#Copyright The Royal Society of Chemistry, 1998 data_hansi14 # 1. SUBMISSION DETAILS _publ_contact_author ; Alexander C. Filippou Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; _publ_contact_author_phone '# 49 30 2093-7385' _publ_contact_author_fax '# 49 30 2093-6939' _publ_contact_author_email 'filippou@chemie.hu-berlin.de' _publ_requested_journal ? _publ_requested_coeditor_name ; Johannes G. Winter, Gabriele Kociok-K\"ohn, Isolde Hinz ; _publ_contact_letter ; Dear Professor Orpen, This cif-file includes the three structures of our publication: Dimetallagermanes of Molybdenum and Tungsten: Synthesis, Structure and Reactions, which has been sent today to Dalton Transactions. sincerely, A. C. Filippou ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Dimetallagermanes of Molybdenum and Tungsten: Synthesis, Structure and Reactions ; loop_ _publ_author_name _publ_author_address 'Alexander C. Filippou' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Johannes G. Winter' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Gabriele Kociok-K\"ohn' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Isolde Hinz' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; #======================================================================= _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H10 Cl2 Ge O6 W2' _chemical_formula_structural '[(C5 H5) W (C O)3)]2 Ge Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C16 H10 Cl2 Ge O6 W2' _chemical_formula_weight 809.45 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'W' 'W' -1.4210 6.8720 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.370(3) _cell_length_b 14.848(4) _cell_length_c 23.811(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4019.8(21) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 13.7 _cell_measurement_theta_max 15.2 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour 'orange yellow' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.675 _exptl_crystal_density_method ? _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 12.693 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'STOE Stadi4 Diffractometer' _diffrn_measurement_method '\w-2\q' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5.1 _diffrn_reflns_number 3532 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3532 _reflns_number_observed 2979 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1995)' _computing_cell_refinement 'STADI4 (STOE, 1995)' _computing_data_reduction 'X-RED, (STOE, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; L.Zsolnai, H.Pritzkow, ZORTEP, ORTEP program for PC, Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 20 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factors etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3512 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_obs 0.0391 _refine_ls_wR_factor_all 0.1092 _refine_ls_wR_factor_obs 0.0969 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.048 _refine_ls_restrained_S_all 1.080 _refine_ls_restrained_S_obs 1.048 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.16540(3) 0.05246(2) 0.13527(2) 0.04617(14) Uani 1 d . . C1 C 0.3053(11) 0.0858(16) 0.0680(6) 0.121(7) Uani 1 d . . H1 H 0.2842(11) 0.0894(16) 0.0303(6) 0.080 Uiso 1 calc R . C2 C 0.3070(10) 0.1566(10) 0.1070(8) 0.090(4) Uani 1 d . . H2 H 0.2865(10) 0.2162(10) 0.0999(8) 0.080 Uiso 1 calc R . C3 C 0.3450(9) 0.1216(8) 0.1582(6) 0.073(3) Uani 1 d . . H3 H 0.3549(9) 0.1542(8) 0.1913(6) 0.080 Uiso 1 calc R . C4 C 0.3656(9) 0.0294(9) 0.1517(7) 0.081(4) Uani 1 d . . H4 H 0.3909(9) -0.0097(9) 0.1797(7) 0.080 Uiso 1 calc R . C5 C 0.3425(10) 0.0065(10) 0.0976(7) 0.081(3) Uani 1 d . . H5 H 0.3496(10) -0.0509(10) 0.0823(7) 0.080 Uiso 1 calc R . C6 C 0.1351(9) -0.0711(7) 0.1649(5) 0.064(3) Uani 1 d . . O1 O 0.1190(8) -0.1414(5) 0.1814(4) 0.090(3) Uani 1 d . . C7 C 0.0365(8) 0.0095(6) 0.0854(4) 0.052(2) Uani 1 d . . O2 O -0.0364(6) -0.0174(4) 0.0573(3) 0.066(2) Uani 1 d . . C8 C 0.0970(8) 0.0756(7) 0.2105(5) 0.057(2) Uani 1 d . . O3 O 0.0691(7) 0.0866(6) 0.2555(3) 0.079(2) Uani 1 d . . Ge Ge 0.01499(8) 0.18835(6) 0.12158(4) 0.0454(2) Uani 1 d . . Cl1 Cl 0.0797(2) 0.2709(2) 0.04801(12) 0.0729(7) Uani 1 d . . Cl2 Cl 0.0690(3) 0.2896(2) 0.18747(13) 0.0765(8) Uani 1 d . . W2 W -0.21804(3) 0.19127(2) 0.11373(2) 0.04666(14) Uani 1 d . . C9 C -0.1979(13) 0.3450(8) 0.1346(8) 0.090(4) Uani 1 d . . H9 H -0.1249(13) 0.3732(8) 0.1344(8) 0.080 Uiso 1 calc R . C10 C -0.2755(15) 0.3377(8) 0.0906(6) 0.094(5) Uani 1 d . . H10 H -0.2635(15) 0.3596(8) 0.0545(6) 0.080 Uiso 1 calc R . C11 C -0.3741(13) 0.2926(9) 0.1089(6) 0.080(3) Uani 1 d . . H11 H -0.4402(13) 0.2803(9) 0.0872(6) 0.080 Uiso 1 calc R . C12 C -0.3605(11) 0.2692(8) 0.1622(6) 0.081(3) Uani 1 d . . H12 H -0.4139(11) 0.2372(8) 0.1840(6) 0.080 Uiso 1 calc R . C13 C -0.2522(15) 0.3011(7) 0.1795(5) 0.087(4) Uani 1 d . . H13 H -0.2205(15) 0.2945(7) 0.2153(5) 0.080 Uiso 1 calc R . C14 C -0.1618(8) 0.1661(7) 0.0359(4) 0.054(2) Uani 1 d . . O4 O -0.1379(7) 0.1540(6) -0.0087(3) 0.077(2) Uani 1 d . . C15 C -0.3254(9) 0.0944(8) 0.0857(5) 0.068(3) Uani 1 d . . O5 O -0.3856(8) 0.0389(6) 0.0704(5) 0.098(3) Uani 1 d . . C16 C -0.1835(7) 0.0905(6) 0.1653(4) 0.054(2) Uani 1 d . . O6 O -0.1668(6) 0.0325(5) 0.1972(4) 