo2 O9 P2' _chemical_formula_sum 'C18 H30 Cl2 Mo2 O9 P2' _chemical_formula_weight 715.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.050(7) _cell_length_b 11.580(9) _cell_length_c 23.320(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.82(3) _cell_angle_gamma 90.00 _cell_volume 2689(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 10.981 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.102 _exptl_absorpt_correction_T_max 0.193 _exptl_absorpt_process_details 'XABS (Parkin, Moezzi & Hope, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.01 _diffrn_orient_matrix_UB_12 0 _diffrn_orient_matrix_UB_13 0 _diffrn_orient_matrix_UB_21 0 _diffrn_orient_matrix_UB_22 0.01 _diffrn_orient_matrix_UB_23 0 _diffrn_orient_matrix_UB_31 0 _diffrn_orient_matrix_UB_32 0 _diffrn_orient_matrix_UB_33 0.01 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3961 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 68.24 _reflns_number_total 3961 _reflns_number_gt 2992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3961 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0808 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1726 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.19567(6) 0.05618(6) 0.31451(3) 0.0141(3) Uani 1 1 d . . . Mo2 Mo 0.33247(6) 0.29203(6) 0.43244(3) 0.0135(3) Uani 1 1 d . . . Cl1 Cl 0.2726(2) 0.07406(17) 0.42483(8) 0.0185(5) Uani 1 1 d . . . Cl2 Cl 0.2641(2) 0.27168(18) 0.32181(8) 0.0206(5) Uani 1 1 d . . . C1 C 0.1189(9) -0.0963(8) 0.3135(4) 0.020(2) Uani 1 1 d . . . O1 O 0.0706(7) -0.1866(6) 0.3123(3) 0.0381(18) Uani 1 1 d . . . C2 C 0.0940(12) 0.0515(9) 0.2379(4) 0.041(3) Uani 1 1 d . . . O2 O 0.0246(9) 0.0461(7) 0.1935(3) 0.062(3) Uani 1 1 d . . . C11 C 0.3373(12) 0.0552(9) 0.2434(5) 0.054(4) Uani 1 1 d . . . H11A H 0.3229 -0.0053 0.2145 0.065 Uiso 1 1 calc R . . H11B H 0.3598 0.1295 0.2282 0.065 Uiso 1 1 calc R . . C12 C 0.4040(9) 0.0244(10) 0.2972(5) 0.040(3) Uani 1 1 d . . . H12 H 0.4706 0.0713 0.3166 0.047 Uiso 1 1 calc R . . C13 C 0.3684(10) -0.0780(9) 0.3210(4) 0.038(3) Uani 1 1 d . . . H13A H 0.4125 -0.0964 0.3595 0.046 Uiso 1 1 calc R . . H13B H 0.3554 -0.1441 0.2953 0.046 Uiso 1 1 calc R . . C3 C 0.3438(9) 0.4596(9) 0.4336(4) 0.029(2) Uani 1 1 d . . . O3 O 0.3454(7) 0.5598(6) 0.4363(3) 0.0408(19) Uani 1 1 d . . . C4 C 0.3405(8) 0.3228(7) 0.5153(4) 0.020(2) Uani 1 1 d . . . O4 O 0.3433(6) 0.3481(6) 0.5630(3) 0.0351(17) Uani 1 1 d . . . C21 C 0.5285(9) 0.2162(9) 0.4829(4) 0.033(2) Uani 1 1 d . . . H21A H 0.5792 0.2660 0.5114 0.039 Uiso 1 1 calc R . . H21B H 0.5258 0.1361 0.4949 0.039 Uiso 1 1 calc R . . C22 C 0.5414(8) 0.2369(8) 0.4243(4) 0.0223(19) Uani 1 1 d . . . H22 H 0.5520 0.1760 0.3993 0.027 Uiso 1 1 calc R . . C23 C 0.5380(8) 0.3483(8) 0.4051(4) 0.0238(19) Uiso 1 1 d . . . H23A H 0.5406 0.3599 0.3641 0.029 Uiso 1 1 calc R . . H23B H 0.5900 0.4043 0.4297 0.029 Uiso 1 1 calc R . . O5 O -0.0210(5) 0.2266(5) 0.3929(2) 0.0190(14) Uani 1 1 d . . . P1 P -0.0182(2) 0.12600(18) 0.34500(9) 0.0138(5) Uani 1 1 d . . . O6 O -0.0936(5) 0.0248(5) 0.3714(2) 0.0162(13) Uani 1 1 d . . . C61 C -0.2286(9) 0.0387(8) 0.3880(4) 0.028(2) Uani 1 1 d . . . H61A H -0.2921 0.0572 0.3541 0.034 Uiso 1 1 calc R . . H61B H -0.2286 0.1016 0.4155 0.034 Uiso 1 1 calc R . . C62 C -0.2691(9) -0.0698(9) 0.4144(4) 0.034(3) Uani 1 1 d . . . H62A H -0.3571 -0.0607 0.4254 0.051 Uiso 1 1 calc R . . H62B H -0.2062 -0.0877 0.4479 0.051 Uiso 1 1 calc R . . H62C H -0.2704 -0.1315 0.3868 0.051 Uiso 1 1 calc R . . O7 O -0.1346(5) 0.1720(5) 0.2967(2) 0.0241(15) Uani 1 1 d . . . C71 C -0.1157(10) 0.2749(9) 0.2636(4) 0.035(3) Uani 1 1 d . . . H71A H -0.0801 0.2542 0.2283 0.043 Uiso 1 1 calc R . . H71B H -0.0521 0.3260 0.2860 0.043 Uiso 1 1 calc R . . C72 C -0.2473(10) 0.3344(9) 0.2491(4) 0.039(3) Uani 1 1 d . . . H72A H -0.2354 0.4033 0.2274 0.058 Uiso 1 1 calc R . . H72B H -0.2820 0.3545 0.2841 0.058 Uiso 1 1 calc R . . H72C H -0.3094 0.2839 0.2264 0.058 Uiso 1 1 calc R . . P2 P 0.0852(2) 0.31448(19) 0.42849(9) 0.0144(5) Uani 1 1 d . . . O8 O 0.0413(5) 0.3083(6) 0.4907(2) 0.0292(16) Uani 1 1 d . . . C81 C -0.0941(9) 0.2894(8) 0.5052(4) 0.026(2) Uani 1 1 d . . . H81A H -0.1578 0.2868 0.4700 0.032 Uiso 1 1 calc R . . H81B H -0.1189 0.3529 0.5287 0.032 Uiso 1 1 calc R . . C82 C -0.0992(11) 0.1800(9) 0.5371(5) 0.051(3) Uani 1 1 d . . . H82A H -0.1883 0.1685 0.5465 0.077 Uiso 1 1 calc R . . H82B H -0.0367 0.1831 0.5721 0.077 Uiso 1 1 calc R . . H82C H -0.0759 0.1172 0.5135 0.077 Uiso 1 1 calc R . . O9 O 0.0355(6) 0.4340(5) 0.4007(3) 0.0273(16) Uani 1 1 d . . . C91 C -0.1006(8) 0.4773(8) 0.3946(4) 0.024(2) Uani 1 1 d . . . H91A H -0.1208 0.5059 0.4315 0.028 Uiso 1 1 calc R . . H91B H -0.1632 0.4155 0.3821 0.028 Uiso 1 1 calc R . . C92 C -0.1152(9) 0.5722(8) 0.3511(4) 0.030(2) Uani 1 1 d . . . H92A H -0.2054 0.6013 0.3468 0.045 Uiso 1 1 calc R . . H92B H -0.0957 0.5433 0.3146 0.045 Uiso 1 1 calc R . . H92C H -0.0537 0.6334 0.3639 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0166(5) 0.0130(4) 0.0129(4) -0.0044(3) 0.0031(3) -0.0005(3) Mo2 0.0117(4) 0.0127(4) 0.0160(4) -0.0043(3) 0.0016(3) -0.0010(3) Cl1 0.0237(12) 0.0137(12) 0.0179(11) 0.0001(8) 0.0028(9) 0.0005(9) Cl2 0.0273(13) 0.0190(12) 0.0154(11) 0.0002(9) 0.0030(9) -0.0022(9) C1 0.025(5) 0.010(5) 0.027(5) -0.008(4) 0.006(4) 0.003(4) O1 0.046(5) 0.019(4) 0.052(5) -0.010(3) 0.020(4) -0.012(3) C2 0.063(8) 0.039(7) 0.020(6) 0.005(5) 0.007(6) 0.021(6) O2 0.096(7) 0.059(6) 0.025(5) -0.014(4) -0.013(5) 0.037(5) C11 0.086(9) 0.026(7) 0.066(9) -0.015(6) 0.068(8) -0.015(6) C12 0.012(5) 0.044(8) 0.068(9) -0.039(6) 0.025(5) -0.011(5) C13 0.035(6) 0.042(7) 0.034(6) -0.031(5) -0.005(5) 0.023(5) C3 0.020(6) 0.038(7) 0.028(6) -0.005(5) 0.006(4) -0.009(5) O3 0.047(5) 0.008(4) 0.067(5) -0.008(3) 0.005(4) -0.008(3) C4 0.011(5) 0.024(5) 0.026(5) -0.012(4) 0.005(4) -0.005(4) O4 0.033(4) 0.053(5) 0.020(4) -0.017(3) 0.005(3) -0.007(3) C21 0.0238(19) 0.033(6) 0.037(6) -0.002(5) -0.010(5) 0.002(5) C22 0.0238(19) 0.017(5) 0.026(5) -0.007(4) 0.005(4) 0.006(4) O5 0.009(3) 0.024(4) 0.024(3) -0.009(3) 