Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem.Soc., Dalton Trans.' _publ_contact_author 'Prof Rosa Llusar' _publ_contact_author_address ; Prof Rosa Llusar Departament de Ciencies Experimentals Universitat Jaume I Campus de Riu Sec PO Box 224 Castello 12071 SPAIN ; _publ_contact_letter ; Please consider this CIF submission for publication in J.Chem.Soc., Dalton Trans. ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+34 964 728086' _publ_contact_author_fax '+34 964 728066' _publ_contact_author_email 'llusar@exp.uji.es' loop_ _publ_author_name _publ_author_address 'Llusar, R.' ; Departament de Cičncies Experimentals, Universitat Jaume I Campus de Riu Sec, Box 224, Castelló, Spain ; 'Uriel, Santiago' ; ? ; 'Vicent, Cristian' ; ? ; _publ_section_title ; Transition metal incorporation into seleno-bridged cubane clusters of molybdenum and tungsten. X-ray crystal structures of the first [Mo3CuSe4] derivatives ; _publ_section_abstract ; ? ; _publ_section_experimental ; ? ; _publ_section_references ; ? ; data_[Mo3Se4Cl3(dmpe)3]PF6_(1) _database_code_CSD 164458 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 Cl3 F6 Mo3 P7 Se4' _chemical_formula_weight 1305.36 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I23 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' _cell_length_a 20.9212(10) _cell_length_b 20.9212(10) _cell_length_c 20.9212(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9157.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.894 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5024 _exptl_absorpt_coefficient_mu 4.446 _exptl_absorpt_correction_type Bruker SADABS _exptl_absorpt_correction_T_min 1.371098 _exptl_absorpt_correction_T_max 1.955038 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22579 _diffrn_reflns_av_R_equivalents 0.0891 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 23.20 _reflns_number_total 2199 _reflns_number_gt 2124 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0881P)^2^+63.4965P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 2199 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1436 _refine_ls_wR_factor_gt 0.1427 _refine_ls_goodness_of_fit_ref 1.207 _refine_ls_restrained_S_all 1.207 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 0.68788(7) 0.20462(7) -0.23568(7) 0.0267(3) Uani 1 1 d . . . Se1 Se 0.69784(8) 0.30216(8) -0.30216(8) 0.0322(7) Uani 1 3 d S . . Se2 Se 0.76966(9) 0.13049(8) -0.26758(9) 0.0340(4) Uani 1 1 d . . . P1 P 0.6427(2) 0.1132(2) -0.1723(2) 0.0355(12) Uani 1 1 d . . . P2 P 0.6152(2) 0.1491(2) -0.3199(2) 0.0342(11) Uani 1 1 d . . . Cl1 Cl 0.5790(2) 0.2473(2) -0.2134(2) 0.0437(12) Uani 1 1 d . . . C1 C 0.5897(10) 0.1349(11) -0.1087(11) 0.055(6) Uani 1 1 d . . . H1A H 0.5552 0.1601 -0.1254 0.082 Uiso 1 1 calc R . . H1B H 0.6126 0.1592 -0.0773 0.082 Uiso 1 1 calc R . . H1C H 0.5728 0.0969 -0.0892 0.082 Uiso 1 1 calc R . . C2 C 0.7025(15) 0.0593(14) -0.1341(12) 0.081(9) Uani 1 1 d . . . H2A H 0.7339 0.0470 -0.1652 0.121 Uiso 1 1 calc R . . H2B H 0.6813 0.0219 -0.1181 0.121 Uiso 1 1 calc R . . H2C H 0.7230 0.0814 -0.0995 0.121 Uiso 1 1 calc R . . C3 C 0.5890(9) 0.0621(9) -0.2236(10) 0.047(6) Uani 1 1 d . . . H3A H 0.6141 0.0278 -0.2421 0.057 Uiso 1 1 calc R . . H3B H 0.5563 0.0430 -0.1969 0.057 Uiso 1 1 calc R . . C4 C 0.5583(7) 0.0983(9) -0.2749(8) 0.033(5) Uani 1 1 d . . . H4A H 0.5251 0.1251 -0.2568 0.039 Uiso 1 1 calc R . . H4B H 0.5381 0.0686 -0.3043 0.039 Uiso 1 1 calc R . . C5 C 0.5693(12) 0.2028(13) -0.3749(10) 0.067(7) Uani 1 1 d . . . H5A H 0.5461 0.2338 -0.3502 0.100 Uiso 1 1 calc R . . H5B H 0.5397 0.1778 -0.3996 0.100 Uiso 1 1 calc R . . H5C H 0.5983 0.2244 -0.4031 0.100 Uiso 1 1 calc R . . C6 C 0.6438(14) 0.0950(13) -0.3732(12) 0.081(9) Uani 1 1 d . . . H6A H 0.6693 0.0639 -0.3512 0.122 Uiso 1 1 calc R . . H6B H 0.6696 0.1166 -0.4045 0.122 Uiso 1 1 calc R . . H6C H 0.6087 0.0741 -0.3941 0.122 Uiso 1 1 calc R . . P10 P 0.5000 0.0000 0.0000 0.041(2) Uani 1 4 d S . . F10 F 0.5000 0.0749(8) 0.0000 0.055(5) Uani 1 2 d S . . F11 F 0.5000 0.0000 -0.0793(8) 0.074(6) Uani 1 2 d S . . F12 F 0.5748(9) 0.0000 0.0000 0.098(8) Uani 1 2 d S . . P20 P 0.0000 0.0000 0.0000 0.250 Uiso 1 12 d S . . F20 F 0.0741 0.0000 0.0000 0.300 Uiso 1 2 d S . . 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 0.0237(8) 0.0255(8) 0.0308(8) 0.0005(7) -0.0004(6) -0.0046(6) Se1 0.0322(7) 0.0322(7) 0.0322(7) 0.0009(7) -0.0009(7) 0.0009(7) Se2 0.0321(10) 0.0273(9) 0.0425(10) -0.0029(8) 0.0061(9) 0.0011(8) P1 0.040(3) 0.026(2) 0.041(3) -0.001(2) 0.000(2) -0.010(2) P2 0.029(3) 0.037(3) 0.036(3) -0.008(2) -0.002(2) -0.003(2) Cl1 0.025(2) 0.049(3) 0.057(3) -0.004(2) 0.011(2) 0.002(2) C1 0.062(15) 0.051(13) 0.050(14) -0.012(11) 0.004(11) -0.009(11) C2 0.10(2) 0.10(2) 0.043(13) 0.022(14) 0.009(15) -0.007(17) C3 0.027(10) 0.049(12) 0.066(15) -0.021(11) 0.002(10) -0.019(9) C4 0.012(8) 0.062(12) 0.024(10) -0.003(8) 0.005(7) -0.011(8) C5 0.066(15) 0.095(19) 0.039(13) -0.017(14) -0.023(11) 0.005(15) C6 0.10(2) 0.11(2) 0.041(14) -0.017(14) -0.002(14) -0.042(17) P10 0.048(6) 0.044(6) 0.032(6) 0.000 0.000 0.000 F10 0.069(12) 0.050(9) 0.047(10) 0.000 0.021(9) 0.000 F11 0.105(17) 0.084(15) 0.032(9) 0.000 0.000 0.033(15) F12 0.036(12) 0.103(18) 0.16(2) 0.01(2) 0.000 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 Se2 2.404(2) . ? Mo1 Se2 2.450(2) 6_665 ? Mo1 Se1 2.478(3) . ? Mo1 Cl1 2.491(5) . ? Mo1 P1 2.512(5) . ? Mo1 P2 2.601(5) . ? Mo1 Mo1 2.835(2) 6_665 ? Mo1 Mo1 2.835(2) 12_654 ? Se1 Mo1 2.478(3) 12_654 ? Se1 Mo1 2.478(3) 6_665 ? Se2 Mo1 2.450(2) 12_654 ? P1 C1 1.79(2) . ? P1 C2 1.86(3) . ? P1 C3 1.885(18) . ? P2 C6 1.70(3) . ? P2 C4 1.854(17) . ? P2 C5 1.87(2) . ? C3 C4 1.46(3) . ? P10 F12 1.56(2) 2_655 ? P10 F12 1.56(2) . ? P10 F10 1.566(16) . ? P10 F10 1.566(16) 2_655 ? P10 F11 1.659(16) . ? P10 F11 1.659(16) 3_655 ? P20 F20 1.5504 10 ? P20 F20 1.5504 6 ? P20 F20 1.5504 2 ? P20 F20 1.5504 5 ? P20 F20 1.5504 . ? P20 F20 1.5504 9 ? 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 Se2 Mo1 Se2 96.91(11) . 