0.075(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0434(2) 0.0415(2) 0.0536(2) 0.00092(15) 0.00131(14) 0.00070(14) C1 0.066(7) 0.236(22) 0.061(8) 0.010(12) 0.008(6) -0.053(11) C2 0.051(6) 0.071(8) 0.147(14) 0.029(9) -0.001(7) -0.012(6) C3 0.059(6) 0.075(7) 0.086(8) -0.017(7) -0.001(6) -0.016(5) C4 0.046(5) 0.077(8) 0.120(11) 0.025(8) -0.007(6) 0.003(5) C5 0.061(7) 0.080(8) 0.102(10) -0.018(8) 0.013(6) -0.001(6) C6 0.056(5) 0.061(6) 0.076(7) 0.002(6) -0.007(5) 0.008(5) O1 0.089(6) 0.056(5) 0.125(8) 0.033(5) -0.006(5) -0.003(4) C7 0.058(5) 0.042(5) 0.056(5) -0.002(4) -0.005(4) -0.005(4) O2 0.073(5) 0.050(4) 0.075(5) -0.008(3) -0.009(4) -0.005(3) C8 0.054(5) 0.060(6) 0.059(6) 0.005(5) -0.001(4) -0.001(4) O3 0.082(5) 0.102(6) 0.053(5) 0.000(4) 0.003(4) -0.007(5) Ge 0.0484(5) 0.0393(5) 0.0487(5) 0.0012(4) 0.0008(4) -0.0007(4) Cl1 0.0699(15) 0.074(2) 0.075(2) 0.0245(14) 0.0062(13) -0.0102(13) Cl2 0.098(2) 0.0544(14) 0.078(2) -0.0134(13) -0.020(2) -0.0029(14) W2 0.0465(2) 0.0422(2) 0.0512(2) 0.00367(15) 0.00499(14) 0.00773(14) C9 0.078(8) 0.047(6) 0.146(14) -0.006(8) -0.002(8) 0.010(6) C10 0.148(13) 0.050(6) 0.084(9) 0.026(6) 0.037(9) 0.042(8) C11 0.083(8) 0.075(7) 0.083(9) 0.012(7) -0.003(6) 0.032(7) C12 0.074(7) 0.055(6) 0.115(11) 0.004(7) 0.016(7) 0.009(6) C13 0.141(12) 0.057(7) 0.063(7) -0.008(6) -0.010(8) 0.034(8) C14 0.049(5) 0.057(5) 0.058(6) 0.005(5) 0.005(4) 0.013(4) O4 0.083(5) 0.092(6) 0.056(5) -0.011(4) -0.002(4) 0.020(4) C15 0.052(5) 0.059(6) 0.093(8) -0.002(6) -0.004(5) 0.003(5) O5 0.073(5) 0.088(6) 0.133(9) 0.001(6) -0.023(5) -0.016(5) C16 0.045(4) 0.048(5) 0.068(6) 0.005(5) 0.013(4) 0.000(4) O6 0.074(5) 0.069(5) 0.081(5) 0.033(4) 0.000(4) 0.002(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 W1 C8 1.984(11) . ? W1 C7 1.991(9) . ? W1 C6 1.996(11) . ? W1 C5 2.307(11) . ? W1 C1 2.311(12) . ? W1 C2 2.332(11) . ? W1 C4 2.335(11) . ? W1 C3 2.350(10) . ? W1 Ge 2.6649(11) . ? C1 C2 1.40(2) . ? C1 C5 1.44(2) . ? C2 C3 1.40(2) . ? C3 C4 1.40(2) . ? C4 C5 1.36(2) . ? C6 O1 1.130(13) . ? C7 O2 1.138(10) . ? C8 O3 1.129(12) . ? Ge Cl2 2.258(3) . ? Ge Cl1 2.261(3) . ? Ge W2 2.6565(12) . ? W2 C16 1.975(10) . ? W2 C14 1.995(10) . ? W2 C15 2.001(11) . ? W2 C13 2.294(11) . ? W2 C12 2.301(12) . ? W2 C11 2.329(12) . ? W2 C10 2.336(10) . ? W2 C9 2.348(12) . ? C9 C10 1.37(2) . ? C9 C13 1.40(2) . ? C10 C11 1.38(2) . ? C11 C12 1.32(2) . ? C12 C13 1.38(2) . ? C14 O4 1.110(12) . ? C15 O5 1.132(13) . ? C16 O6 1.163(12) . ? 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 C8 W1 C7 107.8(4) . . ? C8 W1 C6 76.8(4) . . ? C7 W1 C6 77.8(4) . . ? C8 W1 C5 138.1(5) . . ? C7 W1 C5 108.4(5) . . ? C6 W1 C5 90.9(5) . . ? C8 W1 C1 149.2(5) . . ? C7 W1 C1 99.3(5) . . ? C6 W1 C1 124.1(7) . . ? C5 W1 C1 36.2(6) . . ? C8 W1 C2 114.6(5) . . ? C7 W1 C2 123.3(5) . . ? C6 W1 C2 146.2(4) . . ? C5 W1 C2 58.8(5) . . ? C1 W1 C2 35.2(5) . . ? C8 W1 C4 104.8(5) . . ? C7 W1 C4 140.4(5) . . ? C6 W1 C4 88.5(4) . . ? C5 W1 C4 34.0(5) . . ? C1 W1 C4 58.5(5) . . ? C2 W1 C4 58.2(4) . . ? C8 W1 C3 93.1(4) . . ? C7 W1 C3 156.7(4) . . ? C6 W1 C3 118.0(4) . . ? C5 W1 C3 57.4(5) . . ? C1 W1 C3 58.0(5) . . ? C2 W1 C3 34.7(5) . . ? C4 W1 C3 34.7(4) . . ? C8 W1 Ge 74.2(3) . . ? C7 W1 Ge 72.4(3) . . ? C6 W1 Ge 128.9(3) . . ? C5 W1 Ge 137.4(4) . . ? C1 W1 Ge 101.2(6) . . ? C2 W1 Ge 84.6(3) . . ? C4 W1 Ge 139.2(3) . . ? C3 W1 Ge 104.8(3) . . ? C2 C1 C5 106.6(12) . . ? C2 C1 W1 73.2(7) . . ? C5 C1 W1 71.7(7) . . ? C3 C2 C1 107.6(13) . . ? C3 C2 W1 73.4(7) . . ? C1 C2 W1 71.6(7) . . ? C2 C3 C4 108.6(13) . . ? C2 C3 W1 72.0(7) . . ? C4 C3 W1 72.0(6) . . ? C5 C4 C3 108.6(12) . . ? C5 C4 W1 71.9(7) . . ? C3 C4 W1 73.2(6) . . ? C4 C5 C1 108.5(13) . . ? C4 C5 W1 74.1(7) . . ? C1 C5 W1 72.0(7) . . ? O1 C6 W1 179.2(11) . . ? O2 C7 W1 178.1(8) . . ? O3 C8 W1 172.9(9) . . ? Cl2 Ge Cl1 95.11(13) . . ? Cl2 Ge W2 108.01(9) . . ? Cl1 Ge W2 105.13(8) . . ? Cl2 Ge W1 104.16(9) . . ? Cl1 Ge W1 107.25(8) . . ? W2 Ge W1 131.38(4) . . ? C16 W2 C14 111.8(4) . . ? C16 W2 C15 77.5(4) . . ? C14 W2 C15 75.6(4) . . ? C16 W2 C13 98.5(4) . . ? C14 W2 C13 145.2(5) . . ? C15 W2 C13 129.5(5) . . ? C16 W2 C12 102.1(4) . . ? C14 W2 C12 141.7(4) . . ? C15 W2 C12 95.7(5) . . ? C13 W2 C12 35.0(5) . . ? C16 W2 C11 132.2(4) . . ? C14 W2 C11 108.6(4) . . ? C15 W2 C11 89.0(5) . . ? C13 W2 C11 56.3(5) . . ? C12 W2 C11 33.2(4) . . ? C16 W2 C10 155.1(4) . . ? C14 W2 C10 92.6(4) . . ? C15 W2 C10 114.8(5) . . ? C13 W2 C10 56.8(5) . . ? C12 W2 C10 56.9(5) . . ? C11 W2 C10 34.3(5) . . ? C16 W2 C9 125.9(5) . . ? C14 W2 C9 110.3(5) . . ? C15 W2 C9 146.0(5) . . ? C13 W2 C9 35.0(5) . . ? C12 W2 C9 58.2(5) . . ? C11 W2 C9 57.1(5) . . ? C10 W2 C9 34.1(5) . . ? C16 W2 Ge 75.3(2) . . ? C14 W2 Ge 75.1(3) . . ? C15 W2 Ge 128.3(3) . . ? C13 W2 Ge 97.6(4) . . ? C12 W2 Ge 132.4(4) . . ? C11 W2 Ge 140.7(4) . . ? C10 W2 Ge 108.1(4) . . ? C9 W2 Ge 84.5(3) . . ? C10 C9 C13 105.3(13) . . ? C10 C9 W2 72.5(7) . . ? C13 C9 W2 70.4(7) . . ? C9 C10 C11 108.7(13) . . ? C9 C10 W2 73.4(7) . . ? C11 C10 W2 72.5(7) . . ? C12 C11 C10 109.6(13) . . ? C12 C11 W2 72.2(7) . . ? C10 C11 W2 73.1(7) . . ? C11 C12 C13 107.5(12) . . ? C11 C12 W2 74.6(8) . . ? C13 C12 W2 72.2(7) . . ? C12 C13 C9 109.0(13) . . ? C12 C13 W2 72.8(7) . . ? C9 C13 W2 74.6(8) . . ? O4 C14 W2 175.2(8) . . ? O5 C15 W2 179.2(10) . . ? O6 C16 W2 