# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_1 _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author # Name and address of author for correspondence ; Dr A. Dolbecq Institut Lavoisier, ILV, UMR CNRS 8180 Universit\'e de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; _publ_contact_author_phone '(33) 1 39 25 43 83' _publ_contact_author_fax '(33) 1 39 25 43 81' _publ_contact_author_email dolbecq@chimie.uvsq.fr _publ_requested_coeditor_name ? _publ_contact_letter ; ; #==================================================================== # 2. processing summary (iucr office use only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ; _journal_techeditor_code ? _journal_techeditor_notes ; ; _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #==================================================================== # 3. title and author list _publ_section_title ; e-Keggin-based coordination networks: synthesis, structure and application toward green synthesis of polyoxometalate@graphene hybrids ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'L.M.Rodriguez Albelo' ; Group of Materials Developed by Design Division of Chemistry and Technology of Materials Institute of Materials Research and Engineering University of Havana Havana, 10400 Cuba ; G.Rousseau ; Institut Lavoisier, ILV, UMR CNRS 8180 Universit\'e de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; P.Mialane ; Institut Lavoisier, ILV, UMR CNRS 8180 Universit\'e de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; J.Marrot ; Institut Lavoisier, IREM, UMR CNRS 8180 Universit\'e de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; ; C.Mellot-Draznieks ; ; Lab. Chimie des Processus Biologiques, FRE 3488 College de France 11 Place Marcellin Berthelot 75005 Paris France ; A.R.Ruiz-Salvador ; Group of Materials Developed by Design Division of Chemistry and Technology of Materials Institute of Materials Research and Engineering University of Havana Havana, 10400 Cuba ; S.Li ; Key laboratory of Green Process Engineering Institute of Process Engineering 100190 Beijing China ; R.Liu ; Key laboratory of Green Process Engineering Institute of Process Engineering 100190 Beijing China ; G.Zhang ; Key laboratory of Green Process Engineering Institute of Process Engineering 100190 Beijing China ; B.Keita ; Laboratoire de Chimie Physique, UMR 8000 Universit\'e Paris Sud 91405 Orsay cedex France ; ; A.Dolbecq ; ; Institut Lavoisier, ILV, UMR CNRS 8180 Universit\'e de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles cedex France ; #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_contact_author_name 'Dr A. Dolbecq' #==================================================================== data_e(isop)2 _database_code_depnum_ccdc_archive 'CCDC 870381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H120 Mo12 N3 O48.50 P Zn4' _chemical_formula_weight 3151.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 21.899(5) _cell_length_b 20.306(5) _cell_length_c 22.900(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10183(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 35339 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 29.87 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.055 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5556 _exptl_absorpt_coefficient_mu 2.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6413 _exptl_absorpt_correction_T_max 0.7926 _exptl_absorpt_process_details 'G. M. Sheldrick, SADABS; program for scaling and correction of area detector data, University of G ttingen, Germany, 1997' _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 512x512 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62280 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.3137 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 29.87 _reflns_number_total 26789 _reflns_number_gt 19926 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^ > 2\s(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. One TBA counter-cation could not be located and the data set was corrected with the program SQUEEZE (P. van der Sluis and A. L. Spek, Acta Crystallogr., Sect. A., 1990, 46, 194). The contribution of the three disordered TBA counter-ions has thus been removed. 22 restraints were introduced via the DFIX instructions in order to obtain reasonable C-C distances within the TBA counter cations which have been located. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.017 -0.025 0.315 5688 2995 ' ' _platon_squeeze_details ; ; _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^)+(0.0000P)^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 constr _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 0.024(14) _refine_ls_number_reflns 26789 _refine_ls_number_parameters 964 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.2293 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.016 _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 0.30011(3) 0.15869(4) 0.05147(4) 0.02750(15) Uani 1 1 d . . . Mo2 Mo 0.40531(3) 0.03496(4) 0.07802(4) 0.03026(17) Uani 1 1 d . . . Mo3 Mo 0.17500(3) 0.14934(4) 0.12304(3) 0.02721(15) Uani 1 1 d . . . Mo4 Mo 0.07563(3) 0.02777(4) 0.07885(4) 0.02854(16) Uani 1 1 d . . . Mo5 Mo 0.28100(3) -0.18666(4) 0.12388(4) 0.02842(16) Uani 1 1 d . . . Mo6 Mo 0.15970(4) 0.01616(4) 0.21365(3) 0.02814(16) Uani 1 1 d . . . Mo7 Mo 0.09833(3) -0.05528(4) -0.00529(4) 0.02960(16) Uani 1 1 d . . . Mo8 Mo 0.24327(4) -0.07348(4) 0.22891(3) 0.02957(16) Uani 1 1 d . . . Mo9 Mo 0.32080(4) 0.04400(4) -0.05652(4) 0.03026(17) Uani 1 1 d . . . Mo10 Mo 0.24089(4) -0.04614(4) -0.08438(4) 0.02993(16) Uani 1 1 d . . . Mo11 Mo 0.38606(4) -0.06355(4) 0.14966(4) 0.03085(17) Uani 1 1 d . . . Mo12 Mo 0.20608(4) -0.17735(4) 0.00449(4) 0.02893(16) Uani 1 1 d . . . Zn1 Zn 0.17200(5) 0.10698(6) -0.02705(5) 0.0297(2) Uani 1 1 d . . . Zn2 Zn 0.12522(5) -0.13538(5) 0.13216(5) 0.0295(2) Uani 1 1 d . . . Zn3 Zn 0.30616(5) 0.08923(6) 0.19161(5) 0.0307(2) Uani 1 1 d . . . Zn4 Zn 0.35808(5) -0.11810(6) 0.00512(5) 0.0321(2) Uani 1 1 d . . . P1 P 0.24073(9) -0.01454(11) 0.07547(9) 0.0212(4) Uani 1 1 d . . . O1 O 0.0899(3) -0.0673(3) 0.0781(3) 0.0283(13) Uani 1 1 d . . . O2 O 0.2719(3) -0.0607(3) 0.1205(3) 0.0280(12) Uani 1 1 d . . . O3 O 0.2487(3) 0.0227(3) 0.2234(3) 0.0278(12) Uani 1 1 d . . . O4 O 0.2662(3) 0.1422(3) 0.1315(3) 0.0268(12) Uani 1 1 d . . . O5 O 0.1624(3) 0.2302(4) 0.1338(4) 0.0396(16) Uani 1 1 d . . . O6 O 0.0784(3) 0.0177(3) 0.1679(3) 0.0282(13) Uani 1 1 d . . . O7 O 0.3212(3) -0.0523(3) -0.0498(3) 0.0296(13) Uani 1 1 d . . . O8 O 0.3380(3) -0.0675(3) 0.2280(3) 0.0308(13) Uani 1 1 d . . . O9 O 0.2901(3) -0.1692(3) 0.0368(3) 0.0288(13) Uani 1 1 d . . . O10 O 0.2121(3) -0.0536(3) 0.0245(2) 0.0212(11) Uani 1 1 d . . . O11 O 0.2888(4) -0.2693(4) 0.1276(4) 0.0424(17) Uani 1 1 d . . . O12 O 0.1118(3) 0.0407(3) 0.0019(3) 0.0297(13) Uani 1 1 d . . . O13 O 0.3679(3) 0.0315(3) 0.1545(3) 0.0284(12) Uani 1 1 d . . . O14 O 0.1461(3) -0.0455(4) -0.0824(3) 0.0364(15) Uani 1 1 d . . . O15 O 0.1034(3) 0.1212(3) 0.0914(3) 0.0305(13) Uani 1 1 d . . . O16 O 0.2324(3) 0.0467(3) -0.0644(3) 0.0323(14) Uani 1 1 d . . . O17 O 0.1626(3) -0.0770(3) 0.1928(3) 0.0288(13) Uani 1 1 d . . . O18 O 0.1938(3) -0.1764(3) 0.0920(3) 0.0274(12) Uani 1 1 d . . . O19 O 0.2901(3) 0.0319(3) 0.0493(3) 0.0257(12) Uani 1 1 d . . . O20 O 0.3110(3) 0.1350(4) -0.0245(3) 0.0352(15) Uani 1 1 d . . . O21 O 0.2096(3) 0.1505(3) 0.0406(3) 0.0315(14) Uani 1 1 d . . . O22 O 0.2529(3) -0.1631(4) 0.1957(3) 0.0326(14) Uani 1 1 d . . . O23 O 0.3585(3) -0.1569(3) 0.1341(3) 0.0340(14) Uani 1 1 d . . . O24 O 0.1907(3) 0.0256(3) 0.1066(3) 0.0269(12) Uani 1 1 d . . . O25 O 0.3739(3) 0.1275(3) 0.0784(3) 0.0319(13) Uani 1 1 d . . . O26 O 0.1269(3) -0.1482(4) -0.0042(3) 0.0352(14) Uani 1 1 d . . . O27 O 0.1415(3) 0.1625(4) -0.0895(3) 0.0374(16) Uani 1 1 d . . . O28 O 0.2359(3) -0.1411(4) -0.0637(3) 0.0365(16) Uani 1 1 d . . . O29 O 0.2023(4) -0.2589(4) -0.0118(4) 0.0471(19) Uani 1 1 d . . . O30 O 0.0613(3) -0.1855(4) 0.1720(3) 0.0383(16) Uani 1 1 d . . . O31 O 0.3951(3) -0.0610(4) 0.0651(4) 0.0382(16) Uani 1 1 d . . . O32 O 0.4576(4) -0.0750(5) 0.1757(4) 0.048(2) Uani 1 1 d . . . O33 O 0.3100(4) 0.2408(4) 0.0511(4) 0.0469(19) Uani 1 1 d . . . O34 O 0.1307(4) 0.0175(4) 0.2806(3) 0.0436(17) Uani 1 1 d . . . O35 O 0.4234(3) -0.1606(4) -0.0358(4) 0.0451(19) Uani 1 1 d . . . O36 O 0.0280(4) -0.0636(4) -0.0336(5) 0.051(2) Uani 1 1 d . . . O37 O 0.0001(3) 0.0390(4) 0.0701(4) 0.048(2) Uani 1 1 d . . . O38 O 0.3413(4) 0.1393(4) 0.2541(4) 0.0457(19) Uani 1 1 d . . . O39 O 0.4024(3) 0.0395(3) -0.0114(3) 0.0317(14) Uani 1 1 d . . . O40 O 0.1664(3) 0.1114(3) 0.1948(3) 0.0294(13) Uani 1 1 d . . . O41 O 0.2518(5) -0.0492(5) -0.1557(4) 0.052(2) Uani 1 1 d . . . O42 O 0.3487(4) 0.0606(4) -0.1229(4) 0.0469(19) Uani 1 1 d . . . O43 O 0.2337(4) -0.0913(5) 0.2987(3) 0.047(2) Uani 1 1 d . . . O44 O 0.4616(4) -0.0595(4) -0.0577(4) 0.051(2) Uani 1 1 d . . . O45 O 0.4790(3) 0.0484(4) 0.0877(4) 0.047(2) Uani 1 1 d . . . O46 O 0.1135(5) 0.0686(5) -0.1343(5) 0.058(2) Uani 1 1 d . . . O47 O 0.3822(4) 0.0465(5) 0.2855(4) 0.049(2) Uani 1 1 d . . . O48 O 0.0248(4) -0.0869(4) 0.1976(4) 0.053(2) Uani 1 1 d . . . C1 C 0.5143(4) -0.1530(5) -0.0924(5) 0.038(2) Uani 1 1 d . . . C2 C 0.5291(5) -0.2170(6) -0.0836(5) 0.0444(19) Uani 1 1 d . . . H2 H 0.5074 -0.2420 -0.0566 0.053 Uiso 1 1 calc R . . C3 C 0.5777(5) -0.2459(6) -0.1156(6) 0.047(3) Uani 1 1 d . . . H3 H 0.5886 -0.2895 -0.1090 0.057 Uiso 1 1 calc R . . C4 C 0.3919(5) 0.2097(6) 0.3440(6) 0.044(3) Uani 1 1 d . . . H4 H 0.3601 0.2288 0.3231 0.052 Uiso 1 1 calc R . . C5 C 0.4070(5) 0.1463(6) 0.3336(4) 0.036(2) Uani 1 1 d . . . C6 C 0.4542(5) 0.1165(7) 0.3660(6) 0.046(3) Uani 1 1 d . . . H6 H 0.4643 0.0726 0.3596 0.055 Uiso 1 1 calc R . . C7 C 0.3751(5) 0.1065(6) 0.2872(5) 0.040(2) Uani 1 1 d . . . C8 C 0.4621(5) -0.1220(6) -0.0598(5) 0.0444(19) Uani 1 1 d . . . C9 C 0.0945(4) 0.1694(5) -0.1835(4) 0.0316(18) Uani 1 1 d . . . C10 C 0.1160(5) 0.2321(6) -0.1940(6) 0.048(3) Uani 1 1 d . . . H10 H 0.1464 0.2493 -0.1701 0.058 Uiso 1 1 calc R . . C11 C -0.0932(6) -0.2705(6) 0.2599(6) 0.047(3) Uani 1 1 d . . . H11 H -0.1090 -0.3123 0.2529 0.056 Uiso 1 1 calc R . . C12 C -0.0467(6) -0.2454(5) 0.2249(4) 0.040(2) Uani 1 1 d . . . H12 H -0.0313 -0.2704 0.1943 0.048 Uiso 1 1 calc R . . C13 C -0.0227(5) -0.1809(5) 0.2362(5) 0.037(2) Uani 1 1 d . . . C14 C 0.0498(5) 0.1430(5) -0.2186(4) 0.035(2) Uani 1 1 d . . . H14 H 0.0371 0.0998 -0.2126 0.043 Uiso 1 1 calc R . . C15 C 0.1196(4) 0.1299(4) -0.1324(4) 0.0304(18) Uani 1 1 d . . . C16 C 0.0250(5) -0.1465(6) 0.1991(4) 0.038(2) Uani 1 1 d . . . N1 N 0.1586(5) 0.1833(6) 0.3744(5) 0.056(3) Uani 1 1 d D . . C1A C 0.1953(7) 0.1173(7) 0.3675(7) 0.074(5) Uani 1 1 d D . . H1A1 H 0.1696 0.0812 0.3804 0.089 Uiso 1 1 calc R . . H1A2 H 0.2038 0.1105 0.3264 0.089 Uiso 1 1 calc R . . C2A C 0.2553(7) 0.1140(10) 0.4008(9) 0.083(6) Uani 1 1 d D . . H2A1 H 0.2492 0.1300 0.4403 0.100 Uiso 1 1 calc R . . H2A2 H 0.2852 0.1420 0.3819 0.100 Uiso 1 1 calc R . . C3A C 0.2796(13) 0.0415(12) 0.4028(8) 0.113(9) Uani 1 1 d D . . H3A1 H 0.2464 0.0118 0.4125 0.136 Uiso 1 1 calc R . . H3A2 H 0.2953 0.0292 0.3647 0.136 Uiso 1 1 calc R . . C4A C 0.331(2) 0.035(3) 0.449(2) 0.23(2) Uiso 1 1 d D . . H4A1 H 0.3632 0.0662 0.4409 0.348 Uiso 1 1 calc R . . H4A2 H 0.3478 -0.0087 0.4485 0.348 Uiso 1 1 calc R . . H4A3 H 0.3150 0.0439 0.4875 0.348 Uiso 1 1 calc R . . C1B C 0.1404(8) 0.1958(10) 0.4385(8) 0.082(6) Uani 1 1 d . . . H1B1 H 0.1084 0.2288 0.4391 0.098 Uiso 1 1 calc R . . H1B2 H 0.1754 0.2142 0.4587 0.098 Uiso 1 1 calc R . . C2B C 0.1167(9) 0.1317(14) 0.4752(8) 0.112(7) Uani 1 1 d D . . H2B1 H 0.0803 0.1121 0.4584 0.134 Uiso 1 1 calc R . . H2B2 H 0.1482 0.0986 0.4800 0.134 Uiso 1 1 calc R . . C3B C 0.1031(10) 0.1698(12) 0.5327(7) 0.112(7) Uani 1 1 d D . . H3B1 H 0.1402 0.1876 0.5498 0.134 Uiso 1 1 calc R . . H3B2 H 0.0742 0.2053 0.5263 0.134 Uiso 1 1 calc R . . C4B C 0.0768(11) 0.1175(12) 0.5693(11) 0.106(5) Uiso 1 1 d D . . H4B1 H 0.0536 0.0878 0.5453 0.159 Uiso 1 1 calc R . . H4B2 H 0.0505 0.1367 0.5982 0.159 Uiso 1 1 calc R . . H4B3 H 0.1091 0.0937 0.5883 0.159 Uiso 1 1 calc R . . C1C C 0.2006(7) 0.2387(7) 0.3583(8) 0.064(4) Uani 1 1 d . . . H1C1 H 0.2357 0.2376 0.3840 0.077 Uiso 1 1 calc R . . H1C2 H 0.1795 0.2801 0.3649 0.077 Uiso 1 1 calc R . . C2C C 0.2231(7) 0.2369(9) 0.2945(7) 0.067(5) Uani 1 1 d . . . H2C1 H 0.1885 0.2329 0.2683 0.081 Uiso 1 1 calc R . . H2C2 H 0.2494 0.1990 0.2887 0.081 Uiso 1 1 calc R . . C3C C 0.2599(11) 0.3030(13) 0.2804(14) 0.111(6) Uani 1 1 d . . . H3C1 H 0.2325 0.3402 0.2845 0.133 Uiso 1 1 calc R . . H3C2 H 0.2924 0.3081 0.3089 0.133 Uiso 1 1 calc R . . C4C C 0.2878(11) 0.3039(12) 0.2188(15) 0.111(6) Uani 1 1 d . . . C1D C 0.1007(6) 0.1793(8) 0.3349(8) 0.067(3) Uani 1 1 d D . . H1D1 H 0.0826 