6_665 ? Se2 Mo1 Se1 108.39(8) . . ? Se2 Mo1 Se1 106.94(7) 6_665 . ? Se2 Mo1 Cl1 159.11(14) . . ? Se2 Mo1 Cl1 95.81(14) 6_665 . ? Se1 Mo1 Cl1 83.48(13) . . ? Se2 Mo1 P1 85.62(13) . . ? Se2 Mo1 P1 80.57(13) 6_665 . ? Se1 Mo1 P1 162.69(15) . . ? Cl1 Mo1 P1 80.21(17) . . ? Se2 Mo1 P2 86.56(13) . . ? Se2 Mo1 P2 158.30(14) 6_665 . ? Se1 Mo1 P2 92.08(13) . . ? Cl1 Mo1 P2 75.65(17) . . ? P1 Mo1 P2 78.34(17) . . ? Se2 Mo1 Mo1 100.01(6) . 6_665 ? Se2 Mo1 Mo1 53.51(6) 6_665 6_665 ? Se1 Mo1 Mo1 55.11(5) . 6_665 ? Cl1 Mo1 Mo1 100.87(13) . 6_665 ? P1 Mo1 Mo1 134.05(13) . 6_665 ? P2 Mo1 Mo1 147.04(12) . 6_665 ? Se2 Mo1 Mo1 55.01(7) . 12_654 ? Se2 Mo1 Mo1 98.90(6) 6_665 12_654 ? Se1 Mo1 Mo1 55.11(5) . 12_654 ? Cl1 Mo1 Mo1 138.48(12) . 12_654 ? P1 Mo1 Mo1 140.44(13) . 12_654 ? P2 Mo1 Mo1 100.58(13) . 12_654 ? Mo1 Mo1 Mo1 60.0 6_665 12_654 ? Mo1 Se1 Mo1 69.77(9) 12_654 . ? Mo1 Se1 Mo1 69.77(9) 12_654 6_665 ? Mo1 Se1 Mo1 69.77(9) . 6_665 ? Mo1 Se2 Mo1 71.48(8) . 12_654 ? C1 P1 C2 104.5(11) . . ? C1 P1 C3 101.4(9) . . ? C2 P1 C3 107.5(12) . . ? C1 P1 Mo1 115.7(8) . . ? C2 P1 Mo1 115.7(9) . . ? C3 P1 Mo1 110.8(7) . . ? C6 P2 C4 100.2(11) . . ? C6 P2 C5 100.2(12) . . ? C4 P2 C5 109.1(10) . . ? C6 P2 Mo1 122.4(10) . . ? C4 P2 Mo1 106.7(6) . . ? C5 P2 Mo1 116.6(8) . . ? C4 C3 P1 112.8(14) . . ? C3 C4 P2 112.8(12) . . ? F12 P10 F12 180.0 2_655 . ? F12 P10 F10 90.0 2_655 . ? F12 P10 F10 90.0 . . ? F12 P10 F10 90.0 2_655 2_655 ? F12 P10 F10 90.0 . 2_655 ? F10 P10 F10 180.0 . 2_655 ? F12 P10 F11 90.0 2_655 . ? F12 P10 F11 90.0 . . ? F10 P10 F11 90.0 . . ? F10 P10 F11 90.0 2_655 . ? F12 P10 F11 90.0 2_655 3_655 ? F12 P10 F11 90.0 . 3_655 ? F10 P10 F11 90.0 . 3_655 ? F10 P10 F11 90.0 2_655 3_655 ? F11 P10 F11 180.0 . 3_655 ? F20 P20 F20 90.0 10 6 ? F20 P20 F20 90.0 10 2 ? F20 P20 F20 90.0 6 2 ? F20 P20 F20 90.0 10 5 ? F20 P20 F20 180.0 6 5 ? F20 P20 F20 90.0 2 5 ? F20 P20 F20 90.0 10 . ? F20 P20 F20 90.0 6 . ? F20 P20 F20 180.0 2 . ? F20 P20 F20 90.0 5 . ? F20 P20 F20 180.0 10 9 ? F20 P20 F20 90.0 6 9 ? F20 P20 F20 90.0 2 9 ? F20 P20 F20 90.0 5 9 ? F20 P20 F20 90.0 . 9 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.20 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.650 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.190 #======END data_ [W3Se4Br3(dmpe)3]PF6_(3) _database_code_CSD 164459 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 Br3 F6 P7 Se4 W3' _chemical_formula_weight 1702.47 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' 'F' 'F' 0.0171 0.0103 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M I23 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' _cell_length_a 21.0599(5) _cell_length_b 21.0599(5) _cell_length_c 21.0599(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9340.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6224 _exptl_absorpt_coefficient_mu 13.332 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min 0.5783 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22949 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 23.22 _reflns_number_total 2251 _reflns_number_gt 2066 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0618P)^2^+40.1289P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 2251 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0919 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.044 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.73421(3) 0.29456(2) 0.18826(2) 0.02788(18) Uani 1 1 d . . . Se1 Se 0.80178(6) 0.19822(6) 0.19822(6) 0.0327(5) Uani 1 3 d S . . Se2 Se 0.76623(7) 0.36987(6) 0.26863(6) 0.0339(3) Uani 1 1 d . . . Br1 Br 0.71304(8) 0.24632(8) 0.07423(7) 0.0512(4) Uani 1 1 d . . . P1 P 0.66936(19) 0.38420(19) 0.1423(2) 0.0407(9) Uani 1 1 d . . . P2 P 0.8161(2) 0.3511(2) 0.11543(18) 0.0409(10) Uani 1 1 d . . . C1 C 0.6041(9) 0.3609(9) 0.0924(9) 0.069(5) Uani 1 1 d . . . H1A H 0.6188 0.3315 0.0609 0.103 Uiso 1 1 calc R . . H1B H 0.5868 0.3977 0.0719 0.103 Uiso 1 1 calc R . . H1C H 0.5718 0.3411 0.1179 0.103 Uiso 1 1 calc R . . C2 C 0.6324(8) 0.4381(7) 0.1973(8) 0.053(4) Uani 1 1 d . . . H2A H 0.6636 0.4538 0.2265 0.080 Uiso 1 1 calc R . . H2B H 0.5997 0.4162 0.2203 0.080 Uiso 1 1 calc R . . H2C H 0.6140 0.4729 0.1743 0.080 Uiso 1 1 calc R . . C3 C 0.7199(8) 0.4355(8) 0.0916(8) 0.057(5) Uani 1 1 d . . . H3A H 0.6936 0.4568 0.0603 0.068 Uiso 1 1 calc R . . H3B H 0.7400 0.4678 0.1177 0.068 Uiso 1 1 calc R . . C4 C 0.7687(8) 0.3982(8) 0.0594(7) 0.052(4) Uani 1 1 d . . . H4A H 0.7965 0.4265 0.0361 0.062 Uiso 1 1 calc R . . H4B H 0.7486 0.3699 0.0291 0.062 Uiso 1 1 calc R . . C5 C 0.8709(8) 0.3034(10) 0.0704(8) 0.066(5) Uani 1 1 d . . . H5A H 0.8960 0.2781 0.0989 0.099 Uiso 1 1 calc R . . H5B H 0.8982 0.3305 0.0460 0.099 Uiso 1 1 calc R . . H5C H 0.8476 0.2760 0.0423 0.099 Uiso 1 1 calc R . . C6 C 0.8675(8) 0.4141(9) 0.1484(8) 0.056(5) Uani 1 1 d . . . H6A H 0.8425 0.4419 0.1745 0.084 Uiso 1 1 calc R . . H6B H 0.8862 0.4378 0.1143 0.084 Uiso 1 1 calc R . . H6C H 0.9004 0.3951 0.1736 0.084 Uiso 1 1 calc R . . P10 P 0.5000 0.0000 0.0000 0.044(2) Uani 1 4 d S . . F1 F 0.5000 0.0000 -0.0767(6) 0.074(5) Uani 1 2 d S . . F2 F 0.5000 0.0756(7) 0.0000 0.083(5) Uani 1 2 d S . . F3 F 0.5734(8) 0.0000 0.0000 0.103(6) Uani 1 2 d S . . P20 P 0.5000 0.5000 0.347(3) 0.17(3) Uiso 0.17 2 d SP . . F20 F 0.5000 0.5000 0.271(3) 0.198 Uiso 0.17 2 d SPR . . F21 F 0.5000 0.5000 0.424(3) 0.198 Uiso 0.17 2 d SPR . . F22 F 0.5000 0.5753 0.347(3) 0.198 Uiso 0.17 1 d PR . . F23 F 0.5736 0.5000 0.347(3) 0.198 Uiso 0.17 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0312(3) 0.0270(3) 0.0254(3) 0.0014(2) -0.0024(2) -0.0018(2) Se1 0.0327(5) 0.0327(5) 0.0327(5) -0.0022(6) 0.0022(6) 0.0022(6) Se2 0.0410(8) 0.0282(7) 0.0326(7) -0.0019(6) -0.0037(7) -0.0025(6) Br1 0.0645(11) 0.0541(10) 0.0350(8) -0.0060(7) -0.0083(7) -0.0078(8) P1 0.044(2) 0.030(2) 0.047(2) 0.0089(17) -0.0070(19) -0.0011(17) P2 0.044(2) 0.046(2) 0.033(2) 0.0061(17) 0.0024(17) -0.0071(19) C1 0.066(12) 0.050(11) 0.089(15) 0.007(10) -0.021(11) 0.005(10) C2 0.046(10) 0.056(10) 0.058(11) 0.004(9) -0.010(8) 0.002(8) C3 0.063(12) 0.050(10) 0.057(11) 0.025(8) -0.007(9) -0.014(9) C4 0.062(11) 0.058(10) 0.034(8) 0.013(8) -0.007(8) -0.008(9) C5 