177.1(8) . . ? _refine_diff_density_max 0.940 _refine_diff_density_min -2.226 _refine_diff_density_rms 0.225 #======================================================================= #=END data_hansi16 # 1. SUBMISSION DETAILS _publ_contact_author ; Alexander C. Filippou Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; _publ_contact_author_phone '# 49 30 2093-7385' _publ_contact_author_fax '# 49 30 2093-6939' _publ_contact_author_email 'filippou@chemie.hu-berlin.de' _publ_requested_journal ? _publ_requested_coeditor_name ; Johannes G. Winter, Gabriele Kociok-K\"ohn, Isolde Hinz' ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Dimetallagermanes of Molybdenum and Tungsten: Synthesis, Structure and Reactions ; loop_ _publ_author_name _publ_author_address 'Alexander C. Filippou' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Johannes G. Winter' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Gabriele Kociok-K\"ohn' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Isolde Hinz' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; #======================================================================= _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H10 Cl2 Ge Mo2 O6' _chemical_formula_structural '((C5 H5) Mo (C O)3)2 Ge Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C16 H10 Cl2 Ge Mo2 O6' _chemical_formula_weight 633.63 _chemical_melting_point ? _chemical_compound_source ? 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.8250 0.6880 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.295(2) _cell_length_b 14.832(3) _cell_length_c 23.680(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3967.1(14) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 26.3 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.122 _exptl_crystal_density_method ? _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 2.892 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Stoe IPDS' _diffrn_measurement_method '\f-rotation' _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28391 _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_sigmaI/netI 0.0537 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.25 _reflns_number_total 3968 _reflns_number_observed 3042 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'IPDS (STOE, 1996)' _computing_cell_refinement 'IPDS (STOE, 1996)' _computing_data_reduction 'IPDS (Software 2.65, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; L.Zsolnai, H.Pritzkow, ZORTEP, ORTEP program for PC,Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 26 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factors etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00154(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3942 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0532 _refine_ls_R_factor_obs 0.0367 _refine_ls_wR_factor_all 0.1188 _refine_ls_wR_factor_obs 0.0855 _refine_ls_goodness_of_fit_all 0.939 _refine_ls_goodness_of_fit_obs 1.023 _refine_ls_restrained_S_all 1.235 _refine_ls_restrained_S_obs 1.023 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.16737(3) 0.04957(2) 0.135114(15) 0.02723(13) Uani 1 d . . C1 C 0.3115(5) 0.0804(5) 0.0671(2) 0.067(2) Uani 1 d . . H1 H 0.2927(5) 0.0830(5) 0.0289(2) 0.080 Uiso 1 calc R . C2 C 0.3115(5) 0.1542(4) 0.1058(3) 0.058(2) Uani 1 d . . H2 H 0.2917(5) 0.2136(4) 0.0975(3) 0.080 Uiso 1 calc R . C3 C 0.3465(4) 0.1215(3) 0.1582(2) 0.0456(12) Uani 1 d . . H3 H 0.3546(4) 0.1553(3) 0.1911(2) 0.080 Uiso 1 calc R . C4 C 0.3672(4) 0.0290(4) 0.1531(2) 0.0445(12) Uani 1 d . . H4 H 0.3917(4) -0.0092(4) 0.1820(2) 0.080 Uiso 1 calc R . C5 C 0.3453(4) 0.0031(4) 0.0974(2) 0.0530(14) Uani 1 d . . H5 H 0.3519(4) -0.0549(4) 0.0829(2) 0.080 Uiso 1 calc R . C6 C 0.1357(4) -0.0750(3) 0.1637(2) 0.0409(11) Uani 1 d . . O1 O 0.1183(3) -0.1458(2) 0.1804(2) 0.0581(10) Uani 1 d . . C7 C 0.0373(4) 0.0081(3) 0.0846(2) 0.0329(9) Uani 1 d . . O2 O -0.0376(3) -0.0189(2) 0.05650(13) 0.0399(7) Uani 1 d . . C8 C 0.0987(4) 0.0732(3) 0.2105(2) 0.0376(10) Uani 1 d . . O3 O 0.0666(3) 0.0843(2) 0.25587(14) 0.0500(8) Uani 1 d . . Ge Ge 0.01631(4) 0.18590(3) 0.12099(2) 0.02744(14) Uani 1 d . . Cl1 Cl 0.08154(10) 0.26729(9) 0.04617(5) 0.0449(3) Uani 1 d . . Cl2 Cl 0.07165(12) 0.28788(8) 0.18674(5) 0.0469(3) Uani 1 d . . Mo2 Mo -0.21806(3) 0.18920(2) 0.11359(2) 0.02788(13) Uani 1 d . . C9 C -0.1956(5) 0.3430(3) 0.1322(3) 0.058(2) Uani 1 d . . H9 H -0.1217(5) 0.3703(3) 0.1297(3) 0.080 Uiso 1 calc R . C10 C -0.2792(5) 0.3355(3) 0.0882(2) 0.057(2) Uani 1 d . . H10 H -0.2706(5) 0.3580(3) 0.0518(2) 0.080 Uiso 1 calc R . C11 C -0.3768(5) 0.2885(4) 0.1087(2) 0.0506(13) Uani 1 d . . H11 H -0.4438(5) 0.2729(4) 0.0881(2) 0.080 Uiso 1 calc R . C12 C -0.3568(5) 0.2685(3) 0.1659(2) 0.0480(13) Uani 1 d . . H12 H -0.4087(5) 0.2386(3) 0.1900(2) 0.080 Uiso 1 calc R . C13 C -0.2437(5) 0.3021(3) 0.1802(2) 0.0528(14) Uani 1 d . . H13 H -0.2075(5) 0.2977(3) 0.2154(2) 0.080 Uiso 1 calc R . C14 C -0.1614(4) 0.1641(3) 0.0356(2) 0.0351(10) Uani 1 d . . O4 O -0.1379(3) 0.1531(2) -0.01105(14) 0.0501(9) Uani 1 d . . C15 C -0.3255(4) 0.0916(3) 0.0860(2) 0.0434(12) Uani 1 d . . O5 O -0.3856(3) 0.0359(3) 0.0688(2) 0.0661(11) Uani 1 d . . C16 C -0.1813(4) 0.0874(3) 0.1662(2) 0.0364(10) Uani 1 d . . O6 O -0.1671(3) 0.0286(2) 0.1967(2) 0.0489(9) Uani 