0.2229 0.3351 0.081 Uiso 1 1 calc R . . H1D2 H 0.1152 0.1717 0.2955 0.081 Uiso 1 1 calc R . . C2D C 0.0494(7) 0.1318(9) 0.3445(8) 0.067(3) Uani 1 1 d . . . H2D1 H 0.0259 0.1451 0.3784 0.081 Uiso 1 1 calc R . . H2D2 H 0.0657 0.0882 0.3518 0.081 Uiso 1 1 calc R . . C3D C 0.0089(11) 0.1307(13) 0.2912(12) 0.106(5) Uiso 1 1 d D . . H3D1 H 0.0339 0.1210 0.2573 0.127 Uiso 1 1 calc R . . H3D2 H -0.0084 0.1742 0.2857 0.127 Uiso 1 1 calc R . . C4D C -0.0441(12) 0.0797(14) 0.2940(14) 0.124(9) Uiso 1 1 d D . . N2 N 0.0073(5) 0.2638(6) -0.0044(6) 0.060(3) Uani 1 1 d D . . C1E C 0.0767(5) 0.2701(8) 0.0034(8) 0.071(4) Uani 1 1 d D . . H1E1 H 0.0953 0.2646 -0.0348 0.085 Uiso 1 1 calc R . . H1E2 H 0.0901 0.2333 0.0272 0.085 Uiso 1 1 calc R . . C2E C 0.1038(11) 0.3337(9) 0.0307(10) 0.107(9) Uani 1 1 d D . . H2E1 H 0.0964 0.3339 0.0725 0.128 Uiso 1 1 calc R . . H2E2 H 0.0839 0.3720 0.0140 0.128 Uiso 1 1 calc R . . C3E C 0.1741(11) 0.3372(14) 0.0188(13) 0.1058(12) Uiso 1 1 d D . . C4E1 C 0.227(3) 0.387(3) 0.031(4) 0.16(3) Uiso 0.50 1 d PD . . C4E2 C 0.206(4) 0.341(4) -0.041(2) 0.17(3) Uiso 0.50 1 d PD . . C1F C -0.0241(8) 0.2709(11) 0.0548(8) 0.080(5) Uani 1 1 d . . . H1F1 H -0.0678 0.2729 0.0480 0.096 Uiso 1 1 calc R . . H1F2 H -0.0121 0.3130 0.0713 0.096 Uiso 1 1 calc R . . C2F C -0.0124(10) 0.2176(10) 0.1013(8) 0.093(7) Uani 1 1 d D . . H2F1 H 0.0295 0.2204 0.1148 0.111 Uiso 1 1 calc R . . H2F2 H -0.0186 0.1743 0.0844 0.111 Uiso 1 1 calc R . . C3F C -0.0566(13) 0.2273(14) 0.1534(12) 0.140(8) Uiso 1 1 d D . . H3F1 H -0.0975 0.2339 0.1384 0.168 Uiso 1 1 calc R . . H3F2 H -0.0569 0.1875 0.1767 0.168 Uiso 1 1 calc R . . C4F C -0.0401(14) 0.2852(14) 0.1926(15) 0.140(8) Uiso 1 1 d D . . C1G C -0.0167(7) 0.3165(9) -0.0425(7) 0.069(4) Uani 1 1 d . . . H1G1 H -0.0046 0.3586 -0.0262 0.082 Uiso 1 1 calc R . . H1G2 H -0.0609 0.3146 -0.0416 0.082 Uiso 1 1 calc R . . C2G C 0.0040(14) 0.3144(15) -0.1068(13) 0.148(13) Uani 1 1 d D . . H2G1 H -0.0144 0.2764 -0.1254 0.178 Uiso 1 1 calc R . . H2G2 H 0.0479 0.3084 -0.1079 0.178 Uiso 1 1 calc R . . C3G C -0.0124(14) 0.3768(17) -0.1428(14) 0.172(18) Uani 1 1 d D . . H3G1 H -0.0391 0.3617 -0.1739 0.207 Uiso 1 1 calc R . . H3G2 H -0.0374 0.4037 -0.1173 0.207 Uiso 1 1 calc R . . C4G C 0.033(2) 0.424(3) -0.171(3) 0.24(2) Uiso 1 1 d D . . C1H C -0.0016(9) 0.1952(9) -0.0314(10) 0.098(7) Uani 1 1 d D . . H1H1 H 0.0199 0.1636 -0.0072 0.118 Uiso 1 1 calc R . . H1H2 H 0.0179 0.1950 -0.0695 0.118 Uiso 1 1 calc R . . C2H C -0.0693(11) 0.1701(14) -0.0393(14) 0.127(12) Uani 1 1 d D . . H2H1 H -0.0884 0.1626 -0.0017 0.152 Uiso 1 1 calc R . . H2H2 H -0.0934 0.2020 -0.0608 0.152 Uiso 1 1 calc R . . C3H C -0.0640(18) 0.1057(15) -0.0734(19) 0.172(15) Uiso 1 1 d D . . H3H1 H -0.0421 0.0722 -0.0517 0.207 Uiso 1 1 calc R . . H3H2 H -0.0449 0.1120 -0.1112 0.207 Uiso 1 1 calc R . . C4H C -0.132(2) 0.090(4) -0.079(4) 0.34(4) Uiso 1 1 d D . . O1W O 0.1757(9) -0.3998(11) 0.2000(10) 0.064(5) 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 0.0268(3) 0.0251(4) 0.0306(4) 0.0019(3) -0.0034(3) -0.0037(3) Mo2 0.0246(3) 0.0311(4) 0.0351(4) 0.0026(3) 0.0001(3) -0.0025(3) Mo3 0.0276(3) 0.0252(3) 0.0288(3) -0.0036(3) -0.0032(3) 0.0012(2) Mo4 0.0229(3) 0.0303(4) 0.0325(4) -0.0039(3) -0.0009(3) 0.0008(3) Mo5 0.0285(3) 0.0256(4) 0.0312(4) 0.0024(3) 0.0068(3) 0.0024(3) Mo6 0.0308(4) 0.0290(4) 0.0246(3) -0.0050(3) 0.0024(3) 0.0008(3) Mo7 0.0266(3) 0.0332(4) 0.0289(4) -0.0051(3) -0.0026(3) -0.0032(3) Mo8 0.0339(4) 0.0308(4) 0.0240(3) 0.0005(3) 0.0011(3) 0.0013(3) Mo9 0.0320(4) 0.0302(4) 0.0286(4) 0.0028(3) 0.0056(3) -0.0014(3) Mo10 0.0364(4) 0.0305(4) 0.0229(3) -0.0015(3) 0.0030(3) -0.0015(3) Mo11 0.0273(3) 0.0304(4) 0.0348(4) 0.0044(3) -0.0024(3) 0.0027(3) Mo12 0.0312(4) 0.0273(4) 0.0283(4) -0.0043(3) 0.0070(3) -0.0032(3) Zn1 0.0297(5) 0.0325(5) 0.0268(5) -0.0002(4) -0.0070(4) 0.0025(4) Zn2 0.0267(5) 0.0301(5) 0.0318(5) -0.0029(4) 0.0078(4) -0.0021(4) Zn3 0.0317(5) 0.0315(5) 0.0290(5) -0.0025(4) -0.0077(4) -0.0015(4) Zn4 0.0288(5) 0.0319(5) 0.0357(5) 0.0004(4) 0.0115(4) 0.0002(4) P1 0.0196(8) 0.0230(10) 0.0210(9) -0.0019(8) -0.0005(7) 0.0004(7) O1 0.030(3) 0.022(3) 0.033(3) -0.005(3) 0.011(2) -0.005(2) O2 0.030(3) 0.021(3) 0.033(3) 0.000(3) -0.001(2) -0.001(2) O3 0.030(3) 0.027(3) 0.027(3) 0.002(3) -0.003(2) -0.004(2) O4 0.022(3) 0.027(3) 0.032(3) -0.006(2) -0.005(2) -0.006(2) O5 0.043(4) 0.024(3) 0.051(5) -0.001(3) -0.006(3) 0.004(3) O6 0.025(3) 0.035(3) 0.024(3) -0.006(3) 0.009(2) 0.000(2) O7 0.030(3) 0.029(3) 0.030(3) 0.003(3) 0.005(2) 0.008(2) O8 0.044(4) 0.026(3) 0.022(3) 0.009(2) -0.003(3) 0.000(3) O9 0.031(3) 0.024(3) 0.031(3) 0.001(2) 0.013(2) 0.000(2) O10 0.024(3) 0.024(3) 0.016(2) -0.006(2) -0.0008(19) 0.004(2) O11 0.041(4) 0.043(4) 0.043(4) -0.002(3) 0.012(3) 0.007(3) O12 0.023(3) 0.033(3) 0.033(3) 0.005(3) -0.013(2) 0.000(2) O13 0.036(3) 0.024(3) 0.026(3) 0.000(2) -0.006(2) -0.005(2) O14 0.040(4) 0.034(4) 0.035(4) -0.006(3) -0.005(3) -0.011(3) O15 0.037(3) 0.024(3) 0.031(3) -0.005(3) -0.010(2) 0.006(2) O16 0.039(4) 0.034(4) 0.025(3) -0.007(3) -0.003(3) -0.004(3) O17 0.026(3) 0.029(3) 0.032(3) -0.005(3) 0.011(2) -0.002(2) O18 0.028(3) 0.034(3) 0.020(3) -0.005(2) 0.002(2) 0.001(2) O19 0.028(3) 0.023(3) 0.026(3) 0.003(2) 0.000(2) -0.002(2) O20 0.037(3) 0.048(4) 0.020(3) 0.008(3) 0.005(2) -0.009(3) O21 0.030(3) 0.028(3) 0.036(4) 0.001(3) -0.016(3) 0.007(2) O22 0.035(3) 0.037(4) 0.026(3) 0.004(3) 0.002(3) 0.003(3) O23 0.040(4) 0.027(3) 0.035(3) 0.002(3) 0.010(3) 0.003(3) O24 0.030(3) 0.026(3) 0.025(3) -0.005(2) -0.001(2) -0.006(2) O25 0.030(3) 0.029(3) 0.037(3) 0.004(3) -0.003(3) 0.002(2) O26 0.043(4) 0.033(3) 0.030(3) -0.007(3) 0.003(3) -0.009(3) O27 0.035(4) 0.048(4) 0.029(3) 0.000(3) -0.013(3) 0.013(3) O28 0.041(4) 0.035(4) 0.033(3) -0.013(3) 0.009(3) -0.009(3) O29 0.044(4) 0.042(4) 0.055(5) -0.014(4) 0.018(4) 0.002(3) O30 0.035(3) 0.049(4) 0.031(3) 0.002(3) 0.017(3) -0.006(3) O31 0.037(4) 0.035(4) 0.043(4) 0.004(3) 0.008(3) 0.000(3) O32 0.032(4) 0.058(5) 0.054(5) 0.012(4) -0.013(3) 0.015(3) O33 0.049(4) 0.029(4) 0.063(5) 0.008(4) 0.005(4) -0.008(3) O34 0.057(5) 0.043(4) 0.031(3) -0.006(3) 0.007(3) 0.002(3) O35 0.027(3) 0.043(4) 0.065(5) 0.009(4) 0.027(3) 0.002(3) O36 0.037(4) 0.047(5) 0.069(6) -0.002(4) -0.014(4) -0.004(3) O37 0.023(3) 0.058(5) 0.062(5) -0.010(4) -0.002(3) 0.009(3) O38 0.041(4) 0.047(5) 0.049(4) -0.011(4) -0.024(3) 0.016(3) O39 0.022(3) 0.029(3) 0.045(4) -0.001(3) 0.005(3) 0.000(2) O40 0.035(3) 0.028(3) 0.025(3) -0.003(2) -0.003(2) 0.006(2) O41 0.065(5) 0.063(6) 0.029(4) -0.001(4) 0.007(4) 0.006(4) O42 0.047(5) 0.053(5) 0.040(4) 0.009(4) 0.005(3) -0.003(4) O43 0.058(5) 0.059(6) 0.025(3) 0.007(3) 0.010(3) 0.006(4) O44 0.056(5) 0.034(4) 0.063(5) 0.000(4) 0.028(4) 0.006(3) O45 0.022(3) 0.052(5) 0.067(6) -0.008(4) -0.002(3) -0.008(3) O46 0.059(5) 0.049(5) 0.065(6) 0.002(4) -0.035(5) 0.011(4) O47 0.044(4) 0.055(5) 0.047(5) 0.003(4) -0.025(4) -0.005(3) O48 0.056(5) 0.043(5) 0.061(5) -0.007(4) 0.024(4) -0.018(4) C1 0.023(4) 0.044(6) 0.046(6) 0.000(4) 0.013(4) -0.004(3) C2 0.043(4) 0.051(5) 0.039(4) 0.018(3) 0.027(3) 0.006(3) C3 0.028(5) 0.053(7) 0.060(7) -0.006(6) 0.011(4) 0.011(4) C4 0.032(5) 0.046(6) 0.054(6) -0.010(5) -0.021(4) 0.000(4) C5 0.033(5) 0.046(6) 0.028(4) 0.007(4) -0.003(3) 0.007(4) C6 0.029(5) 0.058(7) 0.051(6) -0.011(5) -0.019(4) 0.000(4) C7 0.032(5) 0.057(7) 0.032(5) -0.004(5) -0.010(4) -0.005(4) C8 0.043(4) 0.051(5) 0.039(4) 0.018(3) 0.027(3) 0.006(3) C9 0.034(5) 0.033(5) 0.028(4) 0.000(4) -0.006(3) 0.001(3) C10 0.040(5) 0.053(7) 0.053(7) 0.007(5) -0.019(5) -0.018(5) C11 0.054(6) 0.034(5) 0.052(7) -0.012(5) 0.029(5) -0.012(5) C12 0.060(6) 0.033(5) 0.026(4) -0.003(4) 0.005(4) -0.010(4) C13 0.042(5) 0.022(4) 0.048(6) 0.002(4) 0.002(4) -0.011(3) C14 0.038(5) 0.036(5) 0.032(4) 0.009(4) -0.009(4) -0.017(4) C15 0.043(5) 0.014(4) 0.035(4) 0.006(3) 0.000(4) 0.004(3) C16 0.032(5) 0.055(6) 0.026(4) 0.012(4) 0.010(3) -0.013(4) N1 0.052(6) 0.052(6) 0.065(7) -0.022(5) 0.013(5) 0.002(5) C1A 0.094(12) 0.075(11) 0.053(8) 0.004(8) 0.010(8) -0.026(9) C2A 0.062(10) 0.102(15) 0.086(13) -0.033(12) 0.002(9) -0.006(9) C3A 0.15(2) 0.15(2) 0.045(10) -0.030(12) 0.023(12) 0.008(18) C1B 0.070(10) 0.094(12) 0.082(11) -0.057(10) 0.028(9) -0.027(9) C2B 0.067(8) 0.22(2) 0.052(7) -0.034(9) 0.021(6) -0.044(10) C3B 0.067(8) 0.22(2) 0.052(7) -0.034(9) 0.021(6) -0.044(10) C1C 0.059(8) 0.046(7) 0.087(10) -0.032(7) 0.025(7) -0.028(6) C2C 0.053(7) 0.084(11) 0.065(9) -0.037(8) 0.010(6) -0.037(7) C3C 0.101(12) 0.087(10) 0.147(18) 0.036(12) -0.025(11) -0.023(9) C4C 0.101(12) 0.087(10) 0.147(18) 0.036(12) -0.025(11) -0.023(9) C1D 0.061(6) 0.068(7) 0.072(7) -0.005(6) 0.001(5) -0.012(5) C2D 0.061(6) 0.068(7) 0.072(7) -0.005(6) 0.001(5) -0.012(5) N2 0.059(6) 0.048(6) 0.074(8) -0.005(6) 0.020(6) 0.023(5) C1E 0.044(7) 0.088(11) 0.081(11) -0.010(9) 0.007(7) 0.023(7) C2E 0.19(3) 0.055(10) 0.078(13) 0.016(10) -0.009(15) -0.007(13) C1F 0.062(8) 0.109(14) 0.069(10) 0.020(10) 0.007(8) 0.041(9) C2F 0.098(13) 0.092(13) 0.088(12) 0.002(11) 0.012(11) 0.068(12) C1G 0.056(8) 0.093(12) 0.057(8) 0.005(8) 0.006(6) 0.038(8) C2G 0.098(19) 0.22(4) 0.12(2) -0.03(2) 0.016(17) 0.06(2) C3G 0.14(2) 0.24(4) 0.13(2) 0.13(3) 0.072(19) 0.11(3) C1H 0.107(16) 0.084(12) 0.104(16) -0.004(12) 0.037(13) 0.046(12) C2H 0.088(15) 0.15(2) 0.14(2) -0.09(2) 0.026(15) -0.052(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O33 1.682(8) . ? Mo1 O20 1.821(7) . ? Mo1 O25 1.841(6) . ? Mo1 O4 2.004(7) . ? Mo1 O21 2.004(7) . ? Mo1 Mo3 3.1983(12) . ? Mo2 O45 1.652(7) . ? Mo2 O13 1.935(7) . ? Mo2 O31 1.983(8) . ? Mo2 O25 2.001(7) . ? Mo2 O39 2.050(8) . ? Mo2 Mo11 2.6212(12) . ? Mo3 O5 1.684(7) . ? Mo3 O15 1.820(6) . ? Mo3 O40 1.825(7) . ? Mo3 O4 2.013(6) . ? Mo3 O21 2.035(8) . ? Mo4 O37 1.681(7) . ? Mo4 O12 1.950(7) . ? Mo4 O1 1.955(6) . ? Mo4 O15 2.013(7) . ? Mo4 O6 2.051(6) . ? Mo4 Mo7 2.6082(12) . ? Mo5 O11 1.690(8) . ? Mo5 O23 1.817(7) . ? Mo5 O22 1.821(7) . ? Mo5 O9 2.035(7) . ? Mo5 O18 2.054(7) . ? Mo5 Mo12 3.1940(13) . ? Mo6 O34 1.660(8) . ? Mo6 O17 1.953(7) . ? Mo6 O3 1.966(6) . ? Mo6 O40 1.986(7) . ? Mo6 O6 2.066(7) . ? Mo6 Mo8 2.6047(12) . ? Mo7 O36 1.679(8) . ? Mo7 O1 1.933(7) . ? Mo7 O12 1.978(7) . ? Mo7 O26 1.987(7) . ? Mo7 O14 2.061(8) . ? Mo8 O43 1.652(8) . ? Mo8 O17 1.951(7) . ? Mo8 O3 1.961(7) . ? Mo8 O22 1.983(8) . ? Mo8 O8 2.078(7) . ? Mo9 O42 1.672(8) . ? Mo9 O16 1.945(7) . ? Mo9 O7 1.962(7) . ? Mo9 O20 1.999(8) . ? Mo9 O39 2.067(7) . ? Mo9 Mo10 2.6115(12) . ? Mo10 O41 1.653(9) . ? Mo10 O7 1.933(7) . ? Mo10 O16 1.948(7) . ? Mo10 O28 1.987(8) . ? Mo10 O14 2.077(7) . ? Mo11 O32 1.692(7) . ? Mo11 O31 1.947(8) . ? Mo11 O13 1.974(6) . ? Mo11 O23 2.020(7) . ? Mo11 O8 2.081(7) . ? Mo12 O29 1.700(8) . ? Mo12 O26 1.843(8) . ? Mo12 O28 1.847(8) . ? Mo12 O9 1.991(7) . ? Mo12 O18 2.022(6) . ? Zn1 O27 1.940(7) . ? Zn1 O21 1.964(7) . ? Zn1 O16 1.995(7) . ? Zn1 O12 1.997(7) . ? Zn2 O18 1.949(6) . ? Zn2 O30 1.956(7) . ? Zn2 O17 2.001(7) . ? Zn2 O1 2.012(7) . ? Zn3 O38 1.917(8) . ? Zn3 O4 1.954(7) . ? Zn3 O13 1.980(7) . ? Zn3 O3 1.985(7) . ? Zn4 O35 1.915(7) . ? Zn4 O9 1.954(6) . ? Zn4 O31 1.972(8) . ? Zn4 O7 2.004(7) . ? P1 O24 1.539(7) . ? P1 O10 1.544(6) . ? P1 O2 1.552(7) . ? P1 O19 1.555(6) . ? O27 C15 1.278(12) . ? O30 C16 1.282(13) . ? O35 C8 1.280(12) . ? O38 C7 1.251(13) . ? O44 C8 1.270(15) . ? O46 C15 1.251(13) . ? O47 C7 1.229(15) . ? O48 C16 1.212(14) . ? C1 C2 1.355(16) . ? C1 C6 1.389(14) 2_654 ? C1 C8 1.502(13) . ? C2 C3 1.419(14) . ? C2 H2 0.9300 . ? C3 C4 1.357(16) 2_654 ? C3 H3 0.9300 . ? C4 C5 1.350(16) . ? C4 C3 1.357(16) 2_655 ? C4 H4 0.9300 . ? C5 C6 1.409(14) . ? C5 C7 1.507(15) . ? C6 C1 1.389(14) 2_655 ? C6 H6 0.9300 . ? C9 C14 1.376(13) . ? C9 C10 1.378(15) . ? C9 C15 1.522(13) . ? C10 C11 1.404(15) 2_554 ? C10 H10 0.9300 . ? C11 C12 1.393(14) . ? C11 C10 1.404(15) 2 ? C11 H11 0.9300 . ? C12 C13 1.434(13) . ? C12 H12 0.9300 . ? C13 C14 1.421(14) 2 ? C13 C16 1.516(13) . ? C14 C13 1.421(14) 2_554 ? C14 H14 0.9300 . ? N1 C1C 1.500(17) . ? N1 C1B 1.54(2) . ? N1 C1D 1.559(12) . ? N1 C1A 1.571(15) . ? C1A C2A 1.519(16) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.566(17) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.563(19) . ? C3A H3A1 0.9700 . ? C3A H3A2 0.9700 . ? C4A H4A1 0.9600 . ? C4A H4A2 0.9600 . ? C4A H4A3 0.9600 . ? C1B C2B 1.63(3) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.556(16) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C4B 1.472(17) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? C4B H4B1 0.9600 . ? C4B H4B2 0.9600 . ? C4B H4B3 0.9600 . ? C1C C2C 1.54(2) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C2C C3C 1.60(3) . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C3C C4C 1.54(5) . ? C3C H3C1 0.9700 . ? C3C H3C2 0.9700 . ? C1D C2D 1.50(2) . ? C1D H1D1 0.9700 . ? C1D H1D2 0.9700 . ? C2D C3D 1.51(3) . ? C2D H2D1 0.9700 . ? C2D H2D2 0.9700 . ? C3D C4D 1.558(18) . ? C3D H3D1 0.9700 . ? C3D H3D2 0.9700 . ? N2 C1G 1.477(19) . ? N2 C1F 1.53(2) . ? N2 C1E 1.537(13) . ? N2 C1H 1.537(16) . ? C1E C2E 1.553(16) . ? C1E H1E1 0.9700 . ? C1E H1E2 0.9700 . ? C2E C3E 1.566(18) . ? C2E H2E1 0.9700 . ? C2E H2E2 0.9700 . ? C3E C4E2 1.55(2) . ? C3E C4E1 1.56(2) . ? C4E1 C4E2 1.95(10) . ? C1F C2F 1.54(2) . ? C1F H1F1 0.9700 . ? C1F H1F2 0.9700 . ? C2F C3F 1.548(18) . ? C2F H2F1 0.9700 . ? C2F H2F2 0.9700 . ? C3F C4F 1.521(18) . ? C3F H3F1 0.9700 . ? C3F H3F2 0.9700 . ? C1G C2G 1.54(3) . ? C1G H1G1 0.9700 . ? C1G H1G2 0.9700 . ? C2G C3G 1.553(18) . ? C2G H2G1 0.9700 . ? C2G H2G2 0.9700 . ? C3G C4G 1.528(19) . ? C3G H3G1 0.9700 . ? C3G H3G2 0.9700 . ? C1H C2H 1.58(3) . ? C1H H1H1 0.9700 . ? C1H H1H2 0.9700 . ? C2H C3H 1.527(18) . ? C2H H2H1 0.9700 . ? C2H H2H2 0.9700 . ? C3H C4H 1.54(2) . ? C3H H3H1 0.9700 . ? C3H H3H2 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O33 Mo1 O20 104.0(4) . . ? O33 Mo1 O25 103.3(4) . . ? O20 Mo1 O25 96.5(3) . . ? O33 Mo1 O4 102.6(4) . . ? O20 Mo1 O4 151.3(3) . . ? O25 Mo1 O4 87.8(3) . . ? O33 Mo1 O21 102.1(3) . . ? O20 Mo1 O21 89.4(3) . . ? O25 Mo1 O21 151.7(3) . . ? O4 Mo1 O21 74.6(3) . . ? O33 Mo1 Mo3 99.9(3) . . ? O20 Mo1 Mo3 125.9(2) . . ? O25 Mo1 Mo3 124.0(2) . . ? O4 Mo1 Mo3 37.32(17) . . ? O21 Mo1 Mo3 38.0(2) . . ? O45 Mo2 O13 107.4(4) . . ? O45 Mo2 O31 107.0(4) . . ? O13 Mo2 O31 93.0(3) . . ? O45 Mo2 O25 100.4(4) . . ? O13 Mo2 O25 83.4(3) . . ? O31 Mo2 O25 152.1(3) . . ? O45 Mo2 O39 99.0(4) . . ? O13 Mo2 O39 153.2(3) . . ? O31 Mo2 O39 83.8(3) . . ? O25 Mo2 O39 87.2(3) . . ? O45 Mo2 Mo11 101.5(3) . . ? O13 Mo2 Mo11 48.54(19) . . ? O31 Mo2 Mo11 47.6(2) . . ? O25 Mo2 Mo11 131.2(2) . . ? O39 Mo2 Mo11 130.89(19) . . ? O5 Mo3 O15 102.9(3) . . ? O5 Mo3 O40 105.3(4) . . ? O15 Mo3 O40 97.9(3) . . ? O5 Mo3 O4 102.6(3) . . ? O15 Mo3 O4 150.6(3) . . ? O40 Mo3 O4 89.2(3) . . ? O5 Mo3 O21 100.7(3) . . ? O15 Mo3 O21 87.5(3) . . ? O40 Mo3 O21 151.5(3) . . ? O4 Mo3 O21 73.7(3) . . ? O5 Mo3 Mo1 99.1(3) . . ? O15 Mo3 Mo1 123.6(2) . . ? O40 Mo3 Mo1 125.1(2) . . ? O4 Mo3 Mo1 37.1(2) . . ? O21 Mo3 Mo1 37.31(18) . . ? O37 Mo4 O12 105.9(4) . . ? O37 Mo4 O1 106.9(4) . . ? O12 Mo4 O1 93.4(3) . . ? O37 Mo4 O15 100.7(4) . . ? O12 Mo4 O15 83.1(3) . . ? O1 Mo4 O15 152.1(3) . . ? O37 Mo4 O6 99.3(4) . . ? O12 Mo4 O6 154.2(2) . . ? O1 Mo4 O6 84.6(3) . . ? O15 Mo4 O6 86.7(3) . . ? O37 Mo4 Mo7 100.8(3) . . ? O12 Mo4 Mo7 48.9(2) . . ? O1 Mo4 Mo7 47.5(2) . . ? O15 Mo4 Mo7 131.1(2) . . ? O6 Mo4 Mo7 131.68(19) . . ? O11 Mo5 O23 103.3(4) . . ? O11 Mo5 O22 104.4(4) . . ? O23 Mo5 O22 96.4(3) . . ? O11 Mo5 O9 102.3(3) . . ? O23 Mo5 O9 88.7(3) . . ? O22 Mo5 O9 150.8(3) . . ? O11 Mo5 O18 102.3(3) . . ? O23 Mo5 O18 151.7(3) . . ? O22 Mo5 O18 88.9(3) . . ? O9 Mo5 O18 74.1(3) . . ? O11 Mo5 Mo12 98.9(3) . . ? O23 Mo5 Mo12 124.8(2) . . ? O22 Mo5 Mo12 125.8(2) . . ? O9 Mo5 Mo12 37.01(19) . . ? O18 Mo5 Mo12 38.05(17) . . ? O34 Mo6 O17 104.7(4) . . ? O34 Mo6 O3 105.8(4) . . ? O17 Mo6 O3 93.5(3) . . ? O34 Mo6 O40 102.3(3) . . ? O17 Mo6 O40 152.6(3) . . ? O3 Mo6 O40 83.4(3) . . ? O34 Mo6 O6 97.9(4) . . ? O17 Mo6 O6 85.4(3) . . ? O3 Mo6 O6 155.6(3) . . ? O40 Mo6 O6 86.5(3) . . ? O34 Mo6 Mo8 99.0(3) . . ? O17 Mo6 Mo8 48.1(2) . . ? O3 Mo6 Mo8 48.4(2) . . ? O40 Mo6 Mo8 131.08(19) . . ? O6 Mo6 Mo8 133.19(18) . . ? O36 Mo7 O1 106.3(4) . . ? O36 Mo7 O12 105.5(3) . . ? O1 Mo7 O12 93.2(3) . . ? O36 Mo7 O26 101.4(4) . . ? O1 Mo7 O26 84.2(3) . . ? O12 Mo7 O26 152.5(3) . . ? O36 Mo7 O14 98.3(4) . . ? O1 Mo7 O14 155.0(3) . . ? O12 Mo7 O14 84.3(3) . . ? O26 Mo7 O14 86.7(3) . . ? O36 Mo7 Mo4 100.1(3) . . ? O1 Mo7 Mo4 48.23(18) . . ? O12 Mo7 Mo4 47.9(2) . . ? O26 Mo7 Mo4 131.6(2) . . ? O14 Mo7 Mo4 131.8(2) . . ? O43 Mo8 O17 106.7(4) . . ? O43 Mo8 O3 106.7(4) . . ? O17 Mo8 O3 93.7(3) . . ? O43 Mo8 O22 100.5(4) . . ? O17 Mo8 O22 84.3(3) . . ? O3 Mo8 O22 152.0(3) . . ? O43 Mo8 O8 98.6(4) . . ? O17 Mo8 O8 154.3(3) . . ? O3 Mo8 O8 83.2(3) . . ? O22 Mo8 O8 86.8(3) . . ? O43 Mo8 Mo6 101.2(3) . . ? O17 Mo8 Mo6 48.17(19) . . ? O3 Mo8 Mo6 48.52(19) . . ? O22 Mo8 Mo6 131.7(2) . . ? O8 Mo8 Mo6 131.23(18) . . ? O42 Mo9 O16 105.9(4) . . ? O42 Mo9 O7 105.7(4) . . ? O16 Mo9 O7 92.2(3) . . ? O42 Mo9 O20 100.7(4) . . ? O16 Mo9 O20 84.4(3) . . ? O7 Mo9 O20 153.2(3) . . ? O42 Mo9 O39 98.5(4) . . ? O16 Mo9 O39 155.3(3) . . ? O7 Mo9 O39 85.0(3) . . ? O20 Mo9 O39 87.1(3) . . ? O42 Mo9 Mo10 99.5(3) . . ? O16 Mo9 Mo10 47.9(2) . . ? O7 Mo9 Mo10 47.4(2) . . ? O20 Mo9 Mo10 131.7(2) . . ? O39 Mo9 Mo10 132.14(19) . . ? O41 Mo10 O7 105.7(4) . . ? O41 Mo10 O16 106.4(4) . . ? O7 Mo10 O16 93.1(3) . . ? O41 Mo10 O28 101.9(4) . . ? O7 Mo10 O28 83.6(3) . . ? O16 Mo10 O28 151.3(3) . . ? O41 Mo10 O14 99.6(4) . . ? O7 Mo10 O14 154.3(3) . . ? O16 Mo10 O14 83.8(3) . . ? O28 Mo10 O14 86.9(3) . . ? O41 Mo10 Mo9 99.8(4) . . ? O7 Mo10 Mo9 48.4(2) . . ? O16 Mo10 Mo9 47.8(2) . . ? O28 Mo10 Mo9 131.2(2) . . ? O14 Mo10 Mo9 131.3(2) . . ? O32 Mo11 O31 105.1(4) . . ? O32 Mo11 O13 107.5(4) . . ? O31 Mo11 O13 92.9(3) . . ? O32 Mo11 O23 102.1(4) . . ? O31 Mo11 O23 83.1(3) . . ? O13 Mo11 O23 150.1(3) . . ? O32 Mo11 O8 99.2(4) . . ? O31 Mo11 O8 155.4(3) . . ? O13 Mo11 O8 83.5(3) . . ? O23 Mo11 O8 88.0(3) . . ? O32 Mo11 Mo2 100.2(3) . . ? O31 Mo11 Mo2 48.8(2) . . ? O13 Mo11 Mo2 47.3(2) . . ? O23 Mo11 Mo2 130.8(2) . . ? O8 Mo11 Mo2 130.54(18) . . ? O29 Mo12 O26 104.1(4) . . ? O29 Mo12 O28 102.8(4) . . ? O26 Mo12 O28 96.5(3) . . ? O29 Mo12 O9 102.0(4) . . ? O26 Mo12 O9 152.0(3) . . ? O28 Mo12 O9 87.4(3) . . ? O29 Mo12 O18 102.7(4) . . ? O26 Mo12 O18 88.8(3) . . ? O28 Mo12 O18 151.8(3) . . ? O9 Mo12 O18 75.7(3) . . ? O29 Mo12 Mo5 98.9(3) . . ? O26 Mo12 Mo5 126.5(2) . . ? O28 Mo12 Mo5 124.5(2) . . ? O9 Mo12 Mo5 37.97(18) . . ? O18 Mo12 Mo5 38.77(19) . . ? O27 Zn1 O21 117.7(3) . . ? O27 Zn1 O16 105.6(3) . . ? O21 Zn1 O16 109.6(3) . . ? O27 Zn1 O12 114.1(3) . . ? O21 Zn1 O12 108.5(3) . . ? O16 Zn1 O12 99.6(3) . . ? O18 Zn2 O30 123.3(3) . . ? O18 Zn2 O17 105.4(3) . . ? O30 Zn2 O17 106.1(3) . . ? O18 Zn2 O1 107.4(3) . . ? O30 Zn2 O1 111.7(3) . . ? O17 Zn2 O1 100.2(3) . . ? O38 Zn3 O4 114.5(3) . . ? O38 Zn3 O13 111.1(3) . . ? O4 Zn3 O13 109.2(3) . . ? O38 Zn3 O3 110.0(4) . . ? O4 Zn3 O3 110.4(3) . . ? O13 Zn3 O3 100.8(3) . . ? O35 Zn4 O9 120.7(3) . . ? O35 Zn4 O31 107.4(4) . . ? O9 Zn4 O31 111.5(3) . . ? O35 Zn4 O7 107.1(3) . . ? O9 Zn4 O7 106.2(3) . . ? O31 Zn4 O7 102.2(3) . . ? O24 P1 O10 109.5(3) . . ? O24 P1 O2 108.9(4) . . ? O10 P1 O2 111.7(4) . . ? O24 P1 O19 110.6(4) . . ? O10 P1 O19 107.6(4) . . ? O2 P1 O19 108.4(3) . . ? Mo7 O1 Mo4 84.3(3) . . ? Mo7 O1 Zn2 131.2(3) . . ? Mo4 O1 Zn2 137.3(4) . . ? Mo8 O3 Mo6 83.1(2) . . ? Mo8 O3 Zn3 137.7(4) . . ? Mo6 O3 Zn3 129.3(4) . . ? Zn3 O4 Mo1 124.8(3) . . ? Zn3 O4 Mo3 123.5(3) . . ? Mo1 O4 Mo3 105.5(3) . . ? Mo4 O6 Mo6 122.1(3) . . ? Mo10 O7 Mo9 84.2(2) . . ? Mo10 O7 Zn4 131.9(4) . . ? Mo9 O7 Zn4 135.7(4) . . ? Mo8 O8 Mo11 121.0(3) . . ? Zn4 O9 Mo12 127.6(4) . . ? Zn4 O9 Mo5 122.1(4) . . ? Mo12 O9 Mo5 105.0(3) . . ? Mo4 O12 Mo7 83.2(3) . . ? Mo4 O12 Zn1 131.2(4) . . ? Mo7 O12 Zn1 137.3(4) . . ? Mo2 O13 Mo11 84.2(3) . . ? Mo2 O13 Zn3 131.0(3) . . ? Mo11 O13 Zn3 137.8(4) . . ? Mo7 O14 Mo10 121.7(4) . . ? Mo3 O15 Mo4 127.8(3) . . ? Mo9 O16 Mo10 84.3(3) . . ? Mo9 O16 Zn1 129.6(3) . . ? Mo10 O16 Zn1 139.3(4) . . ? Mo8 O17 Mo6 83.7(3) . . ? Mo8 O17 Zn2 133.3(3) . . ? Mo6 O17 Zn2 136.9(4) . . ? Zn2 O18 Mo12 125.0(3) . . ? Zn2 O18 Mo5 126.3(3) . . ? Mo12 O18 Mo5 103.2(3) . . ? Mo1 O20 Mo9 127.5(4) . . ? Zn1 O21 Mo1 123.4(4) . . ? Zn1 O21 Mo3 124.8(4) . . ? Mo1 O21 Mo3 104.7(3) . . ? Mo5 O22 Mo8 128.6(4) . . ? Mo5 O23 Mo11 127.9(4) . . ? Mo1 O25 Mo2 128.6(4) . . ? Mo12 O26 Mo7 127.1(4) . . ? C15 O27 Zn1 113.2(6) . . ? Mo12 O28 Mo10 127.4(4) . . ? C16 O30 Zn2 110.4(6) . . ? Mo11 O31 Zn4 129.5(4) . . ? Mo11 O31 Mo2 83.7(3) . . ? Zn4 O31 Mo2 136.7(4) . . ? C8 O35 Zn4 115.4(7) . . ? C7 O38 Zn3 114.1(7) . . ? Mo2 O39 Mo9 121.9(3) . . ? Mo3 O40 Mo6 127.9(3) . . ? C2 C1 C6 119.7(10) . 2_654 ? C2 C1 C8 120.6(9) . . ? C6 C1 C8 119.7(10) 2_654 . ? C1 C2 C3 119.9(9) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C4 C3 C2 119.8(11) 2_654 . ? C4 C3 H3 120.1 2_654 . ? C2 C3 H3 120.1 . . ? C5 C4 C3 121.0(10) . 2_655 ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 2_655 . ? C4 C5 C6 119.8(10) . . ? C4 C5 C7 121.4(9) . . ? C6 C5 C7 118.8(10) . . ? C1 C6 C5 119.8(12) 2_655 . ? C1 C6 H6 120.1 2_655 . ? C5 C6 H6 120.1 . . ? O47 C7 O38 125.6(10) . . ? O47 C7 C5 119.7(9) . . ? O38 C7 C5 114.6(10) . . ? O44 C8 O35 126.1(9) . . ? O44 C8 C1 116.3(9) . . ? O35 C8 C1 117.5(10) . . ? C14 C9 C10 120.1(9) . . ? C14 C9 C15 120.0(9) . . ? C10 C9 C15 119.9(9) . . ? C9 C10 C11 121.5(10) . 2_554 ? C9 C10 H10 119.2 . . ? C11 C10 H10 119.2 2_554 . ? C12 C11 C10 119.2(10) . 2 ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 2 . ? C11 C12 C13 120.0(10) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 118.2(9) 2 . ? C14 C13 C16 116.5(8) 2 . ? C12 C13 C16 125.0(10) . . ? C9 C14 C13 120.7(9) . 2_554 ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 2_554 . ? O46 C15 O27 125.6(9) . . ? O46 C15 C9 117.3(9) . . ? O27 C15 C9 116.9(8) . . ? O48 C16 O30 127.2(9) . . ? O48 C16 C13 118.3(10) . . ? O30 C16 C13 114.5(9) . . ? C1C N1 C1B 105.5(11) . . ? C1C N1 C1D 113.3(13) . . ? C1B N1 C1D 110.5(12) . . ? C1C N1 C1A 107.6(11) . . ? C1B N1 C1A 111.6(13) . . ? C1D N1 C1A 108.3(11) . . ? C2A C1A N1 115.5(13) . . ? C2A C1A H1A1 108.4 . . ? N1 C1A H1A1 108.4 . . ? C2A C1A H1A2 108.4 . . ? N1 C1A H1A2 108.4 . . ? H1A1 C1A H1A2 107.5 . . ? C1A C2A C3A 110.5(16) . . ? C1A C2A H2A1 109.5 . . ? C3A C2A H2A1 109.5 . . ? C1A C2A H2A2 109.5 . . ? C3A C2A H2A2 109.5 . . ? H2A1 C2A H2A2 108.1 . . ? C4A C3A C2A 110(3) . . ? C4A C3A H3A1 109.6 . . ? C2A C3A H3A1 109.6 . . ? C4A C3A H3A2 109.6 . . ? C2A C3A H3A2 109.6 . . ? H3A1 C3A H3A2 108.1 . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? N1 C1B C2B 116.1(12) . . ? N1 C1B H1B1 108.3 . . ? C2B C1B H1B1 108.3 . . ? N1 C1B H1B2 108.3 . . ? C2B C1B H1B2 108.3 . . ? H1B1 C1B H1B2 107.4 . . ? C3B C2B C1B 95.7(17) . . ? C3B C2B H2B1 112.6 . . ? C1B C2B H2B1 112.6 . . ? C3B C2B H2B2 112.6 . . ? C1B C2B H2B2 112.6 . . ? H2B1 C2B H2B2 110.1 . . ? C4B C3B C2B 101.4(19) . . ? C4B C3B H3B1 111.5 . . ? C2B C3B H3B1 111.5 . . ? C4B C3B H3B2 111.5 . . ? C2B C3B H3B2 111.5 . . ? H3B1 C3B H3B2 109.3 . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? N1 C1C C2C 114.2(11) . . ? N1 C1C H1C1 108.7 . . ? C2C C1C H1C1 108.7 . . ? N1 C1C H1C2 108.7 . . ? C2C C1C H1C2 108.7 . . ? H1C1 C1C H1C2 107.6 . . ? C1C C2C C3C 109.4(15) . . ? C1C C2C H2C1 109.8 . . ? C3C C2C H2C1 109.8 . . ? C1C C2C H2C2 109.8 . . ? C3C C2C H2C2 109.8 . . ? H2C1 C2C H2C2 108.2 . . ? C4C C3C C2C 113(2) . . ? C4C C3C H3C1 108.9 . . ? C2C C3C H3C1 108.9 . . ? C4C C3C H3C2 108.9 . . ? C2C C3C H3C2 108.9 . . ? H3C1 C3C H3C2 107.7 . . ? C2D C1D N1 124.0(14) . . ? C2D C1D H1D1 106.3 . . ? N1 C1D H1D1 106.3 . . ? C2D C1D H1D2 106.3 . . ? N1 C1D H1D2 106.3 . . ? H1D1 C1D H1D2 106.4 . . ? C1D C2D C3D 109.4(16) . . ? C1D C2D H2D1 109.8 . . ? C3D C2D H2D1 109.8 . . ? C1D C2D H2D2 109.8 . . ? C3D C2D H2D2 109.8 . . ? H2D1 C2D H2D2 108.3 . . ? C2D C3D C4D 114(2) . . ? C2D C3D H3D1 108.6 . . ? C4D C3D H3D1 108.6 . . ? C2D C3D H3D2 108.6 . . ? C4D C3D H3D2 108.6 . . ? H3D1 C3D H3D2 107.6 . . ? C1G N2 C1F 107.2(10) . . ? C1G N2 C1E 111.1(13) . . ? C1F N2 C1E 109.6(13) . . ? C1G N2 C1H 112.0(15) . . ? C1F N2 C1H 112.6(15) . . ? C1E N2 C1H 104.3(11) . . ? N2 C1E C2E 119.5(13) . . ? N2 C1E H1E1 107.4 . . ? C2E C1E H1E1 107.4 . . ? N2 C1E H1E2 107.4 . . ? C2E C1E H1E2 107.4 . . ? H1E1 C1E H1E2 107.0 . . ? C1E C2E C3E 110.0(18) . . ? C1E C2E H2E1 109.7 . . ? C3E C2E H2E1 109.7 . . ? C1E C2E H2E2 109.7 . . ? C3E C2E H2E2 109.7 . . ? H2E1 C2E H2E2 108.2 . . ? C4E2 C3E C4E1 78(5) . . ? C4E2 C3E C2E 127(4) . . ? C4E1 C3E C2E 137(4) . . ? C3E C4E1 C4E2 51(3) . . ? C3E C4E2 C4E1 52(3) . . ? N2 C1F C2F 118.2(13) . . ? N2 C1F H1F1 107.8 . . ? C2F C1F H1F1 107.8 . . ? N2 C1F H1F2 107.8 . . ? C2F C1F H1F2 107.8 . . ? H1F1 C1F H1F2 107.1 . . ? C1F C2F C3F 109.8(17) . . ? C1F C2F H2F1 109.7 . . ? C3F C2F H2F1 109.7 . . ? C1F C2F H2F2 109.7 . . ? C3F C2F H2F2 109.7 . . ? H2F1 C2F H2F2 108.2 . . ? C4F C3F C2F 114(2) . . ? C4F C3F H3F1 108.8 . . ? C2F C3F H3F1 108.8 . . ? C4F C3F H3F2 108.8 . . ? C2F C3F H3F2 108.8 . . ? H3F1 C3F H3F2 107.7 . . ? N2 C1G C2G 116.1(13) . . ? N2 C1G H1G1 108.3 . . ? C2G C1G H1G1 108.3 . . ? N2 C1G H1G2 108.3 . . ? C2G C1G H1G2 108.3 . . ? H1G1 C1G H1G2 107.4 . . ? C1G C2G C3G 115(2) . . ? C1G C2G H2G1 108.6 . . ? C3G C2G H2G1 108.6 . . ? C1G C2G H2G2 108.6 . . ? C3G C2G H2G2 108.6 . . ? H2G1 C2G H2G2 107.6 . . ? C4G C3G C2G 126(3) . . ? C4G C3G H3G1 105.8 . . ? C2G C3G H3G1 105.8 . . ? C4G C3G H3G2 105.8 . . ? C2G C3G H3G2 105.8 . . ? H3G1 C3G H3G2 106.2 . . ? N2 C1H C2H 117.3(14) . . ? N2 C1H H1H1 108.0 . . ? C2H C1H H1H1 108.0 . . ? N2 C1H H1H2 108.0 . . ? C2H C1H H1H2 108.0 . . ? H1H1 C1H H1H2 107.2 . . ? C3H C2H C1H 105(2) . . ? C3H C2H H2H1 110.7 . . ? C1H C2H H2H1 110.7 . . ? C3H C2H H2H2 110.7 . . ? C1H C2H H2H2 110.7 . . ? H2H1 C2H H2H2 108.8 . . ? C2H C3H C4H 98(4) . . ? C2H C3H H3H1 112.1 . . ? C4H C3H H3H1 112.1 . . ? C2H C3H H3H2 112.1 . . ? C4H C3H H3H2 112.1 . . ? H3H1 C3H H3H2 109.