0.048(11) 0.087(14) 0.063(11) 0.012(11) 0.018(9) 0.014(10) C6 0.052(10) 0.072(12) 0.044(10) 0.015(9) -0.008(8) -0.026(9) P10 0.057(5) 0.042(5) 0.034(5) 0.000 0.000 0.000 F1 0.096(12) 0.095(11) 0.031(7) 0.000 0.000 -0.035(10) F2 0.110(13) 0.046(8) 0.093(12) 0.000 -0.011(12) 0.000 F3 0.059(11) 0.145(17) 0.105(13) -0.005(14) 0.000 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 W1 Se2 2.4157(14) . ? W1 Se2 2.4539(14) 10_656 ? W1 Se1 2.4871(17) . ? W1 P1 2.523(4) . ? W1 P2 2.597(4) . ? W1 Br1 2.6453(16) . ? W1 W1 2.8365(8) 7_665 ? W1 W1 2.8365(8) 10_656 ? Se1 W1 2.4871(17) 7_665 ? Se1 W1 2.4871(17) 10_656 ? Se2 W1 2.4539(14) 7_665 ? P1 C1 1.798(18) . ? P1 C2 1.798(16) . ? P1 C3 1.854(16) . ? P2 C5 1.801(17) . ? P2 C4 1.836(15) . ? P2 C6 1.847(16) . ? C3 C4 1.46(2) . ? P10 F3 1.545(17) . ? P10 F3 1.545(17) 2_655 ? P10 F2 1.592(14) 2_655 ? P10 F2 1.592(14) . ? P10 F1 1.615(13) . ? P10 F1 1.615(13) 3_655 ? P20 F23 1.5503 2_665 ? P20 F23 1.5503 . ? P20 F22 1.5848 2_665 ? P20 F22 1.5848 . ? P20 F21 1.6123 . ? P20 F20 1.6124 . ? 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 Se2 W1 Se2 96.99(7) . 10_656 ? Se2 W1 Se1 108.47(4) . . ? Se2 W1 Se1 107.25(4) 10_656 . ? Se2 W1 P1 85.91(10) . . ? Se2 W1 P1 80.38(10) 10_656 . ? Se1 W1 P1 162.27(10) . . ? Se2 W1 P2 85.83(10) . . ? Se2 W1 P2 157.79(10) 10_656 . ? Se1 W1 P2 92.54(10) . . ? P1 W1 P2 77.85(13) . . ? Se2 W1 Br1 159.27(5) . . ? Se2 W1 Br1 96.81(5) 10_656 . ? Se1 W1 Br1 81.94(5) . . ? P1 W1 Br1 81.25(11) . . ? P2 W1 Br1 75.64(10) . . ? Se2 W1 W1 55.00(4) . 7_665 ? Se2 W1 W1 99.11(3) 10_656 7_665 ? Se1 W1 W1 55.23(3) . 7_665 ? P1 W1 W1 140.73(10) . 7_665 ? P2 W1 W1 100.48(9) . 7_665 ? Br1 W1 W1 137.01(4) . 7_665 ? Se2 W1 W1 100.05(4) . 10_656 ? Se2 W1 W1 53.75(3) 10_656 10_656 ? Se1 W1 W1 55.23(3) . 10_656 ? P1 W1 W1 134.09(9) . 10_656 ? P2 W1 W1 147.55(10) . 10_656 ? Br1 W1 W1 100.58(4) . 10_656 ? W1 W1 W1 60.0 7_665 10_656 ? W1 Se1 W1 69.53(6) . 7_665 ? W1 Se1 W1 69.53(6) . 10_656 ? W1 Se1 W1 69.53(6) 7_665 10_656 ? W1 Se2 W1 71.25(4) . 7_665 ? C1 P1 C2 102.5(8) . . ? C1 P1 C3 105.2(9) . . ? C2 P1 C3 104.5(8) . . ? C1 P1 W1 115.7(6) . . ? C2 P1 W1 117.4(6) . . ? C3 P1 W1 110.3(6) . . ? C5 P2 C4 108.1(8) . . ? C5 P2 C6 102.9(9) . . ? C4 P2 C6 100.0(8) . . ? C5 P2 W1 118.7(7) . . ? C4 P2 W1 105.4(6) . . ? C6 P2 W1 119.8(6) . . ? C4 C3 P1 110.9(12) . . ? C3 C4 P2 112.0(11) . . ? F3 P10 F3 180.0 . 2_655 ? F3 P10 F2 90.0 . 2_655 ? F3 P10 F2 90.0 2_655 2_655 ? F3 P10 F2 90.0 . . ? F3 P10 F2 90.0 2_655 . ? F2 P10 F2 180.0 2_655 . ? F3 P10 F1 90.0 . . ? F3 P10 F1 90.0 2_655 . ? F2 P10 F1 90.0 2_655 . ? F2 P10 F1 90.0 . . ? F3 P10 F1 90.0 . 3_655 ? F3 P10 F1 90.0 2_655 3_655 ? F2 P10 F1 90.0 2_655 3_655 ? F2 P10 F1 90.0 . 3_655 ? F1 P10 F1 180.0 . 3_655 ? F23 P20 F23 180.0 2_665 . ? F23 P20 F22 90.0 2_665 2_665 ? F23 P20 F22 90.0 . 2_665 ? F23 P20 F22 90.0 2_665 . ? F23 P20 F22 90.0 . . ? F22 P20 F22 180.0 2_665 . ? F23 P20 F21 90.0 2_665 . ? F23 P20 F21 90.0 . . ? F22 P20 F21 90.0 2_665 . ? F22 P20 F21 90.0 . . ? F23 P20 F20 90.0 2_665 . ? F23 P20 F20 90.0 . . ? F22 P20 F20 90.0 2_665 . ? F22 P20 F20 90.0 . . ? F21 P20 F20 180.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.22 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.441 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.202 #======END data_[Mo3CuSe4Cl4(dmpe)4]PF6_(4) _database_code_CSD 164460 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H48 Cl4 Cu F6 Mo3 P7 Se4' _chemical_formula_weight 1404.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'F' 'F' 0.0171 0.0103 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.607(6) _cell_length_b 15.879(8) _cell_length_c 21.314(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.180(14) _cell_angle_gamma 90.00 _cell_volume 4267(4) _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 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2696 _exptl_absorpt_coefficient_mu 5.320 _exptl_absorpt_correction_type Bruker SADABS _exptl_absorpt_correction_T_min 1.349658 _exptl_absorpt_correction_T_max 1.955437 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18013 _diffrn_reflns_av_R_equivalents 0.1368 _diffrn_reflns_av_sigmaI/netI 0.2202 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 22.01 _reflns_number_total 5215 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0306P)^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 5215 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 0.763 _refine_ls_restrained_S_all 0.763 _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 0.12239(11) 0.76352(11) 0.07122(7) 0.0252(4) Uani 1 1 d . . . Mo2 Mo 0.33616(12) 0.76517(11) 0.02896(7) 0.0275(5) Uani 1 1 d . . . Mo3 Mo 0.29107(12) 0.76945(10) 0.15936(7) 0.0261(5) Uani 1 1 d . . . Cu1 Cu 0.25321(18) 0.62039(14) 0.09003(10) 0.0330(6) Uani 1 1 d . . . Se1 Se 0.24708(15) 0.88418(12) 0.08386(9) 0.0325(5) Uani 1 1 d . . . Se2 Se 0.13141(14) 0.67706(13) 0.16495(8) 0.0317(5) Uani 1 1 d . . . Se3 Se 0.19973(14) 0.66999(14) -0.01125(8) 0.0352(6) Uani 1 1 d . . . Se4 Se 0.42462(14) 0.67915(13) 0.11135(8) 0.0324(6) Uani 1 1 d . . . Cl1 Cl 0.0461(4) 0.8575(3) -0.0105(2) 0.0491(15) Uani 1 1 d . . . Cl2 Cl 0.4868(4) 0.8654(4) 0.0273(2) 0.0548(17) Uani 1 1 d . . . Cl3 Cl 0.2109(4) 0.8679(3) 0.2362(2) 0.0515(16) Uani 1 1 d . . . Cl4 Cl 0.2541(5) 0.4813(3) 0.0985(3) 0.0612(17) Uani 1 1 d . . . P2 P -0.0256(4) 0.8464(4) 0.1280(2) 0.0363(15) Uani 1 1 d . . . P1 P -0.0424(4) 0.6780(4) 0.0463(2) 0.0341(14) Uani 1 1 d . . . P3 P 0.4589(4) 0.6828(4) -0.0413(2) 0.0418(16) Uani 1 1 d . . . P4 P 0.3181(4) 0.8430(4) -0.0765(2) 0.0426(16) Uani 1 1 d . . . P5 P 0.3362(4) 0.6906(4) 0.2585(2) 0.0407(16) Uani 1 1 d . . . P6 P 0.4507(4) 0.8556(4) 0.2025(2) 0.0395(15) Uani 1 1 d . . . C1 C -0.0468(14) 0.5689(13) 0.0668(9) 0.055(7) Uani 1 1 d . . . H1A H -0.0285 0.5624 0.1103 0.082 Uiso 1 1 calc R . . H1B H 0.0029 0.5383 0.0415 0.082 Uiso 1 1 calc R . . H1C H -0.1170 0.5476 0.0596 0.082 Uiso 1 1 calc R . . C2 C -0.0780(13) 0.6772(12) -0.0364(8) 0.052(7) Uani 1 1 d . . . H2A H -0.0797 0.7340 -0.0519 0.078 Uiso 1 1 calc