# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2033 #======================================================================= # Title: Contemporary bimetallic molecules: an unusual class of exo-closo # metallacarbaboranes having no metal-metal bonds #======================================================================= data_global #======================================================================= # SUBMISSION DETAILS _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry Baylor University PO Box 97348 Waco TX, 76798-7348 ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '(254) 710 2403' _publ_contact_author_phone '(254) 710 4427' _publ_contact_letter ; Please consider this CIF submission for publication in the Journal of the Chemical Society, Dalton Transactions. Title: Contemporary bimetallic molecules: an unusual class of exo-closo metallacarbaboranes having no metal-metal bonds ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_category ? _publ_requested_coeditor_name ? #======================================================================= # PROCESSING SUMMARY (IUCr Office Use Only) _journal_data_validation_number ? _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_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_paper_category ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ; # 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 'Ellis, Dianne D' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Franken, Andreas' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Jelliss, Paul A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Kautz, Jason A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Stone, F Gordon A' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; 'Yu, Pui-Yin ' ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #======================================================================= # TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Harms, K. (1993). XCAD4 A Program to extract intensities from a CAD-4 file. University of Marburg, Germany. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of G\"ottingen, Germany. Bruker Analytical X-ray Instruments Inc. (1995), Madison, Wisconsin, USA. ; _publ_section_figure_captions ; Figure 1. Molecular Structure [2,2,2-(CO)~3~-2-PPh~3~-7,8,12-(\m-H)~3~ -7,8,12-{Cu(PPh~3~)}-closo-2,1-MoCB~10~H~8~] (8) showing the crystallographic labeling scheme. Hydrogen atoms, except for H(3), H(7) and H(8)are omitted for clarity, as are all but the ipso-carbons of the Ph rings. Thermal ellipsoids are shown at the 40% probability level. Figure 2. Molecular Structure [2,2,2-(CO)~3~-2-PPh~3~-7,12-(\m-H)~2~ -7,12-{Ag(PPh~3~)}-closo-2,1-MoCB~10~H~9~] (10) showing the crystallographic labeling scheme. Hydrogen atoms, except for H(3), H(7) and H(8)are omitted for clarity, as are all but the ipso-carbons of the Ph