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 0.0241(2) 0.0268(2) 0.0307(2) 0.00071(15) 0.00044(14) 0.00066(14) C1 0.038(3) 0.126(6) 0.036(3) 0.016(3) 0.012(2) -0.016(3) C2 0.030(3) 0.046(3) 0.099(5) 0.030(3) 0.006(3) -0.011(2) C3 0.028(2) 0.043(3) 0.066(3) -0.001(2) -0.005(2) -0.009(2) C4 0.023(2) 0.046(3) 0.064(3) 0.004(2) -0.006(2) 0.003(2) C5 0.028(3) 0.063(4) 0.068(4) -0.015(3) 0.015(2) 0.005(2) C6 0.031(2) 0.044(3) 0.048(3) -0.002(2) -0.007(2) 0.003(2) O1 0.057(2) 0.038(2) 0.080(3) 0.020(2) -0.011(2) -0.008(2) C7 0.040(2) 0.023(2) 0.035(2) 0.003(2) 0.006(2) 0.003(2) O2 0.043(2) 0.037(2) 0.040(2) -0.0037(14) -0.0043(15) -0.0033(15) C8 0.035(2) 0.040(3) 0.038(3) 0.000(2) -0.004(2) -0.002(2) O3 0.051(2) 0.064(2) 0.035(2) -0.002(2) 0.003(2) -0.004(2) Ge 0.0276(2) 0.0255(2) 0.0293(3) 0.0011(2) 0.0007(2) -0.0005(2) Cl1 0.0411(7) 0.0503(7) 0.0434(7) 0.0175(5) 0.0036(5) -0.0071(5) Cl2 0.0595(8) 0.0349(6) 0.0462(7) -0.0088(5) -0.0118(6) -0.0038(5) Mo2 0.0260(2) 0.0275(2) 0.0301(2) 0.00288(14) 0.00334(14) 0.00482(14) C9 0.048(3) 0.030(3) 0.097(5) -0.001(3) 0.009(3) 0.009(2) C10 0.074(4) 0.040(3) 0.058(4) 0.020(3) 0.022(3) 0.031(3) C11 0.043(3) 0.048(3) 0.060(3) 0.002(3) 0.001(2) 0.027(2) C12 0.051(3) 0.046(3) 0.047(3) 0.005(2) 0.022(2) 0.022(2) C13 0.069(4) 0.043(3) 0.045(3) -0.015(2) -0.008(3) 0.028(3) C14 0.029(2) 0.037(3) 0.039(3) 0.000(2) -0.003(2) 0.007(2) O4 0.048(2) 0.065(3) 0.036(2) -0.007(2) 0.000(2) 0.012(2) C15 0.034(3) 0.041(3) 0.055(3) 0.009(2) 0.000(2) 0.007(2) O5 0.045(2) 0.055(2) 0.098(3) -0.003(2) -0.010(2) -0.014(2) C16 0.031(2) 0.037(3) 0.042(3) -0.005(2) 0.006(2) -0.002(2) O6 0.046(2) 0.043(2) 0.058(2) 0.021(2) -0.001(2) -0.001(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 C8 1.978(5) . ? Mo1 C7 1.991(5) . ? Mo1 C6 2.000(5) . ? Mo1 C5 2.305(5) . ? Mo1 C4 2.318(4) . ? Mo1 C1 2.335(5) . ? Mo1 C3 2.351(4) . ? Mo1 C2 2.354(5) . ? Mo1 Ge 2.6668(6) . ? C1 C5 1.404(9) . ? C1 C2 1.428(9) . ? C2 C3 1.390(8) . ? C3 C4 1.397(7) . ? C4 C5 1.396(8) . ? C6 O1 1.139(6) . ? C7 O2 1.149(5) . ? C8 O3 1.145(6) . ? Ge Cl2 2.2589(12) . ? Ge Cl1 2.2669(12) . ? Ge Mo2 2.6536(7) . ? Mo2 C14 1.989(5) . ? Mo2 C15 1.998(5) . ? Mo2 C16 2.000(5) . ? Mo2 C13 2.318(5) . ? Mo2 C12 2.318(4) . ? Mo2 C11 2.323(5) . ? Mo2 C9 2.337(5) . ? Mo2 C10 2.355(5) . ? C9 C13 1.398(8) . ? C9 C10 1.410(8) . ? C10 C11 1.391(8) . ? C11 C12 1.404(7) . ? C12 C13 1.412(8) . ? C14 O4 1.149(5) . ? C15 O5 1.145(6) . ? C16 O6 1.144(5) . ? 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 C8 Mo1 C7 107.9(2) . . ? C8 Mo1 C6 77.8(2) . . ? C7 Mo1 C6 77.6(2) . . ? C8 Mo1 C5 138.1(2) . . ? C7 Mo1 C5 108.6(2) . . ? C6 Mo1 C5 90.6(2) . . ? C8 Mo1 C4 103.8(2) . . ? C7 Mo1 C4 142.0(2) . . ? C6 Mo1 C4 89.5(2) . . ? C5 Mo1 C4 35.2(2) . . ? C8 Mo1 C1 149.4(2) . . ? C7 Mo1 C1 99.3(2) . . ? C6 Mo1 C1 122.6(2) . . ? C5 Mo1 C1 35.2(2) . . ? C4 Mo1 C1 58.2(2) . . ? C8 Mo1 C3 92.7(2) . . ? C7 Mo1 C3 156.1(2) . . ? C6 Mo1 C3 119.6(2) . . ? C5 Mo1 C3 58.4(2) . . ? C4 Mo1 C3 34.8(2) . . ? C1 Mo1 C3 58.1(2) . . ? C8 Mo1 C2 114.8(2) . . ? C7 Mo1 C2 122.5(2) . . ? C6 Mo1 C2 146.4(2) . . ? C5 Mo1 C2 58.7(2) . . ? C4 Mo1 C2 57.8(2) . . ? C1 Mo1 C2 35.5(2) . . ? C3 Mo1 C2 34.4(2) . . ? C8 Mo1 Ge 74.23(13) . . ? C7 Mo1 Ge 71.75(12) . . ? C6 Mo1 Ge 128.93(13) . . ? C5 Mo1 Ge 137.4(2) . . ? C4 Mo1 Ge 138.27(13) . . ? C1 Mo1 Ge 102.2(2) . . ? C3 Mo1 Ge 103.64(13) . . ? C2 Mo1 Ge 84.58(14) . . ? C5 C1 C2 107.4(5) . . ? C5 C1 Mo1 71.2(3) . . ? C2 C1 Mo1 73.0(3) . . ? C3 C2 C1 107.8(5) . . ? C3 C2 Mo1 72.7(3) . . ? C1 C2 Mo1 71.6(3) . . ? C2 C3 C4 108.3(5) . . ? C2 C3 Mo1 72.9(3) . . ? C4 C3 Mo1 71.3(3) . . ? C5 C4 C3 108.8(5) . . ? C5 C4 Mo1 71.9(3) . . ? C3 C4 Mo1 73.9(3) . . ? C4 C5 C1 107.8(5) . . ? C4 C5 Mo1 72.9(3) . . ? C1 C5 Mo1 73.6(3) . . ? O1 C6 Mo1 179.3(4) . . ? O2 C7 Mo1 177.4(4) . . ? O3 C8 Mo1 174.9(4) . . ? Cl2 Ge Cl1 95.29(5) . . ? Cl2 Ge Mo2 108.01(4) . . ? Cl1 Ge Mo2 105.24(4) . . ? Cl2 Ge Mo1 104.13(4) . . ? Cl1 Ge Mo1 107.09(4) . . ? Mo2 Ge Mo1 131.34(2) . . ? C14 Mo2 C15 75.9(2) . . ? C14 Mo2 C16 111.7(2) . . ? C15 Mo2 C16 77.4(2) . . ? C14 Mo2 C13 143.8(2) . . ? C15 Mo2 C13 132.0(2) . . ? C16 Mo2 C13 98.5(2) . . ? C14 Mo2 C12 143.9(2) . . ? C15 Mo2 C12 97.5(2) . . ? C16 Mo2 C12 101.0(2) . . ? C13 Mo2 C12 35.5(2) . . ? C14 Mo2 C11 108.7(2) . . ? C15 Mo2 C11 88.5(2) . . ? C16 Mo2 C11 132.0(2) . . ? C13 Mo2 C11 58.6(2) . . ? C12 Mo2 C11 35.2(2) . . ? C14 Mo2 C9 108.8(2) . . ? C15 Mo2 C9 146.5(2) . . ? C16 Mo2 C9 126.6(2) . . ? C13 Mo2 C9 35.0(2) . . ? C12 Mo2 C9 58.5(2) . . ? C11 Mo2 C9 58.3(2) . . ? C14 Mo2 C10 91.7(2) . . ? C15 Mo2 C10 113.9(2) . . ? C16 Mo2 C10 156.2(2) . . ? C13 Mo2 C10 58.1(2) . . ? C12 Mo2 C10 58.0(2) . . ? C11 Mo2 C10 34.6(2) . . ? C9 Mo2 C10 35.0(2) . . ? C14 Mo2 Ge 74.75(12) . . ? C15 Mo2 Ge 127.88(13) . . ? C16 Mo2 Ge 74.81(12) . . ? C13 Mo2 Ge 95.34(15) . . ? C12 Mo2 Ge 130.43(15) . . ? C11 Mo2 Ge 141.7(2) . . ? C9 Mo2 Ge 84.11(15) . . ? C10 Mo2 Ge 109.1(2) . . ? C13 C9 C10 107.8(5) . . ? C13 C9 Mo2 71.8(3) . . ? C10 C9 Mo2 73.2(3) . . ? C11 C10 C9 108.2(5) . . ? C11 C10 Mo2 71.4(3) . . ? C9 C10 Mo2 71.8(3) . . ? C10 C11 C12 108.3(5) . . ? C10 C11 Mo2 74.0(3) . . ? C12 C11 Mo2 72.2(3) . . ? C11 C12 C13 107.6(5) . . ? C11 C12 Mo2 72.6(3) . . ? C13 C12 Mo2 72.3(3) . . ? C9 C13 C12 