R . . H2B H -0.1466 0.6520 -0.0415 0.078 Uiso 1 1 calc R . . H2C H -0.0264 0.6454 -0.0594 0.078 Uiso 1 1 calc R . . C3 C -0.1566(14) 0.7221(13) 0.0895(9) 0.045(6) Uani 1 1 d . . . H3A H -0.2223 0.7043 0.0697 0.055 Uiso 1 1 calc R . . H3B H -0.1561 0.7017 0.1323 0.055 Uiso 1 1 calc R . . C4 C -0.1493(14) 0.8173(14) 0.0890(9) 0.051(6) Uani 1 1 d . . . H4A H -0.2092 0.8415 0.1110 0.061 Uiso 1 1 calc R . . H4B H -0.1498 0.8381 0.0462 0.061 Uiso 1 1 calc R . . C5 C -0.0534(14) 0.8220(13) 0.2071(7) 0.052(6) Uani 1 1 d . . . H5A H -0.0588 0.7620 0.2119 0.078 Uiso 1 1 calc R . . H5B H -0.1193 0.8478 0.2190 0.078 Uiso 1 1 calc R . . H5C H 0.0026 0.8429 0.2334 0.078 Uiso 1 1 calc R . . C6 C -0.0175(15) 0.9594(13) 0.1220(9) 0.061(7) Uani 1 1 d . . . H6A H -0.0020 0.9749 0.0795 0.092 Uiso 1 1 calc R . . H6B H 0.0378 0.9798 0.1491 0.092 Uiso 1 1 calc R . . H6C H -0.0839 0.9839 0.1342 0.092 Uiso 1 1 calc R . . C7 C 0.4316(15) 0.5750(12) -0.0518(9) 0.057(7) Uani 1 1 d . . . H7A H 0.4320 0.5472 -0.0118 0.085 Uiso 1 1 calc R . . H7B H 0.4847 0.5504 -0.0782 0.085 Uiso 1 1 calc R . . H7C H 0.3631 0.5685 -0.0710 0.085 Uiso 1 1 calc R . . C8 C 0.5951(13) 0.6847(14) -0.0206(8) 0.059(7) Uani 1 1 d . . . H8A H 0.6170 0.7418 -0.0134 0.088 Uiso 1 1 calc R . . H8B H 0.6362 0.6609 -0.0540 0.088 Uiso 1 1 calc R . . H8C H 0.6059 0.6523 0.0170 0.088 Uiso 1 1 calc R . . C9 C 0.4560(15) 0.7261(16) -0.1208(8) 0.059(7) Uani 1 1 d . . . H9A H 0.5223 0.7131 -0.1416 0.070 Uiso 1 1 calc R . . H9B H 0.3991 0.6997 -0.1444 0.070 Uiso 1 1 calc R . . C10 C 0.4400(15) 0.8187(14) -0.1207(9) 0.054(7) Uani 1 1 d . . . H10A H 0.4335 0.8392 -0.1634 0.065 Uiso 1 1 calc R . . H10B H 0.5003 0.8463 -0.1012 0.065 Uiso 1 1 calc R . . C11 C 0.3088(16) 0.9563(12) -0.0757(9) 0.065(7) Uani 1 1 d . . . H11A H 0.3602 0.9788 -0.0469 0.098 Uiso 1 1 calc R . . H11B H 0.2389 0.9727 -0.0628 0.098 Uiso 1 1 calc R . . H11C H 0.3224 0.9778 -0.1170 0.098 Uiso 1 1 calc R . . C12 C 0.2162(13) 0.8128(14) -0.1328(8) 0.054(7) Uani 1 1 d . . . H12A H 0.2154 0.7526 -0.1371 0.081 Uiso 1 1 calc R . . H12B H 0.2313 0.8381 -0.1727 0.081 Uiso 1 1 calc R . . H12C H 0.1483 0.8318 -0.1183 0.081 Uiso 1 1 calc R . . C13 C 0.2440(15) 0.6984(14) 0.3230(8) 0.066(7) Uani 1 1 d . . . H13A H 0.2248 0.7563 0.3292 0.098 Uiso 1 1 calc R . . H13B H 0.2766 0.6769 0.3605 0.098 Uiso 1 1 calc R . . H13C H 0.1815 0.6661 0.3136 0.098 Uiso 1 1 calc R . . C14 C 0.3610(16) 0.5831(12) 0.2537(10) 0.065(7) Uani 1 1 d . . . H14A H 0.3007 0.5553 0.2355 0.098 Uiso 1 1 calc R . . H14B H 0.3740 0.5611 0.2949 0.098 Uiso 1 1 calc R . . H14C H 0.4221 0.5736 0.2279 0.098 Uiso 1 1 calc R . . C15 C 0.4605(12) 0.7344(12) 0.2945(7) 0.034(5) Uani 1 1 d . . . H15A H 0.4636 0.7202 0.3388 0.041 Uiso 1 1 calc R . . H15B H 0.5223 0.7104 0.2741 0.041 Uiso 1 1 calc R . . C16 C 0.4599(16) 0.8280(13) 0.2864(8) 0.055(6) Uiso 1 1 d . . . H16A H 0.5243 0.8516 0.3042 0.066 Uiso 1 1 calc R . . H16B H 0.4000 0.8518 0.3087 0.066 Uiso 1 1 calc R . . C17 C 0.4458(15) 0.9698(12) 0.2003(10) 0.068(7) Uani 1 1 d . . . H17A H 0.3773 0.9886 0.2139 0.101 Uiso 1 1 calc R . . H17B H 0.4583 0.9889 0.1582 0.101 Uiso 1 1 calc R . . H17C H 0.4994 0.9924 0.2277 0.101 Uiso 1 1 calc R . . C18 C 0.5830(13) 0.8341(13) 0.1775(7) 0.054(7) Uani 1 1 d . . . H18A H 0.5889 0.8452 0.1333 0.081 Uiso 1 1 calc R . . H18B H 0.5996 0.7761 0.1855 0.081 Uiso 1 1 calc R . . H18C H 0.6316 0.8695 0.2001 0.081 Uiso 1 1 calc R . . P10 P 0.7312(4) 0.5283(4) 0.2065(2) 0.067(2) Uani 1 1 d . . . F10 F 0.7242(4) 0.5535(4) 0.1376(2) 0.101(5) Uiso 1 1 d R A 1 F11 F 0.7403(4) 0.4972(4) 0.2763(2) 0.098(5) Uiso 1 1 d R A 1 F12 F 0.8499(4) 0.5565(4) 0.2118(2) 0.095(10) Uiso 0.55(2) 1 d PR A 1 F13 F 0.6105(4) 0.4948(4) 0.2002(2) 0.077(9) Uiso 0.55(2) 1 d PR A 1 F14 F 0.6894(4) 0.6228(4) 0.2195(2) 0.118(12) Uiso 0.55(2) 1 d PR A 1 F15 F 0.7676(4) 0.4357(4) 0.1869(2) 0.109(11) Uiso 0.55(2) 1 d PR A 1 F16 F 0.6512(4) 0.4511(4) 0.1960(2) 0.142(16) Uiso 0.45(2) 1 d PR A 2 F17 F 0.8142(4) 0.6017(4) 0.2243(2) 0.061(10) Uiso 0.45(2) 1 d PR A 2 F18 F 0.8274(4) 0.4694(4) 0.1872(2) 0.116(15) Uiso 0.45(2) 1 d PR A 2 F19 F 0.6322(4) 0.5784(4) 0.2335(2) 0.119(15) Uiso 0.45(2) 1 d PR A 2 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 0.0182(9) 0.0245(11) 0.0328(10) 0.0019(9) -0.0037(7) -0.0004(9) Mo2 0.0314(10) 0.0299(12) 0.0213(10) 0.0030(9) 0.0039(8) -0.0033(9) Mo3 0.0302(10) 0.0250(11) 0.0231(10) -0.0034(9) -0.0101(8) 0.0016(9) Cu1 0.0370(15) 0.0280(15) 0.0339(15) -0.0038(12) -0.0021(12) -0.0017(13) Se1 0.0318(12) 0.0277(13) 0.0379(13) 0.0036(10) -0.0067(10) -0.0038(11) Se2 0.0316(12) 0.0369(14) 0.0267(12) 0.0037(11) -0.0007(9) 0.0001(11) Se3 0.0334(12) 0.0458(15) 0.0262(12) -0.0069(11) -0.0016(9) -0.0066(11) Se4 0.0289(12) 0.0388(15) 0.0294(12) -0.0046(11) -0.0027(9) 0.0069(11) Cl1 0.056(4) 0.046(4) 0.046(3) 0.016(3) -0.007(3) -0.003(3) Cl2 0.050(4) 0.057(4) 0.057(4) 0.010(3) -0.025(3) -0.019(3) Cl3 0.046(3) 0.047(4) 0.061(4) -0.016(3) -0.002(3) 0.012(3) Cl4 0.071(4) 0.031(3) 0.082(5) -0.002(3) -0.003(3) 0.011(3) P2 0.029(3) 0.047(4) 0.033(3) -0.001(3) -0.002(3) 0.009(3) P1 0.027(3) 0.045(4) 0.030(3) -0.002(3) -0.002(2) -0.010(3) P3 0.035(3) 0.066(5) 0.025(3) -0.008(3) 0.004(2) 0.005(3) P4 0.038(3) 0.051(4) 0.038(3) 0.015(3) -0.009(3) -0.010(3) P5 0.035(3) 0.059(5) 0.028(3) 0.007(3) -0.010(3) 0.002(3) P6 0.031(3) 0.046(4) 0.041(4) -0.008(3) -0.010(3) -0.002(3) C1 0.042(14) 0.071(18) 0.052(14) -0.019(13) -0.005(11) -0.029(13) C2 0.035(12) 0.051(16) 0.070(16) 0.038(13) -0.023(11) -0.021(12) C3 0.034(13) 0.051(16) 0.051(14) -0.023(12) 0.009(11) -0.011(12) C4 0.042(14) 0.068(19) 0.043(14) -0.011(13) 0.007(11) 0.003(14) C5 0.054(14) 0.067(17) 0.036(13) 0.013(13) 0.017(11) 0.011(13) C6 0.052(15) 0.052(17) 0.081(18) 0.000(14) 0.013(13) 0.027(13) C7 0.052(15) 0.043(16) 0.075(17) -0.018(13) -0.002(12) 0.017(12) C8 0.048(14) 0.09(2) 0.035(13) -0.016(13) 0.012(10) 0.008(14) C9 0.039(13) 0.12(2) 0.017(12) -0.015(14) -0.006(10) -0.023(15) C10 0.065(16) 0.051(17) 0.047(15) 0.035(13) -0.009(12) -0.036(14) C11 0.085(18) 0.041(16) 0.070(16) 0.039(13) -0.023(13) 0.001(14) C12 