rings. Thermal ellipsoids are shown at the 40% probability level. Figure 3. Molecular Structure [2,2,2-(CO)~3~-2-PPh~3~-7,8,12-(\m-H)~3~ -7,8,12-{RuCl(PPh~2~)}-closo-2,1-MoCB~10~H~8~] (12a) showing the crystallographic labeling scheme. Hydrogen atoms, except for H(3), H(7) and H(8)are omitted for clarity, as are all but the ipso-carbons of the Ph rings. Thermal ellipsoids are shown at the 40% probability level. Figure 5. Molecular Structure [2,2,2-(CO)~3~-2-PPh~3~-12-(\m-H)-{Fe (CO)~2~(\h-C~5~Me~5~)}-closo-2,1-MoCB~10~H~10~] (14) showing the crystallographic labeling scheme. Hydrogen atoms, except for H(8)are omitted for clarity as are all but the ipso-carbons of the Ph rings. Thermal ellipsoids are shown at the 40% probability level. ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; Diffracted intensities for 8, 9, 10, and 14 were collected on an Enraf-Nonius CAD-4 using graphite-monochromatic MoKa X-radiation operatin in \w (8, 9), and \w-2\q (10, 12) scan modes. Final unit cell dimensions were determined from the setting angles of 25 accurately centered reflections. Crystal stability during the data collection was monitored by measuring the intensities of three standard reflections every two hours. Data were collected at a constant rate of 5.17\% min-1 in \w with a scan range of 1.15 + 0.34tan\q for 8, a variable scan speed of 4.13 to 5.17\% min-1 with a scan rage of 1.15 + 0.34tan\q for 9, a constant scan speed of 5.17\% min-1 in \w with a scan range of 0.95 + 0.34tan\q for 10, and a constant scan speed of 5.17\% min-1 in \w with a scan range of 1.15 + 0.34tan\q for 14. The data were corrected for Lorentz, polarization and X-ray absorption effects, the latter either using a face-indexed method based on the measurements of 6 crystal faces for 10 or a semi-empirical method based on azimuthal scans of \y-data for 8 and 14. No absorption correction was applied for 9. Low-temperature data (173K) for 12a were collected on a Siemens SMART CCD area-detector three-circle diffractometer (Mo-Ka X-radiation, graphite monochromator. For four settings of phi. narrow data 'frames' were collected for 0.3\% increments in \w. A total of 2132 frames of data were collected affording a sphere of data. It was confirmed that crystal decay had not taken place during the course of the data collection. The substantial redundancy in data allows empirical absorption corrections (SADABS) to be applied using multiple measurements of equivalent reflections. The data frames were integrated using SAINT. The structures were solved by direct methods and successive difference Fourier syntheses were used to locate all non-hydrogen atoms using SHELXTL version 5.03 Refinements were made by full-matrix least-squares on all F^2^ data using SHELXL-97 Anisotropic thermal parameters were included for all non-hydrogen atoms. For all structures, cage