0.001(3) 0.002(3) P1 0.0128(12) 0.0132(12) 0.0150(12) -0.0027(9) 0.0000(9) 0.0000(9) O6 0.011(3) 0.016(3) 0.023(3) 0.003(3) 0.004(2) 0.000(2) C61 0.016(5) 0.031(6) 0.039(6) -0.006(5) 0.007(4) 0.001(4) C62 0.021(5) 0.052(7) 0.031(6) 0.019(5) 0.009(5) -0.007(5) O7 0.015(3) 0.031(4) 0.024(4) 0.009(3) -0.003(3) 0.003(3) C71 0.039(6) 0.040(7) 0.028(6) 0.003(5) 0.004(5) 0.009(5) C72 0.046(7) 0.036(7) 0.031(6) 0.000(5) -0.008(5) 0.009(5) P2 0.0107(12) 0.0162(13) 0.0160(12) -0.0061(9) 0.0003(9) -0.0011(9) O8 0.010(3) 0.058(5) 0.018(3) -0.008(3) -0.002(3) -0.010(3) C81 0.024(5) 0.031(6) 0.025(5) -0.007(4) 0.007(4) -0.003(4) C82 0.038(7) 0.055(8) 0.057(8) 0.029(6) -0.009(6) -0.005(6) O9 0.020(4) 0.019(4) 0.042(4) 0.004(3) 0.001(3) -0.001(3) C91 0.019(5) 0.022(5) 0.029(5) 0.003(4) 0.000(4) 0.006(4) C92 0.022(5) 0.024(6) 0.045(6) -0.001(5) 0.010(5) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.926(9) . ? Mo1 C2 1.934(11) . ? Mo1 C12 2.216(8) . ? Mo1 C13 2.319(9) . ? Mo1 C11 2.327(9) . ? Mo1 P1 2.489(2) . ? Mo1 Cl2 2.588(3) . ? Mo1 Cl1 2.592(2) . ? Mo2 C3 1.944(11) . ? Mo2 C4 1.956(9) . ? Mo2 C22 2.227(8) . ? Mo2 C21 2.326(9) . ? Mo2 C23 2.335(8) . ? Mo2 P2 2.488(3) . ? Mo2 Cl2 2.589(2) . ? Mo2 Cl1 2.595(3) . ? C1 O1 1.151(10) . ? C2 O2 1.170(12) . ? C11 C12 1.386(15) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.376(14) . ? C12 H12 0.9300 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C3 O3 1.162(11) . ? C4 O4 1.146(10) . ? C21 C22 1.411(12) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.364(12) . ? C22 H22 0.9300 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? O5 P1 1.616(6) . ? O5 P2 1.620(6) . ? P1 O6 1.566(6) . ? P1 O7 1.600(6) . ? O6 C61 1.469(9) . ? C61 C62 1.480(12) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? O7 C71 1.446(11) . ? C71 C72 1.489(13) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? P2 O8 1.574(6) . ? P2 O9 1.581(6) . ? O8 C81 1.463(10) . ? C81 C82 1.474(13) . ? C81 H81A 0.9700 . ? C81 H81B 0.9700 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? O9 C91 1.445(10) . ? C91 C92 1.490(12) . ? C91 H91A 0.9700 . ? C91 H91B 0.9700 . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo1 C2 78.6(4) . . ? C1 Mo1 C12 103.4(4) . . ? C2 Mo1 C12 102.7(4) . . ? C1 Mo1 C13 71.4(4) . . ? C2 Mo1 C13 109.8(4) . . ? C12 Mo1 C13 35.2(4) . . ? C1 Mo1 C11 105.6(4) . . ? C2 Mo1 C11 68.9(5) . . ? C12 Mo1 C11 35.4(4) . . ? C13 Mo1 C11 61.2(4) . . ? C1 Mo1 P1 86.6(3) . . ? C2 Mo1 P1 84.5(3) . . ? C12 Mo1 P1 168.5(3) . . ? C13 Mo1 P1 150.1(3) . . ? C11 Mo1 P1 147.2(3) . . ? C1 Mo1 Cl2 170.9(2) . . ? C2 Mo1 Cl2 101.0(3) . . ? C12 Mo1 Cl2 85.6(3) . . ? C13 Mo1 Cl2 116.9(3) . . ? C11 Mo1 Cl2 82.5(3) . . ? P1 Mo1 Cl2 84.27(8) . . ? C1 Mo1 Cl1 98.6(3) . . ? C2 Mo1 Cl1 165.4(3) . . ? C12 Mo1 Cl1 91.9(3) . . ? C13 Mo1 Cl1 82.5(2) . . ? C11 Mo1 Cl1 125.4(4) . . ? P1 Mo1 Cl1 80.96(7) . . ? Cl2 Mo1 Cl1 79.45(6) . . ? C3 Mo2 C4 79.0(4) . . ? C3 Mo2 C22 103.5(3) . . ? C4 Mo2 C22 102.9(3) . . ? C3 Mo2 C21 109.0(4) . . ? C4 Mo2 C21 69.5(3) . . ? C22 Mo2 C21 36.0(3) . . ? C3 Mo2 C23 70.9(3) . . ? C4 Mo2 C23 107.4(3) . . ? C22 Mo2 C23 34.7(3) . . ? C21 Mo2 C23 61.6(3) . . ? C3 Mo2 P2 87.3(3) . . ? C4 Mo2 P2 85.7(2) . . ? C22 Mo2 P2 167.2(2) . . ? C21 Mo2 P2 146.2(2) . . ? C23 Mo2 P2 151.3(2) . . ? C3 Mo2 Cl2 96.4(3) . . ? C4 Mo2 Cl2 166.2(3) . . ? C22 Mo2 Cl2 90.8(2) . . ? C21 Mo2 Cl2 124.2(2) . . ? C23 Mo2 Cl2 83.0(2) . . ? P2 Mo2 Cl2 81.05(7) . . ? C3 Mo2 Cl1 169.9(3) . . ? C4 Mo2 Cl1 102.9(3) . . ? C22 Mo2 Cl1 85.9(2) . . ? C21 Mo2 Cl1 80.8(3) . . ? C23 Mo2 Cl1 117.3(2) . . ? P2 Mo2 Cl1 82.98(7) . . ? Cl2 Mo2 Cl1 79.38(7) . . ? Mo1 Cl1 Mo2 100.41(7) . . ? Mo1 Cl2 Mo2 100.69(7) . . ? O1 C1 Mo1 178.6(9) . . ? O2 C2 Mo1 175.0(10) . . ? C12 C11 Mo1 67.9(5) . . ? C12 C11 H11A 116.9 . . ? Mo1 C11 H11A 116.9 . . ? C12 C11 H11B 116.9 . . ? Mo1 C11 H11B 116.9 . . ? H11A C11 H11B 113.9 . . ? C13 C12 C11 117.8(9) . . ? C13 C12 Mo1 76.5(5) . . ? C11 C12 Mo1 76.7(6) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? Mo1 C12 H12 116.7 . . ? C12 C13 Mo1 68.3(5) . . ? C12 C13 H13A 116.8 . . ? Mo1 C13 H13A 116.8 . . ? C12 C13 H13B 116.8 . . ? Mo1 C13 H13B 116.8 . . ? H13A C13 H13B 113.9 . . ? O3 C3 Mo2 176.3(8) . . ? O4 C4 Mo2 175.6(8) . . ? C22 C21 Mo2 68.2(5) . . ? C22 C21 H21A 116.9 . . ? Mo2 C21 H21A 116.9 . . ? C22 C21 H21B 116.9 . . ? Mo2 C21 H21B 116.9 . . ? H21A C21 H21B 113.9 . . ? C23 C22 C21 118.5(8) . . ? C23 C22 Mo2 77.0(5) . . ? C21 C22 Mo2 75.8(5) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? Mo2 C22 H22 117.4 . . ? C22 C23 Mo2 68.3(5) . . ? C22 C23 H23A 116.8 . . ? Mo2 C23 H23A 116.8 . . ? C22 C23 H23B 116.8 . . ? Mo2 C23 H23B 116.8 . . ? H23A C23 H23B 113.9 . . ? P1 O5 P2 137.3(4) . . ? O6 P1 O7 100.4(3) . . ? O6 P1 O5 102.3(3) . . ? O7 P1 O5 99.6(3) . . ? O6 P1 Mo1 110.6(2) . . ? O7 P1 Mo1 118.9(2) . . ? O5 P1 Mo1 121.9(2) . . ? C61 O6 P1 122.4(5) . . ? O6 C61 C62 109.4(7) . . ? O6 C61 H61A 109.8 . . ? C62 C61 H61A 109.8 . . ? O6 C61 H61B 109.8 . . ? C62 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C71 O7 P1 120.9(6) . . ? O7 C71 C72 109.0(8) . . ? O7 C71 H71A 109.9 . . ? C72 C71 H71A 109.9 . . ? O7 C71 H71B 109.9 . . ? C72 C71 H71B 109.9 . . ? H71A C71 H71B 108.3 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O8 P2 O9 107.8(4) . . ? O8 P2 O5 101.3(3) . . ? O9 P2 O5 101.0(3) . . ? O8 P2 Mo2 111.4(2) . . ? O9 P2 Mo2 111.4(2) . . ? O5 P2 Mo2 122.6(2) . . ? C81 O8 P2 127.3(5) . . ? O8 C81 C82 110.1(8) . . ? O8 C81 H81A 109.7 . . ? C82 C81 H81A 109.7 . . ? O8 C81 H81B 109.7 . . ? C82 C81 H81B 109.7 . . ? H81A C81 H81B 108.2 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C91 O9 P2 125.9(5) . . ? O9 C91 C92 109.0(7) . . ? O9 C91 H91A 109.9 . . ? C92 C91 H91A 109.9 . . ? O9 C91 H91B 109.9 . . ? C92 C91 H91B 109.9 . . ? H91A C91 H91B 108.3 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Mo1 Cl1 Mo2 -168.9(3) . . . . ? C2 Mo1 Cl1 Mo2 -90.9(13) . . . . ? C12 Mo1 Cl1 Mo2 87.2(3) . . . . ? C13 Mo1 Cl1 Mo2 121.3(3) . . . . ? C11 Mo1 Cl1 Mo2 74.9(3) . . . . ? P1 Mo1 Cl1 