0.032(12) 0.10(2) 0.033(13) 0.036(13) 0.001(10) 0.000(13) C13 0.084(17) 0.10(2) 0.016(12) 0.003(12) -0.006(11) -0.006(15) C14 0.066(16) 0.041(16) 0.088(18) 0.005(14) -0.018(14) -0.003(14) C15 0.014(10) 0.058(16) 0.030(11) 0.015(11) -0.007(8) 0.002(11) C17 0.062(17) 0.045(17) 0.096(19) -0.017(14) -0.005(14) -0.028(14) C18 0.052(14) 0.085(19) 0.024(12) -0.009(12) -0.024(10) 0.032(14) P10 0.068(5) 0.095(6) 0.039(4) 0.013(4) 0.005(3) -0.016(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 Se2 2.426(3) . ? Mo1 Cl1 2.485(5) . ? Mo1 Se1 2.492(3) . ? Mo1 Se3 2.501(3) . ? Mo1 P1 2.536(5) . ? Mo1 P2 2.587(5) . ? Mo1 Mo3 2.835(2) . ? Mo1 Cu1 2.836(3) . ? Mo1 Mo2 2.844(2) . ? Mo2 Se3 2.443(3) . ? Mo2 Cl2 2.477(5) . ? Mo2 Se4 2.486(3) . ? Mo2 Se1 2.492(3) . ? Mo2 P3 2.522(6) . ? Mo2 P4 2.575(6) . ? Mo2 Mo3 2.839(2) . ? Mo2 Cu1 2.843(3) . ? Mo3 Se4 2.439(3) . ? Mo3 Cl3 2.482(5) . ? Mo3 Se1 2.492(3) . ? Mo3 Se2 2.494(3) . ? Mo3 P5 2.520(5) . ? Mo3 P6 2.599(5) . ? Mo3 Cu1 2.830(3) . ? Cu1 Cl4 2.216(6) . ? Cu1 Se3 2.393(3) . ? Cu1 Se2 2.394(3) . ? Cu1 Se4 2.396(3) . ? P2 C5 1.766(16) . ? P2 C6 1.80(2) . ? P2 C4 1.824(18) . ? P1 C1 1.79(2) . ? P1 C2 1.818(17) . ? P1 C3 1.848(17) . ? P3 C7 1.76(2) . ? P3 C8 1.772(17) . ? P3 C9 1.829(18) . ? P4 C11 1.80(2) . ? P4 C12 1.819(17) . ? P4 C10 1.84(2) . ? P5 C14 1.738(19) . ? P5 C13 1.808(17) . ? P5 C15 1.876(15) . ? P6 C18 1.785(17) . ? P6 C17 1.82(2) . ? P6 C16 1.846(18) . ? C3 C4 1.51(2) . ? C9 C10 1.48(3) . ? C15 C16 1.50(2) . ? P10 F10 1.5234 . ? P10 F12 1.5669 . ? P10 F11 1.5716 . ? P10 F18 1.5870 . ? P10 F19 1.5891 . ? P10 F15 1.5954 . ? P10 F16 1.6017 . ? P10 F17 1.6112 . ? P10 F14 1.6150 . ? P10 F13 1.6162 . ? 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 Se2 Mo1 Cl1 159.06(15) . . ? Se2 Mo1 Se1 108.54(9) . . ? Cl1 Mo1 Se1 81.76(14) . . ? Se2 Mo1 Se3 103.02(10) . . ? Cl1 Mo1 Se3 90.85(15) . . ? Se1 Mo1 Se3 106.57(9) . . ? Se2 Mo1 P1 84.57(13) . . ? Cl1 Mo1 P1 81.96(17) . . ? Se1 Mo1 P1 161.81(15) . . ? Se3 Mo1 P1 81.73(14) . . ? Se2 Mo1 P2 86.26(13) . . ? Cl1 Mo1 P2 75.19(17) . . ? Se1 Mo1 P2 90.79(15) . . ? Se3 Mo1 P2 156.09(13) . . ? P1 Mo1 P2 77.22(18) . . ? Se2 Mo1 Mo3 55.94(7) . . ? Cl1 Mo1 Mo3 137.09(14) . . ? Se1 Mo1 Mo3 55.33(6) . . ? Se3 Mo1 Mo3 101.08(8) . . ? P1 Mo1 Mo3 140.22(14) . . ? P2 Mo1 Mo3 102.34(13) . . ? Se2 Mo1 Cu1 53.44(7) . . ? Cl1 Mo1 Cu1 143.51(15) . . ? Se1 Mo1 Cu1 103.56(9) . . ? Se3 Mo1 Cu1 52.82(8) . . ? P1 Mo1 Cu1 94.36(15) . . ? P2 Mo1 Cu1 139.61(14) . . ? Mo3 Mo1 Cu1 59.88(7) . . ? Se2 Mo1 Mo2 102.94(7) . . ? Cl1 Mo1 Mo2 97.90(14) . . ? Se1 Mo1 Mo2 55.20(7) . . ? Se3 Mo1 Mo2 53.92(6) . . ? P1 Mo1 Mo2 135.64(14) . . ? P2 Mo1 Mo2 145.98(15) . . ? Mo3 Mo1 Mo2 60.00(6) . . ? Cu1 Mo1 Mo2 60.06(7) . . ? Se3 Mo2 Cl2 158.62(15) . . ? Se3 Mo2 Se4 102.80(9) . . ? Cl2 Mo2 Se4 91.18(14) . . ? Se3 Mo2 Se1 108.43(9) . . ? Cl2 Mo2 Se1 82.31(16) . . ? Se4 Mo2 Se1 106.67(9) . . ? Se3 Mo2 P3 84.46(14) . . ? Cl2 Mo2 P3 81.6(2) . . ? Se4 Mo2 P3 81.94(14) . . ? Se1 Mo2 P3 161.85(16) . . ? Se3 Mo2 P4 86.01(14) . . ? Cl2 Mo2 P4 75.25(17) . . ? Se4 Mo2 P4 156.72(15) . . ? Se1 Mo2 P4 90.42(16) . . ? P3 Mo2 P4 77.47(19) . . ? Se3 Mo2 Mo3 102.43(8) . . ? Cl2 Mo2 Mo3 98.86(14) . . ? Se4 Mo2 Mo3 54.02(7) . . ? Se1 Mo2 Mo3 55.27(6) . . ? P3 Mo2 Mo3 135.94(14) . . ? P4 Mo2 Mo3 145.67(16) . . ? Se3 Mo2 Cu1 53.18(8) . . ? Cl2 Mo2 Cu1 143.97(14) . . ? Se4 Mo2 Cu1 52.92(7) . . ? Se1 Mo2 Cu1 103.37(9) . . ? P3 Mo2 Cu1 94.57(16) . . ? P4 Mo2 Cu1 139.13(14) . . ? Mo3 Mo2 Cu1 59.74(7) . . ? Se3 Mo2 Mo1 55.85(7) . . ? Cl2 Mo2 Mo1 137.50(16) . . ? Se4 Mo2 Mo1 101.22(8) . . ? Se1 Mo2 Mo1 55.21(7) . . ? P3 Mo2 Mo1 140.07(15) . . ? P4 Mo2 Mo1 101.52(14) . . ? Mo3 Mo2 Mo1 59.83(5) . . ? Cu1 Mo2 Mo1 59.82(7) . . ? Se4 Mo3 Cl3 158.48(14) . . ? Se4 Mo3 Se1 108.14(9) . . ? Cl3 Mo3 Se1 82.87(15) . . ? Se4 Mo3 Se2 103.44(9) . . ? Cl3 Mo3 Se2 90.48(14) . . ? Se1 Mo3 Se2 106.43(8) . . ? Se4 Mo3 P5 84.56(14) . . ? Cl3 Mo3 P5 81.41(19) . . ? Se1 Mo3 P5 162.55(16) . . ? Se2 Mo3 P5 81.26(14) . . ? Se4 Mo3 P6 85.58(14) . . ? Cl3 Mo3 P6 75.62(17) . . ? Se1 Mo3 P6 90.81(14) . . ? Se2 Mo3 P6 156.48(14) . . ? P5 Mo3 P6 78.01(18) . . ? Se4 Mo3 Cu1 53.47(8) . . ? Cl3 Mo3 Cu1 143.42(15) . . ? Se1 Mo3 Cu1 103.73(9) . . ? Se2 Mo3 Cu1 53.00(7) . . ? P5 Mo3 Cu1 93.42(15) . . ? P6 Mo3 Cu1 138.93(14) . . ? Se4 Mo3 Mo1 102.70(8) . . ? Cl3 Mo3 Mo1 98.76(14) . . ? Se1 Mo3 Mo1 55.34(6) . . ? Se2 Mo3 Mo1 53.72(6) . . ? P5 Mo3 Mo1 134.94(14) . . ? P6 Mo3 Mo1 146.13(14) . . ? Cu1 Mo3 Mo1 60.08(7) . . ? Se4 Mo3 Mo2 55.57(6) . . ? Cl3 Mo3 Mo2 138.12(15) . . ? Se1 Mo3 Mo2 55.27(7) . . ? Se2 Mo3 Mo2 101.35(7) . . ? P5 Mo3 Mo2 139.78(15) . . ? P6 Mo3 Mo2 101.63(13) . . ? Cu1 Mo3 Mo2 60.19(7) . . ? Mo1 Mo3 Mo2 60.17(6) . . ? Cl4 Cu1 Se3 113.75(18) . . ? Cl4 Cu1 Se2 108.86(18) . . ? Se3 Cu1 Se2 107.37(11) . . ? Cl4 Cu1 Se4 111.62(18) . . ? Se3 Cu1 Se4 107.12(11) . . ? Se2 Cu1 Se4 107.88(11) . . ? Cl4 Cu1 Mo3 142.21(18) . . ? Se3 Cu1 Mo3 104.03(11) . . ? Se2 Cu1 Mo3 56.28(8) . . ? Se4 Cu1 Mo3 54.88(7) . . ? Cl4 Cu1 Mo1 144.39(18) . . ? Se3 Cu1 Mo1 56.40(8) . . ? Se2 Cu1 Mo1 54.49(7) . . ? Se4 Cu1 Mo1 103.80(10) . . ? Mo3 Cu1 Mo1 60.04(7) . . ? Cl4 Cu1 Mo2 147.30(18) . . ? Se3 Cu1 Mo2 54.81(8) . . ? Se2 Cu1 Mo2 103.83(10) . . ? Se4 Cu1 Mo2 55.88(8) . . ? Mo3 Cu1 Mo2 60.07(7) . . ? Mo1 Cu1 Mo2 60.12(7) . . ? Mo2 Se1 Mo3 69.46(8) . . ? Mo2 Se1 Mo1 69.59(8) . . ? Mo3 Se1 Mo1 69.32(7) . . ? Cu1 Se2 Mo1 72.06(9) . . ? Cu1 Se2 Mo3 70.72(9) . . ? Mo1 Se2 Mo3 70.34(7) . . ? Cu1 Se3 Mo2 72.01(9) . . ? Cu1 Se3 Mo1 70.78(9) . . ? Mo2 Se3 Mo1 70.23(8) . . ? Cu1 Se4 Mo3 71.65(9) . . ? Cu1 Se4 Mo2 71.20(8) . . ? Mo3 Se4 Mo2 70.41(8) . . ? C5 P2 C6 107.3(10) . . ? C5 P2 C4 101.9(9) . . ? C6 P2 C4 105.6(10) . . ? C5 P2 Mo1 118.7(7) . . ? C6 P2 Mo1 115.6(6) . . ? C4 P2 Mo1 105.9(7) . . ? C1 P1 C2 102.8(9) . . ? C1 P1 C3 102.8(9) . . ? C2 P1 C3 107.1(9) . . ? C1 P1 Mo1 119.6(6) . . ? C2 P1 Mo1 113.9(6) . . ? C3 P1 Mo1 109.4(6) . . ? C7 P3 C8 103.7(10) . . ? C7 P3 C9 104.2(10) . . ? C8 P3 C9 103.9(9) . . ? C7 P3 Mo2 117.4(7) . . ? C8 P3 Mo2 116.0(6) . . ? C9 P3 Mo2 110.2(8) . . ? C11 P4 