108.0(5) . . ? C9 C13 Mo2 73.3(3) . . ? C12 C13 Mo2 72.3(3) . . ? O4 C14 Mo2 173.9(4) . . ? O5 C15 Mo2 178.1(5) . . ? O6 C16 Mo2 176.1(4) . . ? _refine_diff_density_max 0.706 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.128 #======================================================================= #=END data_hansi18 # 1. SUBMISSION DETAILS _publ_contact_author ; Alexander C. Filippou Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; _publ_contact_author_phone '# 49 30 2093-7385' _publ_contact_author_fax '# 49 30 2093-6939' _publ_contact_author_email 'filippou@chemie.hu-berlin.de' _publ_requested_journal ? _publ_requested_coeditor_name ; Johannes G. Winter, Gabriele Kociok-K\"ohn, Isolde Hinz ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Dimetallagermanes of Molybdenum and Tungsten: Synthesis, Structure and Reactions ; loop_ _publ_author_name _publ_author_address 'Alexander C. Filippou' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Johannes G. Winter' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Gabriele Kociok-K\"ohn' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; 'Isolde Hinz' ; Institut f\"ur Anorganische und Allgemeine Chemie der Humboldt Universit\"at zu Berlin Hessische Strasse 1-2 10115 Berlin Bundesrepublik Deutschland ; #======================================================================= _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H19 Cl2 Ge Mo2 O5 P' _chemical_formula_structural ; ((C5 H5) Mo (C O)3)) Ge Cl2 ((C5 H5) Mo (C O)2 (P(C H3)3)' ; _chemical_formula_analytical ? _chemical_formula_sum 'C18 H19 Cl2 Ge Mo2 O5 P' _chemical_formula_weight 681.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Mo' 'Mo' -1.8250 0.6880 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.0810 1.8010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' 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 17.876(3) _cell_length_b 15.859(3) _cell_length_c 18.691(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.203(12) _cell_angle_gamma 90.00 _cell_volume 4754.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 2000 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method ? _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 2.482 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'STOE-IPDS' _diffrn_measurement_method '\f-rotation' _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33291 _diffrn_reflns_av_R_equivalents 0.0669 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.08 _reflns_number_total 9213 _reflns_number_observed 6708 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'IPDS (STOE, 1996)' _computing_cell_refinement 'IPDS (STOE, 1996)' _computing_data_reduction 'IPDS (Software 2.65, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ; L.Zsolnai,H.Pritzkow,ZORTEP,ORTEP program for PC,Universit\"at Heidelberg 1994 ; _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factors etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9200 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_obs 0.0328 _refine_ls_wR_factor_all 0.0822 _refine_ls_wR_factor_obs 0.0707 _refine_ls_goodness_of_fit_all 0.917 _refine_ls_goodness_of_fit_obs 1.033 _refine_ls_restrained_S_all 1.014 _refine_ls_restrained_S_obs 1.033 _refine_ls_shift/esd_max -0.022 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.07022(2) 0.89825(2) -0.27407(2) 0.02498(9) Uani 1 d . . C11 C 0.1223(4) 1.0309(3) -0.2861(3) 0.0622(15) Uani 1 d . . H11 H 0.1411(4) 1.0710(3) -0.2439(3) 0.080 Uiso 1 calc R . C12 C 0.1703(3) 0.9702(3) -0.2983(3) 0.0481(13) Uani 1 d . . H12 H 0.2281(3) 0.9614(3) -0.2655(3) 0.080 Uiso 1 calc R . C13 C 0.1213(3) 0.9238(3) -0.3663(3) 0.0497(13) Uani 1 d . . H13 H 0.1395(3) 0.8783(3) -0.3877(3) 0.080 Uiso 1 calc R . C14 C 0.0398(3) 0.9567(4) -0.3973(3) 0.067(2) Uani 1 d . . H14 H -0.0071(3) 0.9377(4) -0.4437(3) 0.080 Uiso 1 calc R . C15 C 0.0410(3) 1.0235(4) -0.3462(4) 0.070(2) Uani 1 d . . H15 H -0.0052(3) 1.0572(4) -0.3520(4) 0.080 Uiso 1 calc R . C1 C 0.0326(2) 0.7805(3) -0.3043(2) 0.0383(11) Uani 1 d . . O1 O 0.0053(2) 0.7148(2) -0.3268(2) 0.0570(9) Uani 1 d . . C2 C -0.0426(3) 0.8967(4) -0.2782(3) 0.0525(13) Uani 1 d . . O2 O -0.1062(2) 0.8949(3) -0.2780(2) 0.093(2) Uani 1 d . . C3 C 0.0927(2) 0.9202(3) -0.1614(3) 0.0372(10) Uani 1 d . . O3 O 0.1019(2) 0.9384(2) -0.0989(2) 0.0532(9) Uani 1 d . . Mo2 Mo 0.20505(2) 0.66581(2) -0.09962(2) 0.02686(9) Uani 1 d . . C21 C 0.3137(3) 0.7236(3) 0.0119(3) 0.0484(13) Uani 1 d . . H21 H 0.3107(3) 0.7802(3) 0.0271(3) 0.080 Uiso 1 calc R . C22 C 0.2868(3) 0.6531(4) 0.0374(3) 0.065(2) Uani 1 d . . H22 H 0.2619(3) 0.6526(4) 0.0730(3) 0.080 Uiso 1 calc R . C23 C 0.3030(3) 0.5820(4) 0.0008(3) 0.075(2) Uani 1 d . . H23 H 0.2906(3) 0.5251(4) 0.0075(3) 0.080 Uiso 1 calc R . C24 C 0.3401(3) 0.6093(4) -0.0467(3) 0.062(2) Uani 1 d . . H24 H 0.3578(3) 0.5746(4) -0.0777(3) 0.080 Uiso 1 calc R . C25 C 0.3466(2) 0.6970(3) -0.0405(3) 0.0488(13) Uani 1 d . . H25 H 0.3692(2) 0.7326(3) -0.0669(3) 0.080 Uiso 1 calc R . C4 C 0.1707(2) 0.6224(3) -0.2089(3) 0.0362(10) Uani 1 d . . O4 O 0.1543(2) 0.5917(2) -0.2695(2) 0.0488(8) Uani 1 d . . C5 C 0.1080(3) 0.7256(3) -0.1009(2) 0.0353(10) Uani 1 d . . O5 O 0.0530(2) 0.7593(2) -0.0973(2) 0.0509(8) Uani 1 d . . P1 P 0.10674(8) 0.55187(8) -0.11166(8) 0.0430(3) Uani 