carbon atoms were assigned by comparison of the bond lengths to adjacent boron atoms in conjunction with the magnitudes of their isotropic thermal parameters. With the exception of the agostic B->H Ag/Cu/Ru protons in 8, 10, and 12a and H(7) in 10, all hydrogen atoms were included in calculated positions and allowed to ride on their parent boron or carbon atoms with fixed isotropic thermal parameters (Uiso = 1.2Uiso of the parent atom or Uiso = 1.5Uiso for the methyl protons). The agostic protons in 8, 10, and 12a and H(7) in 10 were located in difference Fourier syntheses. The postional parameters of these hydrogens were allowed to refine while their isotropic thermal parameters were constrained to 1.2Uiso of the parent boron atoms. Compound 8 co-crystallized with a molecule of dichloromethane. The carbon atom (C90) of the solvent molecule was disordered over two sites (60:40), in addition, the C-Cl bond distances were restrained. Both solvent molecules of 12a were disordered over two positions: the CH2Cl2 molecule (50 : 50), and the C5H12 molecule (75 : 25), and individual distances, C-Cl of the CH2Cl2 and C-C of the pentane molecule, were restrained. The carbon atoms of the minor component of the pentane molecule were refined with isotropic thermal parameters and no hydrogen atoms were added. The carbonyl groups on the iron cation of 14 (C(7), O(7), C(8), O(8); C(9), O(9), C(10), O(10)) were disordered over two sites in the ratio 70:30. The thermal parameters for the minor disordered components were refined isotropically with the value for C(9) fixed at 10.15. All calculations were carried out on Dell or Viglen PC computers. ; #======================================================================= # If more than one structure is reported, the remaining sections should # be completed per structure. For each data set, replace the '?' in the # data_? line below by a unique identifier. data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H41 B10 Cu Mo O3 P2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H41 B10 Cu Mo O3 P2' _chemical_formula_weight 899.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7020(12) _cell_length_b 12.1224(8) _cell_length_c 16.203(2) _cell_angle_alpha 92.074(9) _cell_angle_beta 104.602(10) _cell_angle_gamma 106.685(7) _cell_volume 2115.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 4.32 _cell_measurement_theta_max 22.07 _exptl_crystal_description parallelopiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.84252 _exptl_absorpt_correction_T_max 0.88520 _exptl_absorpt_process_details 'SHELXTL-PC, (Bruker, 1995)' _exptl_special_details ; Data were collected on an Enraf-Nonius CAD-4 operating in the \w-2\q scan mode, using graphite-monochromated Mo-Ka X-radiation. The final unit cell dimensions were determined from the setting angle values of 25 accurately centered