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 29.87 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.089 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.161 #==================================================================== data_TPA[e(trim)]infini _database_code_depnum_ccdc_archive 'CCDC 870382' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H45 Mo12 N3 O46 P Zn4' _chemical_formula_weight 2807.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Zn Zn 0.2839 1.4301 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 17.5630(15) _cell_length_b 30.229(2) _cell_length_c 31.886(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16929(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63902 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 30.13 _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8512 _exptl_absorpt_coefficient_mu 2.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4762 _exptl_absorpt_correction_T_max 0.7600 _exptl_absorpt_process_details 'G. M. Sheldrick, SADABS; program for scaling and correction of area detector data, University of G ttingen, Germany, 1997' _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 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 198388 _diffrn_reflns_av_R_equivalents 0.0993 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 30.13 _reflns_number_total 24676 _reflns_number_gt 13560 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _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^ > 2\s(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. The disordered TPA counter-cations could not be located and the data set was corrected with the program SQUEEZE (P. van der Sluis and A. L. Spek, Acta Crystallogr., Sect. A., 1990, 46, 194). ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.025 -0.014 -0.002 9754 10975 ' ' _platon_squeeze_details ; ; _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^)+(0.0561P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000106(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 24676 _refine_ls_number_parameters 650 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1408 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.005 _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 0.92057(3) 0.680218(18) 0.070401(16) 0.01640(12) Uani 1 1 d . . . Mo2 Mo 0.56451(3) 0.679797(18) 0.069670(16) 0.01648(12) Uani 1 1 d . . . Mo3 Mo 0.84442(3) 0.739957(18) 0.112384(16) 0.01737(12) Uani 1 1 d . . . Mo4 Mo 0.63840(3) 0.740202(18) 0.112331(16) 0.01780(12) Uani 1 1 d . . . Mo5 Mo 0.56512(3) 0.682087(18) -0.039845(16) 0.01553(11) Uani 1 1 d . . . Mo6 Mo 0.92082(3) 0.681884(18) -0.039294(16) 0.01592(12) Uani 1 1 d . . . Mo7 Mo 0.63933(3) 0.743407(18) -0.080901(16) 0.01636(12) Uani 1 1 d . . . Mo8 Mo 0.84609(3) 0.743643(18) -0.079983(16) 0.01711(12) Uani 1 1 d . . . Mo9 Mo 0.74249(3) 0.823881(16) 0.067074(15) 0.01742(11) Uani 1 1 d . . . Mo10 Mo 0.74201(3) 0.825806(16) -0.032655(15) 0.01760(11) Uani 1 1 d . . . Mo11 Mo 0.83403(3) 0.597273(17) 0.014618(16) 0.01657(11) Uani 1 1 d . . . Mo12 Mo 0.65188(3) 0.597278(17) 0.013612(16) 0.01632(11) Uani 1 1 d . . . Zn1 Zn 1.07500(4) 0.71151(2) 0.01642(2) 0.01765(15) Uani 1 1 d . . . Zn2 Zn 0.74296(4) 0.63832(2) -0.07439(2) 0.01755(14) Uani 1 1 d . . . Zn3 Zn 0.91008(4) 0.78873(2) 0.01672(2) 0.01725(15) Uani 1 1 d . . . Zn4 Zn 0.74166(4) 0.63474(2) 0.10418(2) 0.01853(15) Uani 1 1 d . . . P1 P 0.74259(7) 0.71125(5) 0.01564(4) 0.0134(3) Uani 1 1 d . . . O1 O 0.9769(2) 0.68002(13) 0.01560(12) 0.0170(8) Uani 1 1 d . . . O2 O 0.7425(2) 0.60314(12) -0.02363(11) 0.0186(8) Uani 1 1 d . . . O3 O 0.6542(2) 0.67654(14) 0.10491(12) 0.0189(9) Uani 1 1 d . . . O4 O 0.7406(3) 0.60125(14) -0.12366(12) 0.0291(11) Uani 1 1 d . . . O5 O 0.7425(2) 0.73957(12) 0.05572(12) 0.0188(8) Uani 1 1 d . . . O6 O 0.6549(2) 0.67978(13) -0.07577(12) 0.0179(9) Uani 1 1 d . . . O7 O 0.8153(2) 0.68271(12) 0.01535(12) 0.0174(8) Uani 1 1 d . . . O8 O 0.7380(2) 0.59665(14) 0.15323(13) 0.0295(10) Uani 1 1 d . . . O9 O 0.7422(2) 0.74090(12) -0.02376(11) 0.0166(8) Uani 1 1 d . . . O10 O 0.7419(2) 0.60220(12) 0.05163(11) 0.0178(8) Uani 1 1 d . . . O11 O 0.5830(2) 0.75064(15) -0.12221(13) 0.0258(11) Uani 1 1 d . . . O12 O 0.8302(2) 0.67910(13) -0.07549(11) 0.0180(9) Uani 1 1 d . . . O13 O 0.6733(2) 0.81995(13) 0.01710(12) 0.0200(9) Uani 1 1 d . . . O14 O 0.5744(2) 0.74447(14) 0.06224(12) 0.0192(9) Uani 1 1 d . . . O15 O 1.0082(2) 0.81843(13) 0.01482(12) 0.0170(8) Uani 1 1 d . . . O16 O 0.8292(2) 0.67609(13) 0.10600(12) 0.0182(9) Uani 1 1 d . . . O17 O 0.9081(2) 0.74413(13) 0.06294(12) 0.0160(9) Uani 1 1 d . . . O18 O 0.5801(2) 0.74533(17) 0.15336(13) 0.0296(11) Uani 1 1 d . . . O19 O 0.5757(2) 0.74549(14) -0.03078(12) 0.0179(9) Uani 1 1 d . . . O20 O 0.9016(2) 0.74666(15) 0.15352(13) 0.0245(10) Uani 1 1 d . . . O21 O 0.9030(2) 0.75219(15) -0.12103(14) 0.0273(11) Uani 1 1 d . . . O22 O 0.7407(2) 0.73738(13) 0.14430(11) 0.0204(9) Uani 1 1 d . . . O23 O 0.8110(2) 0.81923(12) 0.01754(12) 0.0182(8) Uani 1 1 d . . . O24 O 0.6376(2) 0.54193(13) 0.01197(14) 0.0264(10) Uani 1 1 d . . . O25 O 0.9096(2) 0.74620(13) -0.03043(12) 0.0181(9) Uani 1 1 d . . . O26 O 0.8946(2) 0.61792(14) 0.05673(12) 0.0194(9) Uani 1 1 d . . . O27 O 0.7424(2) 0.74117(13) -0.11245(12) 0.0214(9) Uani 1 1 d . . . O28 O 0.6706(2) 0.68119(12) 0.01559(11) 0.0155(8) Uani 1 1 d . . . O29 O 0.7445(2) 0.87903(13) 0.07732(14) 0.0293(10) Uani 1 1 d . . . O30 O 0.7389(2) 0.88105(13) -0.04050(14) 0.0278(10) Uani 1 1 d . . . O31 O 0.8214(2) 0.80329(13) 0.09957(12) 0.0231(10) Uani 1 1 d . . . O32 O 0.9947(2) 0.67251(13) 0.10288(13) 0.0214(10) Uani 1 1 d . . . O33 O 0.5927(2) 0.61567(13) 0.05613(12) 0.0192(9) Uani 1 1 d . . . O34 O 0.5931(2) 0.61872(13) -0.02861(11) 0.0155(9) Uani 1 1 d . . . O35 O 0.8919(2) 0.61688(14) -0.02852(13) 0.0226(10) Uani 1 1 d . . . O36 O 0.8195(2) 0.80686(13) -0.06503(13) 0.0218(10) Uani 1 1 d . . . O37 O 0.6657(2) 0.80335(14) 0.09921(12) 0.0216(10) Uani 1 1 d . . . O38 O 0.9936(2) 0.67405(15) -0.07102(13) 0.0285(11) Uani 1 1 d . . . O39 O 0.6657(2) 0.80534(13) -0.06551(12) 0.0187(9) Uani 1 1 d . . . O40 O 0.8492(2) 0.54155(14) 0.01465(14) 0.0284(10) Uani 1 1 d . . . O41 O 0.4905(2) 0.67087(15) 0.10183(13) 0.0309(11) Uani 1 1 d . . . O42 O 0.7500(3) 0.66480(13) -0.15976(13) 0.0310(11) Uani 1 1 d . . . O43 O 0.4917(2) 0.67537(13) -0.07294(13) 0.0212(9) Uani 1 1 d . . . O44 O 0.7417(3) 0.66076(15) 0.18870(13) 0.0409(13) Uani 1 1 d . . . O45 O 0.7317(5) 0.45450(19) -0.26160(18) 0.107(3) Uani 1 1 d . . . O46 O 0.7052(5) 0.46201(17) -0.19681(17) 0.085(2) Uani 1 1 d . . . C1 C 0.7415(4) 0.6193(2) 0.18731(18) 0.0257(14) Uani 1 1 d . . . C2 C 0.7470(4) 0.5948(2) 0.22724(18) 0.0294(15) Uani 1 1 d . . . C3 C 0.7471(4) 0.6190(2) 0.26422(17) 0.0265(14) Uani 1 1 d . . . H3 H 0.7419 0.6497 0.2638 0.032 Uiso 1 1 calc R . . C4 C 0.7448(4) 0.5963(2) -0.19795(18) 0.0274(14) Uani 1 1 d . . . C5 C 0.7466(4) 0.6242(2) -0.15768(18) 0.0275(14) Uani 1 1 d . . . C6 C 0.7310(4) 0.5517(2) -0.19741(18) 0.0345(18) Uani 1 1 d . . . H6 H 0.7162 0.5381 -0.1725 0.041 Uiso 1 1 calc R . . C7 C 0.7389(5) 0.5265(2) -0.23386(19) 0.046(2) Uani 1 1 d . . . C8 C 0.7196(7) 0.4774(2) -0.2330(2) 0.071(4) Uani 1 1 d . . . C9 C 0.7534(4) 0.5492(2) 0.22855(19) 0.0380(18) Uani 1 1 d . . . H9 H 0.7525 0.5333 0.2036 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0143(2) 0.0194(3) 0.0155(3) 0.0010(2) -0.00041(19) 0.0010(2) Mo2 0.0146(2) 0.0199(3) 0.0150(3) 0.0010(2) -0.00108(19) 0.0006(2) Mo3 0.0155(3) 0.0209(3) 0.0157(3) 0.0001(2) -0.0006(2) 0.0003(2) Mo4 0.0165(3) 0.0223(3) 0.0146(3) -0.0014(2) -0.0004(2) 0.0011(2) Mo5 0.0133(2) 0.0198(3) 0.0135(3) -0.0004(2) -0.00008(19) -0.0011(2) Mo6 0.0136(2) 0.0181(3) 0.0161(3) -0.0003(2) -0.00109(19) 0.0003(2) Mo7 0.0146(2) 0.0198(3) 0.0147(3) 0.0018(2) 0.00091(19) -0.0001(2) Mo8 0.0152(3) 0.0207(3) 0.0154(3) 0.0005(2) -0.0002(2) -0.0004(2) Mo9 0.0152(2) 0.0172(2) 0.0199(2) -0.00323(19) -0.0011(2) 0.0012(2) Mo10 0.0157(2) 0.0173(2) 0.0198(2) 0.00162(19) 0.0001(2) -0.0005(2) Mo11 0.0158(2) 0.0172(3) 0.0167(3) -0.0001(2) 0.0005(2) 0.00114(19) Mo12 0.0165(2) 0.0163(3) 0.0162(3) 0.0005(2) 0.0004(2) -0.00098(19) Zn1 0.0134(3) 0.0199(4) 0.0196(4) 0.0008(3) 0.0009(3) -0.0003(3) Zn2 0.0190(3) 0.0203(3) 0.0134(3) -0.0017(3) 0.0001(3) 0.0000(3) Zn3 0.0142(3) 0.0201(4) 0.0174(4) 0.0006(3) 0.0005(3) -0.0006(3) Zn4 0.0183(4) 0.0231(3) 0.0142(3) 0.0010(3) 0.0000(3) 0.0005(3) P1 0.0110(6) 0.0162(7) 0.0130(6) 0.0005(5) 0.0004(6) 0.0013(5) O1 0.0127(19) 0.022(2) 0.017(2) 0.0085(19) 0.0028(17) -0.0011(16) O2 0.019(2) 0.019(2) 0.017(2) 0.0036(15) 0.0021(16) 0.0031(17) O3 0.020(2) 0.025(3) 0.012(2) -0.0004(18) -0.0055(16) -0.0021(18) O4 0.053(3) 0.027(2) 0.0073(19) 0.0003(16) 0.008(2) 0.000(2) O5 0.020(2) 0.0177(19) 0.019(2) 0.0029(15) -0.0002(17) -0.0054(17) O6 0.013(2) 0.021(2) 0.020(2) 0.0026(18) 0.0020(16) 0.0027(17) O7 0.0150(19) 0.018(2) 0.019(2) 0.0041(19) -0.0022(17) 0.0004(16) O8 0.039(3) 0.031(2) 0.018(2) 0.0009(18) 0.002(2) -0.001(2) O9 0.0149(19) 0.0178(19) 0.0170(19) -0.0038(15) -0.0003(16) 0.0021(16) O10 0.017(2) 0.023(2) 0.0138(19) 0.0007(16) 0.0045(16) -0.0036(17) O11 0.023(2) 0.029(3) 0.025(3) 0.002(2) -0.0044(19) -0.0050(19) O12 0.012(2) 0.027(2) 0.015(2) -0.0012(18) -0.0058(16) 0.0033(17) O13 0.016(2) 0.022(2) 0.022(2) -0.004(2) -0.0024(18) 0.0024(16) O14 0.0114(19) 0.027(3) 0.019(2) -0.0058(19) -0.0025(16) 0.0023(17) O15 0.0144(19) 0.021(2) 0.016(2) 0.0039(19) 0.0061(17) -0.0006(16) O16 0.017(2) 0.017(2) 0.020(2) -0.0024(18) 0.0006(17) 0.0045(17) O17 0.024(2) 0.009(2) 0.016(2) 0.0001(16) 0.0052(16) 0.0010(16) O18 0.014(2) 0.050(3) 0.024(3) -0.003(2) 0.0089(18) 0.004(2) O19 0.020(2) 0.022(2) 0.011(2) -0.0033(18) -0.0008(16) -0.0013(17) O20 0.023(2) 0.030(3) 0.021(2) -0.003(2) -0.0008(18) -0.0005(19) O21 0.023(2) 0.035(3) 0.024(3) 0.007(2) 0.0028(18) 0.001(2) O22 0.023(2) 0.025(2) 0.0134(19) -0.0006(16) -0.0044(17) 0.0046(19) O23 0.0137(19) 0.017(2) 0.023(2) 0.0024(19) 0.0002(18) -0.0012(16) O24 0.032(2) 0.015(2) 0.032(3) 0.001(2) 0.004(2) -0.0014(18) O25 0.016(2) 0.016(2) 0.022(2) 0.0029(18) -0.0042(16) -0.0033(16) O26 0.018(2) 0.023(2) 0.017(2) 0.0036(18) 0.0046(17) 0.0113(17) O27 0.020(2) 0.030(2) 0.0142(19) 0.0030(17) -0.0030(17) 0.0004(19) O28 0.0143(19) 0.021(2) 0.0117(19) -0.0042(18) 0.0006(16) -0.0027(15) O29 0.026(2) 0.018(2) 0.043(3) 0.0005(19) -0.008(2) -0.0065(19) O30 0.033(3) 0.016(2) 0.035(3) 0.0025(18) 0.003(2) -0.0026(19) O31 0.025(2) 0.020(2) 0.024(2) -0.0088(19) -0.0023(19) 0.0007(18) O32 0.020(2) 0.022(2) 0.023(2) -0.0022(19) -0.0012(18) 0.0048(18) O33 0.024(2) 0.017(2) 0.017(2) -0.0001(18) 0.0048(17) -0.0025(17) O34 0.022(2) 0.016(2) 0.009(2) -0.0008(16) -0.0003(15) -0.0023(17) O35 0.017(2) 0.025(3) 0.026(3) 0.0008(19) 0.0030(17) -0.0032(18) O36 0.015(2) 0.019(2) 0.032(3) 0.0097(19) 0.0002(18) -0.0050(17) O37 0.015(2) 0.027(3) 0.023(2) 0.0050(19) 0.0028(17) 0.0018(18) O38 0.018(2) 0.045(3) 0.023(2) -0.005(2) 0.0064(18) -0.002(2) O39 0.017(2) 0.021(2) 0.017(2) -0.0052(18) -0.0012(16) 0.0034(17) O40 0.035(3) 0.018(2) 0.031(3) 0.007(2) 0.002(2) 0.0015(19) O41 0.031(3) 0.039(3) 0.023(3) 0.014(2) 0.008(2) 0.001(2) O42 0.058(3) 0.0127(19) 0.022(2) -0.0033(16) -0.009(2) 0.004(2) O43 0.017(2) 0.020(2) 0.027(2) 0.0014(19) -0.0036(18) -0.0016(17) O44 0.073(4) 0.032(3) 0.018(2) 0.0078(19) -0.003(2) 0.005(3) O45 0.259(11) 0.021(3) 0.040(4) -0.003(3) -0.014(5) -0.020(5) O46 0.196(8) 0.020(3) 0.038(4) -0.006(3) 0.001(4) -0.006(4) C1 0.033(4) 0.027(3) 0.017(3) 0.000(2) 0.000(3) 0.001(3) C2 0.043(4) 0.030(3) 0.015(3) 0.001(2) 0.005(3) -0.002(3) C3 0.050(4) 0.017(3) 0.012(3) 0.002(2) 0.001(3) 0.000(3) C4 0.040(4) 0.028(3) 0.014(3) -0.002(2) 0.006(3) 0.011(3) C5 0.036(4) 0.030(3) 0.017(3) -0.004(2) -0.009(3) 0.003(3) C6 0.073(6) 0.020(3) 0.011(3) 0.003(2) 0.000(3) 0.000(3) C7 0.106(7) 0.017(3) 0.016(3) -0.002(3) -0.015(4) -0.020(4) C8 0.186(11) 0.015(4) 0.013(4) -0.004(3) -0.005(5) 0.010(5) C9 0.066(5) 0.032(4) 0.016(3) -0.006(3) 0.004(3) -0.001(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O32 1.679(4) . ? Mo1 O17 1.959(4) . ? Mo1 O16 1.969(4) . ? Mo1 O26 1.986(4) . ? Mo1 O1 2.008(4) . ? Mo1 Mo3 2.6157(8) . ? Mo2 O41 1.677(4) . ? Mo2 O3 1.938(4) . ? Mo2 O14 1.977(4) . ? Mo2 O15 2.010(4) 8_575 ? Mo2 O33 2.047(4) . ? Mo2 Mo4 2.6209(8) . ? Mo3 O20 1.664(4) . ? Mo3 O17 1.937(4) . ? Mo3 O16 1.960(4) . ? Mo3 O31 1.999(4) . ? Mo3 O22 2.087(4) . ? Mo4 O18 1.669(4) . ? Mo4 O3 1.959(4) . ? Mo4 O14 1.958(4) . ? Mo4 O37 2.012(4) . ? Mo4 O22 