C12 102.9(10) . . ? C11 P4 C10 105.5(10) . . ? C12 P4 C10 101.3(9) . . ? C11 P4 Mo2 118.4(7) . . ? C12 P4 Mo2 120.6(6) . . ? C10 P4 Mo2 105.9(6) . . ? C14 P5 C13 103.2(10) . . ? C14 P5 C15 103.8(9) . . ? C13 P5 C15 101.7(8) . . ? C14 P5 Mo3 118.6(7) . . ? C13 P5 Mo3 117.3(7) . . ? C15 P5 Mo3 110.2(6) . . ? C18 P6 C17 102.4(10) . . ? C18 P6 C16 100.9(9) . . ? C17 P6 C16 105.3(10) . . ? C18 P6 Mo3 121.1(7) . . ? C17 P6 Mo3 119.4(7) . . ? C16 P6 Mo3 105.3(7) . . ? C4 C3 P1 109.1(13) . . ? C3 C4 P2 107.6(15) . . ? C10 C9 P3 111.9(14) . . ? C9 C10 P4 108.7(13) . . ? C16 C15 P5 108.5(12) . . ? C15 C16 P6 110.3(14) . . ? F10 P10 F12 92.6 . . ? F10 P10 F11 176.7 . . ? F12 P10 F11 87.4 . . ? F10 P10 F18 86.9 . . ? F12 P10 F18 57.0 . . ? F11 P10 F18 90.4 . . ? F10 P10 F19 100.1 . . ? F12 P10 F19 125.6 . . ? F11 P10 F19 82.5 . . ? F18 P10 F19 172.1 . . ? F10 P10 F15 90.3 . . ? F12 P10 F15 90.4 . . ? F11 P10 F15 86.4 . . ? F18 P10 F15 33.8 . . ? F19 P10 F15 141.5 . . ? F10 P10 F16 91.8 . . ? F12 P10 F16 146.1 . . ? F11 P10 F16 86.3 . . ? F18 P10 F16 89.7 . . ? F19 P10 F16 86.5 . . ? F15 P10 F16 56.0 . . ? F10 P10 F17 94.1 . . ? F12 P10 F17 32.4 . . ? F11 P10 F17 87.7 . . ? F18 P10 F17 89.5 . . ? F19 P10 F17 93.6 . . ? F15 P10 F17 122.7 . . ? F16 P10 F17 173.9 . . ? F10 P10 F14 84.5 . . ? F12 P10 F14 91.9 . . ? F11 P10 F14 98.8 . . ? F18 P10 F14 147.3 . . ? F19 P10 F14 38.4 . . ? F15 P10 F14 174.4 . . ? F16 P10 F14 122.0 . . ? F17 P10 F14 59.9 . . ? F10 P10 F13 87.4 . . ? F12 P10 F13 177.3 . . ? F11 P10 F13 92.4 . . ? F18 P10 F13 120.3 . . ? F19 P10 F13 57.0 . . ? F15 P10 F13 86.9 . . ? F16 P10 F13 31.3 . . ? F17 P10 F13 150.3 . . ? F14 P10 F13 90.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.883 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.189 #======END data_[Mo3CuSe4Br4(dmpe)3]PF6·CH2Cl2_(5) _database_code_CSD 164461 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H48 Br4 Cl2 Cu F6 Mo3 P7 Se4' _chemical_formula_weight 1665.10 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' 'F' 'F' 0.0171 0.0103 '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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.7990(5) _cell_length_b 23.8115(9) _cell_length_c 16.5128(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.7810(10) _cell_angle_gamma 90.00 _cell_volume 5032.0(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 'Dark Red' _exptl_crystal_size_max 0.171 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.122 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3144 _exptl_absorpt_coefficient_mu 7.584 _exptl_absorpt_correction_type 'Bruker SADABS' _exptl_absorpt_correction_T_min 0.7115 _exptl_absorpt_correction_T_max 0.9703 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31879 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10286 _reflns_number_gt 6299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0771P)^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 10286 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.16665(6) 0.04550(3) 0.27919(4) 0.03039(18) Uani 1 1 d . . . Mo2 Mo 0.37593(6) 0.00774(3) 0.25459(4) 0.03130(19) Uani 1 1 d . . . Mo3 Mo 0.20347(6) -0.06320(3) 0.21153(4) 0.03038(18) Uani 1 1 d . . . Cu1 Cu 0.24456(10) 0.03546(5) 0.11714(6) 0.0433(3) Uani 1 1 d . . . Se1 Se 0.25140(7) -0.03374(4) 0.35088(5) 0.0341(2) Uani 1 1 d . . . Se2 Se 0.30471(7) 0.10155(4) 0.21764(5) 0.0400(2) Uani 1 1 d . . . Se3 Se 0.35894(7) -0.04428(4) 0.12760(5) 0.0377(2) Uani 1 1 d . . . Se4 Se 0.07564(7) 0.00448(4) 0.15937(5) 0.0380(2) Uani 1 1 d . . . Br1 Br 0.01210(8) 0.01903(5) 0.37652(6) 0.0526(3) Uani 1 1 d . . . Br2 Br 0.46196(8) 0.04460(5) 0.39056(6) 0.0547(3) Uani 1 1 d . . . Br3 Br 0.27980(9) -0.16038(4) 0.26505(7) 0.0552(3) Uani 1 1 d . . . Br4 Br 0.23385(11) 0.06871(5) -0.01465(6) 0.0702(4) Uani 1 1 d . . . P1 P 0.0470(2) 0.12810(12) 0.24753(16) 0.0463(6) Uani 1 1 d . . . P2 P 0.1936(2) 0.11035(12) 0.40391(14) 0.0449(6) Uani 1 1 d . . . P3 P 0.5425(2) 0.04934(13) 0.19730(16) 0.0524(7) Uani 1 1 d . . . P4 P 0.5158(2) -0.06710(13) 0.29121(16) 0.0500(7) Uani 1 1 d . . . P5 P 0.1555(2) -0.12355(12) 0.09009(16) 0.0491(7) Uani 1 1 d . . . P6 P 0.0406(2) -0.11749(12) 0.26020(16) 0.0491(7) Uani 1 1 d . . . C1 C 0.0703(9) 0.1676(5) 0.1567(6) 0.065(3) Uani 1 1 d . . . H1A H 0.1423 0.1789 0.1555 0.098 Uiso 1 1 calc R . . H1B H 0.0265 0.2004 0.1558 0.098 Uiso 1 1 calc R . . H1C H 0.0545 0.1447 0.1103 0.098 Uiso 1 1 calc R . . C2 C -0.0921(8) 0.1111(5) 0.2399(7) 0.068(3) Uani 1 1 d . . . H2A H -0.1122 0.0897 0.2865 0.102 Uiso 1 1 calc R . . H2B H -0.1051 0.0894 0.1918 0.102 Uiso 1 1 calc R . . H2C H -0.1321 0.1452 0.2374 0.102 Uiso 1 1 calc R . . C3 C 0.0558(9) 0.1814(5) 0.3262(6) 0.064(3) Uani 1 1 d . . . H3A H 0.1105 0.2078 0.3127 0.077 Uiso 1 1 calc R . . H3B H -0.0096 0.2018 0.3280 0.077 Uiso 1 1 calc R . . C4 C 0.0795(8) 0.1561(5) 0.4103(6) 0.059(3) Uani 1 1 d . . . H4A H 0.0197 0.1347 0.4285 0.071 Uiso 1 1 calc R . . H4B H 0.0929 0.1859 0.4490 0.071 Uiso 1 1 calc R . . C5 C 0.2064(9) 0.0773(5) 0.5029(6) 0.059(3) Uani 1 1 d . . . H5A H 0.1528 0.0494 0.5087 0.088 Uiso 1 1 calc R . . H5B H 0.1992 0.1052 0.5444 0.088 Uiso 1 1 calc R . . H5C H 0.2737 0.0598 0.5079 0.088 Uiso 1 1 calc R . . C6 C 0.2998(9) 0.1613(4) 0.4011(6) 0.059(3) Uani 1 1 d . . . H6A H 0.2984 0.1804 0.3500 0.089 Uiso 1 1 calc R . . H6B H 0.3654 0.1422 0.4079 0.089 Uiso 1 1 calc R . . H6C H 0.2915 0.1880 0.4441 0.089 Uiso 1 1 calc R . . C7 C 0.5804(10) 0.1169(5) 0.2363(8) 0.084(4) Uani 1 1 d . . . H7A H 0.5243 0.1431 0.2281 0.126 Uiso 1 1 calc R . . H7B H 0.6412 0.1299 0.2085 0.126 Uiso 1 1 calc R . . H7C H 0.5961 0.1138 0.2932 0.126 Uiso 1 1 calc R . . C8 C 0.5488(10) 0.0575(6) 0.0889(6) 0.080(4) Uani 1 1 d . . . H8A H 0.4917 0.0805 0.0704 0.120 Uiso 1 1 calc R . . H8B H 0.5443 0.0213 0.0635 0.120 Uiso 1 1 calc R . . H8C H 0.6137 0.0750 0.0750 0.120 Uiso 1 1 calc R . . C9 C 0.6543(9) 0.0055(6) 0.2180(8) 0.083(4) Uani 1 1 d . . . H9A H 0.6663 -0.0183 0.1713 0.099 Uiso 1 1 calc R . . H9B H 0.7153 0.0293 0.2253 0.099 Uiso 1 1 calc R . . C10 C 0.6426(8) -0.0315(5) 0.2928(7) 