Mo2 -83.75(8) . . . . ? Cl2 Mo1 Cl1 Mo2 2.05(6) . . . . ? C3 Mo2 Cl1 Mo1 64.3(15) . . . . ? C4 Mo2 Cl1 Mo1 164.0(3) . . . . ? C22 Mo2 Cl1 Mo1 -93.7(2) . . . . ? C21 Mo2 Cl1 Mo1 -129.6(2) . . . . ? C23 Mo2 Cl1 Mo1 -78.4(3) . . . . ? P2 Mo2 Cl1 Mo1 80.11(8) . . . . ? Cl2 Mo2 Cl1 Mo1 -2.05(6) . . . . ? C2 Mo1 Cl2 Mo2 163.1(3) . . . . ? C12 Mo1 Cl2 Mo2 -94.8(3) . . . . ? C13 Mo1 Cl2 Mo2 -78.0(3) . . . . ? C11 Mo1 Cl2 Mo2 -130.3(4) . . . . ? P1 Mo1 Cl2 Mo2 79.78(8) . . . . ? Cl1 Mo1 Cl2 Mo2 -2.06(6) . . . . ? C3 Mo2 Cl2 Mo1 -168.6(3) . . . . ? C4 Mo2 Cl2 Mo1 -98.8(11) . . . . ? C22 Mo2 Cl2 Mo1 87.7(2) . . . . ? C21 Mo2 Cl2 Mo1 73.1(3) . . . . ? C23 Mo2 Cl2 Mo1 121.6(2) . . . . ? P2 Mo2 Cl2 Mo1 -82.42(8) . . . . ? Cl1 Mo2 Cl2 Mo1 2.06(6) . . . . ? C1 Mo1 C11 C12 -91.3(7) . . . . ? C2 Mo1 C11 C12 -162.2(8) . . . . ? C13 Mo1 C11 C12 -33.4(6) . . . . ? P1 Mo1 C11 C12 159.9(5) . . . . ? Cl2 Mo1 C11 C12 93.0(6) . . . . ? Cl1 Mo1 C11 C12 21.7(7) . . . . ? Mo1 C11 C12 C13 66.6(7) . . . . ? C1 Mo1 C12 C13 -25.2(7) . . . . ? C2 Mo1 C12 C13 -106.3(7) . . . . ? C11 Mo1 C12 C13 -123.4(9) . . . . ? P1 Mo1 C12 C13 125.2(16) . . . . ? Cl2 Mo1 C12 C13 153.4(6) . . . . ? Cl1 Mo1 C12 C13 74.2(6) . . . . ? C1 Mo1 C12 C11 98.2(7) . . . . ? C2 Mo1 C12 C11 17.0(7) . . . . ? C13 Mo1 C12 C11 123.4(9) . . . . ? P1 Mo1 C12 C11 -111.4(16) . . . . ? Cl2 Mo1 C12 C11 -83.2(6) . . . . ? Cl1 Mo1 C12 C11 -162.5(6) . . . . ? C11 C12 C13 Mo1 -66.7(8) . . . . ? C1 Mo1 C13 C12 154.1(7) . . . . ? C2 Mo1 C13 C12 84.1(7) . . . . ? C11 Mo1 C13 C12 33.5(6) . . . . ? P1 Mo1 C13 C12 -160.9(5) . . . . ? Cl2 Mo1 C13 C12 -30.0(7) . . . . ? Cl1 Mo1 C13 C12 -104.1(6) . . . . ? C3 Mo2 C21 C22 -86.9(6) . . . . ? C4 Mo2 C21 C22 -156.8(6) . . . . ? C23 Mo2 C21 C22 -32.3(5) . . . . ? P2 Mo2 C21 C22 158.0(4) . . . . ? Cl2 Mo2 C21 C22 25.3(6) . . . . ? Cl1 Mo2 C21 C22 95.7(5) . . . . ? Mo2 C21 C22 C23 66.3(7) . . . . ? C3 Mo2 C22 C23 -20.4(6) . . . . ? C4 Mo2 C22 C23 -102.0(6) . . . . ? C21 Mo2 C22 C23 -124.3(8) . . . . ? P2 Mo2 C22 C23 126.5(10) . . . . ? Cl2 Mo2 C22 C23 76.4(5) . . . . ? Cl1 Mo2 C22 C23 155.7(5) . . . . ? C3 Mo2 C22 C21 103.9(6) . . . . ? C4 Mo2 C22 C21 22.3(6) . . . . ? C23 Mo2 C22 C21 124.3(8) . . . . ? P2 Mo2 C22 C21 -109.2(11) . . . . ? Cl2 Mo2 C22 C21 -159.3(5) . . . . ? Cl1 Mo2 C22 C21 -80.0(5) . . . . ? C21 C22 C23 Mo2 -65.6(7) . . . . ? C3 Mo2 C23 C22 158.9(6) . . . . ? C4 Mo2 C23 C22 87.6(6) . . . . ? C21 Mo2 C23 C22 33.5(5) . . . . ? P2 Mo2 C23 C22 -158.4(4) . . . . ? Cl2 Mo2 C23 C22 -101.7(5) . . . . ? Cl1 Mo2 C23 C22 -27.5(6) . . . . ? P2 O5 P1 O6 130.7(6) . . . . ? P2 O5 P1 O7 -126.4(6) . . . . ? P2 O5 P1 Mo1 6.7(7) . . . . ? C1 Mo1 P1 O6 20.6(3) . . . . ? C2 Mo1 P1 O6 99.5(4) . . . . ? C12 Mo1 P1 O6 -130.6(18) . . . . ? C13 Mo1 P1 O6 -21.5(6) . . . . ? C11 Mo1 P1 O6 134.6(6) . . . . ? Cl2 Mo1 P1 O6 -158.9(2) . . . . ? Cl1 Mo1 P1 O6 -78.7(2) . . . . ? C1 Mo1 P1 O7 -94.7(4) . . . . ? C2 Mo1 P1 O7 -15.9(4) . . . . ? C12 Mo1 P1 O7 114.0(18) . . . . ? C13 Mo1 P1 O7 -136.9(5) . . . . ? C11 Mo1 P1 O7 19.3(6) . . . . ? Cl2 Mo1 P1 O7 85.8(3) . . . . ? Cl1 Mo1 P1 O7 166.0(3) . . . . ? C1 Mo1 P1 O5 140.7(4) . . . . ? C2 Mo1 P1 O5 -140.4(4) . . . . ? C12 Mo1 P1 O5 -10.5(18) . . . . ? C13 Mo1 P1 O5 98.6(6) . . . . ? C11 Mo1 P1 O5 -105.3(6) . . . . ? Cl2 Mo1 P1 O5 -38.8(3) . . . . ? Cl1 Mo1 P1 O5 41.4(3) . . . . ? O7 P1 O6 C61 -47.6(7) . . . . ? O5 P1 O6 C61 54.7(7) . . . . ? Mo1 P1 O6 C61 -174.1(6) . . . . ? P1 O6 C61 C62 -177.0(6) . . . . ? O6 P1 O7 C71 174.1(6) . . . . ? O5 P1 O7 C71 69.6(7) . . . . ? Mo1 P1 O7 C71 -65.2(7) . . . . ? P1 O7 C71 C72 -148.0(7) . . . . ? P1 O5 P2 O8 -137.8(6) . . . . ? P1 O5 P2 O9 111.3(6) . . . . ? P1 O5 P2 Mo2 -13.1(7) . . . . ? C3 Mo2 P2 O8 -94.5(4) . . . . ? C4 Mo2 P2 O8 -15.3(4) . . . . ? C22 Mo2 P2 O8 117.6(11) . . . . ? C21 Mo2 P2 O8 26.6(5) . . . . ? C23 Mo2 P2 O8 -134.4(5) . . . . ? Cl2 Mo2 P2 O8 168.5(3) . . . . ? Cl1 Mo2 P2 O8 88.3(3) . . . . ? C3 Mo2 P2 O9 25.9(4) . . . . ? C4 Mo2 P2 O9 105.1(4) . . . . ? C22 Mo2 P2 O9 -122.0(11) . . . . ? C21 Mo2 P2 O9 146.9(5) . . . . ? C23 Mo2 P2 O9 -14.0(5) . . . . ? Cl2 Mo2 P2 O9 -71.1(3) . . . . ? Cl1 Mo2 P2 O9 -151.4(3) . . . . ? C3 Mo2 P2 O5 145.5(4) . . . . ? C4 Mo2 P2 O5 -135.4(4) . . . . ? C22 Mo2 P2 O5 -2.5(11) . . . . ? C21 Mo2 P2 O5 -93.5(5) . . . . ? C23 Mo2 P2 O5 105.6(5) . . . . ? Cl2 Mo2 P2 O5 48.5(3) . . . . ? Cl1 Mo2 P2 O5 -31.8(3) . . . . ? O9 P2 O8 C81 73.8(8) . . . . ? O5 P2 O8 C81 -31.7(8) . . . . ? Mo2 P2 O8 C81 -163.7(6) . . . . ? P2 O8 C81 C82 116.2(9) . . . . ? O8 P2 O9 C91 -54.1(7) . . . . ? O5 P2 O9 C91 51.7(7) . . . . ? Mo2 P2 O9 C91 -176.6(6) . . . . ? P2 O9 C91 C92 -162.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.805 _diffrn_reflns_theta_full 68.24 _diffrn_measured_fraction_theta_full 0.805 _refine_diff_density_max 1.723 _refine_diff_density_min -1.967 _refine_diff_density_rms 0.231 #==END #========================================================================== data_6 _database_code_CSD 196135 #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H35 Cl Mo O3 P2' _chemical_formula_sum 'C34 H35 Cl Mo O3 P2' _chemical_formula_weight 684.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.119(5) _cell_length_b 10.830(5) _cell_length_c 23.494(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.229(5) _cell_angle_gamma 90.00 _cell_volume 3218(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8452 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 70 _exptl_crystal_description prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 5.294 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.460 _exptl_absorpt_correction_T_max 0.651 _exptl_absorpt_process_details 'XABS (Parkin, Moezzi & Hope, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' # Orientation matrix from 'scale_all_nabs_3.out' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0339153 _diffrn_orient_matrix_UB_21 -0.0383669 _diffrn_orient_matrix_UB_31 -0.0425366 _diffrn_orient_matrix_UB_12 0.0192657 _diffrn_orient_matrix_UB_22 -0.0588777 _diffrn_orient_matrix_UB_32 0.0684670 _diffrn_orient_matrix_UB_13 -0.0392624 _diffrn_orient_matrix_UB_23 -0.0291683 _diffrn_orient_matrix_UB_33 -0.0140352 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11578 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 70.00 _reflns_number_total 6058 _reflns_number_gt 4952 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+1.5536P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6058 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.743126(17) 0.09532(2) 0.600413(11) 0.01835(9) Uani 1 1 d . . . P2 P 0.80360(6) 0.26237(7) 0.69426(4) 0.01946(17) Uani 1 1 d . . . Cl1 Cl 0.92377(6) 0.01406(7) 0.68994(4) 0.02973(18) Uani 1 1 d . . . P1 P 0.86265(6) 0.26351(7) 0.60264(4) 0.01902(17) Uani 1 1 d . . . C26 C 0.7796(3) 0.5008(3) 0.72933(16) 0.0265(7) Uani 1 1 d . . . H26 H 0.8452 0.4882 0.7694 0.032 Uiso 1 1 calc R . . C23 C 0.5833(2) 0.5386(3) 0.61045(16) 0.0281(7) Uani 1 1 d . . . H23 H 0.5173 0.5514 0.5707 0.034 Uiso 1 1 calc R . . O3 O 0.55011(17) 0.2157(2) 0.47240(11) 0.0324(5) Uani 1 1 d . . . C11' C 0.7990(2) 0.4008(3) 0.55079(15) 0.0211(6) Uani 1 1 d . . . C21 C 0.7332(2) 0.4065(3) 0.68149(15) 0.0200(6) Uani 1 1 d . . . O2 O 0.7190(2) -0.0682(2) 0.48274(12) 0.0399(6) Uani 1 1 d . . . C2 C 0.7304(2) -0.0090(3) 0.52741(16) 0.0271(7) Uani 1 1 d . . . C1 C 0.9168(2) 0.3099(3) 0.69075(14) 0.0229(6) Uani 1 1 d . . . H1A H 0.9298 0.3981 0.6975 0.027 Uiso 1 1 calc R . . H1B H 0.9807 0.2650 0.7229 0.027 Uiso 1 1 calc R . . C11 C 0.9759(2) 0.2375(3) 0.59612(14) 0.0217(6) Uani 1 1 d . . . C3 C 0.6224(2) 0.1732(3) 0.52156(16) 0.0246(7) Uani 1 1 d . . . O1 O 0.4593(2) 0.5324(2) 0.74945(13) 0.0481(7) Uani 1 1 d . . . C12 C 0.9960(3) 0.1209(3) 0.58075(16) 0.0288(7) Uani 1 1 d . . . H12 H 0.9506 0.0556 0.5728 0.035 Uiso 1 1 calc R . . C21' C 0.8505(2) 0.2257(3) 0.78197(15) 0.0223(6) Uani 1 1 d . . . C16 C 1.0448(2) 0.3347(3) 0.60768(15) 0.0274(7) Uani 1 1 d . . . H16 H 1.0318 0.4130 0.6178 0.033 Uiso 1 1 calc R . . C5 C 0.6748(3) -0.0169(3) 0.64650(16) 0.0276(7) Uani 1 1 d . . . H5 H 0.7114 -0.0162 0.6937 0.033 Uiso 1 1 calc R . . C22' C 0.9536(3) 0.2460(3) 0.83699(15) 0.0293(7) Uani 1 1 d . . . H22' H 1.0043 0.2763 0.8298 0.035 Uiso 1 1 calc R . . C14' C 0.6897(3) 0.6005(3) 0.46578(18) 0.0340(8) Uani 1 1 d . . . H14' H 0.6529 0.6672 0.4376 0.041 Uiso 1 1 calc R . . C22 C 0.6334(2) 0.4261(3) 0.62154(15) 0.0252(7) Uani 1 1 d . . . H22 H 0.6011 0.3634 0.5894 0.030 Uiso 1 1 calc R . . C26' C 0.7760(3) 0.1801(3) 0.79389(16) 0.0288(7) Uani 1 1 d . . . H26' H 0.7071 0.1658 0.7575 0.035 Uiso 1 1 calc R . . C15' C 0.7562(3) 0.6174(3) 0.53492(18) 0.0344(8) Uani 1 1 d . . . H15' H 0.7645 0.6959 0.5533 0.041 Uiso 1 1 calc R . . C12' C 0.7319(2) 0.3845(3) 0.48021(15) 0.0245(7) Uani 1 1 d . . . H12' H 0.7240 0.3064 0.4616 0.029 Uiso 1 1 calc R . . C13' C 0.6776(3) 0.4828(3) 0.43828(17) 0.0305(7) Uani 1 1 d . . . H13' H 0.6329 0.4708 0.3916 0.037 Uiso 1 1 calc R . . C16' C 0.8108(3) 0.5193(3) 0.57738(17) 0.0293(7) Uani 1 1 d . . . H16' H 0.8557 0.5321 0.6240 0.035 Uiso 1 1 calc R . . C24 C 0.6307(3) 0.6323(3) 0.65809(16) 0.0294(7) Uani 1 1 d . . . H24 H 0.5968 0.7080 0.6501 0.035 Uiso 1 1 calc R . . C15 C 1.1320(3) 0.3148(3) 0.60414(17) 0.0330(8) Uani 1 1 d . . . H15 H 1.1778 0.3796 0.6121 0.040 Uiso 1 1 calc R . . C4 C 0.6955(3) -0.1045(3) 0.61194(17) 0.0288(7) Uani 1 1 d . . . H4A H 0.6349 -0.1413 0.5718 0.035 Uiso 1 1 calc R . . H4B H 0.7527 -0.1621 0.6394 0.035 Uiso 1 1 calc R . . C13 C 1.0836(3) 0.1022(3) 0.57735(17) 0.0321(8) Uani 1 1 d . . . H13 H 1.0970 0.0241 0.5673 0.038 Uiso 1 1 calc R . . C6 C 0.5957(2) 0.0707(3) 0.60645(17) 0.0280(7) Uani 1 1 d . . . H6A H 0.5833 0.1341 0.6305 0.034 Uiso 1 1 calc R . . H6B H 0.5317 0.0404 0.5659 0.034 Uiso 1 1 calc R . . C25' C 0.8038(3) 0.1557(3) 0.85953(17) 0.0355(8) Uani 1 1 d . . . H25' H 0.7536 0.1255 0.8672 0.043 Uiso 1 1 calc R . . C8 C 0.6279(3) 0.4412(4) 0.8200(2) 0.0465(10) Uani 1 1 d . . . H8A H 0.6529 0.4199 0.7911 0.056 Uiso 1 1 calc R . . H8B H 0.6875 0.4440 0.8670 0.056 Uiso 1 1 calc R . . C23' C 0.9803(3) 0.2209(4) 0.90228(17) 0.0387(9) Uani 1 1 d . . . H23' H 1.0492 0.2342 0.9390 0.046 Uiso 1 1 calc R . . C14 C 1.1511(2) 0.1984(3) 0.58881(16) 0.0326(8) Uani 1 1 d . . . H14 H 1.2096 0.1851 0.5862 0.039 Uiso 1 1 calc R . . C25 C 0.7290(3) 0.6132(3) 0.71788(16) 0.0299(7) Uani 1 1 d . . . H25 H 0.7606 0.6758 0.7501 0.036 Uiso 1 1 calc R . . C7 C 0.5679(3) 0.5626(4) 0.7986(2) 0.0435(9) Uani 1 1 d . . . H7A H 0.5750 0.6040 0.8375 0.052 Uiso 1 1 calc R . . H7B H 0.5950 0.6167 0.7786 0.052 Uiso 1 1 calc R . . C9 C 0.5452(3) 0.3523(4) 0.8110(2) 0.0586(12) Uani 1 1 d . . . H9A H 0.5404 0.3519 0.8505 0.070 Uiso 1 1 calc R . . H9B H 0.5598 0.2692 0.8029 0.070 Uiso 1 1 calc R . . C10 C 0.4454(3) 0.4027(4) 0.7493(2) 0.0475(10) Uani 1 1 d . . . H10A H 0.4342 0.3663 0.7081 0.057 Uiso 1 1 calc R . . H10B H 0.3848 0.3841 0.7517 0.057 Uiso 1 1 calc R . . C24' C 0.9058(3) 0.1763(3) 0.91339(17) 0.0386(9) Uani 1 1 d . . . H24' H 0.9246 0.1599 0.9575 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01843(14) 0.01651(14) 0.01850(14) 0.00069(9) 0.00909(11) 0.00076(9) P2 0.0190(4) 0.0199(4) 0.0184(4) 0.0006(3) 0.0095(3) 0.0011(3) Cl1 0.0253(4) 0.0289(4) 0.0280(4) 0.0080(3) 0.0101(3) 0.0085(3) P1 0.0181(4) 0.0196(4) 0.0181(4) 0.0000(3) 0.0092(3) 0.0002(3) C26 0.0296(17) 0.0251(17) 0.0243(16) 0.0003(13) 0.0144(14) 0.0003(13) C23 0.0221(16) 0.0316(18) 0.0268(16) 0.0035(14) 0.0109(14) 0.0031(13) O3 0.0217(12) 0.0292(13) 0.0277(12) 0.0070(10) 0.0016(10) 0.0039(9) C11' 0.0200(15) 0.0206(15) 0.0248(15) 0.0002(12) 0.0137(13) -0.0003(11) C21 0.0261(16) 0.0177(15) 0.0231(15) 0.0018(12) 0.0178(13) 0.0001(12) O2 0.0535(16) 0.0373(14) 0.0338(13) -0.0132(11) 0.0270(12) -0.0017(12) C2 0.0211(16) 0.0267(17) 0.0280(17) 0.0046(14) 0.0099(14) 0.0001(13) C1 0.0193(15) 0.0249(17) 0.0210(15) -0.0035(12) 0.0089(13) -0.0021(12) C11 0.0206(16) 0.0262(16) 0.0182(14) 0.0024(12) 0.0105(13) 0.0012(12) C3 0.0274(17) 0.0191(16) 0.0302(17) -0.0077(13) 0.0177(15) -0.0086(13) O1 0.0402(15) 0.0408(16) 0.0499(15) 0.0075(13) 