2.068(4) . ? Mo5 O43 1.678(4) . ? Mo5 O19 1.947(4) . ? Mo5 O6 1.950(4) . ? Mo5 O34 2.010(4) . ? Mo5 O15 2.010(4) 8_575 ? Mo5 Mo7 2.6170(7) . ? Mo6 O38 1.647(4) . ? Mo6 O12 1.968(4) . ? Mo6 O25 1.974(4) . ? Mo6 O1 2.009(4) . ? Mo6 O35 2.059(4) . ? Mo6 Mo8 2.6251(7) . ? Mo7 O11 1.661(4) . ? Mo7 O6 1.949(4) . ? Mo7 O19 1.951(4) . ? Mo7 O39 1.990(4) . ? Mo7 O27 2.073(4) . ? Mo8 O21 1.667(4) . ? Mo8 O25 1.936(4) . ? Mo8 O12 1.976(4) . ? Mo8 O36 2.024(4) . ? Mo8 O27 2.095(4) . ? Mo9 O29 1.699(4) . ? Mo9 O37 1.804(4) . ? Mo9 O31 1.839(4) . ? Mo9 O23 1.991(4) . ? Mo9 O13 2.007(4) . ? Mo9 Mo10 3.1805(7) . ? Mo10 O30 1.689(4) . ? Mo10 O36 1.802(4) . ? Mo10 O39 1.810(4) . ? Mo10 O13 2.001(4) . ? Mo10 O23 2.018(4) . ? Mo11 O40 1.705(4) . ? Mo11 O35 1.810(4) . ? Mo11 O26 1.823(4) . ? Mo11 O10 2.009(4) . ? Mo11 O2 2.026(4) . ? Mo11 Mo12 3.1992(7) . ? Mo12 O24 1.693(4) . ? Mo12 O33 1.797(4) . ? Mo12 O34 1.816(4) . ? Mo12 O2 1.993(4) . ? Mo12 O10 1.997(4) . ? Zn1 O1 1.969(4) . ? Zn1 O13 1.972(4) 8_675 ? Zn1 O14 1.976(4) 8_675 ? Zn1 O19 1.989(4) 8_675 ? Zn2 O2 1.937(4) . ? Zn2 O4 1.930(4) . ? Zn2 O12 1.967(4) . ? Zn2 O6 1.992(4) . ? Zn3 O15 1.944(4) . ? Zn3 O23 1.969(4) . ? Zn3 O25 1.978(4) . ? Zn3 O17 1.998(4) . ? Zn4 O10 1.943(4) . ? Zn4 O8 1.943(4) . ? Zn4 O16 1.983(4) . ? Zn4 O3 1.989(4) . ? P1 O7 1.542(4) . ? P1 O5 1.538(4) . ? P1 O9 1.543(4) . ? P1 O28 1.557(4) . ? O4 C5 1.292(7) . ? O8 C1 1.286(7) . ? O13 Zn1 1.972(4) 8_575 ? O14 Zn1 1.976(4) 8_575 ? O15 Mo2 2.010(4) 8_675 ? O15 Mo5 2.010(4) 8_675 ? O19 Zn1 1.989(4) 8_575 ? O42 C5 1.230(7) . ? O44 C1 1.253(7) . ? O45 C8 1.164(8) . ? O46 C8 1.271(8) . ? C1 C2 1.477(8) . ? C2 C9 1.384(9) . ? C2 C3 1.389(8) . ? C3 C4 1.396(8) 7_756 ? C3 H3 0.9300 . ? C4 C6 1.369(8) . ? C4 C3 1.396(8) 7_755 ? C4 C5 1.537(8) . ? C6 C7 1.397(8) . ? C6 H6 0.9300 . ? C7 C9 1.387(9) 7_755 ? C7 C8 1.523(10) . ? C9 C7 1.387(9) 7_756 ? C9 H9 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O32 Mo1 O17 107.35(18) . . ? O32 Mo1 O16 105.49(18) . . ? O17 Mo1 O16 92.38(16) . . ? O32 Mo1 O26 100.49(18) . . ? O17 Mo1 O26 151.99(16) . . ? O16 Mo1 O26 83.06(16) . . ? O32 Mo1 O1 98.89(17) . . ? O17 Mo1 O1 87.26(16) . . ? O16 Mo1 O1 154.52(16) . . ? O26 Mo1 O1 85.38(16) . . ? O32 Mo1 Mo3 100.15(14) . . ? O17 Mo1 Mo3 47.48(11) . . ? O16 Mo1 Mo3 48.10(11) . . ? O26 Mo1 Mo3 130.50(11) . . ? O1 Mo1 Mo3 134.37(11) . . ? O41 Mo2 O3 105.5(2) . . ? O41 Mo2 O14 107.5(2) . . ? O3 Mo2 O14 92.77(16) . . ? O41 Mo2 O15 98.92(18) . 8_575 ? O3 Mo2 O15 154.97(15) . 8_575 ? O14 Mo2 O15 84.98(16) . 8_575 ? O41 Mo2 O33 99.43(19) . . ? O3 Mo2 O33 82.96(16) . . ? O14 Mo2 O33 152.89(16) . . ? O15 Mo2 O33 87.76(16) 8_575 . ? O41 Mo2 Mo4 100.28(17) . . ? O3 Mo2 Mo4 48.07(12) . . ? O14 Mo2 Mo4 47.92(11) . . ? O15 Mo2 Mo4 132.59(11) 8_575 . ? O33 Mo2 Mo4 130.51(11) . . ? O20 Mo3 O17 106.55(18) . . ? O20 Mo3 O16 106.50(19) . . ? O17 Mo3 O16 93.34(16) . . ? O20 Mo3 O31 99.60(19) . . ? O17 Mo3 O31 83.58(16) . . ? O16 Mo3 O31 153.47(16) . . ? O20 Mo3 O22 98.44(17) . . ? O17 Mo3 O22 154.54(15) . . ? O16 Mo3 O22 83.98(15) . . ? O31 Mo3 O22 87.63(16) . . ? O20 Mo3 Mo1 100.30(15) . . ? O17 Mo3 Mo1 48.18(11) . . ? O16 Mo3 Mo1 48.42(11) . . ? O31 Mo3 Mo1 131.31(12) . . ? O22 Mo3 Mo1 132.05(11) . . ? O18 Mo4 O3 105.8(2) . . ? O18 Mo4 O14 106.32(19) . . ? O3 Mo4 O14 92.73(16) . . ? O18 Mo4 O37 102.8(2) . . ? O3 Mo4 O37 150.82(16) . . ? O14 Mo4 O37 84.54(17) . . ? O18 Mo4 O22 98.68(18) . . ? O3 Mo4 O22 84.02(15) . . ? O14 Mo4 O22 154.70(15) . . ? O37 Mo4 O22 86.23(15) . . ? O18 Mo4 Mo2 99.66(16) . . ? O3 Mo4 Mo2 47.39(11) . . ? O14 Mo4 Mo2 48.55(13) . . ? O37 Mo4 Mo2 132.15(12) . . ? O22 Mo4 Mo2 131.11(11) . . ? O43 Mo5 O19 106.59(18) . . ? O43 Mo5 O6 104.30(19) . . ? O19 Mo5 O6 92.61(16) . . ? O43 Mo5 O34 100.64(17) . . ? O19 Mo5 O34 152.68(16) . . ? O6 Mo5 O34 82.70(16) . . ? O43 Mo5 O15 99.35(18) . 8_575 ? O19 Mo5 O15 85.77(16) . 8_575 ? O6 Mo5 O15 155.72(16) . 8_575 ? O34 Mo5 O15 87.69(15) . 8_575 ? O43 Mo5 Mo7 98.84(14) . . ? O19 Mo5 Mo7 47.90(11) . . ? O6 Mo5 Mo7 47.84(12) . . ? O34 Mo5 Mo7 129.98(11) . . ? O15 Mo5 Mo7 133.41(11) 8_575 . ? O38 Mo6 O12 105.12(19) . . ? O38 Mo6 O25 107.9(2) . . ? O12 Mo6 O25 92.60(16) . . ? O38 Mo6 O1 98.69(18) . . ? O12 Mo6 O1 154.98(15) . . ? O25 Mo6 O1 87.23(16) . . ? O38 Mo6 O35 99.0(2) . . ? O12 Mo6 O35 81.80(16) . . ? O25 Mo6 O35 153.05(16) . . ? O1 Mo6 O35 87.07(16) . . ? O38 Mo6 Mo8 100.75(16) . . ? O12 Mo6 Mo8 48.40(12) . . ? O25 Mo6 Mo8 47.21(11) . . ? O1 Mo6 Mo8 134.07(11) . . ? O35 Mo6 Mo8 129.63(11) . . ? O11 Mo7 O6 106.24(19) . . ? O11 Mo7 O19 107.69(19) . . ? O6 Mo7 O19 92.48(17) . . ? O11 Mo7 O39 102.13(19) . . ? O6 Mo7 O39 151.03(16) . . ? O19 Mo7 O39 84.31(16) . . ? O11 Mo7 O27 98.02(18) . . ? O6 Mo7 O27 83.47(15) . . ? O19 Mo7 O27 154.04(15) . . ? O39 Mo7 O27 86.97(15) . . ? O11 Mo7 Mo5 101.15(15) . . ? O6 Mo7 Mo5 47.85(11) . . ? O19 Mo7 Mo5 47.77(12) . . ? O39 Mo7 Mo5 131.21(11) . . ? O27 Mo7 Mo5 130.90(11) . . ? O21 Mo8 O25 106.81(19) . . ? O21 Mo8 O12 107.14(19) . . ? O25 Mo8 O12 93.53(16) . . ? O21 Mo8 O36 100.19(19) . . ? O25 Mo8 O36 84.44(16) . . ? O12 Mo8 O36 151.94(16) . . ? O21 Mo8 O27 97.96(18) . . ? O25 Mo8 O27 154.87(16) . . ? O12 Mo8 O27 82.98(15) . . ? O36 Mo8 O27 87.11(16) . . ? O21 Mo8 Mo6 101.45(15) . . ? O25 Mo8 Mo6 48.46(12) . . ? O12 Mo8 Mo6 48.14(10) . . ? O36 Mo8 Mo6 132.09(11) . . ? O27 Mo8 Mo6 130.78(11) . . ? O29 Mo9 O37 104.1(2) . . ? O29 Mo9 O31 102.01(18) . . ? O37 Mo9 O31 97.28(18) . . ? O29 Mo9 O23 102.07(19) . . ? O37 Mo9 O23 151.46(17) . . ? O31 Mo9 O23 88.14(17) . . ? O29 Mo9 O13 102.90(18) . . ? O37 Mo9 O13 88.76(17) . . ? O31 Mo9 O13 152.05(16) . . ? O23 Mo9 O13 74.44(16) . . ? O29 Mo9 Mo10 100.03(15) . . ? O37 Mo9 Mo10 124.92(13) . . ? O31 Mo9 Mo10 124.87(13) . . ? O23 Mo9 Mo10 37.78(11) . . ? O13 Mo9 Mo10 37.41(11) . . ? O30 Mo10 O36 104.68(19) . . ? O30 Mo10 O39 103.22(19) . . ? O36 Mo10 O39 96.84(17) . . ? O30 Mo10 O13 100.70(18) . . ? O36 Mo10 O13 151.83(17) . . ? O39 Mo10 O13 88.98(16) . . ? O30 Mo10 O23 103.53(18) . . ? O36 Mo10 O23 88.25(17) . . ? O39 Mo10 O23 150.49(17) . . ? O13 Mo10 O23 74.00(16) . . ? O30 Mo10 Mo9 99.57(15) . . ? O36 Mo10 Mo9 124.40(13) . . ? O39 Mo10 Mo9 125.05(12) . . ? O13 Mo10 Mo9 37.55(11) . . ? O23 Mo10 Mo9 37.20(11) . . ? O40 Mo11 O35 103.7(2) . . ? O40 Mo11 O26 104.29(19) . . ? O35 Mo11 O26 96.91(18) . . ? O40 Mo11 O10 101.44(18) . . ? O35 Mo11 O10 151.00(17) . . ? O26 Mo11 O10 90.69(16) . . ? O40 Mo11 O2 102.15(18) . . ? O35 Mo11 O2 87.67(16) . . ? O26 Mo11 O2 151.21(16) . . ? O10 Mo11 O2 72.99(15) . . ? O40 Mo11 Mo12 98.97(14) . . ? O35 Mo11 Mo12 123.62(13) . . ? O26 Mo11 Mo12 126.20(12) . . ? O10 Mo11 Mo12 36.88(10) . . ? O2 Mo11 Mo12 36.90(10) . . ? O24 Mo12 O33 104.08(19) . . ? O24 Mo12 O34 104.21(19) . . ? O33 Mo12 O34 96.90(17) . . ? O24 Mo12 O2 100.84(18) . . ? O33 Mo12 O2 152.12(17) . . ? O34 Mo12 O2 88.87(16) . . ? O24 Mo12 O10 102.12(18) . . ? O33 Mo12 O10 88.66(16) . . ? O34 Mo12 O10 150.82(16) . . ? O2 Mo12 O10 73.95(15) . . ? O24 Mo12 Mo11 98.56(14) . . ? O33 Mo12 Mo11 124.82(13) . . ? O34 Mo12 Mo11 125.15(12) . . ? O2 Mo12 Mo11 37.61(11) . . ? O10 Mo12 Mo11 37.13(10) . . ? O1 Zn1 O13 122.25(17) . 8_675 ? O1 Zn1 O14 109.31(16) . 8_675 ? O13 Zn1 O14 108.75(16) 8_675 8_675 ? O1 Zn1 O19 108.13(16) . 8_675 ? O13 Zn1 O19 108.56(16) 8_675 8_675 ? O14 Zn1 O19 96.86(17) 8_675 8_675 ? O2 Zn2 O4 111.18(17) . . ? O2 Zn2 O12 111.26(16) . . ? O4 Zn2 O12 111.45(17) . . ? O2 Zn2 O6 111.14(16) . . ? O4 Zn2 O6 109.33(18) . . ? O12 Zn2 O6 102.14(16) . . ? O15 Zn3 O23 124.56(17) . . ? O15 Zn3 O25 106.27(16) . . ? O23 Zn3 O25 108.11(16) . . ? O15 Zn3 O17 110.48(16) . . ? O23 Zn3 O17 106.92(16) . . ? O25 Zn3 O17 97.00(16) . . ? O10 Zn4 O8 113.21(17) . . ? O10 Zn4 O16 110.07(15) . . ? O8 Zn4 O16 112.06(17) . . ? O10 Zn4 O3 109.46(15) . . ? O8 Zn4 O3 109.98(17) . . ? O16 Zn4 O3 101.42(15) . . ? O7 P1 O5 108.5(2) . . ? O7 P1 O9 108.9(2) . . ? O5 P1 O9 110.7(2) . . ? O7 P1 O28 110.3(2) . . ? O5 P1 O28 109.0(2) . . ? O9 P1 O28 109.5(2) . . ? Zn1 O1 Mo1 114.72(19) . . ? Zn1 O1 Mo6 115.27(18) . . ? Mo1 O1 Mo6 121.11(18) . . ? Zn2 O2 Mo12 123.38(19) . . ? Zn2 O2 Mo11 123.21(19) . . ? Mo12 O2 Mo11 105.50(17) . . ? Mo2 O3 Mo4 84.54(16) . . ? Mo2 O3 Zn4 130.8(2) . . ? Mo4 O3 Zn4 137.3(2) . . ? C5 O4 Zn2 111.7(4) . . ? Mo7 O6 Mo5 84.31(15) . . ? Mo7 O6 Zn2 137.0(2) . . ? Mo5 O6 Zn2 129.6(2) . . ? C1 O8 Zn4 111.3(4) . . ? Zn4 O10 Mo12 124.04(19) . . ? Zn4 O10 Mo11 123.06(18) . . ? Mo12 O10 Mo11 105.99(17) . . ? Zn2 O12 Mo6 130.3(2) . . ? Zn2 O12 Mo8 136.9(2) . . ? Mo6 O12 Mo8 83.46(15) . . ? Zn1 O13 Mo10 124.2(2) 8_575 . ? Zn1 O13 Mo9 124.6(2) 8_575 . ? Mo10 O13 Mo9 105.04(17) . . ? Mo4 O14 Zn1 130.1(2) . 8_575 ? Mo4 O14 Mo2 83.53(16) . . ? Zn1 O14 Mo2 139.0(2) 8_575 . ? Zn3 O15 Mo2 114.93(18) . 8_675 ? Zn3 O15 Mo5 117.68(19) . 8_675 ? Mo2 O15 Mo5 120.66(18) 8_675 8_675 ? Mo3 O16 Mo1 83.48(15) . . ? Mo3 O16 Zn4 136.9(2) . . ? Mo1 O16 Zn4 130.9(2) . . ? Mo3 O17 Mo1 84.34(15) . . ? Mo3 O17 Zn3 130.9(2) . . ? Mo1 O17 Zn3 138.9(2) . . ? Mo5 O19 Mo7 84.33(15) . . ? Mo5 O19 Zn1 139.0(2) . 8_575 ? Mo7 O19 Zn1 130.1(2) . 8_575 ? Mo4 O22 Mo3 121.09(18) . . ? Zn3 O23 Mo9 125.3(2) . . ? Zn3 O23 Mo10 124.5(2) . . ? Mo9 O23 Mo10 105.02(17) . . ? Mo8 O25 Zn3 130.4(2) . . ? Mo8 O25 Mo6 84.34(16) . . ? Zn3 O25 Mo6 138.5(2) . . ? Mo11 O26 Mo1 128.3(2) . . ? Mo7 O27 Mo8 121.21(18) . . ? Mo9 O31 Mo3 126.3(2) . . ? Mo12 O33 Mo2 126.3(2) . . ? Mo12 O34 Mo5 127.7(2) . . ? Mo11 O35 Mo6 125.3(2) . . ? Mo10 O36 Mo8 127.5(2) . . ? Mo9 O37 Mo4 128.5(2) . . ? Mo10 O39 Mo7 129.5(2) . . ? O44 C1 O8 124.2(6) . . ? O44 C1 C2 118.1(5) . . ? O8 C1 C2 117.6(6) . . ? C9 C2 C3 120.0(6) . . ? C9 C2 C1 122.1(6) . . ? C3 C2 C1 117.8(6) . . ? C2 C3 C4 118.3(6) . 7_756 ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 7_756 . ? C6 C4 C3 120.9(5) . 7_755 ? C6 C4 C5 122.3(5) . . ? C3 C4 C5 116.7(5) 7_755 . ? O42 C5 O4 125.8(5) . . ? O42 C5 C4 120.3(5) . . ? O4 C5 C4 113.8(5) . . ? C4 C6 C7 120.6(6) . . ? C4 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C9 C7 C6 117.3(6) 7_755 . ? C9 C7 C8 121.2(6) 7_755 . ? C6 C7 C8 119.7(6) . . ? O45 C8 O46 121.9(7) . . ? O45 C8 C7 121.7(8) . . ? O46 C8 C7 114.7(6) . . ? C7 C9 C2 121.7(6) 7_756 . ? C7 C9 H9 119.1 7_756 . ? C2 C9 H9 119.1 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.13 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.081 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.203 #==================================================================== data_e(bim)4 _database_code_depnum_ccdc_archive 'CCDC 870383' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H78 Mo12 N9 O52 P Zn4' _chemical_formula_weight 3008.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Zn Zn 0.2839 1.4301 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 15.270(3) _cell_length_b 15.270(3) _cell_length_c 18.496(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4312.6(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8670 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 30.36 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2430 _exptl_absorpt_coefficient_mu 2.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5985 _exptl_absorpt_correction_T_max 0.6736 _exptl_absorpt_process_details 'G. M. Sheldrick, SADABS; program for scaling and correction of area detector data, University of G ttingen, Germany, 1997' _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 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13600 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 30.36 _reflns_number_total 5881 _reflns_number_gt 3288 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^ > 2\s(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. The data set was corrected with the program SQUEEZE (P. van der Sluis and A. L. Spek, Acta Crystallogr., Sect. A., 1990, 46, 194) The contribution of the disordered TBA counter-ions has thus been removed. The AFIX 66 instruction was used for the phenyl ring. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.014 0.222 0.420 1514 576 ' ' 2 0.000 0.500 0.750 36 6 ' ' 3 0.000 0.500 -0.001 3 0 ' ' 4 0.000 0.500 0.501 4 0 ' ' 5 0.500 0.000 0.250 36 6 ' ' 6 0.500 0.000 0.499 3 0 ' ' 7 0.500 0.000 1.001 4 0 ' ' _platon_squeeze_details ; ; _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^)+(0.0624P)^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 constr _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 0.02(3) _refine_ls_number_reflns 5881 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1568 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.76650(6) 0.97085(7) 0.94261(5) 0.0512(3) Uani 1 1 d . . . Mo2 Mo 0.82326(6) 0.85000(6) 1.06058(5) 0.0471(2) Uani 1 1 d . . . Mo3 Mo 0.91684(8) 1.02926(7) 0.81320(5) 0.0580(3) Uani 1 1 d . . . Zn1 Zn 0.92692(9) 0.81870(9) 0.89175(6) 0.0526(3) Uani 1 1 d . . . P1 P 1.0000 1.0000 1.0000 0.0332(10) Uani 1 4 d S . . O1 O 0.9692(4) 0.9222(4) 1.0493(3) 0.0400(13) Uani 1 1 d . . . O2 O 0.8315(5) 0.8617(4) 0.9538(4) 0.0471(17) Uani 1 1 d . . . O3 O 1.0299(4) 0.7861(4) 0.9506(4) 0.0449(17) Uani 1 1 d . . . O4 O 0.9675(6) 0.9170(5) 0.8252(3) 0.062(2) Uani 1 1 d . . . O5 O 0.8040(6) 0.9805(5) 0.8450(4) 0.0521(19) Uani 1 1 d . . . O6 O 0.8564(5) 0.8691(6) 1.1551(4) 0.057(2) Uani 1 1 d . . . O7 O 0.6643(6) 0.9406(7) 0.9371(5) 0.084(2) Uani 1 1 d . . . O8 O 0.8989(7) 1.0369(7) 0.7255(5) 0.084(2) Uani 1 1 d . . . O9 O 0.9054(4) 0.7559(4) 1.0487(4) 0.0460(17) Uani 1 1 d . . . O10 O 0.7304(6) 0.7921(6) 1.0701(5) 0.069(2) Uani 1 1 d . . . N1 N 0.8673(8) 0.7289(7) 0.8322(5) 0.066(3) Uani 1 1 d . . . N2 N 0.7683(8) 0.6716(8) 0.7603(5) 0.071(3) Uani 1 1 d . . . H2 H 0.7259 0.6700 0.7297 0.085 Uiso 1 1 calc R . . C1 C 0.8159(13) 0.7368(11) 0.7764(8) 0.100(6) Uani 1 1 d . . . H1 H 0.8141 0.7882 0.7495 0.119 Uiso 1 1 calc R . . C2 C 0.8556(6) 0.6414(4) 0.8509(5) 0.063(3) Uani 1 1 d G . . C3 C 0.7978(7) 0.6065(5) 0.8005(4) 0.080(5) Uani 1 1 d G . . C4 C 0.7687(8) 0.5206(6) 0.8077(6) 0.113(5) Uani 1 1 d G . . H4 H 0.7301 0.4973 0.7740 0.136 Uiso 1 1 calc R . . C5 C 0.7975(9) 0.4698(5) 0.8654(7) 0.122(7) Uani 1 1 d G . . H5 H 0.7781 0.4123 0.8702 0.147 Uiso 1 1 calc R . . C6 C 0.8553(10) 0.5047(6) 0.9157(6) 0.153(11) Uani 1 1 d G . . H6 H 0.8745 0.4707 0.9543 0.184 Uiso 1 1 calc R . . C7 C 0.8843(8) 0.5905(7) 0.9085(5) 0.113(5) Uani 1 1 d G . . H7 H 0.9230 0.6139 0.9422 0.136 Uiso 1 1 calc R . . O1W O 1.0000 1.0000 0.5000 0.054(4) Uiso 1 4 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 0.0416(5) 0.0553(6) 0.0567(6) -0.0108(5) -0.0029(4) -0.0063(4) Mo2 0.0442(5) 0.0487(5) 0.0483(5) 0.0035(4) 0.0107(4) -0.0064(4) Mo3 0.0765(8) 0.0551(6) 0.0425(4) 0.0021(4) -0.0068(5) 0.0021(6) Zn1 0.0628(8) 0.0485(7) 0.0467(6) -0.0024(6) -0.0062(6) -0.0054(7) P1 0.0285(14) 0.0285(14) 0.043(2) 0.000 0.000 0.000 O1 0.032(3) 0.040(3) 0.048(3) 0.000(3) 0.004(3) -0.003(3) O2 0.064(5) 0.033(3) 0.045(4) 0.004(3) -0.012(3) -0.011(3) O3 0.037(3) 0.041(4) 0.056(4) 0.016(3) 0.011(3) -0.002(3) O4 0.097(7) 0.053(5) 0.036(3) -0.005(3) 0.002(4) 0.024(5) O5 0.070(5) 0.047(4) 0.039(4) 0.002(3) -0.006(4) -0.010(4) O6 0.057(5) 0.069(5) 0.044(4) 0.017(4) 0.008(3) 0.007(4) O7 0.093(5) 0.083(5) 0.076(4) -0.032(4) -0.046(4) 0.028(4) O8 0.093(5) 0.083(5) 0.076(4) -0.032(4) -0.046(4) 0.028(4) O9 0.044(4) 0.040(3) 0.054(4) 0.013(3) 0.007(3) -0.001(3) O10 0.069(5) 0.074(5) 0.064(5) 0.015(4) 0.010(4) -0.025(5) N1 0.069(7) 0.064(6) 0.064(6) -0.013(5) -0.003(5) -0.017(6) N2 0.089(8) 0.077(8) 0.046(5) -0.002(5) -0.013(5) -0.029(7) C1 0.146(16) 0.084(10) 0.069(8) 0.021(8) -0.056(10) -0.064(11) C2 0.057(7) 0.040(6) 0.093(9) -0.004(6) -0.014(6) -0.001(5) C3 0.138(14) 0.042(6) 0.060(7) -0.032(6) -0.019(8) 0.013(8) C4 0.123(11) 0.058(7) 0.159(13) -0.003(7) -0.053(10) -0.021(7) C5 0.159(19) 0.038(8) 0.17(2) -0.016(10) -0.039(15) -0.013(10) C6 0.28(3) 0.082(12) 0.097(13) 0.055(11) 0.000(17) 0.000(18) C7 0.123(11) 0.058(7) 0.159(13) -0.003(7) -0.053(10) -0.021(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O7 1.631(10) . ? Mo1 O5 1.900(7) . ? Mo1 O9 1.903(7) 3_577 ? Mo1 O2 1.951(7) . ? Mo1 O3 1.998(7) 3_577 ? Mo1 Mo2 2.9863(15) . ? Mo2 O10 1.681(8) . ? Mo2 O6 1.842(8) . ? Mo2 O9 1.920(7) . ? Mo2 O3 1.931(7) 3_577 ? Mo2 O2 1.987(7) . ? Mo2 O1 2.495(7) . ? Mo3 O8 1.649(9) . ? Mo3 O4 1.893(8) . ? Mo3 O4 1.960(10) 2_775 ? Mo3 O5 1.967(8) . ? Mo3 O6 1.981(8) 3_577 ? Mo3 Mo3 2.692(2) 2_775 ? Zn1 O2 1.967(8) . ? Zn1 O3 1.976(7) . ? Zn1 N1 1.981(10) . ? Zn1 O4 2.038(8) . ? P1 O1 1.569(6) 2_775 ? P1 O1 1.569(6) 3_577 ? P1 O1 1.569(6) . ? P1 O1 1.569(6) 4_757 ? O3 Mo2 1.931(7) 4_757 ? O3 Mo1 1.998(7) 4_757 ? O4 Mo3 1.960(10) 2_775 ? O6 Mo3 1.981(8) 4_757 ? O9 Mo1 1.903(7) 4_757 ? N1 C1 1.301(16) . ? N1 C2 1.391(13) . ? N2 C1 1.268(15) . ? N2 C3 1.320(13) . ? N2 H2 0.8600 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Mo1 O5 104.5(4) . . ? O7 Mo1 O9 101.8(4) . 3_577 ? O5 Mo1 O9 91.6(3) . 3_577 ? O7 Mo1 O2 104.6(4) . . ? O5 Mo1 O2 90.8(3) . . ? O9 Mo1 O2 151.9(3) 3_577 . ? O7 Mo1 O3 101.8(4) . 3_577 ? O5 Mo1 O3 153.5(3) . 3_577 ? O9 Mo1 O3 86.3(3) 3_577 3_577 ? O2 Mo1 O3 79.3(3) . 3_577 ? O7 Mo1 Mo2 98.6(4) . . ? O5 Mo1 Mo2 130.9(3) . . ? O9 Mo1 Mo2 125.2(2) 3_577 . ? O2 Mo1 Mo2 41.1(2) . . ? O3 Mo1 Mo2 39.7(2) 3_577 . ? O10 Mo2 O6 102.5(4) . . ? O10 Mo2 O9 99.8(4) . . ? O6 Mo2 O9 92.7(3) . . ? O10 Mo2 O3 105.3(4) . 3_577 ? O6 Mo2 O3 91.8(3) . 3_577 ? O9 Mo2 O3 152.9(3) . 3_577 ? O10 Mo2 O2 101.8(4) . . ? O6 Mo2 O2 155.6(3) . . ? O9 Mo2 O2 85.0(3) . . ? O3 Mo2 O2 80.0(3) 3_577 . ? O10 Mo2 O1 174.3(4) . . ? O6 Mo2 O1 76.4(3) . . ? O9 Mo2 O1 74.8(3) . . ? O3 Mo2 O1 80.4(3) 3_577 . ? O2 Mo2 O1 79.7(3) . . ? O10 Mo2 Mo1 99.0(3) . . ? O6 Mo2 Mo1 132.4(3) . . ? O9 Mo2 Mo1 124.7(2) . . ? O3 Mo2 Mo1 41.4(2) 3_577 . ? O2 Mo2 Mo1 40.2(2) . . ? O1 Mo2 Mo1 85.69(15) . . ? O8 Mo3 O4 104.3(4) . . ? O8 Mo3 O4 103.4(5) . 2_775 ? O4 Mo3 O4 89.9(4) . 2_775 ? O8 Mo3 O5 100.1(5) . . ? O4 Mo3 O5 88.9(4) . . ? O4 Mo3 O5 156.1(3) 2_775 . ? O8 Mo3 O6 99.7(4) . 3_577 ? O4 Mo3 O6 156.0(3) . 3_577 ? O4 Mo3 O6 85.9(3) 2_775 3_577 ? O5 Mo3 O6 85.6(4) . 3_577 ? O8 Mo3 Mo3 100.4(4) . 2_775 ? O4 Mo3 Mo3 46.7(3) . 2_775 ? O4 Mo3 Mo3 44.7(2) 2_775 2_775 ? O5 Mo3 Mo3 134.5(2) . 2_775 ? O6 Mo3 Mo3 129.8(3) 3_577 2_775 ? O2 Zn1 O3 110.6(3) . . ? O2 Zn1 N1 102.4(4) . . ? O3 Zn1 N1 119.9(4) . . ? O2 Zn1 O4 109.3(3) . . ? O3 Zn1 O4 106.1(3) . . ? N1 Zn1 O4 108.3(4) . . ? O1 P1 O1 109.7(2) 2_775 3_577 ? O1 P1 O1 108.9(5) 2_775 . ? O1 P1 O1 109.7(2) 3_577 . ? O1 P1 O1 109.7(2) 2_775 4_757 ? O1 P1 O1 108.9(5) 3_577 4_757 ? O1 P1 O1 109.7(2) . 4_757 ? P1 O1 Mo2 130.6(3) . . ? Mo1 O2 Zn1 126.9(4) . . ? Mo1 O2 Mo2 98.6(3) . . ? Zn1 O2 Mo2 126.6(4) . . ? Mo2 O3 Zn1 128.5(3) 4_757 . ? Mo2 O3 Mo1 98.9(3) 4_757 4_757 ? Zn1 O3 Mo1 125.3(3) . 4_757 ? Mo3 O4 Mo3 88.6(4) . 2_775 ? Mo3 O4 Zn1 127.9(4) . . ? Mo3 O4 Zn1 130.6(4) 2_775 . ? Mo1 O5 Mo3 125.3(4) . . ? Mo2 O6 Mo3 125.5(4) . 4_757 ? Mo1 O9 Mo2 125.1(4) 4_757 . ? C1 N1 C2 102.0(10) . . ? C1 N1 Zn1 130.9(10) . . ? C2 N1 Zn1 125.8(7) . . ? C1 N2 C3 105.2(11) . . ? C1 N2 H2 127.4 . . ? C3 N2 H2 127.4 . . ? N2 C1 N1 117.4(13) . . ? N2 C1 H1 121.3 . . ? N1 C1 H1 121.3 . . ? C3 C2 C7 120.0 . . ? C3 C2 N1 106.5(7) . . ? C7 C2 N1 133.4(7) . . ? N2 C3 C4 130.9(8) . . ? N2 C3 C2 107.8(7) . . ? C4 C3 C2 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 120.0 . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 30.36 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.701 _refine_diff_density_min -1.138 _refine_diff_density_rms 0.196 #==================================================================== data_e2(pazo)4 _database_code_depnum_ccdc_archive 'CCDC 870384' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H93 Mo24 N25 O83 P3 Zn8' _chemical_formula_weight 5603.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' Zn Zn 0.2839 1.4301 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.475(7) _cell_length_b 17.497(9) _cell_length_c 28.988(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.516(11) _cell_angle_gamma 90.00 _cell_volume 6791(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22104 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 30.48 _exptl_crystal_description parallelepiped _exptl_crystal_colour black _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.740 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5080 _exptl_absorpt_coefficient_mu 3.659 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2179 _exptl_absorpt_correction_T_max 0.9305 _exptl_absorpt_process_details 'G. M. Sheldrick, SADABS; program for scaling and correction of area detector data, University of G ttingen, Germany, 1997' _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 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36434 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11956 _reflns_number_gt 8392 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^ > 2\s(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. The TBA counter-cations could not be located and the data set was corrected with the program SQUEEZE (P. van der Sluis and A. L. Spek, Acta Crystallogr., Sect. A., 1990, 46, 194). The AFIX66 instruction was used for the pyridine ring involving C6B. The largest residual density peak is located in the vicinity of the P2 atom of the disordered phosphite ion. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.412 0.500 386 245 ' ' 2 0.500 0.932 0.000 386 244 ' ' _platon_squeeze_details ; ; _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^)+(0.0823P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11956 _refine_ls_number_parameters 802 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1657 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.121 _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 -0.00358(8) 0.57783(5) 0.22897(3) 0.0208(2) Uani 1 1 d . . . Mo2 Mo -0.16633(7) 0.54181(5) 0.05534(3) 0.0169(2) Uani 1 1 d . . . Mo3 Mo -0.07814(7) 0.47263(5) 0.12934(3) 0.0165(2) Uani 1 1 d . . . Mo4 Mo 0.15452(8) 0.70120(5) 0.01583(3) 0.0207(2) Uani 1 1 d . . . Mo5 Mo 0.17083(7) 0.49678(5) 0.16735(3) 0.0198(2) Uani 1 1 d . . . Mo6 Mo -0.03433(7) 0.66931(5) -0.00831(3) 0.0193(2) Uani 1 1 d . . . Mo7 Mo 0.22637(8) 0.80429(6) 0.11678(4) 0.0251(2) Uani 1 1 d . . . Mo8 Mo -0.22408(8) 0.73391(6) 0.05072(3) 0.0240(2) Uani 1 1 d . . . Mo9 Mo 0.28778(7) 0.61443(6) 0.10868(3) 0.0216(2) Uani 1 1 d . . . Mo10 Mo -0.03607(8) 0.72616(6) 0.23233(3) 0.0250(3) Uani 1 1 d . . . Mo11 Mo 0.09382(8) 0.85503(6) 0.16946(4) 0.0268(3) Uani 1 1 d . . . Mo12 Mo -0.15760(8) 0.82931(6) 0.14253(4) 0.0265(3) Uani 1 1 d . . . Zn1 Zn -0.22563(10) 0.63902(7) 0.15556(4) 0.0217(3) Uani 1 1 d . . . Zn2 Zn 0.21739(11) 0.68073(8) 0.21261(5) 0.0274(3) Uani 1 1 d . . . Zn3 Zn 0.09752(10) 0.50708(7) 0.04758(4) 0.0192(3) Uani 1 1 d . . . Zn4 Zn -0.01150(11) 0.84948(8) 0.05116(5) 0.0285(3) Uani 1 1 d . . . P1 P 0.0193(2) 0.66797(15) 0.11759(9) 0.0147(6) Uani 1 1 d . . . O1 O 0.1210(5) 0.4244(4) 0.0049(2) 0.0149(15) Uani 1 1 d . . . O2 O 0.1939(5) 0.5256(4) 0.1019(2) 0.0193(16) Uani 1 1 d . . . O3 O -0.0374(5) 0.4946(4) 0.0678(2) 0.0170(16) Uani 1 1 d . . . O4 O -0.0619(5) 0.6567(4) 0.0753(2) 0.0168(16) Uani 1 1 d . . . O5 O 0.1206(6) 0.6858(4) 0.0998(2) 0.0211(17) Uani 1 1 d . . . O6 O 0.1248(6) 0.5203(4) 0.2223(2) 0.0222(17) Uani 1 1 d . . . O7 O 0.0790(5) 0.6046(4) 0.0139(2) 0.0197(17) Uani 1 1 d . . . O8 O 0.2460(6) 0.5955(4) 0.1725(2) 0.0235(18) Uani 1 1 d . . . O9 O -0.1182(6) 0.6393(4) 0.2074(3) 0.0242(18) Uani 1 1 d . . . O10 O 0.0345(6) 0.7628(4) 0.0152(2) 0.0245(18) Uani 1 1 d . . . O11 O -0.1841(6) 0.5506(4) 0.1216(2) 0.0231(17) Uani 1 1 d . . . O12 O 0.1986(6) 0.7772(4) 0.1801(3) 0.0286(19) Uani 1 1 d . . . O13 O -0.2604(6) 0.6333(4) 0.0495(2) 0.0228(12) Uani 1 1 d . . . O14 O -0.1359(6) 0.3866(4) 0.1263(3) 0.0266(18) Uani 1 1 d . . . O15 O 0.0657(6) 0.4396(4) 0.1435(2) 0.0215(17) Uani 1 1 d . . . O16 O 0.0872(6) 0.6672(4) 0.2352(3) 0.0262(18) Uani 1 1 d . . . O17 O 0.0973(6) 0.8532(4) 0.1020(3) 0.0276(19) Uani 1 1 d . . . O18 O -0.0202(6) 0.5543(4) 0.2841(3) 0.030(2) Uani 1 1 d . . . O19 O -0.1370(6) 0.8197(4) 0.0748(3) 0.0254(18) Uani 1 1 d . . . O20 O -0.1580(6) 0.7314(4) 0.0000(3) 0.0252(18) Uani 1 1 d . . . O21 O -0.0393(6) 0.6766(5) -0.0663(3) 0.031(2) Uani 1 1 d . . . O22 O -0.0598(7) 0.7351(5) 0.2873(3) 0.040(2) Uani 1 1 d . . . O23 O 0.0245(6) 0.5929(4) 0.1463(2) 0.0215(17) Uani 1 1 d . . . O24 O 0.3194(6) 0.7118(4) 0.1270(3) 0.0258(18) Uani 1 1 d . . . O25 O 0.0461(6) 0.8168(4) 0.2264(3) 0.0292(19) Uani 1 1 d . . . O26 O -0.0724(6) 0.4916(4) 0.1960(2) 0.0228(12) Uani 1 1 d . . . O27 O 0.2254(6) 0.7831(4) 0.0506(3) 0.0259(18) Uani 1 1 d . . . O28 O -0.0088(6) 0.7349(4) 0.1486(2) 0.0216(17) Uani 1 1 d . . . O29 O 0.3089(7) 0.8767(4) 0.1239(3) 0.037(2) Uani 1 1 d . . . O30 O 0.1931(6) 0.7124(5) -0.0363(3) 0.032(2) Uani 1 1 d . . . O31 O -0.2275(6) 0.7328(4) 0.1190(3) 0.0260(18) Uani 1 1 d . . . O32 O 0.3987(6) 0.5694(5) 0.1132(3) 0.033(2) Uani 1 1 d . . . O33 O 0.2615(6) 0.6328(4) 0.0466(3) 0.0252(18) Uani 1 1 d . . . O34 O 0.1468(7) 0.9381(5) 0.1877(3) 0.044(2) Uani 1 1 d . . . O35 O -0.2460(6) 0.4733(4) 0.0360(3) 0.0282(19) Uani 1 1 d . . . O36 O 0.2606(6) 0.4302(4) 0.1807(3) 0.034(2) Uani 1 1 d . . . O37 O -0.3309(6) 0.7802(5) 0.0322(3) 0.037(2) Uani 1 1 d . . . O38 O -0.1508(6) 0.7898(4) 0.2009(3) 0.0291(19) Uani 1 1 d . . . O39 O -0.0477(6) 0.8900(4) 0.1512(3) 0.033(2) Uani 1 1 d . . . O40 O -0.2542(7) 0.8897(5) 0.1407(3) 0.044(2) Uani 1 1 d . . . N1A N -0.3559(7) 0.6251(5) 0.1757(3) 0.022(2) Uani 1 1 d . . . N2A N -0.4292(7) 0.6840(5) 0.1652(3) 0.022(2) Uani 1 1 d . . . N3A N -0.4462(9) 0.4317(6) 0.2403(4) 0.038(3) Uani 1 1 d . . . N4A N -0.4360(8) 0.8704(6) 0.2485(4) 0.039(3) Uani 1 1 d . . . H4A1 H -0.4390 0.9098 0.2661 0.047 