0.069(3) Uani 1 1 d . . . H10A H 0.6488 -0.0086 0.3412 0.082 Uiso 1 1 calc R . . H10B H 0.6981 -0.0593 0.2942 0.082 Uiso 1 1 calc R . . C11 C 0.5044(9) -0.1037(5) 0.3883(6) 0.071(4) Uani 1 1 d . . . H11A H 0.4386 -0.1229 0.3900 0.107 Uiso 1 1 calc R . . H11B H 0.5084 -0.0769 0.4317 0.107 Uiso 1 1 calc R . . H11C H 0.5602 -0.1304 0.3941 0.107 Uiso 1 1 calc R . . C12 C 0.5411(9) -0.1221(5) 0.2172(6) 0.063(3) Uani 1 1 d . . . H12A H 0.4792 -0.1443 0.2093 0.095 Uiso 1 1 calc R . . H12B H 0.5969 -0.1456 0.2367 0.095 Uiso 1 1 calc R . . H12C H 0.5605 -0.1053 0.1668 0.095 Uiso 1 1 calc R . . C13 C 0.2521(10) -0.1734(5) 0.0592(7) 0.074(4) Uani 1 1 d . . . H13A H 0.3167 -0.1542 0.0492 0.111 Uiso 1 1 calc R . . H13B H 0.2287 -0.1918 0.0105 0.111 Uiso 1 1 calc R . . H13C H 0.2625 -0.2007 0.1012 0.111 Uiso 1 1 calc R . . C14 C 0.1250(10) -0.0881(5) -0.0039(6) 0.070(3) Uani 1 1 d . . . H14A H 0.1828 -0.0648 -0.0188 0.105 Uiso 1 1 calc R . . H14B H 0.0639 -0.0652 0.0028 0.105 Uiso 1 1 calc R . . H14C H 0.1120 -0.1154 -0.0456 0.105 Uiso 1 1 calc R . . C15 C 0.0410(10) -0.1655(5) 0.1097(7) 0.073(4) Uani 1 1 d . . . H15A H -0.0207 -0.1449 0.0922 0.088 Uiso 1 1 calc R . . H15B H 0.0443 -0.1997 0.0780 0.088 Uiso 1 1 calc R . . C16 C 0.0303(11) -0.1809(5) 0.1988(7) 0.073(4) Uani 1 1 d . . . H16A H 0.0849 -0.2071 0.2145 0.088 Uiso 1 1 calc R . . H16B H -0.0367 -0.1988 0.2075 0.088 Uiso 1 1 calc R . . C17 C 0.0384(9) -0.1396(5) 0.3641(7) 0.069(3) Uani 1 1 d . . . H17A H 0.1040 -0.1567 0.3784 0.103 Uiso 1 1 calc R . . H17B H -0.0170 -0.1662 0.3714 0.103 Uiso 1 1 calc R . . H17C H 0.0269 -0.1076 0.3983 0.103 Uiso 1 1 calc R . . C18 C -0.0861(8) -0.0859(5) 0.2434(7) 0.070(3) Uani 1 1 d . . . H18A H -0.0913 -0.0725 0.1886 0.104 Uiso 1 1 calc R . . H18B H -0.0948 -0.0550 0.2800 0.104 Uiso 1 1 calc R . . H18C H -0.1397 -0.1133 0.2525 0.104 Uiso 1 1 calc R . . P10 P -0.25960(18) -0.23929(8) 0.34767(13) 0.0522(7) Uani 1 1 d G . . F1 F -0.2599(4) -0.17438(9) 0.3289(3) 0.102(3) Uani 1 1 d G . . F2 F -0.2563(4) -0.30483(9) 0.3661(3) 0.0723(19) Uani 1 1 d G . . F3 F -0.3380(4) -0.24979(19) 0.2728(2) 0.131(4) Uani 1 1 d G . . F4 F -0.1765(4) -0.22924(18) 0.4177(3) 0.108(3) Uani 1 1 d G . . F5 F -0.3588(3) -0.2310(2) 0.4011(3) 0.126(3) Uani 1 1 d G . . F6 F -0.1639(4) -0.2465(2) 0.2864(3) 0.140(4) Uani 1 1 d G . . C20 C 0.342(4) 0.227(2) -0.037(3) 0.200 Uiso 0.50 1 d P . . Cl20 Cl 0.4527(13) 0.2076(7) -0.0268(9) 0.200 Uiso 0.50 1 d P . . Cl21 Cl 0.3239(12) 0.2307(6) 0.0818(9) 0.200 Uiso 0.50 1 d P . . C30 C 0.250(5) 0.311(2) -0.068(3) 0.200 Uiso 0.50 1 d P . . Cl30 Cl 0.1160(12) 0.3028(7) -0.0542(9) 0.200 Uiso 0.50 1 d P . . Cl31 Cl 0.2597(12) 0.3768(7) -0.0558(9) 0.200 Uiso 0.50 1 d P . . 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 0.0282(4) 0.0373(4) 0.0257(4) -0.0015(3) 0.0005(3) 0.0024(3) Mo2 0.0254(4) 0.0430(5) 0.0255(4) -0.0032(3) 0.0009(3) -0.0022(3) Mo3 0.0295(4) 0.0356(4) 0.0260(4) -0.0001(3) -0.0007(3) -0.0015(3) Cu1 0.0496(7) 0.0505(8) 0.0298(6) 0.0040(5) 0.0008(5) -0.0015(6) Se1 0.0324(5) 0.0450(6) 0.0248(4) 0.0026(4) 0.0011(4) 0.0016(4) Se2 0.0438(6) 0.0398(6) 0.0365(5) -0.0010(4) 0.0037(4) -0.0058(4) Se3 0.0363(5) 0.0495(6) 0.0274(4) -0.0046(4) 0.0043(4) 0.0008(4) Se4 0.0334(5) 0.0459(6) 0.0346(5) 0.0002(4) -0.0077(4) 0.0007(4) Br1 0.0406(6) 0.0693(8) 0.0483(6) 0.0033(5) 0.0135(5) 0.0022(5) Br2 0.0449(6) 0.0758(8) 0.0431(6) -0.0166(5) -0.0082(5) -0.0020(5) Br3 0.0629(7) 0.0460(6) 0.0566(6) 0.0061(5) -0.0025(5) 0.0067(5) Br4 0.1001(10) 0.0747(9) 0.0357(6) 0.0133(5) 0.0019(6) 0.0026(7) P1 0.0454(15) 0.0489(17) 0.0445(15) 0.0001(12) -0.0037(12) 0.0121(12) P2 0.0477(15) 0.0526(17) 0.0345(13) -0.0109(11) -0.0019(12) 0.0064(13) P3 0.0354(14) 0.078(2) 0.0442(15) -0.0004(14) 0.0070(12) -0.0136(13) P4 0.0381(14) 0.069(2) 0.0429(14) -0.0059(13) -0.0051(12) 0.0143(13) P5 0.0595(18) 0.0478(17) 0.0398(14) -0.0084(12) -0.0083(13) -0.0091(13) P6 0.0398(15) 0.0581(18) 0.0493(15) 0.0072(13) 0.0015(12) -0.0128(13) C1 0.066(8) 0.068(8) 0.061(7) 0.021(6) 0.008(6) -0.003(6) C2 0.040(6) 0.096(10) 0.067(8) 0.009(7) -0.002(6) 0.020(6) C3 0.072(8) 0.054(7) 0.065(7) -0.002(6) -0.012(6) 0.024(6) C4 0.054(7) 0.061(7) 0.062(7) -0.025(6) 0.003(6) 0.015(6) C5 0.058(7) 0.080(8) 0.039(6) 0.001(5) -0.005(5) 0.011(6) C6 0.073(8) 0.049(7) 0.056(7) -0.017(5) -0.002(6) -0.007(6) C7 0.067(8) 0.094(10) 0.091(10) -0.006(8) 0.003(7) -0.047(8) C8 0.072(9) 0.114(12) 0.054(7) 0.016(7) 0.019(6) -0.015(8) C9 0.039(7) 0.122(12) 0.087(9) 0.005(8) 0.025(6) 0.004(7) C10 0.030(6) 0.105(10) 0.071(8) -0.003(7) -0.008(5) 0.018(6) C11 0.070(8) 0.085(9) 0.058(7) 0.002(6) -0.012(6) 0.024(7) C12 0.057(7) 0.085(9) 0.048(6) -0.010(6) 0.000(5) 0.031(6) C13 0.108(11) 0.052(7) 0.063(7) -0.026(6) -0.008(7) 0.012(7) C14 0.092(9) 0.076(9) 0.042(6) -0.006(6) -0.019(6) -0.012(7) C15 0.070(8) 0.072(9) 0.078(9) -0.015(7) -0.009(7) -0.033(7) C16 0.088(9) 0.064(8) 0.068(8) -0.002(6) 0.005(7) -0.035(7) C17 0.060(7) 0.077(9) 0.071(8) 0.027(7) 0.006(6) -0.014(6) C18 0.040(6) 0.090(9) 0.079(8) 0.022(7) -0.005(6) -0.013(6) P10 0.0595(18) 0.0373(16) 0.0598(17) 0.0022(13) -0.0007(14) -0.0121(13) F1 0.111(6) 0.049(4) 0.144(7) 0.023(4) -0.033(6) -0.015(4) F2 0.103(5) 0.034(3) 0.080(4) 0.003(3) 0.004(4) -0.005(3) F3 0.181(10) 0.097(6) 0.113(7) 0.038(5) -0.085(7) -0.061(6) F4 0.125(7) 0.082(6) 0.116(6) 0.010(5) -0.049(6) -0.031(5) F5 0.091(6) 0.120(8) 0.168(9) -0.020(6) 0.057(6) 0.004(5) F6 0.156(9) 0.101(7) 0.167(9) 0.019(6) 0.101(7) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Se2 2.4465(12) . ? Mo1 Se1 2.4704(11) . ? Mo1 Se4 2.4823(11) . ? Mo1 P1 2.543(3) . ? Mo1 P2 2.594(3) . ? Mo1 Br1 2.6419(12) . ? Mo1 Mo2 2.8597(10) . ? Mo1 Mo3 2.8607(10) . ? Mo1 Cu1 2.8783(13) . ? Mo2 Se3 2.4427(11) . ? Mo2 Se1 2.4725(11) . ? Mo2 Se2 2.4854(12) . ? Mo2 P3 2.545(3) . ? Mo2 P4 2.591(3) . ? Mo2 Br2 2.6374(12) . ? Mo2 Mo3 2.8616(10) . ? Mo2 Cu1 2.8827(13) . ? Mo3 Se4 2.4449(12) . ? Mo3 Se1 2.4750(11) . ? Mo3 Se3 2.4815(11) . ? Mo3 P5 2.536(3) . ? Mo3 P6 2.591(3) . ? Mo3 Br3 2.6584(13) . ? Mo3 Cu1 2.8718(14) . ? Cu1 Br4 2.3181(15) . ? Cu1 Se4 2.3971(15) . ? Cu1 Se3 2.4023(15) . ? Cu1 Se2 2.4059(15) . ? P1 C1 1.799(10) . ? P1 C3 1.818(11) . ? P1 C2 1.828(11) . ? P2 C5 1.820(10) . ? P2 C6 1.822(11) . ? P2 C4 1.826(10) . ? P3 C7 1.798(12) . ? P3 C9 1.800(12) . ? P3 C8 1.804(11) . ? P4 C12 1.823(10) . ? P4 C10 1.830(11) . ? P4 C11 1.832(11) . ? P5 C13 1.793(11) . ? P5 C14 1.805(10) . ? P5 C15 1.807(11) . ? P6 C17 1.796(11) . ? P6 C18 1.806(11) . ? P6 C16 1.822(11) . ? C3 C4 1.540(14) . ? C9 C10 1.527(16) . ? C15 C16 1.524(15) . ? P10 F5 1.5683 . ? P10 F1 1.5764 . ? P10 F4 1.5788 . ? P10 F2 1.5903 . ? P10 F3 1.6013 . ? P10 F6 1.6078 . ? C20 Cl20 1.50(5) . ? C20 Cl21 1.99(5) . ? C30 Cl31 1.59(5) . ? C30 Cl30 1.74(6) . ? 