reflections. The stability of the crystal during the period of the data collection was monitored by measuring the intensities of three standard reflections every two hours. Data were collected at a constant scan speed of 5.17\% min-1 in \w, with a scan range of 1.15 + 0.34tan\q. The data were corrected for Lorentz, polarization and X-ray absorption effects, the latter by a semi empirical method based on azimuthal scans of \y data. ; _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 'Enraf-Nonius' _diffrn_measurement_method '\w scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% none _diffrn_reflns_number 7835 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0771 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7435 _reflns_number_gt 4903 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.2500P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7435 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0994 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.66211(4) 0.80275(3) 0.25527(3) 0.03565(12) Uani 1 d . . . C3 C 0.6734(4) 0.7543(4) 0.1410(3) 0.0472(12) Uani 1 d . . . O3 O 0.6811(4) 0.7371(3) 0.0732(2) 0.0746(12) Uani 1 d . . . C4 C 0.4933(5) 0.7805(4) 0.1781(3) 0.0545(14) Uani 1 d . . . O4 O 0.3965(3) 0.7678(3) 0.1334(3) 0.0803(13) Uani 1 d . . . C5 C 0.5486(4) 0.6801(4) 0.3024(3) 0.0491(13) Uani 1 d . . . O5 O 0.4793(4) 0.6154(3) 0.3295(3) 0.0762(12) Uani 1 d . . . P2 P 0.78466(11) 0.65744(10) 0.28747(8) 0.0364(3) Uani 1 d . . . C41 C 0.7932(4) 0.5987(4) 0.3904(3) 0.0368(11) Uani 1 d . . . C42 C 0.8225(5) 0.4975(4) 0.4047(3) 0.0570(14) Uani 1 d . . . H42 H 0.8368 0.4569 0.3606 0.068 Uiso 1 calc R . . C43 C 0.8311(5) 0.4553(5) 0.4831(3) 0.0657(16) Uani 1 d . . . H43 H 0.8501 0.3863 0.4911 0.079 Uiso 1 calc R . . C44 C 0.8117(5) 0.5142(5) 0.5489(3) 0.0619(15) Uani 1 d . . . H44 H 0.8185 0.4864 0.6022 0.074 Uiso 1 calc R . . C45 C 0.7822(6) 0.6146(5) 0.5356(3) 0.0680(16) Uani 1 d . . . H45 H 0.7683 0.6551 0.5801 0.082 Uiso 1 calc R . . C46 C 0.7728(5) 0.6562(4) 0.4576(3) 0.0559(14) Uani 1 d . . . H46 H 0.7522 0.7245 0.4498 0.067 Uiso 1 calc R . . C51 C 0.7259(5) 0.5271(4) 0.2092(3) 0.0438(12) Uani 1 d . . . C52 C 0.8050(5) 0.4676(4) 0.1919(3) 0.0589(15) Uani 1 d . . . H52 H 0.8890 0.4940 0.2211 0.071 Uiso 1 calc R . . C53 C 0.7604(6) 0.3702(4) 0.1322(4) 0.0682(17) Uani 1 d . . . H53 H 0.8139 0.3316 0.1207 0.082 Uiso 1 calc R . . C54 C 0.6358(7) 0.3311(5) 0.0900(4) 0.0744(18) Uani 1 d . . . H54 H 0.6051 0.2657 0.0497 0.089 Uiso 1 calc R . . C55 C 0.5567(6) 0.3871(5) 0.1068(4) 0.0765(18) Uani 1 d . . . H55 H 0.4726 0.3591 0.0784 0.092 Uiso 1 calc R . . C56 C 0.6013(5) 0.4853(4) 0.1657(3) 0.0587(14) Uani 1 d . . . H56 H 0.5470 0.5235 0.1762 0.070 Uiso 1 calc R . . C61 C 0.9475(4) 0.7126(3) 0.2874(3) 0.0370(11) Uani 1 d . . . C62 C 1.0429(4) 0.7388(4) 0.3621(3) 0.0471(12) Uani 1 d . . . H62 H 1.0250 0.7277 0.4145 0.057 Uiso 1 calc R . . C63 C 1.1657(5) 0.7818(4) 0.3599(4) 0.0643(16) Uani 1 d . . . H63 H 1.2293 0.8000 0.4107 0.077 Uiso 1 calc R . . C64 C 1.1928(5) 0.7973(4) 0.2829(5) 0.0711(18) Uani 1 d . . . H64 H 1.2751 0.8257 0.2817 0.085 Uiso 1 calc R . . C65 C 1.0996(5) 0.7712(4) 0.2076(4) 0.0609(15) Uani 1 d . . . H65 H 1.1183 0.7809 0.1553 0.073 Uiso 1 calc R . . C66 C 0.9779(5) 0.7304(4) 0.2103(3) 0.0542(14) Uani 1 d . . . H66 H 0.9147 0.7146 0.1594 0.065 Uiso 1 calc R . . C1 C 0.7096(4) 0.9302(4) 0.3846(3) 0.0399(11) Uani 1 d . . . H1 H 0.6701 0.8736 0.4285 0.048 Uiso 1 calc R . . B2 B 0.8400(5) 0.9197(4) 0.3636(3) 0.0369(12) Uani 1 d . . . H2 H 0.8898 0.8594 0.3911 0.044 Uiso 1 calc R . . B3 B 0.8339(5) 0.9641(4) 0.2575(4) 0.0377(13) Uani 1 d . . . H3 H 0.891(4) 0.943(3) 0.214(2) 0.045 Uiso 1 d . . . B4 B 0.6904(5) 0.9940(4) 0.2177(4) 0.0449(14) Uani 1 d . . . H4 H 0.6431 0.9861 0.1489 0.054 Uiso 1 calc R . . B5 B 0.6120(5) 0.9659(5) 0.3023(4) 0.0449(14) Uani 1 d . . . H5 H 0.5104 0.9362 0.2896 0.054 Uiso 1 calc R . . B6 B 0.8439(5) 1.0378(5) 0.4322(4) 0.0467(14) Uani 1 d . . . H6 H 0.8933 1.0511 0.5009 0.056 Uiso 1 calc R . . B7 B 0.9216(5) 1.0625(4) 0.3522(4) 0.0407(13) Uani 1 d . . . H7 H 1.019(4) 1.091(3) 0.370(3) 0.049 Uiso 1 d . . . B8 B 0.8296(5) 1.1107(5) 0.2653(4) 0.0482(15) Uani 1 d . . . H8 H 0.875(4) 1.168(4) 0.224(3) 0.058 Uiso 1 d . . . B9 B 0.6923(5) 1.1110(5) 0.2900(4) 0.0519(16) Uani 1 d . . . H9 H 0.6423 1.1727 0.2660 0.062 Uiso 1 calc R . . B10 B 0.7022(5) 1.0673(5) 0.3933(4) 0.0515(16) Uani 1 d . . . H10 H 0.6587 1.1006 0.4373 0.062 Uiso 1 calc R . . B11 B 0.8362(5) 1.1555(5) 0.3713(4) 0.0490(15) Uani 1 d . . . H11 H 0.8810 1.2462 0.4001 0.059 Uiso 1 calc R . . Cu Cu 1.00859(6) 1.07792(6) 0.24273(5) 0.0627(2) Uani 1 d . . . P1 P 1.17731(12) 1.16058(11) 0.20751(9) 0.0472(3) Uani 1 d . . . C11 C 1.2206(5) 1.0746(4) 0.1330(3) 0.0471(12) Uani 1 d . . . C12 C 1.1276(5) 0.9905(5) 0.0745(4) 0.0658(16) Uani 1 d . . . H12 H 1.0457 0.9765 0.0757 0.079 Uiso 1 calc R . . C13 C 1.1550(7) 0.9268(5) 0.0144(4) 0.0793(19) Uani 1 d . . . H13 H 1.0918 0.8702 -0.0250 0.095 Uiso 1 calc R . . C14 C 1.2754(7) 0.9469(6) 0.0128(4) 0.0798(19) Uani 1 d . . . H14 H 1.2937 0.9059 -0.0292 0.096 Uiso 1 calc R . . C15 C 1.3695(6) 1.0276(6) 0.0729(5) 0.0805(19) Uani 1 d . . . H15 H 1.4516 1.0388 0.0732 0.097 Uiso 1 calc R . . C16 C 1.3417(5) 1.0920(5) 0.1330(4) 0.0669(16) Uani 1 d . . . H16 H 1.4052 1.1472 0.1734 0.080 Uiso 1 calc R . . C21 C 1.1719(4) 1.2927(4) 0.1591(3) 0.0471(12) Uani 1 d . . . C22 C 1.1345(5) 1.3726(5) 0.1998(4) 0.0746(18) Uani 1 d . . . H22 H 1.1105 1.3570 0.2498 0.089 Uiso 1 calc R . . C23 C 1.1326(6) 1.4759(5) 0.1665(5) 0.091(2) Uani 1 d . . . H23 H 1.1101 1.5305 0.1953 0.109 Uiso 1 calc R . . C24 C 1.1636(6) 1.4981(6) 0.0918(5) 0.087(2) Uani 1 d . . . H24 H 1.1614 1.5672 