Uiso 1 1 calc R . . C1A C -0.3896(8) 0.5645(6) 0.1977(3) 0.018(2) Uani 1 1 d . . . C2A C -0.3194(10) 0.5048(7) 0.2120(5) 0.037(3) Uani 1 1 d . . . H2A H -0.2526 0.5102 0.2074 0.044 Uiso 1 1 calc R . . C3A C -0.3508(13) 0.4399(8) 0.2326(5) 0.056(4) Uani 1 1 d . . . H3A H -0.3052 0.4011 0.2412 0.067 Uiso 1 1 calc R . . C4A C -0.5136(10) 0.4884(7) 0.2275(4) 0.031(3) Uani 1 1 d . . . H4A H -0.5802 0.4817 0.2322 0.038 Uiso 1 1 calc R . . C5A C -0.4856(9) 0.5540(7) 0.2081(4) 0.028(3) Uani 1 1 d . . . H5A H -0.5322 0.5928 0.2016 0.034 Uiso 1 1 calc R . . C6A C -0.4291(10) 0.7429(7) 0.1931(4) 0.033(2) Uani 1 1 d . . . C7A C -0.4918(11) 0.8066(6) 0.1797(5) 0.041(4) Uani 1 1 d . . . H7A H -0.5336 0.8050 0.1518 0.049 Uiso 1 1 calc R . . C8A C -0.4912(10) 0.8685(7) 0.2064(4) 0.033(2) Uani 1 1 d . . . H8A H -0.5291 0.9109 0.1962 0.039 Uiso 1 1 calc R . . C9A C -0.3777(11) 0.8126(7) 0.2626(5) 0.041(4) Uani 1 1 d . . . H9A H -0.3397 0.8160 0.2914 0.050 Uiso 1 1 calc R . . C10A C -0.3707(10) 0.7470(7) 0.2364(4) 0.033(3) Uani 1 1 d . . . H10A H -0.3288 0.7071 0.2471 0.040 Uiso 1 1 calc R . . N1B N 0.5834(10) 0.6374(8) 0.4018(5) 0.070(4) Uani 1 1 d . . . N2B N 0.5360(11) 0.7032(7) 0.3801(5) 0.063(4) Uani 1 1 d . . . N3B N 0.3225(11) 0.6879(8) 0.2668(5) 0.071(3) Uani 1 1 d . . . C1B C 0.4666(11) 0.6975(9) 0.3432(6) 0.056(3) Uani 1 1 d . . . C2B C 0.4384(15) 0.6266(10) 0.3231(9) 0.100(6) Uani 1 1 d . . . H2B H 0.4679 0.5816 0.3350 0.120 Uiso 1 1 calc R . . C3B C 0.3667(14) 0.6248(9) 0.2858(7) 0.076(4) Uani 1 1 d . . . H3B H 0.3477 0.5776 0.2729 0.091 Uiso 1 1 calc R . . C4B C 0.3481(14) 0.7550(11) 0.2882(6) 0.075(4) Uani 1 1 d . . . H4B H 0.3152 0.7992 0.2770 0.090 Uiso 1 1 calc R . . C5B C 0.4183(14) 0.7611(11) 0.3247(6) 0.074(4) Uani 1 1 d . . . H5B H 0.4342 0.8089 0.3376 0.089 Uiso 1 1 calc R . . C6B C 0.6733(6) 0.6162(6) 0.3941(4) 0.056(3) Uani 1 1 d G . . C7B C 0.7126(8) 0.5551(6) 0.4208(4) 0.100(6) Uani 1 1 d G . . H7B H 0.6773 0.5347 0.4437 0.120 Uiso 1 1 calc R . . C8B C 0.8046(8) 0.5244(5) 0.4133(4) 0.076(4) Uani 1 1 d G . . H8B H 0.8308 0.4835 0.4312 0.091 Uiso 1 1 calc R . . N4B N 0.8573(6) 0.5549(6) 0.3791(4) 0.071(3) Uani 1 1 d G . . H4B1 H 0.9142 0.5360 0.3745 0.085 Uiso 1 1 calc R . . C9B C 0.8180(9) 0.6161(6) 0.3524(3) 0.075(4) Uani 1 1 d G . . H9B H 0.8533 0.6365 0.3295 0.090 Uiso 1 1 calc R . . C10B C 0.7260(9) 0.6468(5) 0.3599(4) 0.074(4) Uani 1 1 d G . . N1C N 0.2905(17) 1.2726(13) 0.0930(8) 0.139(8) Uiso 1 1 d D . . N2C N 0.3622(17) 1.3117(12) 0.1246(7) 0.123(7) Uiso 1 1 d D . . N3C N 0.6345(14) 1.3540(13) 0.0771(6) 0.109(7) Uani 1 1 d . . . H3C1 H 0.6945 1.3608 0.0705 0.131 Uiso 1 1 calc R . . C1C C 0.4515(17) 1.3268(11) 0.1079(9) 0.103(6) Uani 1 1 d . . . C2C C 0.4964(16) 1.3940(12) 0.1169(7) 0.083(6) Uani 1 1 d . . . H2C H 0.4688 1.4308 0.1348 0.100 Uiso 1 1 calc R . . C3C C 0.589(2) 1.4073(14) 0.0981(7) 0.123(11) Uani 1 1 d . . . H3C H 0.6171 1.4558 0.1010 0.148 Uiso 1 1 calc R . . C4C C 0.588(2) 1.2907(14) 0.0663(10) 0.136(11) Uani 1 1 d . . . H4C H 0.6174 1.2547 0.0485 0.163 Uiso 1 1 calc R . . C5C C 0.4977(16) 1.2755(11) 0.0801(9) 0.103(6) Uani 1 1 d . . . H5C H 0.4657 1.2300 0.0710 0.124 Uiso 1 1 calc R . . C6C C 0.2707(13) 1.1954(10) 0.1007(6) 0.060(4) Uiso 1 1 d . . . C7C C 0.2058(13) 1.1459(10) 0.0762(6) 0.066(5) Uiso 1 1 d . . . H7C H 0.1681 1.1622 0.0491 0.079 Uiso 1 1 calc R . . C8C C 0.1965(13) 1.0744(10) 0.0909(6) 0.061(4) Uiso 1 1 d . . . H8C H 0.1491 1.0419 0.0756 0.073 Uiso 1 1 calc R . . N4C N 0.2583(13) 1.0492(10) 0.1293(6) 0.090(5) Uiso 1 1 d . . . H4C1 H 0.2594 1.0023 0.1382 0.108 Uiso 1 1 calc R . . C9C C 0.3158(16) 1.1024(12) 0.1516(7) 0.087(6) Uiso 1 1 d . . . H9C H 0.3533 1.0851 0.1785 0.104 Uiso 1 1 calc R . . C10C C 0.3296(18) 1.1783(13) 0.1420(8) 0.098(7) Uiso 1 1 d . . . H10C H 0.3708 1.2122 0.1599 0.117 Uiso 1 1 calc R . . P2 P -0.0321(5) 1.0069(4) 0.0068(2) 0.0330(16) Uiso 0.50 1 d P . . H1 H -0.1210 1.0161 -0.0093 0.030 Uiso 0.50 1 d P . . O41 O -0.0327(16) 0.9455(12) 0.0249(8) 0.052(6) Uiso 0.50 1 d P . . O42 O -0.0321(15) 0.9258(12) -0.0004(7) 0.050(5) Uiso 0.50 1 d P . . O43 O 0.001(2) 1.0269(16) 0.0592(9) 0.089(8) 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 0.0314(6) 0.0153(5) 0.0153(5) -0.0001(4) 0.0014(4) 0.0000(4) Mo2 0.0187(5) 0.0168(5) 0.0157(5) 0.0018(4) 0.0033(4) 0.0010(4) Mo3 0.0229(5) 0.0125(5) 0.0144(5) 0.0012(4) 0.0032(4) 0.0000(4) Mo4 0.0255(6) 0.0162(5) 0.0213(5) 0.0010(4) 0.0067(4) -0.0025(4) Mo5 0.0238(6) 0.0146(5) 0.0200(5) -0.0003(4) -0.0021(4) 0.0021(4) Mo6 0.0243(6) 0.0172(5) 0.0169(5) 0.0041(4) 0.0044(4) 0.0007(4) Mo7 0.0282(6) 0.0163(5) 0.0313(6) -0.0047(4) 0.0062(5) -0.0051(4) Mo8 0.0263(6) 0.0215(6) 0.0250(5) 0.0074(4) 0.0062(4) 0.0071(4) Mo9 0.0217(6) 0.0181(5) 0.0246(5) -0.0045(4) 0.0003(4) -0.0017(4) Mo10 0.0382(7) 0.0153(5) 0.0226(5) -0.0030(4) 0.0082(5) -0.0002(4) Mo11 0.0386(7) 0.0130(5) 0.0302(6) -0.0051(4) 0.0097(5) -0.0021(4) Mo12 0.0342(6) 0.0151(5) 0.0321(6) 0.0018(4) 0.0124(5) 0.0055(4) Zn1 0.0256(8) 0.0178(7) 0.0232(7) 0.0027(5) 0.0091(6) 0.0021(5) Zn2 0.0346(9) 0.0205(7) 0.0260(7) -0.0058(6) -0.0010(6) -0.0032(6) Zn3 0.0228(7) 0.0173(7) 0.0175(6) -0.0005(5) 0.0026(5) -0.0005(5) Zn4 0.0369(9) 0.0170(7) 0.0325(8) 0.0047(6) 0.0082(7) 0.0033(6) P1 0.0178(15) 0.0117(14) 0.0152(13) 0.0015(11) 0.0046(11) 0.0012(11) O1 0.019(4) 0.014(4) 0.013(3) -0.001(3) 0.007(3) -0.001(3) O2 0.016(4) 0.022(4) 0.019(4) -0.004(3) -0.001(3) 0.001(3) O3 0.016(4) 0.022(4) 0.013(4) -0.003(3) 0.001(3) 0.002(3) O4 0.018(4) 0.016(4) 0.017(4) 0.006(3) 0.004(3) 0.003(3) O5 0.028(5) 0.014(4) 0.021(4) -0.005(3) 0.003(3) -0.001(3) O6 0.032(5) 0.014(4) 0.019(4) -0.001(3) -0.001(3) 0.006(3) O7 0.021(4) 0.017(4) 0.022(4) 0.002(3) 0.006(3) 0.006(3) O8 0.031(5) 0.018(4) 0.020(4) -0.006(3) -0.002(3) -0.001(3) O9 0.028(5) 0.015(4) 0.030(4) -0.004(3) 0.005(4) 0.000(3) O10 0.036(5) 0.017(4) 0.020(4) 0.003(3) 0.005(4) 0.000(3) O11 0.025(4) 0.023(4) 0.021(4) 0.004(3) 0.004(3) 0.003(3) O12 0.032(5) 0.019(4) 0.036(5) -0.009(4) 0.012(4) 0.004(4) O13 0.028(3) 0.019(3) 0.021(3) 0.007(2) 0.000(2) 0.001(2) O14 0.034(5) 0.018(4) 0.030(4) 0.006(3) 0.008(4) -0.004(3) O15 0.023(4) 0.017(4) 0.023(4) 0.003(3) -0.005(3) 0.000(3) O16 0.034(5) 0.021(4) 0.024(4) -0.002(3) 0.004(4) -0.001(4) O17 0.037(5) 0.015(4) 0.032(5) -0.006(3) 0.011(4) -0.003(4) O18 0.043(5) 0.026(5) 0.020(4) 0.002(3) 0.004(4) 0.002(4) O19 0.026(5) 0.028(5) 0.023(4) 0.008(3) 0.009(3) 0.007(4) O20 0.029(5) 0.024(4) 0.023(4) 0.009(3) 0.008(4) 0.008(4) O21 0.043(6) 0.035(5) 0.016(4) 0.006(4) 0.001(4) -0.001(4) O22 0.065(7) 0.034(5) 0.025(5) -0.008(4) 0.020(4) 0.000(5) O23 0.022(4) 0.022(4) 0.021(4) 0.002(3) 0.004(3) 0.004(3) O24 0.028(5) 0.019(4) 0.031(4) -0.003(3) 0.007(4) 0.001(3) O25 0.045(5) 0.008(4) 0.038(5) -0.007(3) 0.018(4) -0.003(4) O26 0.028(3) 0.019(3) 0.021(3) 0.007(2) 0.000(2) 0.001(2) O27 0.039(5) 0.015(4) 0.023(4) 0.006(3) 0.004(4) -0.006(3) O28 0.024(4) 0.017(4) 0.025(4) 0.006(3) 0.004(3) -0.003(3) O29 0.041(6) 0.019(5) 0.050(6) -0.001(4) 0.004(4) -0.006(4) O30 0.023(5) 0.042(5) 0.035(5) -0.002(4) 0.012(4) -0.010(4) O31 0.032(5) 0.023(4) 0.023(4) 0.003(3) 0.007(4) 0.002(4) O32 0.032(5) 0.030(5) 0.036(5) -0.008(4) 0.000(4) 0.005(4) O33 0.032(5) 0.017(4) 0.026(4) -0.003(3) 0.003(4) -0.003(3) O34 0.063(7) 0.020(5) 0.051(6) -0.014(4) 0.019(5) -0.015(4) O35 0.031(5) 0.027(5) 0.026(4) 0.000(4) 0.000(4) -0.009(4) O36 0.039(5) 0.025(5) 0.035(5) 0.005(4) -0.003(4) 0.014(4) O37 0.030(5) 0.030(5) 0.051(6) 0.010(4) 0.004(4) 0.016(4) O38 0.037(5) 0.019(4) 0.034(5) 0.000(4) 0.014(4) 0.000(4) O39 0.044(6) 0.022(4) 0.035(5) -0.003(4) 0.014(4) 0.006(4) O40 0.048(6) 0.030(5) 0.058(6) 0.006(4) 0.020(5) 0.011(4) N1A 0.023(5) 0.017(5) 0.027(5) -0.001(4) 0.002(4) 0.001(4) N2A 0.026(6) 0.015(5) 0.026(5) 0.001(4) 0.001(4) 0.004(4) N3A 0.044(7) 0.020(6) 0.051(7) 0.007(5) 0.018(6) 0.002(5) N4A 0.046(7) 0.022(6) 0.050(7) -0.019(5) 0.009(6) -0.002(5) C1A 0.027(7) 0.013(6) 0.014(5) -0.003(4) 0.005(5) -0.003(5) C2A 0.037(8) 0.021(7) 0.057(9) 0.012(6) 0.021(7) 0.004(6) C3A 0.077(13) 0.028(8) 0.067(11) 0.020(7) 0.028(9) 0.027(8) C4A 0.032(7) 0.035(8) 0.027(7) 0.008(6) 0.003(6) 0.000(6) C5A 0.036(8) 0.026(7) 0.022(6) 0.005(5) -0.001(5) 0.005(5) C6A 0.035(6) 0.017(5) 0.045(6) -0.005(4) 0.000(4) 0.002(4) C7A 0.057(10) 0.006(6) 0.055(9) -0.009(6) -0.012(7) -0.001(6) C8A 0.035(6) 0.017(5) 0.045(6) -0.005(4) 0.000(4) 0.002(4) C9A 0.062(10) 0.029(8) 0.032(7) -0.013(6) 0.003(7) -0.017(7) C10A 0.034(8) 0.028(7) 0.034(7) 0.000(6) -0.007(6) -0.004(6) N1B 0.053(9) 0.058(9) 0.093(11) -0.011(8) -0.023(8) 0.014(7) N2B 0.073(10) 0.043(8) 0.066(9) -0.026(7) -0.027(8) 0.022(7) N3B 0.067(7) 0.057(7) 0.088(8) -0.021(6) 0.010(6) 0.006(5) C1B 0.038(7) 0.044(7) 0.080(8) -0.031(6) -0.016(6) 0.013(5) C2B 0.068(10) 0.042(8) 0.177(16) -0.010(9) -0.039(10) 0.015(7) C3B 0.070(9) 0.035(7) 0.117(12) -0.032(7) -0.017(8) 0.020(6) C4B 0.082(10) 0.073(9) 0.067(9) -0.013(7) -0.006(7) 0.020(8) C5B 0.072(9) 0.075(9) 0.073(9) -0.036(7) -0.005(7) 0.017(7) C6B 0.038(7) 0.044(7) 0.080(8) -0.031(6) -0.016(6) 0.013(5) C7B 0.068(10) 0.042(8) 0.177(16) -0.010(9) -0.039(10) 0.015(7) C8B 0.070(9) 0.035(7) 0.117(12) -0.032(7) -0.017(8) 0.020(6) N4B 0.067(7) 0.057(7) 0.088(8) -0.021(6) 0.010(6) 0.006(5) C9B 0.082(10) 0.073(9) 0.067(9) -0.013(7) -0.006(7) 0.020(8) C10B 0.072(9) 0.075(9) 0.073(9) -0.036(7) -0.005(7) 0.017(7) N3C 0.094(14) 0.148(19) 0.096(14) -0.048(13) 0.056(11) -0.066(14) C1C 0.084(11) 0.063(9) 0.181(17) -0.023(10) 0.097(11) -0.012(8) C2C 0.091(16) 0.079(14) 0.087(14) -0.023(11) 0.043(12) -0.012(12) C3C 0.19(3) 0.11(2) 0.068(14) -0.047(14) 0.033(17) -0.07(2) C4C 0.17(3) 0.086(18) 0.17(3) -0.004(18) 0.13(2) -0.020(18) C5C 0.084(11) 0.063(9) 0.181(17) -0.023(10) 0.097(11) -0.012(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O18 1.689(7) . ? Mo1 O9 1.928(8) . ? Mo1 O26 1.961(7) . ? Mo1 O16 1.980(8) . ? Mo1 O6 2.029(8) . ? Mo1 O23 2.482(7) . ? Mo1 Mo10 2.6356(18) . ? Mo2 O35 1.663(8) . ? Mo2 O3 1.921(7) . ? Mo2 O11 1.967(7) . ? Mo2 O1 2.002(7) 3_565 ? Mo2 O13 2.037(7) . ? Mo2 O4 2.484(7) . ? Mo2 Mo3 2.6269(16) . ? Mo3 O14 1.692(7) . ? Mo3 O26 1.954(7) . ? Mo3 O3 1.963(7) . ? Mo3 O11 1.969(7) . ? Mo3 O15 2.020(7) . ? Mo4 O30 1.664(8) . ? Mo4 O27 1.939(7) . ? Mo4 O10 1.941(8) . ? Mo4 O7 1.969(7) . ? Mo4 O33 2.004(8) . ? Mo4 Mo6 2.6217(19) . ? Mo5 O36 1.693(8) . ? Mo5 O15 1.806(7) . ? Mo5 O6 1.821(7) . ? Mo5 O8 1.999(7) . ? Mo5 O2 2.020(7) . ? Mo5 Mo9 3.1971(17) . ? Mo6 O21 1.678(7) . ? Mo6 O7 1.951(7) . ? Mo6 O10 1.964(7) . ? Mo6 O1 2.022(7) 3_565 ? Mo6 O20 2.026(8) . ? Mo6 O4 2.504(7) . ? Mo7 O29 1.683(8) . ? Mo7 O17 1.942(8) . ? Mo7 O27 1.954(7) . ? Mo7 O12 1.972(8) . ? Mo7 O24 2.048(8) . ? Mo7 Mo11 2.6324(17) . ? Mo8 O37 1.685(8) . ? Mo8 O20 1.805(7) . ? Mo8 O13 1.826(7) . ? Mo8 O19 1.983(8) . ? Mo8 O31 1.986(7) . ? Mo8 Mo12 3.1830(19) . ? Mo9 O32 1.682(8) . ? Mo9 O24 1.821(7) . ? Mo9 O33 1.822(7) . ? Mo9 O2 2.000(7) . ? Mo9 O8 2.021(7) . ? Mo10 O22 1.668(8) . ? Mo10 O16 1.949(8) . ? Mo10 O25 1.954(8) . ? Mo10 O9 1.968(7) . ? Mo10 O38 2.035(8) . ? Mo10 O28 2.500(7) . ? Mo11 O34 1.679(8) . ? Mo11 O25 1.956(8) . ? Mo11 O12 1.961(8) . ? Mo11 O17 1.962(8) . ? Mo11 O39 2.015(9) . ? Mo12 O40 1.673(9) . ? Mo12 O39 1.817(9) . ? Mo12 O38 1.820(8) . ? Mo12 O31 2.014(8) . ? Mo12 O19 2.020(7) . ? Zn1 N1A 1.927(10) . ? Zn1 O11 1.950(7) . ? Zn1 O31 1.952(7) . ? Zn1 O9 1.964(8) . ? Zn2 O12 1.936(8) . ? Zn2 O16 1.956(8) . ? Zn2 O8 1.957(7) . ? Zn2 N3B 1.997(15) . ? Zn3 O2 1.951(7) . ? Zn3 O1 1.953(7) . ? Zn3 O7 1.968(7) . ? Zn3 O3 1.985(7) . ? Zn4 O41 1.85(2) . ? Zn4 O17 1.959(8) . ? Zn4 O19 1.967(8) . ? Zn4 O10 1.980(8) . ? Zn4 O42 2.00(2) . ? P1 O5 1.545(8) . ? P1 O28 1.550(8) . ? P1 O23 1.552(7) . ? P1 O4 1.560(7) . ? O1 Mo2 2.002(7) 3_565 ? O1 Mo6 2.022(7) 3_565 ? N1A C1A 1.342(13) . ? N1A N2A 1.436(12) . ? N2A C6A 1.310(14) . ? N3A C3A 1.338(19) . ? N3A C4A 1.368(15) . ? N4A C9A 1.317(17) . ? N4A C8A 1.353(16) . ? N4A H4A1 0.8600 . ? C1A C5A 1.374(16) . ? C1A C2A 1.438(16) . ? C2A C3A 1.371(18) . ? C2A H2A 0.9300 . ? C3A H3A 0.9300 . ? C4A C5A 1.350(16) . ? C4A H4A 0.9300 . ? C5A H5A 0.9300 . ? C6A C10A 1.405(16) . ? C6A C7A 1.426(17) . ? C7A C8A 1.332(16) . ? C7A H7A 0.9300 . ? C8A H8A 0.9300 . ? C9A C10A 1.387(17) . ? C9A H9A 0.9300 . ? C10A H10A 0.9300 . ? N1B C6B 1.310(16) . ? N1B N2B 1.427(17) . ? N2B C1B 1.342(18) . ? N3B C3B 1.34(2) . ? N3B C4B 1.36(2) . ? C1B C5B 1.37(2) . ? C1B C2B 1.40(2) . ? C2B C3B 1.37(2) . ? C2B H2B 0.9300 . ? C3B H3B 0.9300 . ? C4B C5B 1.34(2) . ? C4B H4B 0.9300 . ? C5B H5B 0.9300 . ? C6B C7B 1.3900 . ? C6B C10B 1.3900 . ? C7B C8B 1.3900 . ? C7B H7B 0.9300 . ? C8B N4B 1.3900 . ? C8B H8B 0.9300 . ? N4B C9B 1.3900 . ? N4B H4B1 0.8600 . ? C9B C10B 1.3900 . ? C9B H9B 0.9300 . ? N1C C6C 1.40(2) . ? N1C N2C 1.430(17) . ? N2C C1C 1.37(3) . ? N3C C4C 1.29(3) . ? N3C C3C 1.31(3) . ? N3C H3C1 0.8600 . ? C1C C2C 1.33(3) . ? C1C C5C 1.40(2) . ? C2C C3C 1.43(3) . ? C2C H2C 0.9300 . ? C3C H3C 0.9300 . ? C4C C5C 1.35(3) . ? C4C H4C 0.9300 . ? C5C H5C 0.9300 . ? C6C C7C 1.37(2) . ? C6C C10C 1.39(3) . ? C7C C8C 1.33(2) . ? C7C H7C 0.9300 . ? C8C N4C 1.38(2) . ? C8C H8C 0.9300 . ? N4C C9C 1.33(2) . ? N4C H4C1 0.8600 . ? C9C C10C 1.37(3) . ? C9C H9C 0.9300 . ? C10C H10C 0.9300 . ? P2 P2 1.020(13) 3_575 ? P2 O41 1.20(2) . ? P2 O42 1.43(2) . ? P2 O42 1.49(2) 3_575 ? P2 O43 1.57(3) . ? P2 O41 1.58(2) 3_575 ? P2 O43 2.09(3) 3_575 ? P2 H1 1.2455 . ? O41 O42 0.81(2) . ? O41 P2 1.58(2) 3_575 ? O41 O43 1.77(3) . ? O42 P2 1.49(2) 3_575 ? O43 P2 2.09(3) 3_575 ? 