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 Se2 Mo1 Se1 107.50(4) . . ? Se2 Mo1 Se4 102.55(4) . . ? Se1 Mo1 Se4 106.24(4) . . ? Se2 Mo1 P1 85.93(7) . . ? Se1 Mo1 P1 161.55(7) . . ? Se4 Mo1 P1 82.28(7) . . ? Se2 Mo1 P2 85.17(7) . . ? Se1 Mo1 P2 91.22(7) . . ? Se4 Mo1 P2 157.39(7) . . ? P1 Mo1 P2 77.06(9) . . ? Se2 Mo1 Br1 159.04(5) . . ? Se1 Mo1 Br1 81.59(4) . . ? Se4 Mo1 Br1 92.52(4) . . ? P1 Mo1 Br1 81.70(7) . . ? P2 Mo1 Br1 75.62(7) . . ? Se2 Mo1 Mo2 55.20(3) . . ? Se1 Mo1 Mo2 54.69(3) . . ? Se4 Mo1 Mo2 101.15(3) . . ? P1 Mo1 Mo2 140.96(7) . . ? P2 Mo1 Mo2 100.67(6) . . ? Br1 Mo1 Mo2 136.21(4) . . ? Se2 Mo1 Mo3 101.98(4) . . ? Se1 Mo1 Mo3 54.73(3) . . ? Se4 Mo1 Mo3 53.90(3) . . ? P1 Mo1 Mo3 136.18(7) . . ? P2 Mo1 Mo3 145.89(7) . . ? Br1 Mo1 Mo3 98.66(4) . . ? Mo2 Mo1 Mo3 60.03(3) . . ? Se2 Mo1 Cu1 52.97(3) . . ? Se1 Mo1 Cu1 103.10(4) . . ? Se4 Mo1 Cu1 52.49(3) . . ? P1 Mo1 Cu1 95.08(7) . . ? P2 Mo1 Cu1 138.04(7) . . ? Br1 Mo1 Cu1 144.84(4) . . ? Mo2 Mo1 Cu1 60.32(3) . . ? Mo3 Mo1 Cu1 60.05(3) . . ? Se3 Mo2 Se1 107.39(4) . . ? Se3 Mo2 Se2 102.53(4) . . ? Se1 Mo2 Se2 106.22(4) . . ? Se3 Mo2 P3 86.76(7) . . ? Se1 Mo2 P3 160.95(7) . . ? Se2 Mo2 P3 82.25(8) . . ? Se3 Mo2 P4 84.53(7) . . ? Se1 Mo2 P4 91.40(7) . . ? Se2 Mo2 P4 157.69(8) . . ? P3 Mo2 P4 77.00(10) . . ? Se3 Mo2 Br2 158.56(5) . . ? Se1 Mo2 Br2 81.42(4) . . ? Se2 Mo2 Br2 93.29(4) . . ? P3 Mo2 Br2 81.08(7) . . ? P4 Mo2 Br2 75.59(7) . . ? Se3 Mo2 Mo1 102.05(4) . . ? Se1 Mo2 Mo1 54.62(3) . . ? Se2 Mo2 Mo1 53.93(3) . . ? P3 Mo2 Mo1 136.18(8) . . ? P4 Mo2 Mo1 145.93(7) . . ? Br2 Mo2 Mo1 98.94(4) . . ? Se3 Mo2 Mo3 55.11(3) . . ? Se1 Mo2 Mo3 54.70(3) . . ? Se2 Mo2 Mo3 100.98(4) . . ? P3 Mo2 Mo3 141.69(7) . . ? P4 Mo2 Mo3 100.37(7) . . ? Br2 Mo2 Mo3 136.02(4) . . ? Mo1 Mo2 Mo3 60.00(3) . . ? Se3 Mo2 Cu1 52.85(4) . . ? Se1 Mo2 Cu1 102.92(4) . . ? Se2 Mo2 Cu1 52.62(4) . . ? P3 Mo2 Cu1 95.78(7) . . ? P4 Mo2 Cu1 137.29(7) . . ? Br2 Mo2 Cu1 145.72(5) . . ? Mo1 Mo2 Cu1 60.16(3) . . ? Mo3 Mo2 Cu1 59.99(3) . . ? Se4 Mo3 Se1 107.27(4) . . ? Se4 Mo3 Se3 102.80(4) . . ? Se1 Mo3 Se3 106.10(4) . . ? Se4 Mo3 P5 86.63(7) . . ? Se1 Mo3 P5 161.85(8) . . ? Se3 Mo3 P5 81.30(7) . . ? Se4 Mo3 P6 84.30(7) . . ? Se1 Mo3 P6 92.48(7) . . ? Se3 Mo3 P6 156.75(8) . . ? P5 Mo3 P6 77.01(9) . . ? Se4 Mo3 Br3 158.76(5) . . ? Se1 Mo3 Br3 81.51(4) . . ? Se3 Mo3 Br3 92.86(4) . . ? P5 Mo3 Br3 81.58(7) . . ? P6 Mo3 Br3 75.88(7) . . ? Se4 Mo3 Mo1 55.12(3) . . ? Se1 Mo3 Mo1 54.58(3) . . ? Se3 Mo3 Mo1 101.04(4) . . ? P5 Mo3 Mo1 141.46(7) . . ? P6 Mo3 Mo1 101.11(7) . . ? Br3 Mo3 Mo1 136.01(4) . . ? Se4 Mo3 Mo2 102.04(4) . . ? Se1 Mo3 Mo2 54.62(3) . . ? Se3 Mo3 Mo2 53.84(3) . . ? P5 Mo3 Mo2 135.14(7) . . ? P6 Mo3 Mo2 147.02(7) . . ? Br3 Mo3 Mo2 98.77(4) . . ? Mo1 Mo3 Mo2 59.97(3) . . ? Se4 Mo3 Cu1 52.86(4) . . ? Se1 Mo3 Cu1 103.17(4) . . ? Se3 Mo3 Cu1 52.72(4) . . ? P5 Mo3 Cu1 94.51(7) . . ? P6 Mo3 Cu1 136.95(7) . . ? Br3 Mo3 Cu1 145.42(4) . . ? Mo1 Mo3 Cu1 60.28(3) . . ? Mo2 Mo3 Cu1 60.37(3) . . ? Br4 Cu1 Se4 109.65(6) . . ? Br4 Cu1 Se3 111.45(6) . . ? Se4 Cu1 Se3 106.68(5) . . ? Br4 Cu1 Se2 116.00(6) . . ? Se4 Cu1 Se2 106.38(5) . . ? Se3 Cu1 Se2 106.17(5) . . ? Br4 Cu1 Mo3 141.26(6) . . ? Se4 Cu1 Mo3 54.39(3) . . ? Se3 Cu1 Mo3 55.27(4) . . ? Se2 Cu1 Mo3 102.70(4) . . ? Br4 Cu1 Mo1 145.85(6) . . ? Se4 Cu1 Mo1 55.23(3) . . ? Se3 Cu1 Mo1 102.55(4) . . ? Se2 Cu1 Mo1 54.27(3) . . ? Mo3 Cu1 Mo1 59.67(3) . . ? Br4 Cu1 Mo2 147.54(6) . . ? Se4 Cu1 Mo2 102.66(4) . . ? Se3 Cu1 Mo2 54.13(3) . . ? Se2 Cu1 Mo2 55.18(4) . . ? Mo3 Cu1 Mo2 59.64(3) . . ? Mo1 Cu1 Mo2 59.52(3) . . ? Mo1 Se1 Mo2 70.70(3) . . ? Mo1 Se1 Mo3 70.68(3) . . ? Mo2 Se1 Mo3 70.68(3) . . ? Cu1 Se2 Mo1 72.76(4) . . ? Cu1 Se2 Mo2 72.20(4) . . ? Mo1 Se2 Mo2 70.87(3) . . ? Cu1 Se3 Mo2 73.02(4) . . ? Cu1 Se3 Mo3 72.01(4) . . ? Mo2 Se3 Mo3 71.05(3) . . ? Cu1 Se4 Mo3 72.75(4) . . ? Cu1 Se4 Mo1 72.27(4) . . ? Mo3 Se4 Mo1 70.98(3) . . ? C1 P1 C3 102.8(5) . . ? C1 P1 C2 103.3(5) . . ? C3 P1 C2 104.8(6) . . ? C1 P1 Mo1 118.0(4) . . ? C3 P1 Mo1 111.2(3) . . ? C2 P1 Mo1 115.2(4) . . ? C5 P2 C6 104.6(5) . . ? C5 P2 C4 105.5(5) . . ? C6 P2 C4 101.7(5) . . ? C5 P2 Mo1 117.7(4) . . ? C6 P2 Mo1 117.9(3) . . ? C4 P2 Mo1 107.6(3) . . ? C7 P3 C9 103.9(6) . . ? C7 P3 C8 104.1(6) . . ? C9 P3 C8 101.8(6) . . ? C7 P3 Mo2 116.0(4) . . ? C9 P3 Mo2 111.8(4) . . ? C8 P3 Mo2 117.4(4) . . ? C12 P4 C10 100.2(6) . . ? C12 P4 C11 105.2(5) . . ? C10 P4 C11 106.8(5) . . ? C12 P4 Mo2 117.8(3) . . ? C10 P4 Mo2 107.1(4) . . ? C11 P4 Mo2 117.9(4) . . ? C13 P5 C14 101.9(6) . . ? C13 P5 C15 104.4(6) . . ? C14 P5 C15 104.3(6) . . ? C13 P5 Mo3 116.1(4) . . ? C14 P5 Mo3 117.5(4) . . ? C15 P5 Mo3 111.1(4) . . ? C17 P6 C18 104.1(5) . . ? C17 P6 C16 106.7(6) . . ? C18 P6 C16 101.7(6) . . ? C17 P6 Mo3 117.8(4) . . ? C18 P6 Mo3 118.0(4) . . ? C16 P6 Mo3 107.1(4) . . ? C4 C3 P1 112.4(7) . . ? C3 C4 P2 109.2(7) . . ? C10 C9 P3 113.7(7) . . ? C9 C10 P4 110.6(8) . . ? C16 C15 P5 112.9(8) . . ? C15 C16 P6 109.3(8) . . ? F5 P10 F1 89.3 . . ? F5 P10 F4 96.4 . . ? F1 P10 F4 89.7 . . ? F5 P10 F2 92.0 . . ? F1 P10 F2 178.6 . . ? F4 P10 F2 89.6 . . ? F5 P10 F3 87.2 . . ? F1 P10 F3 90.1 . . ? F4 P10 F3 176.5 . . ? F2 P10 F3 90.6 . . ? F5 P10 F6 175.2 . . ? F1 P10 F6 88.9 . . ? F4 P10 F6 88.1 . . ? F2 P10 F6 89.8 . . ? F3 P10 F6 88.4 . . ? Cl20 C20 Cl21 91(3) . . ? Cl31 C30 Cl30 99(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.497 _refine_diff_density_min -1.161 _refine_diff_density_rms 0.163