1 d . . C31 C 0.0047(3) 0.5645(3) -0.1930(3) 0.064(2) Uani 1 d . . H31A H 0.0096(3) 0.5724(3) -0.2427(3) 0.080 Uiso 1 calc R . H31B H -0.0225(3) 0.6138(3) -0.1832(3) 0.080 Uiso 1 calc R . H31C H -0.0287(3) 0.5140(3) -0.1973(3) 0.080 Uiso 1 calc R . C32 C 0.1372(3) 0.4460(3) -0.1272(4) 0.068(2) Uani 1 d . . H32A H 0.1930(3) 0.4331(3) -0.0852(4) 0.080 Uiso 1 calc R . H32B H 0.1379(3) 0.4434(3) -0.1793(4) 0.080 Uiso 1 calc R . H32C H 0.0972(3) 0.4049(3) -0.1255(4) 0.080 Uiso 1 calc R . C33 C 0.0854(4) 0.5383(4) -0.0266(4) 0.079(2) Uani 1 d . . H33A H 0.1380(4) 0.5308(4) 0.0215(4) 0.080 Uiso 1 calc R . H33B H 0.0502(4) 0.4884(4) -0.0347(4) 0.080 Uiso 1 calc R . H33C H 0.0564(4) 0.5882(4) -0.0206(4) 0.080 Uiso 1 calc R . Ge1 Ge 0.19601(2) 0.79957(3) -0.18283(2) 0.02550(10) Uani 1 d . . Cl1 Cl 0.29285(6) 0.89706(7) -0.10328(7) 0.0465(3) Uani 1 d . . Cl2 Cl 0.26361(6) 0.77140(8) -0.25870(7) 0.0454(3) Uani 1 d . . Mo3 Mo 0.34649(3) 0.31313(3) 0.31792(2) 0.03983(11) Uani 1 d . . C41 C 0.3749(5) 0.4167(4) 0.4144(4) 0.087(2) Uani 1 d . . H41 H 0.4300(5) 0.4233(4) 0.4556(4) 0.080 Uiso 1 calc R . C42 C 0.3403(7) 0.4585(4) 0.3383(6) 0.125(4) Uani 1 d . . H42 H 0.3672(7) 0.4978(4) 0.3190(6) 0.080 Uiso 1 calc R . C43 C 0.2598(7) 0.4292(5) 0.2994(5) 0.120(4) Uani 1 d . . H43 H 0.2215(7) 0.4459(5) 0.2472(5) 0.080 Uiso 1 calc R . C44 C 0.2417(4) 0.3734(4) 0.3449(4) 0.085(2) Uani 1 d . . H44 H 0.1901(4) 0.3453(4) 0.3305(4) 0.080 Uiso 1 calc R . C45 C 0.3139(4) 0.3656(4) 0.4171(3) 0.065(2) Uani 1 d . . H45 H 0.3198(4) 0.3307(4) 0.4606(3) 0.080 Uiso 1 calc R . C6 C 0.2909(3) 0.2020(4) 0.2874(3) 0.0478(12) Uani 1 d . . O6 O 0.2593(2) 0.1379(3) 0.2741(3) 0.0880(14) Uani 1 d . . C7 C 0.4318(3) 0.2335(4) 0.3874(3) 0.0524(13) Uani 1 d . . O7 O 0.4803(2) 0.1845(3) 0.4263(2) 0.0822(13) Uani 1 d . . C8 C 0.4313(3) 0.3228(3) 0.2794(3) 0.062(2) Uani 1 d . . O8 O 0.4845(3) 0.3294(3) 0.2593(2) 0.0909(15) Uani 1 d . . Mo4 Mo 0.29991(2) 0.19468(2) 0.06440(2) 0.02698(9) Uani 1 d . . C51 C 0.2001(3) 0.1944(4) -0.0700(3) 0.0554(14) Uani 1 d . . H51 H 0.2035(3) 0.2310(4) -0.1087(3) 0.080 Uiso 1 calc R . C52 C 0.2336(3) 0.1131(4) -0.0510(3) 0.063(2) Uani 1 d . . H52 H 0.2647(3) 0.0854(4) -0.0742(3) 0.080 Uiso 1 calc R . C53 C 0.2140(4) 0.0792(4) 0.0075(4) 0.081(2) Uani 1 d . . H53 H 0.2286(4) 0.0247(4) 0.0306(4) 0.080 Uiso 1 calc R . C54 C 0.1697(3) 0.1390(5) 0.0254(3) 0.073(2) Uani 1 d . . H54 H 0.1484(3) 0.1326(5) 0.0635(3) 0.080 Uiso 1 calc R . C55 C 0.1607(3) 0.2118(4) -0.0213(3) 0.059(2) Uani 1 d . . H55 H 0.1332(3) 0.2627(4) -0.0200(3) 0.080 Uiso 1 calc R . C9 C 0.3647(3) 0.1477(3) 0.1704(3) 0.0401(11) Uani 1 d . . O9 O 0.4030(2) 0.1147(2) 0.2312(2) 0.0671(11) Uani 1 d . . C10 C 0.3551(3) 0.2978(3) 0.0553(3) 0.0499(13) Uani 1 d . . O10 O 0.3840(3) 0.3568(3) 0.0418(2) 0.0890(14) Uani 1 d . . C61 C 0.4397(3) 0.1655(5) -0.0274(3) 0.092(2) Uani 1 d . . H61A H 0.4316(3) 0.2260(5) -0.0393(3) 0.080 Uiso 1 calc R . H61B H 0.3983(3) 0.1335(5) -0.0723(3) 0.080 Uiso 1 calc R . H61C H 0.4959(3) 0.1492(5) -0.0190(3) 0.080 Uiso 1 calc R . C62 C 0.4441(4) 0.0320(4) 0.0729(3) 0.091(2) Uani 1 d . . H62A H 0.4386(4) 0.0131(4) 0.1203(3) 0.080 Uiso 1 calc R . H62B H 0.5002(4) 0.0189(4) 0.0790(3) 0.080 Uiso 1 calc R . H62C H 0.4026(4) 0.0031(4) 0.0257(3) 0.080 Uiso 1 calc R . C63 C 0.5233(3) 0.1829(5) 0.1396(3) 0.095(3) Uani 1 d . . H63A H 0.5219(3) 0.2447(5) 0.1396(3) 0.080 Uiso 1 calc R . H63B H 0.5704(3) 0.1638(5) 0.1304(3) 0.080 Uiso 1 calc R . H63C H 0.5296(3) 0.1618(5) 0.1913(3) 0.080 Uiso 1 calc R . P2 P 0.42727(7) 0.14325(11) 0.06138(7) 0.0545(4) Uani 1 d . . Ge2 Ge 0.27456(3) 0.29946(4) 0.15914(3) 0.04749(14) Uani 1 d . . Cl3 Cl 0.3039(7) 0.4394(2) 0.1311(2) 0.064(2) Uani 0.52(2) d P 1 Cl4 Cl 0.1483(4) 0.3227(7) 0.1287(3) 0.072(2) Uani 0.52(2) d P 1 Cl3A Cl 0.2468(12) 0.4266(5) 0.1136(5) 0.095(4) Uani 0.48(2) d P 2 Cl4A Cl 0.1316(3) 0.2730(10) 0.1359(3) 0.082(3) Uani 0.48(2) d P 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 0.02123(15) 0.0288(2) 0.0227(2) 0.0036(2) 0.00772(13) 0.00237(14) C11 0.101(4) 0.030(3) 0.054(3) 0.004(3) 0.034(3) -0.015(3) C12 0.038(2) 0.051(3) 0.052(3) 0.022(3) 0.017(2) -0.011(2) C13 0.072(3) 0.045(3) 0.050(3) 0.005(3) 0.043(3) -0.006(3) C14 0.056(3) 0.091(5) 0.029(3) 0.034(3) -0.004(2) -0.027(3) C15 0.072(4) 0.062(4) 0.091(5) 0.053(4) 0.050(4) 0.034(3) C1 0.025(2) 0.054(3) 0.025(2) 0.001(2) 0.002(2) -0.002(2) O1 0.055(2) 0.049(2) 0.047(2) -0.002(2) 0.005(2) -0.015(2) C2 0.043(3) 0.075(4) 0.036(3) 0.002(3) 0.015(2) 0.007(3) O2 0.034(2) 0.172(5) 0.080(3) -0.008(3) 0.033(2) 0.005(2) C3 0.037(2) 0.027(3) 0.046(3) 0.004(2) 0.017(2) 0.001(2) O3 0.073(2) 0.049(2) 0.040(2) -0.012(2) 0.027(2) -0.007(2) Mo2 0.0312(2) 0.0246(2) 0.0223(2) 0.0000(2) 0.00961(14) 0.00209(14) C21 0.040(2) 0.054(3) 0.034(3) -0.014(2) 0.002(2) 0.003(2) C22 0.061(3) 0.101(5) 0.023(3) 0.013(3) 0.009(2) 0.001(3) C23 0.070(4) 0.045(4) 0.059(4) 0.027(3) -0.019(3) 0.001(3) C24 0.044(3) 0.064(4) 0.048(3) -0.012(3) -0.005(2) 0.032(3) C25 0.023(2) 0.064(4) 0.047(3) 0.006(3) 0.005(2) 0.009(2) C4 0.035(2) 0.031(3) 0.037(3) 0.001(2) 0.011(2) 0.004(2) O4 0.064(2) 0.045(2) 0.032(2) -0.012(2) 0.016(2) 0.005(2) C5 0.044(2) 0.030(3) 0.037(2) -0.005(2) 0.022(2) -0.010(2) O5 0.056(2) 0.038(2) 0.079(2) -0.004(2) 0.048(2) 0.000(2) P1 0.0548(7) 