0.0161(13) 0.0052(12) C12 0.0263(17) 0.0296(18) 0.0279(17) -0.0031(14) 0.0133(14) -0.0012(13) C21' 0.0266(17) 0.0207(15) 0.0204(15) 0.0012(12) 0.0133(13) 0.0036(12) C16 0.0272(17) 0.0286(18) 0.0280(16) -0.0029(14) 0.0161(14) -0.0017(13) C5 0.0333(18) 0.0274(17) 0.0282(16) 0.0027(14) 0.0208(15) -0.0062(14) C22' 0.0261(17) 0.037(2) 0.0232(16) 0.0001(14) 0.0126(14) 0.0020(14) C14' 0.0335(19) 0.0311(19) 0.046(2) 0.0154(16) 0.0272(17) 0.0121(14) C22 0.0220(16) 0.0254(17) 0.0250(16) 0.0003(13) 0.0108(14) -0.0010(12) C26' 0.0287(17) 0.0309(18) 0.0275(17) 0.0000(14) 0.0158(15) 0.0005(14) C15' 0.045(2) 0.0221(17) 0.046(2) 0.0008(15) 0.0312(18) 0.0025(14) C12' 0.0255(17) 0.0248(16) 0.0274(16) 0.0012(13) 0.0171(14) 0.0000(12) C13' 0.0280(18) 0.037(2) 0.0299(17) 0.0105(15) 0.0182(15) 0.0061(14) C16' 0.0348(19) 0.0248(17) 0.0315(17) 0.0013(14) 0.0202(15) -0.0009(14) C24 0.0346(19) 0.0236(17) 0.0361(18) 0.0060(14) 0.0234(16) 0.0060(13) C15 0.0267(18) 0.038(2) 0.0375(19) 0.0019(16) 0.0194(16) -0.0024(14) C4 0.0320(18) 0.0179(16) 0.0366(18) 0.0033(13) 0.0189(15) -0.0025(13) C13 0.0306(18) 0.0337(19) 0.0330(18) -0.0024(14) 0.0180(15) 0.0066(14) C6 0.0256(17) 0.0290(17) 0.0342(18) -0.0026(14) 0.0194(15) -0.0045(13) C25' 0.046(2) 0.037(2) 0.0332(19) 0.0025(15) 0.0279(18) 0.0015(16) C8 0.040(2) 0.039(2) 0.055(2) 0.0034(19) 0.0224(19) 0.0040(17) C23' 0.033(2) 0.052(2) 0.0209(17) 0.0006(16) 0.0082(15) 0.0073(17) C14 0.0237(17) 0.046(2) 0.0299(17) 0.0017(15) 0.0162(15) 0.0050(15) C25 0.0383(19) 0.0247(17) 0.0295(17) -0.0035(14) 0.0203(16) -0.0013(14) C7 0.040(2) 0.036(2) 0.049(2) -0.0013(18) 0.0208(19) -0.0006(16) C9 0.054(3) 0.047(3) 0.066(3) 0.006(2) 0.027(2) -0.002(2) C10 0.047(2) 0.040(2) 0.047(2) 0.0033(18) 0.020(2) -0.0040(17) C24' 0.053(2) 0.044(2) 0.0236(17) 0.0069(16) 0.0239(17) 0.0127(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C3 1.941(3) . ? Mo1 C2 1.973(3) . ? Mo1 C5 2.223(3) . ? Mo1 C6 2.325(3) . ? Mo1 C4 2.343(3) . ? Mo1 Cl1 2.5223(10) . ? Mo1 P1 2.5461(11) . ? Mo1 P2 2.6003(10) . ? P2 C21' 1.818(3) . ? P2 C21 1.819(3) . ? P2 C1 1.832(3) . ? P1 C11 1.822(3) . ? P1 C11' 1.827(3) . ? P1 C1 1.830(3) . ? C26 C25 1.383(4) . ? C26 C21 1.391(4) . ? C26 H26 0.9300 . ? C23 C22 1.382(4) . ? C23 C24 1.385(5) . ? C23 H23 0.9300 . ? O3 C3 1.165(4) . ? C11' C16' 1.395(4) . ? C11' C12' 1.402(4) . ? C21 C22 1.406(4) . ? O2 C2 1.159(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C11 C12 1.392(4) . ? C11 C16 1.398(4) . ? O1 C10 1.420(5) . ? O1 C7 1.435(4) . ? C12 C13 1.386(5) . ? C12 H12 0.9300 . ? C21' C26' 1.391(4) . ? C21' C22' 1.393(4) . ? C16 C15 1.384(4) . ? C16 H16 0.9300 . ? C5 C4 1.392(5) . ? C5 C6 1.408(5) . ? C5 H5 0.9300 . ? C22' C23' 1.383(5) . ? C22' H22' 0.9300 . ? C14' C15' 1.376(5) . ? C14' C13' 1.396(5) . ? C14' H14' 0.9300 . ? C22 H22 0.9300 . ? C26' C25' 1.384(4) . ? C26' H26' 0.9300 . ? C15' C16' 1.380(5) . ? C15' H15' 0.9300 . ? C12' C13' 1.375(4) . ? C12' H12' 0.9300 . ? C13' H13' 0.9300 . ? C16' H16' 0.9300 . ? C24 C25 1.392(5) . ? C24 H24 0.9300 . ? C15 C14 1.384(5) . ? C15 H15 0.9300 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C13 C14 1.378(5) . ? C13 H13 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C25' C24' 1.375(5) . ? C25' H25' 0.9300 . ? C8 C9 1.498(6) . ? C8 C7 1.519(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C23' C24' 1.375(5) . ? C23' H23' 0.9300 . ? C14 H14 0.9300 . ? C25 H25 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C9 C10 1.509(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C24' H24' 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 80.01(13) . . ? C3 Mo1 C5 104.91(13) . . ? C2 Mo1 C5 105.10(13) . . ? C3 Mo1 C6 71.12(12) . . ? C2 Mo1 C6 110.33(12) . . ? C5 Mo1 C6 35.98(12) . . ? C3 Mo1 C4 108.90(12) . . ? C2 Mo1 C4 71.44(13) . . ? C5 Mo1 C4 35.38(12) . . ? C6 Mo1 C4 61.43(12) . . ? C3 Mo1 Cl1 165.82(9) . . ? C2 Mo1 Cl1 94.03(9) . . ? C5 Mo1 Cl1 89.03(9) . . ? C6 Mo1 Cl1 123.05(9) . . ? C4 Mo1 Cl1 80.92(9) . . ? C3 Mo1 P1 89.68(9) . . ? C2 Mo1 P1 99.06(9) . . ? C5 Mo1 P1 153.51(9) . . ? C6 Mo1 P1 140.71(8) . . ? C4 Mo1 P1 156.64(8) . . ? Cl1 Mo1 P1 78.49(4) . . ? C3 Mo1 P2 102.52(9) . . ? C2 Mo1 P2 163.12(9) . . ? C5 Mo1 P2 90.49(9) . . ? C6 Mo1 P2 86.06(9) . . ? C4 Mo1 P2 122.16(9) . . ? Cl1 Mo1 P2 79.56(3) . . ? P1 Mo1 P2 64.47(3) . . ? C21' P2 C21 101.76(13) . . ? C21' P2 C1 108.60(14) . . ? C21 P2 C1 103.17(14) . . ? C21' P2 Mo1 123.14(10) . . ? C21 P2 Mo1 123.72(10) . . ? C1 P2 Mo1 93.47(10) . . ? C11 P1 C11' 104.20(14) . . ? C11 P1 C1 106.20(13) . . ? C11' P1 C1 106.05(14) . . ? C11 P1 Mo1 125.22(10) . . ? C11' P1 Mo1 117.40(10) . . ? C1 P1 Mo1 95.29(10) . . ? C25 C26 C21 120.6(3) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C16' C11' C12' 118.5(3) . . ? C16' C11' P1 124.0(2) . . ? C12' C11' P1 117.5(2) . . ? C26 C21 C22 119.2(3) . . ? C26 C21 P2 120.4(2) . . ? C22 C21 P2 120.3(2) . . ? O2 C2 Mo1 177.3(3) . . ? P1 C1 P2 97.12(14) . . ? P1 C1 H1A 112.3 . . ? P2 C1 H1A 112.3 . . ? P1 C1 H1B 112.3 . . ? P2 C1 H1B 112.3 . . ? H1A C1 H1B 109.9 . . ? C12 C11 C16 119.2(3) . . ? C12 C11 P1 120.7(2) . . ? C16 C11 P1 120.1(2) . . ? O3 C3 Mo1 176.9(3) . . ? C10 O1 C7 109.2(3) . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C26' C21' C22' 119.1(3) . . ? C26' C21' P2 116.7(2) . . ? C22' C21' P2 124.1(2) . . ? C15 C16 C11 120.3(3) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C4 C5 C6 116.7(3) . . ? C4 C5 Mo1 77.01(18) . . ? C6 C5 Mo1 75.96(18) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 121.6 . . ? Mo1 C5 H5 116.5 . . ? C23' C22' C21' 119.8(3) . . ? C23' C22' H22' 120.1 . . ? C21' C22' H22' 120.1 . . ? C15' C14' C13' 119.6(3) . . ? C15' C14' H14' 120.2 . . ? C13' C14' H14' 120.2 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C25' C26' C21' 120.5(3) . . ? C25' C26' H26' 119.8 . . ? C21' C26' H26' 119.8 . . ? C14' C15' C16' 120.8(3) . . ? C14' C15' H15' 119.6 . . ? C16' C15' H15' 119.6 . . ? C13' C12' C11' 120.7(3) . . ? C13' C12' H12' 119.6 . . ? C11' C12' H12' 119.6 . . ? C12' C13' C14' 120.0(3) . . ? C12' C13' H13' 120.0 . . ? C14' C13' H13' 120.0 . . ? C15' C16' C11' 120.4(3) . . ? C15' C16' H16' 119.8 . . ? C11' C16' H16' 119.8 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C5 C4 Mo1 67.62(17) . . ? C5 C4 H4A 116.9 . . ? Mo1 C4 H4A 116.9 . . ? C5 C4 H4B 116.9 . . ? Mo1 C4 H4B 116.9 . . ? H4A C4 H4B 113.9 . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C5 C6 Mo1 68.05(17) . . ? C5 C6 H6A 116.9 . . ? Mo1 C6 H6A 116.9 . . ? C5 C6 H6B 116.9 . . ? Mo1 C6 H6B 116.9 . . ? H6A C6 H6B 113.9 . . ? C24' C25' C26' 119.8(3) . . ? C24' C25' H25' 120.1 . . ? C26' C25' H25' 120.1 . . ? C9 C8 C7 102.0(3) . . ? C9 C8 H8A 111.4 . . ? C7 C8 H8A 111.4 . . ? C9 C8 H8B 111.4 . . ? C7 C8 H8B 111.4 . . ? H8A C8 H8B 109.2 . . ? C24' C23' C22' 120.5(3) . . ? C24' C23' H23' 119.7 . . ? C22' C23' H23' 119.7 . . ? C13 C14 C15 120.1(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C26 C25 C24 119.9(3) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? O1 C7 C8 106.4(3) . . ? O1 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? O1 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.6 . . ? C8 C9 C10 102.8(3) . . ? C8 C9 H9A 111.2 . . ? C10 C9 H9A 111.2 . . ? C8 C9 H9B 111.2 . . ? C10 C9 H9B 111.2 . . ? H9A C9 H9B 109.1 . . ? O1 C10 C9 106.7(3) . . ? O1 C10 H10A 110.4 . . ? C9 C10 H10A 110.4 . . ? O1 C10 H10B 110.4 . . ? C9 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? C23' C24' C25' 120.3(3) . . ? C23' C24' H24' 119.8 . . ? C25' C24' H24' 119.8 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 70.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.964 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.087 #==END #========================================================================== data_7 _database_code_CSD 196136 #========================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H32 Cl2 Mo2 O4 P2, C H N' _chemical_formula_sum 'C36 H33 Cl2 Mo2 N O4 P2' _chemical_formula_weight 868.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.763(5) _cell_length_b 15.343(5) _cell_length_c 17.538(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.96(5) _cell_angle_gamma 90.00 _cell_volume 3601(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6938 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 69.97 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 8.229 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.085 _exptl_absorpt_correction_T_max 0.150 _exptl_absorpt_process_details 'XABS (Parkin, Moezzi & Hope, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' # Orientation matrix from 'scale_all_noabs_3.out' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.0204518 _diffrn_orient_matrix_UB_21 -0.0645093 _diffrn_orient_matrix_UB_31 0.0314986 _diffrn_orient_matrix_UB_12 0.0283964 _diffrn_orient_matrix_UB_22 0.0327636 _diffrn_orient_matrix_UB_32 0.0486624 _diffrn_orient_matrix_UB_13 -0.0416920 _diffrn_orient_matrix_UB_23 -0.0240206 _diffrn_orient_matrix_UB_33 0.0405016 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6752 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 69.97 _reflns_number_total 6752 _reflns_number_gt 6548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collet (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens, 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+10.5670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6752 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.81336(2) 0.748411(19) 0.225307(17) 0.02432(9) Uani 1 1 d . . . Mo2 Mo 0.64999(2) 0.89725(2) 0.308342(16) 0.02353(9) Uani 1 1 d . . . P1 P 0.87052(6) 0.89893(6) 0.20142(5) 0.02107(18) Uani 1 1 d . . . P2 P 0.74855(6) 1.01619(6) 0.27376(5) 0.01952(18) Uani 1 1 d . . . Cl2 Cl 0.63920(6) 0.82710(6) 0.16871(5) 0.02658(18) Uani 1 1 d . . . Cl1 Cl 0.81883(6) 0.81661(6) 0.36160(5) 0.0294(2) Uani 1 1 d . . . O2 O 0.8477(3) 0.6938(3) 0.0696(2) 0.0701(12) Uani 1 1 d . . . C21 C 0.6827(3) 1.0811(2) 0.1790(2) 0.0227(7) Uani 1 1 d . . . C14 C 0.7433(4) 1.0093(3) -0.0682(2) 0.0443(11) Uani 1 1 d . . . H14 H 0.7183 1.0314 -0.1227 0.053 Uiso 1 1 calc R . . C11' C 1.0042(3) 0.8959(2) 0.2256(2) 0.0241(7) Uani 1 1 d . . . C11 C 0.8175(3) 0.9437(2) 0.0947(2) 0.0264(8) Uani 1 1 d . . . C5 C 0.6831(3) 0.9500(3) 0.4172(2) 0.0359(9) Uani 1 1 d . . . C3 C 0.9508(3) 0.7097(3) 0.2707(2) 0.0322(9) Uani 1 1 d . . . C1 C 0.8677(2) 0.9874(2) 0.2702(2) 0.0226(7) Uani 1 1 d . . . H1A H 0.8928 1.0394 0.2541 0.027 Uiso 1 1 calc R . . H1B H 0.9147 0.9729 0.3270 0.027 Uiso 1 1 calc R . . C7 C 0.7376(4) 0.6330(3) 0.2482(4) 0.0602(15) Uani 1 1 d . . . H7 H 0.6893 0.6445 0.2678 0.072 Uiso 1 1 calc R . . O4 O 0.4896(2) 1.0420(2) 0.2629(2) 0.0506(8) Uani 1 1 d . . . C26 C 0.5902(3) 1.0547(2) 0.1181(2) 0.0251(7) Uani 1 1 d . . . H26 H 0.5608 1.0037 0.1256 0.030 Uiso 1 1 calc R . . C12 C 0.7343(3) 0.9065(3) 0.0314(2) 0.0303(8) Uani 1 1 d . . . H12 H 0.7029 0.8592 0.0430 0.036 Uiso 1 1 calc R . . C4 C 0.5480(3) 0.9870(3) 0.2767(2) 0.0332(9) Uani 1 1 d . . . C26' C 0.8856(3) 1.1022(3) 0.4208(2) 0.0357(9) Uani 1 1 d . . . H26' H 0.9346 1.0654 0.4189 0.043 Uiso 1 1 calc R . . C16' C 1.0777(3) 0.9204(3) 0.3030(2) 0.0284(8) Uani 1 1 d . . . H16' H 1.0596 0.9443 0.3434 0.034 Uiso 1 1 calc R . . C7' C 0.5649(4) 0.7773(3) 0.3107(3) 0.0465(11) Uani 1 1 d . . . H7' H 0.5765 0.7270 0.2866 0.056 Uiso 1 1 calc R . . C21' C 0.7895(3) 1.0989(2) 0.3572(2) 0.0230(7) Uani 1 1 d . . . C22 C 0.7254(3) 1.1578(3) 0.1671(2) 0.0291(8) Uani 1 1 d . . . H22 H 0.7872 1.1758 0.2074 0.035 Uiso 1 1 calc R . . O5 O 0.7029(3) 0.9830(2) 0.48145(19) 0.0606(10) Uani 1 1 d . . . O3 O 1.0325(2) 0.6857(2) 0.2940(2) 0.0488(8) Uani 1 1 d . . . C22' C 0.7187(3) 1.1565(3) 0.3609(2) 0.0300(8) Uani 1 1 d . . . H22' H 0.6545 1.1566 0.3179 0.036 Uiso 1 1 calc R . . C6 C 0.7127(4) 0.6296(3) 0.1626(4) 0.0699(18) Uani 1 1 d . . . H6A H 0.6437 0.6417 0.1250 0.084 Uiso 1 1 calc R . . H6B H 0.7424 0.5830 0.1434 0.084 Uiso 1 1 calc R . . C2 C 0.8301(3) 0.7149(3) 0.1248(3) 0.0435(11) Uani 1 1 d . . . C23' C 0.7424(3) 1.2133(3) 0.4276(2) 0.0357(9) Uani 1 1 d . . . H23' H 0.6940 1.2511 0.4292 