0.0693 0.105 Uiso 1 calc R . . C25 C 1.1980(7) 1.4184(6) 0.0503(4) 0.092(2) Uani 1 d . . . H25 H 1.2176 1.4326 -0.0013 0.110 Uiso 1 calc R . . C26 C 1.2037(5) 1.3165(5) 0.0845(4) 0.0704(17) Uani 1 d . . . H26 H 1.2294 1.2637 0.0564 0.084 Uiso 1 calc R . . C31 C 1.3107(4) 1.2054(4) 0.3012(3) 0.0442(12) Uani 1 d . . . C32 C 1.3982(5) 1.3129(4) 0.3168(4) 0.0649(16) Uani 1 d . . . H32 H 1.3921 1.3662 0.2773 0.078 Uiso 1 calc R . . C33 C 1.4956(5) 1.3422(5) 0.3912(4) 0.083(2) Uani 1 d . . . H33 H 1.5535 1.4156 0.4020 0.099 Uiso 1 calc R . . C34 C 1.5070(6) 1.2638(6) 0.4485(4) 0.0775(18) Uani 1 d . . . H34 H 1.5725 1.2838 0.4983 0.093 Uiso 1 calc R . . C35 C 1.4224(6) 1.1563(6) 0.4327(4) 0.0684(16) Uani 1 d . . . H35 H 1.4314 1.1023 0.4711 0.082 Uiso 1 calc R . . C36 C 1.3234(5) 1.1271(4) 0.3602(4) 0.0586(14) Uani 1 d . . . H36 H 1.2648 1.0542 0.3508 0.070 Uiso 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 Mo 0.0330(2) 0.0324(2) 0.0387(2) 0.00231(17) 0.00845(18) 0.00707(17) C3 0.048(3) 0.050(3) 0.040(3) 0.004(3) 0.007(3) 0.015(2) O3 0.094(3) 0.088(3) 0.043(2) 0.000(2) 0.020(2) 0.030(2) C4 0.049(3) 0.051(3) 0.060(4) 0.008(3) 0.010(3) 0.014(3) O4 0.048(2) 0.085(3) 0.084(3) 0.005(2) -0.013(2) 0.012(2) C5 0.043(3) 0.041(3) 0.065(4) 0.004(3) 0.021(3) 0.009(2) O5 0.070(3) 0.065(3) 0.095(3) 0.023(2) 0.042(2) 0.005(2) P2 0.0377(7) 0.0322(6) 0.0360(7) -0.0008(5) 0.0088(6) 0.0073(5) C41 0.037(3) 0.034(2) 0.039(3) 0.005(2) 0.009(2) 0.010(2) C42 0.084(4) 0.062(3) 0.043(3) 0.013(3) 0.026(3) 0.042(3) C43 0.098(5) 0.062(4) 0.054(4) 0.023(3) 0.024(3) 0.046(3) C44 0.086(4) 0.063(4) 0.039(3) 0.013(3) 0.014(3) 0.027(3) C45 0.109(5) 0.062(4) 0.046(3) 0.006(3) 0.030(3) 0.038(4) C46 0.083(4) 0.045(3) 0.047(3) 0.012(3) 0.019(3) 0.030(3) C51 0.055(3) 0.033(3) 0.036(3) -0.001(2) 0.009(2) 0.007(2) C52 0.073(4) 0.041(3) 0.059(4) -0.004(3) 0.012(3) 0.018(3) C53 0.098(5) 0.045(3) 0.064(4) -0.003(3) 0.017(4) 0.030(3) C54 0.106(5) 0.043(3) 0.062(4) -0.014(3) 0.015(4) 0.013(4) C55 0.064(4) 0.060(4) 0.079(4) -0.019(3) 0.001(3) -0.002(3) C56 0.060(4) 0.045(3) 0.061(4) -0.008(3) 0.012(3) 0.005(3) C61 0.041(3) 0.029(2) 0.043(3) 0.002(2) 0.014(2) 0.013(2) C62 0.039(3) 0.044(3) 0.054(3) -0.003(2) 0.008(3) 0.010(2) C63 0.041(3) 0.061(4) 0.080(4) -0.009(3) 0.005(3) 0.011(3) C64 0.049(4) 0.048(3) 0.119(6) 0.005(4) 0.030(4) 0.012(3) C65 0.069(4) 0.059(4) 0.077(4) 0.017(3) 0.046(4) 0.029(3) C66 0.055(3) 0.056(3) 0.058(4) 0.007(3) 0.021(3) 0.023(3) C1 0.038(3) 0.038(3) 0.045(3) 0.000(2) 0.016(2) 0.011(2) B2 0.041(3) 0.032(3) 0.039(3) -0.002(2) 0.007(3) 0.018(2) B3 0.036(3) 0.031(3) 0.048(3) 0.002(3) 0.017(3) 0.009(2) B4 0.041(3) 0.038(3) 0.057(4) 0.008(3) 0.012(3) 0.014(3) B5 0.036(3) 0.043(3) 0.058(4) 0.002(3) 0.014(3) 0.015(3) B6 0.042(3) 0.046(3) 0.049(4) -0.007(3) 0.010(3) 0.013(3) B7 0.034(3) 0.028(3) 0.056(4) -0.003(3) 0.010(3) 0.006(2) B8 