0.0274(7) 0.0542(8) -0.0017(6) 0.0309(6) -0.0058(6) C31 0.055(3) 0.043(3) 0.094(4) -0.012(3) 0.032(3) -0.017(3) C32 0.087(4) 0.027(3) 0.098(4) -0.007(3) 0.049(3) -0.005(3) C33 0.113(5) 0.060(4) 0.098(5) 0.002(4) 0.075(4) -0.023(4) Ge1 0.0217(2) 0.0267(2) 0.0254(2) 0.0001(2) 0.0080(2) 0.0002(2) Cl1 0.0334(5) 0.0364(7) 0.0526(7) -0.0057(6) 0.0034(5) -0.0075(5) Cl2 0.0450(6) 0.0552(8) 0.0483(7) 0.0056(6) 0.0319(5) 0.0097(5) Mo3 0.0676(3) 0.0296(2) 0.0253(2) 0.0028(2) 0.0232(2) 0.0040(2) C41 0.149(6) 0.061(4) 0.074(5) -0.038(4) 0.071(5) -0.027(4) C42 0.283(13) 0.031(4) 0.137(9) -0.012(5) 0.162(9) -0.010(6) C43 0.257(12) 0.063(6) 0.086(6) 0.043(5) 0.118(8) 0.095(7) C44 0.111(5) 0.092(5) 0.060(4) -0.009(4) 0.045(4) 0.046(4) C45 0.103(4) 0.059(4) 0.041(3) -0.003(3) 0.040(3) 0.014(3) C6 0.048(3) 0.058(4) 0.049(3) 0.002(3) 0.033(2) 0.001(3) O6 0.086(3) 0.082(3) 0.122(4) -0.024(3) 0.069(3) -0.043(3) C7 0.049(3) 0.063(4) 0.038(3) 0.005(3) 0.013(2) -0.005(3) O7 0.055(2) 0.111(4) 0.064(3) 0.033(3) 0.011(2) 0.012(2) C8 0.080(4) 0.047(4) 0.050(3) -0.011(3) 0.021(3) -0.033(3) O8 0.094(3) 0.120(4) 0.072(3) -0.025(3) 0.049(2) -0.059(3) Mo4 0.0270(2) 0.0271(2) 0.0250(2) -0.0021(2) 0.00985(13) -0.00447(14) C51 0.048(3) 0.069(4) 0.032(3) -0.002(3) 0.002(2) -0.010(3) C52 0.053(3) 0.066(4) 0.049(3) -0.035(3) 0.004(3) -0.012(3) C53 0.084(4) 0.051(4) 0.076(5) -0.006(3) 0.006(3) -0.041(3) C54 0.035(3) 0.112(6) 0.062(4) 0.008(4) 0.013(3) -0.033(3) C55 0.032(2) 0.086(5) 0.041(3) -0.006(3) 0.001(2) 0.007(3) C9 0.042(2) 0.039(3) 0.043(3) -0.004(2) 0.022(2) 0.010(2) O9 0.090(3) 0.065(3) 0.042(2) 0.018(2) 0.026(2) 0.044(2) C10 0.057(3) 0.056(4) 0.039(3) -0.010(2) 0.023(2) -0.019(3) O10 0.116(3) 0.074(3) 0.081(3) -0.008(2) 0.047(3) -0.058(3) C61 0.077(4) 0.157(7) 0.064(4) -0.006(4) 0.052(3) 0.023(4) C62 0.099(5) 0.106(6) 0.058(4) -0.010(4) 0.025(3) 0.047(4) C63 0.032(3) 0.176(8) 0.074(4) -0.029(5) 0.022(3) -0.006(4) P2 0.0430(6) 0.0826(11) 0.0393(7) -0.0120(7) 0.0195(6) 0.0104(7) Ge2 0.0659(3) 0.0486(3) 0.0274(2) 0.0087(2) 0.0201(2) 0.0285(3) Cl3 0.120(5) 0.027(2) 0.046(2) 0.0097(12) 0.038(2) 0.008(2) Cl4 0.045(2) 0.111(5) 0.067(2) 0.003(3) 0.030(2) 0.027(3) Cl3A 0.198(11) 0.052(3) 0.064(3) 0.033(3) 0.083(5) 0.062(5) Cl4A 0.031(2) 0.165(9) 0.051(2) -0.011(3) 0.0189(13) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C1 1.982(5) . ? Mo1 C2 1.985(5) . ? Mo1 C3 1.992(5) . ? Mo1 C14 2.314(4) . ? Mo1 C13 2.314(4) . ? Mo1 C15 2.327(5) . ? Mo1 C12 2.330(4) . ? Mo1 C11 2.351(5) . ? Mo1 Ge1 2.6509(6) . ? C11 C12 1.375(7) . ? C11 C15 1.395(8) . ? C12 C13 1.394(6) . ? C13 C14 1.409(7) . ? C14 C15 1.420(8) . ? C1 O1 1.148(5) . ? C2 O2 1.139(5) . ? C3 O3 1.143(5) . ? Mo2 C5 1.969(5) . ? Mo2 C4 1.979(5) . ? Mo2 C21 2.321(4) . ? Mo2 C25 2.324(4) . ? Mo2 C22 2.330(4) . ? Mo2 C23 2.335(5) . ? Mo2 C24 2.345(4) . ? Mo2 P1 2.4607(13) . ? Mo2 Ge1 2.5928(7) . ? C21 C22 1.382(7) . ? C21 C25 1.411(6) . ? C22 C23 1.414(8) . ? C23 C24 1.391(8) . ? C24 C25 1.397(7) . ? C4 O4 1.146(5) . ? C5 O5 1.147(5) . ? P1 C31 1.797(5) . ? P1 C33 1.804(5) . ? P1 C32 1.827(5) . ? Ge1 Cl2 2.2770(11) . ? Ge1 Cl1 2.3076(11) . ? Mo3 C8 1.950(6) . ? Mo3 C7 1.964(5) . ? Mo3 C6 1.979(6) . ? Mo3 C41 2.325(5) . ? Mo3 C45 2.327(5) . ? Mo3 C43 2.331(7) . ? Mo3 C44 2.347(6) . ? Mo3 C42 2.348(7) . ? Mo3 Ge2 2.6717(8) . ? C41 C45 1.377(8) . ? C41 C42 1.439(10) . ? C42 C43 1.375(12) . ? C43 C44 1.361(9) . ? C44 C45 1.401(8) . ? C6 O6 1.137(6) . ? C7 O7 1.153(6) . ? C8 O8 1.171(6) . ? Mo4 C9 1.948(5) . ? Mo4 C10 1.955(5) . ? Mo4 C54 2.286(4) . ? Mo4 C55 2.305(4) . ? Mo4 C53 2.324(5) . ? Mo4 C52 2.340(5) . ? Mo4 C51 2.353(4) . ? Mo4 P2 2.4424(13) . ? Mo4 Ge2 2.6098(7) . ? C51 C52 1.399(7) . ? C51 C55 1.404(7) . ? C52 C53 1.395(8) . ? C53 C54 1.368(9) . ? C54 C55 1.413(8) . ? C9 O9 1.160(5) . ? C10 O10 1.150(6) . ? C61 P2 1.804(5) . ? C62 P2 1.786(6) . ? C63 P2 1.806(5) . ? Ge2 Cl4 2.102(6) . ? Ge2 Cl3A 2.159(5) . ? Ge2 Cl3 2.391(4) . ? Ge2 Cl4A 2.432(7) . ? 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 76.5(2) . . ? C1 Mo1 C3 110.5(2) . . ? C2 Mo1 C3 76.7(2) . . ? C1 Mo1 C14 101.1(2) . . ? C2 Mo1 C14 100.3(2) . . ? C3 Mo1 C14 146.2(2) . . ? C1 Mo1 C13 98.5(2) . . ? C2 Mo1 C13 134.6(2) . . ? C3 Mo1 C13 142.6(2) . . ? C14 Mo1 C13 35.5(2) . . ? C1 Mo1 C15 132.7(2) . . ? C2 Mo1 C15 91.4(2) . . ? C3 Mo1 C15 110.6(2) . . ? C14 Mo1 C15 35.6(2) . . ? C13 Mo1 C15 58.7(2) . . ? C1 Mo1 C12 126.9(2) . . ? C2 Mo1 C12 148.6(2) . . ? C3 Mo1 C12 107.8(2) . . ? C14 Mo1 C12 58.2(2) . . ? C13 Mo1 C12 34.9(2) . . ? C15 Mo1 C12 57.6(2) . . ? C1 Mo1 C11 156.3(2) . . ? C2 Mo1 C11 116.5(2) . . ? C3 Mo1 C11 92.3(2) . . ? C14 Mo1 C11 58.4(2) . . ? C13 Mo1 C11 58.0(2) . . ? C15 Mo1 C11 34.7(2) . . ? C12 Mo1 C11 34.2(2) . . ? C1 Mo1 Ge1 73.25(11) . . ? C2 Mo1 Ge1 125.21(15) . . ? C3 Mo1 Ge1 72.87(12) . . ? C14 Mo1 Ge1 129.5(2) . . ? C13 Mo1 Ge1 94.63(13) . . ? C15 Mo1 Ge1 141.83(14) . . ? C12 Mo1 Ge1 84.73(12) . . ? C11 Mo1 Ge1 109.31(15) . . ? C12 C11 C15 108.2(5) . . ? C12 C11 Mo1 72.1(3) . . ? C15 C11 Mo1 71.7(3) . . ? C11 C12 C13 109.5(4) . . ? C11 C12 Mo1 73.8(3) . . ? C13 C12 Mo1 71.9(2) . . ? C12 C13 C14 107.4(5) . . ? C12 C13 Mo1 73.1(3) . . ? C14 C13 Mo1 72.3(3) . . ? C13 C14 C15 107.0(4) . . ? C13 C14 Mo1 72.3(2) . . ? C15 C14 Mo1 72.7(3) . . ? C11 C15 C14 107.9(5) . . ? C11 