0.043 Uiso 1 1 calc R . . C13 C 0.6977(3) 0.9404(3) -0.0501(2) 0.0393(10) Uani 1 1 d . . . H13 H 0.6415 0.9156 -0.0925 0.047 Uiso 1 1 calc R . . C15' C 1.1778(3) 0.9097(3) 0.3208(3) 0.0382(10) Uani 1 1 d . . . H15' H 1.2266 0.9267 0.3728 0.046 Uiso 1 1 calc R . . C25 C 0.5420(3) 1.1047(3) 0.0463(2) 0.0314(9) Uani 1 1 d . . . H25 H 0.4805 1.0866 0.0054 0.038 Uiso 1 1 calc R . . C14' C 1.2055(3) 0.8737(3) 0.2614(3) 0.0434(11) Uani 1 1 d . . . H14' H 1.2727 0.8668 0.2730 0.052 Uiso 1 1 calc R . . C23 C 0.6762(3) 1.2073(3) 0.0953(2) 0.0343(9) Uani 1 1 d . . . H23 H 0.7049 1.2586 0.0877 0.041 Uiso 1 1 calc R . . C13' C 1.1325(3) 0.8483(3) 0.1850(3) 0.0439(11) Uani 1 1 d . . . H13' H 1.1509 0.8234 0.1452 0.053 Uiso 1 1 calc R . . C24 C 0.5843(3) 1.1807(3) 0.0349(2) 0.0331(9) Uani 1 1 d . . . H24 H 0.5513 1.2141 -0.0132 0.040 Uiso 1 1 calc R . . C15 C 0.8278(4) 1.0466(3) -0.0049(3) 0.0513(12) Uani 1 1 d . . . H15 H 0.8601 1.0929 -0.0172 0.062 Uiso 1 1 calc R . . C12' C 1.0326(3) 0.8589(3) 0.1662(2) 0.0357(9) Uani 1 1 d . . . H12' H 0.9843 0.8415 0.1141 0.043 Uiso 1 1 calc R . . C25' C 0.9091(3) 1.1602(3) 0.4874(2) 0.0425(11) Uani 1 1 d . . . H25' H 0.9739 1.1623 0.5295 0.051 Uiso 1 1 calc R . . C24' C 0.8371(3) 1.2144(3) 0.4915(2) 0.0380(10) Uani 1 1 d . . . H24' H 0.8524 1.2515 0.5372 0.046 Uiso 1 1 calc R . . C8 C 0.8353(4) 0.6190(3) 0.3033(3) 0.0502(12) Uani 1 1 d . . . H8A H 0.8699 0.5715 0.2904 0.060 Uiso 1 1 calc R . . H8B H 0.8517 0.6251 0.3628 0.060 Uiso 1 1 calc R . . C16 C 0.8632(4) 1.0143(3) 0.0761(3) 0.0429(11) Uani 1 1 d . . . H16 H 0.9183 1.0402 0.1186 0.052 Uiso 1 1 calc R . . C8' C 0.6201(4) 0.7964(3) 0.3969(3) 0.0498(12) Uani 1 1 d . . . H8'1 H 0.6742 0.7569 0.4290 0.060 Uiso 1 1 calc R . . H8'2 H 0.5828 0.8172 0.4274 0.060 Uiso 1 1 calc R . . C6' C 0.4914(3) 0.8382(4) 0.2632(3) 0.0505(12) Uani 1 1 d . . . H6'1 H 0.4494 0.8611 0.2887 0.061 Uiso 1 1 calc R . . H6'2 H 0.4557 0.8267 0.2034 0.061 Uiso 1 1 calc R . . C10 C 0.4510(5) 0.9422(5) 0.4465(5) 0.0670(19) Uani 1 1 d . . . H10 H 0.4412 0.9837 0.4051 0.080 Uiso 1 1 calc R . . N10 N 0.4609(4) 0.9006(4) 0.4880(5) 0.079(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02337(16) 0.02406(16) 0.02052(14) 0.00096(11) 0.00438(12) 0.00170(11) Mo2 0.01887(15) 0.03204(17) 0.01759(14) 0.00205(11) 0.00567(11) -0.00241(11) P1 0.0191(4) 0.0265(5) 0.0151(4) -0.0011(3) 0.0048(3) 0.0011(3) P2 0.0148(4) 0.0259(4) 0.0147(4) -0.0018(3) 0.0031(3) -0.0003(3) Cl2 0.0215(4) 0.0330(5) 0.0179(4) 0.0009(3) 0.0012(3) -0.0005(3) Cl1 0.0251(4) 0.0395(5) 0.0169(4) 0.0043(3) 0.0024(3) 0.0029(4) O2 0.096(3) 0.081(3) 0.0349(17) -0.0172(18) 0.0294(19) 0.022(2) C21 0.0203(17) 0.031(2) 0.0151(15) -0.0027(14) 0.0062(13) 0.0022(14) C14 0.065(3) 0.040(2) 0.0228(19) 0.0102(18) 0.014(2) 0.012(2) C11' 0.0249(18) 0.0253(18) 0.0236(17) 0.0030(14) 0.0116(15) 0.0035(15) C11 0.0303(19) 0.0286(19) 0.0178(16) -0.0014(14) 0.0077(15) 0.0065(15) C5 0.039(2) 0.040(2) 0.028(2) 0.0054(18) 0.0141(17) -0.0042(19) C3 0.035(2) 0.028(2) 0.032(2) 0.0052(16) 0.0123(17) 0.0040(17) C1 0.0193(16) 0.0294(19) 0.0172(15) -0.0045(14) 0.0059(13) -0.0031(14) C7 0.050(3) 0.027(2) 0.106(5) 0.008(3) 0.035(3) -0.012(2) O4 0.0372(17) 0.065(2) 0.0519(19) 0.0077(17) 0.0214(15) 0.0190(17) C26 0.0216(17) 0.0287(19) 0.0198(16) 0.0007(14) 0.0036(14) -0.0030(15) C12 0.0262(19) 0.043(2) 0.0195(17) 0.0022(16) 0.0071(15) 0.0016(17) C4 0.0258(19) 0.048(3) 0.0269(19) 0.0022(17) 0.0124(16) -0.0003(19) C26' 0.028(2) 0.041(2) 0.0283(19) -0.0094(17) 0.0030(16) 0.0053(17) C16' 0.0212(18) 0.031(2) 0.0316(19) -0.0009(16) 0.0095(15) 0.0016(15) C7' 0.050(3) 0.042(3) 0.056(3) -0.004(2) 0.031(2) -0.024(2) C21' 0.0236(17) 0.0276(19) 0.0161(15) -0.0013(13) 0.0067(14) -0.0016(14) C22 0.0213(18) 0.039(2) 0.0230(17) 0.0005(16) 0.0051(14) -0.0068(16) O5 0.092(3) 0.065(2) 0.0284(16) -0.0117(16) 0.0292(17) -0.018(2) O3 0.0301(16) 0.0484(19) 0.065(2) 0.0167(16) 0.0167(15) 0.0167(14) C22' 0.0255(19) 0.040(2) 0.0239(18) -0.0045(16) 0.0094(15) 0.0022(16) C6 0.050(3) 0.036(3) 0.090(4) -0.017(3) -0.004(3) -0.002(2) C2 0.047(3) 0.039(2) 0.032(2) -0.0045(19) 0.0051(19) 0.009(2) C23' 0.041(2) 0.038(2) 0.033(2) -0.0065(17) 0.0203(18) 0.0027(19) C13 0.036(2) 0.056(3) 0.0202(18) 0.0008(18) 0.0062(16) 0.005(2) C15' 0.024(2) 0.039(2) 0.045(2) 0.0062(19) 0.0072(18) 0.0022(17) C25 0.0266(19) 0.041(2) 0.0186(17) 0.0000(15) 0.0016(15) -0.0019(17) C14' 0.034(2) 0.044(3) 0.059(3) 0.012(2) 0.027(2) 0.010(2) C23 0.035(2) 0.037(2) 0.0279(19) 0.0067(17) 0.0098(17) -0.0072(18) C13' 0.045(3) 0.053(3) 0.049(3) 0.009(2) 0.035(2) 0.017(2) C24 0.032(2) 0.041(2) 0.0207(17) 0.0083(16) 0.0058(15) 0.0032(18) C15 0.083(4) 0.033(2) 0.037(2) 0.0048(19) 0.024(2) -0.008(2) C12' 0.039(2) 0.043(2) 0.0282(19) 0.0013(17) 0.0174(17) 0.0094(19) C25' 0.035(2) 0.049(3) 0.026(2) -0.0107(19) -0.0035(17) -0.004(2) C24' 0.052(3) 0.038(2) 0.0236(19) -0.0091(17) 0.0154(18) -0.006(2) C8 0.067(3) 0.030(2) 0.061(3) 0.016(2) 0.034(3) 0.006(2) C16 0.062(3) 0.030(2) 0.027(2) -0.0022(17) 0.010(2) -0.010(2) C8' 0.062(3) 0.049(3) 0.048(3) 0.015(2) 0.031(2) -0.007(2) C6' 0.029(2) 0.071(4) 0.051(3) -0.009(2) 0.016(2) -0.017(2) C10 0.043(3) 0.078(5) 0.097(5) -0.031(4) 0.045(4) 0.002(4) N10 0.024(2) 0.052(4) 0.139(6) -0.023(3) 0.015(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C3 1.934(4) . ? Mo1 C2 1.949(5) . ? Mo1 C7 2.219(5) . ? Mo1 C6 2.316(5) . ? Mo1 C8 2.355(4) . ? Mo1 P1 2.5533(12) . ? Mo1 Cl1 2.5792(11) . ? Mo1 Cl2 2.6267(14) . ? Mo2 C5 1.937(4) . ? Mo2 C4 1.940(4) . ? Mo2 C7' 2.239(4) . ? Mo2 C6' 2.317(4) . ? Mo2 C8' 2.363(4) . ? Mo2 P2 2.5613(11) . ? Mo2 Cl1 2.5790(14) . ? Mo2 Cl2 2.6176(11) . ? P1 C1 1.828(3) . ? P1 C11 1.831(4) . ? P1 C11' 1.836(4) . ? P2 C21 1.826(4) . ? P2 C21' 1.836(4) . ? P2 C1 1.840(3) . ? O2 C2 1.150(5) . ? C21 C26 1.392(5) . ? C21 C22 1.392(5) . ? C14 C13 1.360(6) . ? C14 C15 1.396(7) . ? C14 H14 0.9300 . ? C11' C16' 1.386(5) . ? C11' C12' 1.398(5) . ? C11 C12 1.383(5) . ? C11 C16 1.386(6) . ? C5 O5 1.154(5) . ? C3 O3 1.158(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C7 C8 