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 O18 Mo1 O9 104.8(4) . . ? O18 Mo1 O26 99.6(3) . . ? O9 Mo1 O26 87.4(3) . . ? O18 Mo1 O16 104.6(4) . . ? O9 Mo1 O16 93.0(3) . . ? O26 Mo1 O16 154.8(3) . . ? O18 Mo1 O6 100.1(3) . . ? O9 Mo1 O6 155.0(3) . . ? O26 Mo1 O6 86.1(3) . . ? O16 Mo1 O6 82.9(3) . . ? O18 Mo1 O23 171.9(3) . . ? O9 Mo1 O23 80.3(3) . . ? O26 Mo1 O23 74.2(3) . . ? O16 Mo1 O23 81.0(3) . . ? O6 Mo1 O23 74.7(3) . . ? O18 Mo1 Mo10 99.5(3) . . ? O9 Mo1 Mo10 48.1(2) . . ? O26 Mo1 Mo10 134.8(2) . . ? O16 Mo1 Mo10 47.4(2) . . ? O6 Mo1 Mo10 129.7(2) . . ? O23 Mo1 Mo10 88.57(17) . . ? O35 Mo2 O3 106.8(4) . . ? O35 Mo2 O11 103.9(3) . . ? O3 Mo2 O11 93.3(3) . . ? O35 Mo2 O1 99.6(3) . 3_565 ? O3 Mo2 O1 86.1(3) . 3_565 ? O11 Mo2 O1 155.5(3) . 3_565 ? O35 Mo2 O13 99.6(4) . . ? O3 Mo2 O13 153.5(3) . . ? O11 Mo2 O13 82.9(3) . . ? O1 Mo2 O13 86.8(3) 3_565 . ? O35 Mo2 O4 171.3(3) . . ? O3 Mo2 O4 80.1(3) . . ? O11 Mo2 O4 80.7(3) . . ? O1 Mo2 O4 75.2(2) 3_565 . ? O13 Mo2 O4 73.4(3) . . ? O35 Mo2 Mo3 99.1(3) . . ? O3 Mo2 Mo3 48.1(2) . . ? O11 Mo2 Mo3 48.2(2) . . ? O1 Mo2 Mo3 133.9(2) 3_565 . ? O13 Mo2 Mo3 130.5(2) . . ? O4 Mo2 Mo3 89.46(16) . . ? O14 Mo3 O26 99.8(3) . . ? O14 Mo3 O3 107.5(3) . . ? O26 Mo3 O3 151.9(3) . . ? O14 Mo3 O11 106.7(4) . . ? O26 Mo3 O11 86.7(3) . . ? O3 Mo3 O11 92.0(3) . . ? O14 Mo3 O15 100.4(3) . . ? O26 Mo3 O15 85.3(3) . . ? O3 Mo3 O15 83.1(3) . . ? O11 Mo3 O15 152.7(3) . . ? O14 Mo3 Mo2 101.8(3) . . ? O26 Mo3 Mo2 133.9(2) . . ? O3 Mo3 Mo2 46.8(2) . . ? O11 Mo3 Mo2 48.1(2) . . ? O15 Mo3 Mo2 129.2(2) . . ? O30 Mo4 O27 101.4(4) . . ? O30 Mo4 O10 105.7(4) . . ? O27 Mo4 O10 87.4(3) . . ? O30 Mo4 O7 106.8(3) . . ? O27 Mo4 O7 150.6(3) . . ? O10 Mo4 O7 92.8(3) . . ? O30 Mo4 O33 101.1(4) . . ? O27 Mo4 O33 85.6(3) . . ? O10 Mo4 O33 153.1(3) . . ? O7 Mo4 O33 81.0(3) . . ? O30 Mo4 Mo6 100.2(3) . . ? O27 Mo4 Mo6 134.6(2) . . ? O10 Mo4 Mo6 48.2(2) . . ? O7 Mo4 Mo6 47.7(2) . . ? O33 Mo4 Mo6 128.3(2) . . ? O36 Mo5 O15 102.4(4) . . ? O36 Mo5 O6 105.1(4) . . ? O15 Mo5 O6 97.5(3) . . ? O36 Mo5 O8 103.6(4) . . ? O15 Mo5 O8 151.1(3) . . ? O6 Mo5 O8 87.7(3) . . ? O36 Mo5 O2 101.8(4) . . ? O15 Mo5 O2 88.6(3) . . ? O6 Mo5 O2 150.3(3) . . ? O8 Mo5 O2 74.0(3) . . ? O36 Mo5 Mo9 100.5(3) . . ? O15 Mo5 Mo9 124.4(2) . . ? O6 Mo5 Mo9 123.9(2) . . ? O8 Mo5 Mo9 37.5(2) . . ? O2 Mo5 Mo9 37.1(2) . . ? O21 Mo6 O7 108.3(4) . . ? O21 Mo6 O10 104.3(4) . . ? O7 Mo6 O10 92.7(3) . . ? O21 Mo6 O1 98.8(3) . 3_565 ? O7 Mo6 O1 87.0(3) . 3_565 ? O10 Mo6 O1 155.6(3) . 3_565 ? O21 Mo6 O20 98.0(4) . . ? O7 Mo6 O20 153.6(3) . . ? O10 Mo6 O20 82.8(3) . . ? O1 Mo6 O20 86.7(3) 3_565 . ? O21 Mo6 O4 169.2(3) . . ? O7 Mo6 O4 80.0(3) . . ? O10 Mo6 O4 81.6(3) . . ? O1 Mo6 O4 74.4(2) 3_565 . ? O20 Mo6 O4 73.6(3) . . ? O21 Mo6 Mo4 100.3(3) . . ? O7 Mo6 Mo4 48.3(2) . . ? O10 Mo6 Mo4 47.5(2) . . ? O1 Mo6 Mo4 135.1(2) 3_565 . ? O20 Mo6 Mo4 129.8(2) . . ? O4 Mo6 Mo4 90.37(16) . . ? O29 Mo7 O17 104.9(4) . . ? O29 Mo7 O27 101.2(4) . . ? O17 Mo7 O27 87.7(3) . . ? O29 Mo7 O12 105.1(4) . . ? O17 Mo7 O12 93.0(3) . . ? O27 Mo7 O12 152.6(3) . . ? O29 Mo7 O24 101.1(4) . . ? O17 Mo7 O24 154.0(3) . . ? O27 Mo7 O24 85.9(3) . . ? O12 Mo7 O24 81.6(3) . . ? O29 Mo7 Mo11 99.1(3) . . ? O17 Mo7 Mo11 47.9(2) . . ? O27 Mo7 Mo11 134.8(2) . . ? O12 Mo7 Mo11 47.8(2) . . ? O24 Mo7 Mo11 128.9(2) . . ? O37 Mo8 O20 103.6(4) . . ? O37 Mo8 O13 103.9(4) . . ? O20 Mo8 O13 96.7(3) . . ? O37 Mo8 O19 101.5(4) . . ? O20 Mo8 O19 88.8(3) . . ? O13 Mo8 O19 152.0(3) . . ? O37 Mo8 O31 101.9(4) . . ? O20 Mo8 O31 151.9(3) . . ? O13 Mo8 O31 88.5(3) . . ? O19 Mo8 O31 74.6(3) . . ? O37 Mo8 Mo12 99.4(3) . . ? O20 Mo8 Mo12 125.2(3) . . ? O13 Mo8 Mo12 124.8(2) . . ? O19 Mo8 Mo12 37.7(2) . . ? O31 Mo8 Mo12 37.6(2) . . ? O32 Mo9 O24 103.8(4) . . ? O32 Mo9 O33 103.4(4) . . ? O24 Mo9 O33 97.8(3) . . ? O32 Mo9 O2 100.9(3) . . ? O24 Mo9 O2 151.7(3) . . ? O33 Mo9 O2 89.4(3) . . ? O32 Mo9 O8 100.9(4) . . ? O24 Mo9 O8 88.1(3) . . ? O33 Mo9 O8 152.8(3) . . ? O2 Mo9 O8 73.9(3) . . ? O32 Mo9 Mo5 98.3(3) . . ? O24 Mo9 Mo5 124.1(2) . . ? O33 Mo9 Mo5 125.9(2) . . ? O2 Mo9 Mo5 37.5(2) . . ? O8 Mo9 Mo5 37.1(2) . . ? O22 Mo10 O16 105.3(4) . . ? O22 Mo10 O25 100.4(4) . . ? O16 Mo10 O25 86.8(3) . . ? O22 Mo10 O9 105.2(4) . . ? O16 Mo10 O9 92.7(3) . . ? O25 Mo10 O9 153.5(3) . . ? O22 Mo10 O38 99.1(4) . . ? O16 Mo10 O38 155.4(3) . . ? O25 Mo10 O38 85.7(3) . . ? O9 Mo10 O38 83.8(3) . . ? O22 Mo10 O28 170.7(3) . . ? O16 Mo10 O28 81.7(3) . . ? O25 Mo10 O28 73.6(3) . . ? O9 Mo10 O28 80.2(3) . . ? O38 Mo10 O28 73.7(3) . . ? O22 Mo10 Mo1 100.3(3) . . ? O16 Mo10 Mo1 48.4(2) . . ? O25 Mo10 Mo1 134.3(2) . . ? O9 Mo10 Mo1 46.8(2) . . ? O38 Mo10 Mo1 130.0(2) . . ? O28 Mo10 Mo1 88.92(17) . . ? O34 Mo11 O25 101.4(4) . . ? O34 Mo11 O12 106.2(4) . . ? O25 Mo11 O12 86.0(3) . . ? O34 Mo11 O17 105.7(4) . . ? O25 Mo11 O17 152.0(3) . . ? O12 Mo11 O17 92.7(3) . . ? O34 Mo11 O39 100.1(4) . . ? O25 Mo11 O39 86.2(3) . . ? O12 Mo11 O39 153.5(3) . . ? O17 Mo11 O39 82.6(3) . . ? O34 Mo11 Mo7 100.5(3) . . ? O25 Mo11 Mo7 133.2(2) . . ? O12 Mo11 Mo7 48.2(2) . . ? O17 Mo11 Mo7 47.3(2) . . ? O39 Mo11 Mo7 129.3(2) . . ? O40 Mo12 O39 104.8(4) . . ? O40 Mo12 O38 103.1(4) . . ? O39 Mo12 O38 98.0(4) . . ? O40 Mo12 O31 100.7(4) . . ? O39 Mo12 O31 151.5(3) . . ? O38 Mo12 O31 88.2(3) . . ? O40 Mo12 O19 102.4(4) . . ? O39 Mo12 O19 89.0(3) . . ? O38 Mo12 O19 150.8(3) . . ? O31 Mo12 O19 73.3(3) . . ? O40 Mo12 Mo8 99.2(3) . . ? O39 Mo12 Mo8 124.7(3) . . ? O38 Mo12 Mo8 123.9(2) . . ? O31 Mo12 Mo8 37.0(2) . . ? O19 Mo12 Mo8 36.9(2) . . ? N1A Zn1 O11 112.1(3) . . ? N1A Zn1 O31 108.4(4) . . ? O11 Zn1 O31 112.3(3) . . ? N1A Zn1 O9 112.7(4) . . ? O11 Zn1 O9 99.2(3) . . ? O31 Zn1 O9 112.1(3) . . ? O12 Zn2 O16 101.3(3) . . ? O12 Zn2 O8 113.5(3) . . ? O16 Zn2 O8 110.6(3) . . ? O12 Zn2 N3B 111.8(5) . . ? O16 Zn2 N3B 109.1(5) . . ? O8 Zn2 N3B 110.2(5) . . ? O2 Zn3 O1 119.6(3) . . ? O2 Zn3 O7 107.0(3) . . ? O1 Zn3 O7 110.4(3) . . ? O2 Zn3 O3 109.1(3) . . ? O1 Zn3 O3 109.0(3) . . ? O7 Zn3 O3 100.0(3) . . ? O41 Zn4 O17 110.2(7) . . ? O41 Zn4 O19 106.6(7) . . ? O17 Zn4 O19 110.3(3) . . ? O41 Zn4 O10 121.4(7) . . ? O17 Zn4 O10 99.7(3) . . ? O19 Zn4 O10 108.3(3) . . ? O41 Zn4 O42 23.9(7) . . ? O17 Zn4 O42 124.7(6) . . ? O19 Zn4 O42 112.7(6) . . ? O10 Zn4 O42 98.2(7) . . ? O5 P1 O28 108.9(4) . . ? O5 P1 O23 111.2(4) . . ? O28 P1 O23 109.1(4) . . ? O5 P1 O4 109.3(4) . . ? O28 P1 O4 110.8(4) . . ? O23 P1 O4 107.4(4) . . ? Zn3 O1 Mo2 114.9(3) . 3_565 ? Zn3 O1 Mo6 115.7(3) . 3_565 ? Mo2 O1 Mo6 121.2(3) 3_565 3_565 ? Zn3 O2 Mo9 124.3(4) . . ? Zn3 O2 Mo5 123.9(4) . . ? Mo9 O2 Mo5 105.4(3) . . ? Mo2 O3 Mo3 85.1(3) . . ? Mo2 O3 Zn3 137.4(4) . . ? Mo3 O3 Zn3 130.5(4) . . ? P1 O4 Mo2 127.9(4) . . ? P1 O4 Mo6 125.6(4) . . ? Mo2 O4 Mo6 89.3(2) . . ? Mo5 O6 Mo1 125.1(4) . . ? Mo6 O7 Zn3 135.8(4) . . ? Mo6 O7 Mo4 83.9(3) . . ? Zn3 O7 Mo4 133.9(4) . . ? Zn2 O8 Mo5 124.8(4) . . ? Zn2 O8 Mo9 120.9(4) . . ? Mo5 O8 Mo9 105.4(3) . . ? Mo1 O9 Zn1 137.8(4) . . ? Mo1 O9 Mo10 85.1(3) . . ? Zn1 O9 Mo10 128.2(4) . . ? Mo4 O10 Mo6 84.3(3) . . ? Mo4 O10 Zn4 136.9(4) . . ? Mo6 O10 Zn4 131.0(4) . . ? Zn1 O11 Mo2 129.0(4) . . ? Zn1 O11 Mo3 137.5(4) . . ? Mo2 O11 Mo3 83.7(3) . . ? Zn2 O12 Mo11 137.2(4) . . ? Zn2 O12 Mo7 129.4(4) . . ? Mo11 O12 Mo7 84.0(3) . . ? Mo8 O13 Mo2 126.4(4) . . ? Mo5 O15 Mo3 127.7(4) . . ? Mo10 O16 Zn2 135.6(4) . . ? Mo10 O16 Mo1 84.3(3) . . ? Zn2 O16 Mo1 129.3(4) . . ? Mo7 O17 Zn4 136.6(4) . . ? Mo7 O17 Mo11 84.8(3) . . ? Zn4 O17 Mo11 130.5(4) . . ? Zn4 O19 Mo8 125.1(4) . . ? Zn4 O19 Mo12 122.4(4) . . ? Mo8 O19 Mo12 105.4(3) . . ? Mo8 O20 Mo6 126.7(4) . . ? P1 O23 Mo1 127.2(4) . . ? Mo9 O24 Mo7 125.3(4) . . ? Mo10 O25 Mo11 126.6(4) . . ? Mo3 O26 Mo1 125.2(4) . . ? Mo4 O27 Mo7 126.7(4) . . ? P1 O28 Mo10 126.1(4) . . ? Zn1 O31 Mo8 123.3(4) . . ? Zn1 O31 Mo12 123.0(4) . . ? Mo8 O31 Mo12 105.4(3) . . ? Mo9 O33 Mo4 126.5(4) . . ? Mo12 O38 Mo10 125.4(4) . . ? Mo12 O39 Mo11 126.2(4) . . ? C1A N1A N2A 114.0(9) . . ? C1A N1A Zn1 127.8(8) . . ? N2A N1A Zn1 118.2(7) . . ? C6A N2A N1A 118.7(9) . . ? C3A N3A C4A 119.9(11) . . ? C9A N4A C8A 120.6(11) . . ? C9A N4A H4A1 119.7 . . ? C8A N4A H4A1 119.7 . . ? N1A C1A C5A 125.9(10) . . ? N1A C1A C2A 117.7(10) . . ? C5A C1A C2A 116.4(10) . . ? C3A C2A C1A 120.1(13) . . ? C3A C2A H2A 119.9 . . ? C1A C2A H2A 119.9 . . ? N3A C3A C2A 120.7(13) . . ? N3A C3A H3A 119.7 . . ? C2A C3A H3A 119.7 . . ? C5A C4A N3A 121.4(12) . . ? C5A C4A H4A 119.3 . . ? N3A C4A H4A 119.3 . . ? C4A C5A C1A 121.3(11) . . ? C4A C5A H5A 119.3 . . ? C1A C5A H5A 119.3 . . ? N2A C6A C10A 123.6(11) . . ? N2A C6A C7A 119.2(11) . . ? C10A C6A C7A 117.2(11) . . ? C8A C7A C6A 120.8(12) . . ? C8A C7A H7A 119.6 . . ? C6A C7A H7A 119.6 . . ? C7A C8A N4A 120.7(12) . . ? C7A C8A H8A 119.6 . . ? N4A C8A H8A 119.6 . . ? N4A C9A C10A 122.6(12) . . ? N4A C9A H9A 118.7 . . ? C10A C9A H9A 118.7 . . ? C9A C10A C6A 117.8(12) . . ? C9A C10A H10A 121.1 . . ? C6A C10A H10A 121.1 . . ? C6B N1B N2B 121.9(15) . . ? C1B N2B N1B 121.8(12) . . ? C3B N3B C4B 116.6(16) . . ? C3B N3B Zn2 120.9(12) . . ? C4B N3B Zn2 122.4(12) . . ? N2B C1B C5B 120.6(14) . . ? N2B C1B C2B 121.8(15) . . ? C5B C1B C2B 117.6(15) . . ? C3B C2B C1B 118.8(16) . . ? C3B C2B H2B 120.6 . . ? C1B C2B H2B 120.6 . . ? N3B C3B C2B 123.2(16) . . ? N3B C3B H3B 118.4 . . ? C2B C3B H3B 118.4 . . ? C5B C4B N3B 123.4(18) . . ? C5B C4B H4B 118.3 . . ? N3B C4B H4B 118.3 . . ? C4B C5B C1B 120.4(17) . . ? C4B C5B H5B 119.8 . . ? C1B C5B H5B 119.8 . . ? N1B C6B C7B 115.1(11) . . ? N1B C6B C10B 124.7(11) . . ? C7B C6B C10B 120.0 . . ? C8B C7B C6B 120.0 . . ? C8B C7B H7B 120.0 . . ? C6B C7B H7B 120.0 . . ? C7B C8B N4B 120.0 . . ? C7B C8B H8B 120.0 . . ? N4B C8B H8B 120.0 . . ? C9B N4B C8B 120.0 . . ? C9B N4B H4B1 120.0 . . ? C8B N4B H4B1 120.0 . . ? N4B C9B C10B 120.0 . . ? N4B C9B H9B 120.0 . . ? C10B C9B H9B 120.0 . . ? C9B C10B C6B 120.0 . . ? C6C N1C N2C 119(2) . . ? C1C N2C N1C 115(2) . . ? C4C N3C C3C 119(2) . . ? C4C N3C H3C1 120.6 . . ? C3C N3C H3C1 120.6 . . ? C2C C1C N2C 119.7(19) . . ? C2C C1C C5C 117.2(18) . . ? N2C C1C C5C 123(2) . . ? C1C C2C C3C 117.6(19) . . ? C1C C2C H2C 121.2 . . ? C3C C2C H2C 121.2 . . ? N3C C3C C2C 122(2) . . ? N3C C3C H3C 118.8 . . ? C2C C3C H3C 118.8 . . ? N3C C4C C5C 122(2) . . ? N3C C4C H4C 119.2 . . ? C5C C4C H4C 119.2 . . ? C4C C5C C1C 121(2) . . ? C4C C5C H5C 119.3 . . ? C1C C5C H5C 119.3 . . ? C7C C6C C10C 125.2(18) . . ? C7C C6C N1C 130.6(18) . . ? C10C C6C N1C 104.2(18) . . ? C8C C7C C6C 120.4(17) . . ? C8C C7C H7C 119.8 . . ? C6C C7C H7C 119.8 . . ? C7C C8C N4C 119.1(17) . . ? C7C C8C H8C 120.4 . . ? N4C C8C H8C 120.4 . . ? C9C N4C C8C 115.6(18) . . ? C9C N4C H4C1 122.2 . . ? C8C N4C H4C1 122.2 . . ? N4C C9C C10C 131(2) . . ? N4C C9C H9C 114.3 . . ? C10C C9C H9C 114.3 . . ? C9C C10C C6C 108(2) . . ? C9C C10C H10C 126.1 . . ? C6C C10C H10C 126.1 . . ? P2 P2 O41 90.3(13) 3_575 . ? P2 P2 O42 72.3(11) 3_575 . ? O41 P2 O42 34.5(11) . . ? P2 P2 O42 66.9(11) 3_575 3_575 ? O41 P2 O42 143.1(15) . 3_575 ? O42 P2 O42 139.1(7) . 3_575 ? P2 P2 O43 105.6(13) 3_575 . ? O41 P2 O43 78.0(15) . . ? O42 P2 O43 111.0(14) . . ? O42 P2 O43 80.7(13) 3_575 . ? P2 P2 O41 49.3(9) 3_575 3_575 ? O41 P2 O41 139.7(9) . 3_575 ? O42 P2 O41 115.4(11) . 3_575 ? O42 P2 O41 30.6(9) 3_575 3_575 ? O43 P2 O41 109.3(13) . 3_575 ? P2 P2 O43 46.4(10) 3_575 3_575 ? O41 P2 O43 99.1(14) . 3_575 ? O42 P2 O43 65.3(11) . 3_575 ? O42 P2 O43 86.0(12) 3_575 3_575 ? O43 P2 O43 152.0(6) . 3_575 ? O41 P2 O43 55.5(11) 3_575 3_575 ? P2 P2 H1 135.0 3_575 . ? O41 P2 H1 103.1 . . ? O42 P2 H1 95.1 . . ? O42 P2 H1 113.6 3_575 . ? O43 P2 H1 119.1 . . ? O41 P2 H1 106.6 3_575 . ? O43 P2 H1 88.8 3_575 . ? O42 O41 P2 89(3) . . ? O42 O41 P2 69(2) . 3_575 ? P2 O41 P2 40.3(9) . 3_575 ? O42 O41 O43 145(3) . . ? P2 O41 O43 60.5(13) . . ? P2 O41 O43 77.2(13) 3_575 . ? O42 O41 Zn4 88(2) . . ? P2 O41 Zn4 170.5(17) . . ? P2 O41 Zn4 130.5(14) 3_575 . ? O43 O41 Zn4 118.8(15) . . ? O41 O42 P2 56(2) . . ? O41 O42 P2 81(2) . 3_575 ? P2 O42 P2 40.9(7) . 3_575 ? O41 O42 Zn4 68(2) . . ? P2 O42 Zn4 123.6(14) . . ? P2 O42 Zn4 126.1(13) 3_575 . ? P2 O43 O41 41.4(10) . . ? P2 O43 P2 28.0(6) . 3_575 ? O41 O43 P2 47.3(10) . 3_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.768 _refine_diff_density_min -2.849 _refine_diff_density_rms 0.260 #===END