C15 Mo1 73.6(3) . . ? C14 C15 Mo1 71.7(3) . . ? O1 C1 Mo1 174.6(4) . . ? O2 C2 Mo1 177.7(4) . . ? O3 C3 Mo1 174.6(4) . . ? C5 Mo2 C4 106.6(2) . . ? C5 Mo2 C21 101.8(2) . . ? C4 Mo2 C21 145.1(2) . . ? C5 Mo2 C25 132.2(2) . . ? C4 Mo2 C25 110.0(2) . . ? C21 Mo2 C25 35.4(2) . . ? C5 Mo2 C22 100.2(2) . . ? C4 Mo2 C22 149.6(2) . . ? C21 Mo2 C22 34.6(2) . . ? C25 Mo2 C22 58.2(2) . . ? C5 Mo2 C23 128.9(2) . . ? C4 Mo2 C23 114.4(2) . . ? C21 Mo2 C23 58.0(2) . . ? C25 Mo2 C23 57.8(2) . . ? C22 Mo2 C23 35.3(2) . . ? C5 Mo2 C24 157.9(2) . . ? C4 Mo2 C24 95.5(2) . . ? C21 Mo2 C24 58.3(2) . . ? C25 Mo2 C24 34.8(2) . . ? C22 Mo2 C24 58.3(2) . . ? C23 Mo2 C24 34.6(2) . . ? C5 Mo2 P1 76.25(12) . . ? C4 Mo2 P1 76.51(13) . . ? C21 Mo2 P1 130.77(14) . . ? C25 Mo2 P1 141.60(13) . . ? C22 Mo2 P1 96.5(2) . . ? C23 Mo2 P1 84.7(2) . . ? C24 Mo2 P1 108.6(2) . . ? C5 Mo2 Ge1 77.17(12) . . ? C4 Mo2 Ge1 75.90(13) . . ? C21 Mo2 Ge1 91.23(14) . . ? C25 Mo2 Ge1 82.96(13) . . ? C22 Mo2 Ge1 124.9(2) . . ? C23 Mo2 Ge1 140.7(2) . . ? C24 Mo2 Ge1 110.2(2) . . ? P1 Mo2 Ge1 133.88(3) . . ? C22 C21 C25 108.2(5) . . ? C22 C21 Mo2 73.1(3) . . ? C25 C21 Mo2 72.4(2) . . ? C21 C22 C23 107.6(5) . . ? C21 C22 Mo2 72.4(3) . . ? C23 C22 Mo2 72.6(3) . . ? C24 C23 C22 108.5(5) . . ? C24 C23 Mo2 73.1(3) . . ? C22 C23 Mo2 72.1(3) . . ? C23 C24 C25 107.7(5) . . ? C23 C24 Mo2 72.3(3) . . ? C25 C24 Mo2 71.8(2) . . ? C24 C25 C21 108.1(5) . . ? C24 C25 Mo2 73.4(3) . . ? C21 C25 Mo2 72.2(2) . . ? O4 C4 Mo2 174.6(4) . . ? O5 C5 Mo2 176.3(4) . . ? C31 P1 C33 103.1(3) . . ? C31 P1 C32 103.3(3) . . ? C33 P1 C32 103.0(3) . . ? C31 P1 Mo2 114.4(2) . . ? C33 P1 Mo2 115.3(2) . . ? C32 P1 Mo2 116.0(2) . . ? Cl2 Ge1 Cl1 94.55(5) . . ? Cl2 Ge1 Mo2 107.67(4) . . ? Cl1 Ge1 Mo2 109.35(4) . . ? Cl2 Ge1 Mo1 104.35(3) . . ? Cl1 Ge1 Mo1 101.59(4) . . ? Mo2 Ge1 Mo1 132.79(2) . . ? C8 Mo3 C7 78.0(2) . . ? C8 Mo3 C6 109.7(2) . . ? C7 Mo3 C6 76.3(2) . . ? C8 Mo3 C41 107.0(2) . . ? C7 Mo3 C41 95.8(2) . . ? C6 Mo3 C41 139.7(2) . . ? C8 Mo3 C45 140.7(2) . . ? C7 Mo3 C45 95.6(2) . . ? C6 Mo3 C45 106.1(2) . . ? C41 Mo3 C45 34.4(2) . . ? C8 Mo3 C43 117.2(3) . . ? C7 Mo3 C43 151.3(2) . . ? C6 Mo3 C43 116.4(3) . . ? C41 Mo3 C43 57.3(3) . . ? C45 Mo3 C43 56.8(2) . . ? C8 Mo3 C44 150.6(3) . . ? C7 Mo3 C44 125.5(2) . . ? C6 Mo3 C44 94.5(2) . . ? C41 Mo3 C44 57.8(2) . . ? C45 Mo3 C44 34.9(2) . . ? C43 Mo3 C44 33.8(2) . . ? C8 Mo3 C42 94.7(3) . . ? C7 Mo3 C42 127.1(3) . . ? C6 Mo3 C42 150.2(3) . . ? C41 Mo3 C42 35.9(2) . . ? C45 Mo3 C42 58.3(2) . . ? C43 Mo3 C42 34.2(3) . . ? C44 Mo3 C42 57.7(3) . . ? C8 Mo3 Ge2 70.59(14) . . ? C7 Mo3 Ge2 122.31(15) . . ? C6 Mo3 Ge2 70.93(14) . . ? C41 Mo3 Ge2 138.8(2) . . ? C45 Mo3 Ge2 138.28(14) . . ? C43 Mo3 Ge2 86.4(2) . . ? C44 Mo3 Ge2 103.5(2) . . ? C42 Mo3 Ge2 103.0(2) . . ? C45 C41 C42 107.8(7) . . ? C45 C41 Mo3 72.9(3) . . ? C42 C41 Mo3 72.9(4) . . ? C43 C42 C41 105.0(7) . . ? C43 C42 Mo3 72.3(4) . . ? C41 C42 Mo3 71.2(4) . . ? C44 C43 C42 111.8(8) . . ? C44 C43 Mo3 73.7(4) . . ? C42 C43 Mo3 73.6(5) . . ? C43 C44 C45 106.7(7) . . ? C43 C44 Mo3 72.4(4) . . ? C45 C44 Mo3 71.8(3) . . ? C41 C45 C44 108.7(6) . . ? C41 C45 Mo3 72.7(3) . . ? C44 C45 Mo3 73.3(3) . . ? O6 C6 Mo3 176.1(5) . . ? O7 C7 Mo3 177.6(5) . . ? O8 C8 Mo3 177.3(4) . . ? C9 Mo4 C10 108.2(2) . . ? C9 Mo4 C54 104.0(2) . . ? C10 Mo4 C54 141.0(2) . . ? C9 Mo4 C55 136.6(2) . . ? C10 Mo4 C55 105.8(2) . . ? C54 Mo4 C55 35.9(2) . . ? C9 Mo4 C53 98.1(2) . . ? C10 Mo4 C53 151.2(2) . . ? C54 Mo4 C53 34.5(2) . . ? C55 Mo4 C53 58.8(2) . . ? C9 Mo4 C52 123.9(2) . . ? C10 Mo4 C52 116.9(2) . . ? C54 Mo4 C52 57.5(2) . . ? C55 Mo4 C52 58.2(2) . . ? C53 Mo4 C52 34.8(2) . . ? C9 Mo4 C51 156.2(2) . . ? C10 Mo4 C51 94.8(2) . . ? C54 Mo4 C51 58.3(2) . . ? C55 Mo4 C51 35.1(2) . . ? C53 Mo4 C51 58.2(2) . . ? C52 Mo4 C51 34.7(2) . . ? C9 Mo4 P2 75.74(12) . . ? C10 Mo4 P2 76.5(2) . . ? C54 Mo4 P2 133.8(2) . . ? C55 Mo4 P2 139.01(14) . . ? C53 Mo4 P2 99.3(2) . . ? C52 Mo4 P2 83.79(14) . . ? C51 Mo4 P2 104.44(14) . . ? C9 Mo4 Ge2 75.95(13) . . ? C10 Mo4 Ge2 76.80(14) . . ? C54 Mo4 Ge2 90.3(2) . . ? C55 Mo4 Ge2 86.48(14) . . ? C53 Mo4 Ge2 122.3(2) . . ? C52 Mo4 Ge2 143.96(14) . . ? C51 Mo4 Ge2 116.68(14) . . ? P2 Mo4 Ge2 132.16(4) . . ? C52 C51 C55 107.4(5) . . ? C52 C51 Mo4 72.1(3) . . ? C55 C51 Mo4 70.6(2) . . ? C53 C52 C51 109.1(6) . . ? C53 C52 Mo4 72.0(3) . . ? C51 C52 Mo4 73.2(3) . . ? C54 C53 C52 107.3(6) . . ? C54 C53 Mo4 71.2(3) . . ? C52 C53 Mo4 73.2(3) . . ? C53 C54 C55 109.6(6) . . ? C53 C54 Mo4 74.3(3) . . ? C55 C54 Mo4 72.8(3) . . ? C51 C55 C54 106.6(5) . . ? C51 C55 Mo4 74.3(3) . . ? C54 C55 Mo4 71.3(3) . . ? O9 C9 Mo4 175.6(4) . . ? O10 C10 Mo4 173.0(4) . . ? C62 P2 C61 102.8(3) . . ? C62 P2 C63 101.4(3) . . ? C61 P2 C63 102.6(3) . . ? C62 P2 Mo4 115.8(2) . . ? C61 P2 Mo4 116.8(2) . . ? C63 P2 Mo4 115.3(2) . . ? Cl4 Ge2 Cl3 95.2(2) . . ? Cl3A Ge2 Cl4A 92.9(2) . . ? Cl4 Ge2 Mo4 114.6(2) . . ? Cl3A Ge2 Mo4 113.93(11) . . ? Cl3 Ge2 Mo4 108.8(2) . . ? Cl4A Ge2 Mo4 104.6(2) . . ? Cl4 Ge2 Mo3 102.64(14) . . ? Cl3A Ge2 Mo3 106.0(3) . . ? Cl3 Ge2 Mo3 97.08(10) . . ? Cl4A Ge2 Mo3 99.47(13) . . ? Mo4 Ge2 Mo3 131.51(2) . . ? _refine_diff_density_max 1.717 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.093 #=======================================================================