1.373(7) . ? C7 C6 1.388(9) . ? C7 H7 0.9300 . ? O4 C4 1.158(5) . ? C26 C25 1.387(5) . ? C26 H26 0.9300 . ? C12 C13 1.398(5) . ? C12 H12 0.9300 . ? C26' C21' 1.386(5) . ? C26' C25' 1.391(6) . ? C26' H26' 0.9300 . ? C16' C15' 1.387(5) . ? C16' H16' 0.9300 . ? C7' C6' 1.409(7) . ? C7' C8' 1.412(7) . ? C7' H7' 0.9300 . ? C21' C22' 1.391(5) . ? C22 C23 1.384(5) . ? C22 H22 0.9300 . ? C22' C23' 1.380(5) . ? C22' H22' 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C23' C24' 1.374(6) . ? C23' H23' 0.9300 . ? C13 H13 0.9300 . ? C15' C14' 1.385(6) . ? C15' H15' 0.9300 . ? C25 C24 1.377(6) . ? C25 H25 0.9300 . ? C14' C13' 1.375(7) . ? C14' H14' 0.9300 . ? C23 C24 1.384(6) . ? C23 H23 0.9300 . ? C13' C12' 1.378(6) . ? C13' H13' 0.9300 . ? C24 H24 0.9300 . ? C15 C16 1.383(6) . ? C15 H15 0.9300 . ? C12' H12' 0.9300 . ? C25' C24' 1.375(6) . ? C25' H25' 0.9300 . ? C24' H24' 0.9300 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C16 H16 0.9300 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C6' H6'1 0.9700 . ? C6' H6'2 0.9700 . ? C10 N10 0.931(9) . ? C10 H10 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 77.27(18) . . ? C3 Mo1 C7 101.63(18) . . ? C2 Mo1 C7 102.7(2) . . ? C3 Mo1 C6 107.77(19) . . ? C2 Mo1 C6 70.4(2) . . ? C7 Mo1 C6 35.6(2) . . ? C3 Mo1 C8 68.82(17) . . ? C2 Mo1 C8 105.33(19) . . ? C7 Mo1 C8 34.76(19) . . ? C6 Mo1 C8 61.0(2) . . ? C3 Mo1 P1 89.05(12) . . ? C2 Mo1 P1 85.02(15) . . ? C7 Mo1 P1 167.93(15) . . ? C6 Mo1 P1 145.54(17) . . ? C8 Mo1 P1 152.13(14) . . ? C3 Mo1 Cl1 97.24(13) . . ? C2 Mo1 Cl1 168.13(15) . . ? C7 Mo1 Cl1 88.68(17) . . ? C6 Mo1 Cl1 121.49(19) . . ? C8 Mo1 Cl1 81.99(14) . . ? P1 Mo1 Cl1 84.37(4) . . ? C3 Mo1 Cl2 170.52(12) . . ? C2 Mo1 Cl2 104.90(14) . . ? C7 Mo1 Cl2 86.99(14) . . ? C6 Mo1 Cl2 81.53(15) . . ? C8 Mo1 Cl2 118.67(13) . . ? P1 Mo1 Cl2 82.00(3) . . ? Cl1 Mo1 Cl2 78.85(5) . . ? C5 Mo2 C4 80.09(18) . . ? C5 Mo2 C7' 103.59(17) . . ? C4 Mo2 C7' 102.42(18) . . ? C5 Mo2 C6' 107.35(18) . . ? C4 Mo2 C6' 68.25(19) . . ? C7' Mo2 C6' 35.97(18) . . ? C5 Mo2 C8' 70.42(17) . . ? C4 Mo2 C8' 108.38(18) . . ? C7' Mo2 C8' 35.62(17) . . ? C6' Mo2 C8' 61.72(18) . . ? C5 Mo2 P2 90.21(13) . . ? C4 Mo2 P2 82.89(12) . . ? C7' Mo2 P2 165.82(13) . . ? C6' Mo2 P2 142.28(13) . . ? C8' Mo2 P2 154.81(13) . . ? C5 Mo2 Cl1 92.31(14) . . ? C4 Mo2 Cl1 163.46(12) . . ? C7' Mo2 Cl1 93.61(14) . . ? C6' Mo2 Cl1 128.26(14) . . ? C8' Mo2 Cl1 82.40(14) . . ? P2 Mo2 Cl1 82.46(4) . . ? C5 Mo2 Cl2 169.90(13) . . ? C4 Mo2 Cl2 106.89(12) . . ? C7' Mo2 Cl2 82.32(13) . . ? C6' Mo2 Cl2 82.28(13) . . ? C8' Mo2 Cl2 113.03(13) . . ? P2 Mo2 Cl2 83.56(4) . . ? Cl1 Mo2 Cl2 79.02(5) . . ? C1 P1 C11 106.06(17) . . ? C1 P1 C11' 100.85(16) . . ? C11 P1 C11' 101.53(17) . . ? C1 P1 Mo1 117.54(12) . . ? C11 P1 Mo1 118.60(13) . . ? C11' P1 Mo1 109.68(12) . . ? C21 P2 C21' 102.64(16) . . ? C21 P2 C1 104.42(16) . . ? C21' P2 C1 101.24(16) . . ? C21 P2 Mo2 117.80(12) . . ? C21' P2 Mo2 109.43(12) . . ? C1 P2 Mo2 118.93(12) . . ? Mo2 Cl2 Mo1 99.91(5) . . ? Mo2 Cl1 Mo1 102.21(5) . . ? C26 C21 C22 119.4(3) . . ? C26 C21 P2 120.8(3) . . ? C22 C21 P2 119.8(3) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16' C11' C12' 118.9(3) . . ? C16' C11' P1 122.7(3) . . ? C12' C11' P1 118.0(3) . . ? C12 C11 C16 119.2(3) . . ? C12 C11 P1 121.2(3) . . ? C16 C11 P1 119.6(3) . . ? O5 C5 Mo2 178.7(4) . . ? O3 C3 Mo1 176.7(4) . . ? P1 C1 P2 119.30(18) . . ? P1 C1 H1A 107.5 . . ? P2 C1 H1A 107.5 . . ? P1 C1 H1B 107.5 . . ? P2 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C8 C7 C6 118.4(6) . . ? C8 C7 Mo1 78.0(3) . . ? C6 C7 Mo1 76.0(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? Mo1 C7 H7 116.0 . . ? C25 C26 C21 119.8(3) . . ? C25 C26 H26 120.1 . . ? C21 C26 H26 120.1 . . ? C11 C12 C13 119.8(4) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? O4 C4 Mo2 175.9(3) . . ? C21' C26' C25' 120.5(4) . . ? C21' C26' H26' 119.8 . . ? C25' C26' H26' 119.8 . . ? C11' C16' C15' 120.5(4) . . ? C11' C16' H16' 119.8 . . ? C15' C16' H16' 119.8 . . ? C6' C7' C8' 116.6(5) . . ? C6' C7' Mo2 75.0(3) . . ? C8' C7' Mo2 77.0(3) . . ? C6' C7' H7' 121.7 . . ? C8' C7' H7' 121.7 . . ? Mo2 C7' H7' 117.4 . . ? C26' C21' C22' 118.2(3) . . ? C26' C21' P2 123.2(3) . . ? C22' C21' P2 118.4(3) . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C23' C22' C21' 121.0(4) . . ? C23' C22' H22' 119.5 . . ? C21' C22' H22' 119.5 . . ? C7 C6 Mo1 68.4(3) . . ? C7 C6 H6A 116.8 . . ? Mo1 C6 H6A 116.8 . . ? C7 C6 H6B 116.8 . . ? Mo1 C6 H6B 116.8 . . ? H6A C6 H6B 113.8 . . ? O2 C2 Mo1 174.7(4) . . ? C24' C23' C22' 120.4(4) . . ? C24' C23' H23' 119.8 . . ? C22' C23' H23' 119.8 . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C14' C15' C16' 120.3(4) . . ? C14' C15' H15' 119.9 . . ? C16' C15' H15' 119.9 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C13' C14' C15' 119.2(4) . . ? C13' C14' H14' 120.4 . . ? C15' C14' H14' 120.4 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C14' C13' C12' 121.3(4) . . ? C14' C13' H13' 119.4 . . ? C12' C13' H13' 119.4 . . ? C25 C24 C23 119.8(3) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C13' C12' C11' 119.8(4) . . ? C13' C12' H12' 120.1 . . ? C11' C12' H12' 120.1 . . ? C24' C25' C26' 120.4(4) . . ? C24' C25' H25' 119.8 . . ? C26' C25' H25' 119.8 . . ? C23' C24' C25' 119.5(4) . . ? C23' C24' H24' 120.3 . . ? C25' C24' H24' 120.3 . . ? C7 C8 Mo1 67.2(3) . . ? C7 C8 H8A 117.0 . . ? Mo1 C8 H8A 117.0 . . ? C7 C8 H8B 117.0 . . ? Mo1 C8 H8B 117.0 . . ? H8A C8 H8B 114.0 . . ? C15 C16 C11 120.8(4) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C7' C8' Mo2 67.4(2) . . ? C7' C8' H8'1 117.0 . . ? Mo2 C8' H8'1 117.0 . . ? C7' C8' H8'2 117.0 . . ? Mo2 C8' H8'2 117.0 . . ? H8'1 C8' H8'2 114.0 . . ? C7' C6' Mo2 69.0(2) . . ? C7' C6' H6'1 116.8 . . ? Mo2 C6' H6'1 116.8 . . ? C7' C6' H6'2 116.8 . . ? Mo2 C6' H6'2 116.8 . . ? H6'1 C6' H6'2 113.8 . . ? N10 C10 H10 180.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 69.97 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.724 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.092 #==END