0.051(4) 0.029(3) 0.068(4) 0.008(3) 0.023(3) 0.012(3) B9 0.049(4) 0.040(3) 0.071(4) 0.008(3) 0.013(3) 0.023(3) B10 0.053(4) 0.045(3) 0.064(4) -0.003(3) 0.020(3) 0.023(3) B11 0.046(3) 0.034(3) 0.065(4) -0.006(3) 0.016(3) 0.011(3) Cu 0.0469(4) 0.0575(4) 0.0823(5) 0.0026(4) 0.0324(4) 0.0015(3) P1 0.0430(8) 0.0413(7) 0.0580(9) 0.0036(7) 0.0219(7) 0.0070(6) C11 0.052(3) 0.040(3) 0.053(3) 0.008(2) 0.020(3) 0.015(2) C12 0.064(4) 0.069(4) 0.065(4) 0.000(3) 0.012(3) 0.027(3) C13 0.107(6) 0.072(4) 0.058(4) -0.004(3) 0.011(4) 0.037(4) C14 0.118(6) 0.082(5) 0.067(4) 0.018(4) 0.038(4) 0.060(5) C15 0.077(5) 0.080(5) 0.110(6) 0.019(4) 0.050(4) 0.042(4) C16 0.062(4) 0.061(4) 0.085(4) -0.003(3) 0.030(3) 0.023(3) C21 0.035(3) 0.050(3) 0.055(3) 0.004(3) 0.011(2) 0.012(2) C22 0.083(4) 0.066(4) 0.093(5) 0.005(4) 0.047(4) 0.030(3) C23 0.103(6) 0.060(4) 0.124(7) 0.009(4) 0.038(5) 0.042(4) C24 0.100(5) 0.061(4) 0.107(6) 0.033(4) 0.026(5) 0.033(4) C25 0.133(6) 0.081(5) 0.085(5) 0.032(4) 0.051(5) 0.047(5) C26 0.093(5) 0.054(4) 0.080(4) 0.017(3) 0.044(4) 0.029(3) C31 0.046(3) 0.043(3) 0.048(3) 0.010(2) 0.020(2) 0.012(2) C32 0.054(4) 0.053(3) 0.077(4) 0.018(3) 0.013(3) 0.002(3) C33 0.053(4) 0.066(4) 0.103(5) 0.006(4) 0.001(4) -0.004(3) C34 0.062(4) 0.085(5) 0.079(5) 0.002(4) 0.007(3) 0.025(4) C35 0.079(4) 0.084(5) 0.068(4) 0.030(4) 0.039(4) 0.044(4) C36 0.058(4) 0.051(3) 0.075(4) 0.010(3) 0.031(3) 0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C3 1.970(5) . y Mo C4 1.991(5) . y Mo C5 2.004(5) . y Mo B3 2.360(5) . y Mo B4 2.370(5) . y Mo B5 2.370(5) . y Mo B2 2.389(5) . y Mo C1 2.402(4) . y Mo P2 2.5634(12) . y C3 O3 1.142(5) . y C4 O4 1.144(5) . y C5 O5 1.142(5) . y P2 C41 1.828(4) . ? P2 C61 1.829(4) . ? P2 C51 1.836(4) . ? C41 C42 1.378(6) . ? C41 C46 1.379(6) . ? C42 C43 1.377(6) . ? C43 C44 1.364(7) . ? C44 C45 1.368(7) . ? C45 C46 1.368(6) . ? C51 C56 1.383(6) . ? C51 C52 1.398(6) . ? C52 C53 1.383(7) . ? C53 C54 1.377(8) . ? C54 C55 1.365(8) . ? C55 C56 1.382(7) . ? C61 C62 1.378(6) . ? C61 C66 1.390(6) . ? C62 C63 1.391(6) . ? C63 C64 1.369(7) . ? C64 C65 1.372(7) . ? C65 C66 1.380(7) . ? C1 B5 1.682(7) . ? C1 B2 1.682(6) . ? C1 B10 1.691(7) . ? C1 B6 1.704(7) . ? B2 B7 1.762(7) . ? B2 B6 1.763(7) . ? B2 B3 1.810(7) . ? B3 B4 1.785(7) . ? B3 B7 1.789(7) . ? B3 B8 1.792(7) . ? B3 Cu 2.188(5) . y B4 B8 1.792(8) . ? B4 B9 1.798(8) . ? B4 B5 1.823(8) . ? B5 B10 1.772(8) . ? B5 B9 1.785(8) . ? B6 B7 1.750(8) . ? B6 B10 1.762(8) . ? B6 B11 1.775(8) . ? B7 B8 1.772(8) . ? B7 B11 1.772(7) . ? B7 Cu 2.245(6) . y B8 B9 1.752(8) . ? B8 B11 1.758(8) . ? B8 Cu 2.352(6) . y B9 B10 1.760(8) . ? B9 B11 1.780(8) . ? B10 B11 1.754(8) . ? Cu H3 1.77(4) . y Cu H7 2.03(4) . y Cu H8 2.12(4) . y Cu P1 2.1682(14) . y P1 C31 1.815(5) . ? P1 C21 1.818(5) . ? P1 C11 1.822(5) . ? C11 C16 1.372(7) . ? C11 C12 1.377(7) . ? C12 C13 1.376(7) . ? C13 C14 1.366(8) . ? C14 C15 1.375(8) . ? C15 C16 1.383(7) . ? C21 C26 1.369(7) . ? C21 C22 1.382(7) . ? C22 C23 1.385(8) . ? C23 C24 1.363(8) . ? C24 C25 1.364(8) . ? C25 C26 1.384(7) . ? C31 C32 1.375(6) . ? C31 C36 1.382(6) . ? C32 C33 1.386(7) . ? C33 C34 1.362(8) . ? C34 C35 1.361(8) . ? C35 C36 1.376(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo C4 75.7(2) . . y C3 Mo C5 114.1(2) . . y C4 Mo C5 75.1(2) . . y C3 Mo B3 85.26(19) . . ? C4 Mo B3 122.69(19) . . ? C5 Mo B3 157.6(2) . . ? C3 Mo B4 88.8(2) . . ? C4 Mo B4 81.19(19) . . ? C5 Mo B4 140.99(19) . . ? B3 Mo B4 44.34(18) . . ? C3 Mo B5 129.5(2) . . ? C4 Mo B5 77.3(2) . . ? C5 Mo B5 98.76(19) . . ? B3 Mo B5 74.79(18) . . ? B4 Mo B5 45.24(19) . . ? C3 Mo B2 121.59(19) . . ? C4 Mo B2 149.85(19) . . ? C5 Mo B2 112.89(19) . . ? B3 Mo B2 44.80(18) . . ? B4 Mo B2 75.20(19) . . ? B5 Mo B2 72.83(18) . . ? C3 Mo C1 156.52(18) . . ? C4 Mo C1 113.50(18) . . ? C5 Mo C1 89.36(18) . . ? B3 Mo C1 71.55(17) . . ? B4 Mo C1 72.18(18) . . ? B5 Mo C1 41.27(17) . . ? B2 Mo C1 41.11(15) . . ? C3 Mo P2 77.29(14) . . y C4 Mo P2 129.72(15) . . y C5 Mo P2 78.45(14) . . y B3 Mo P2 96.11(13) . . ? B4 Mo P2 139.48(13) . . ? B5 Mo P2 149.33(14) . . ? B2 Mo P2 80.14(12) . . ? C1 Mo P2 108.09(11) . . ? O3 C3 Mo 173.3(4) . . y O4 C4 Mo 179.7(5) . . y O5 C5 Mo 175.2(4) . . y C41 P2 C61 103.1(2) . . ? C41 P2 C51 103.3(2) . . ? C61 P2 C51 102.5(2) . . ? C41 P2 Mo 116.83(15) . . ? C61 P2 Mo 114.98(14) . . ? C51 P2 Mo 114.31(16) . . ? C42 C41 C46 117.5(4) . . ? C42 C41 P2 121.9(4) . . ? C46 C41 P2 120.7(3) . . ? C43 C42 C41 121.4(5) . . ? C44 C43 C42 120.2(5) . . ? C43 C44 C45 119.1(5) . . ? C46 C45 C44 120.7(5) . . ? C45 C46 C41 121.1(5) . . ? C56 C51 C52 118.3(4) . . ? C56 C51 P2 120.4(4) . . ? C52 C51 P2 121.3(4) . . ? C53 C52 C51 121.0(5) . . ? C54 C53 C52 119.1(6) . . ? C55 C54 C53 120.8(5) . . ? C54 C55 C56 120.3(6) . . ? C55 C56 C51 120.5(5) . . ? C62 C61 C66 118.0(4) . . ? C62 C61 P2 122.1(4) . . ? C66 C61 P2 119.9(4) . . ? C61 C62 C63 120.7(5) . . ? C64 C63 C62 120.0(5) . . ? C63 C64 C65 120.5(5) . . ? C64 C65 C66 119.2(5) . . ? C65 C66 C61 121.6(5) . . ? B5 C1 B2 114.2(4) . . ? B5 C1 B10 63.4(3) . . ? B2 C1 B10 114.1(4) . . ? B5 C1 B6 115.3(4) . . ? B2 C1 B6 62.7(3) . . ? B10 C1 B6 62.5(3) . . ? B5 C1 Mo 68.3(2) . . ? B2 C1 Mo 69.0(2) . . ? B10 C1 Mo 127.6(3) . . ? B6 C1 Mo 128.0(3) . . ? C1 B2 B7 104.7(3) . . ? C1 B2 B6 59.2(3) . . ? B7 B2 B6 59.6(3) . . ? C1 B2 B3 105.7(4) . . ? B7 B2 B3 60.1(3) . . ? B6 B2 B3 108.5(4) . . ? C1 B2 Mo 69.9(2) . . ? B7 B2 Mo 122.6(3) . . ? B6 B2 Mo 125.6(3) . . ? B3 B2 Mo 66.8(2) . . ? B4 B3 B7 108.0(4) . . ? B4 B3 B8 60.1(3) . . ? B7 B3 B8 59.3(3) . . ? B4 B3 B2 107.8(4) . . ? B7 B3 B2 58.6(3) . . ? B8 B3 B2 105.7(4) . . ? B4 B3 Cu 121.8(3) . . ? B7 B3 Cu 67.9(2) . . ? B8 B3 Cu 71.6(3) . . ? B2 B3 Cu 115.3(3) . . ? B4 B3 Mo 68.1(2) . . ? B7 B3 Mo 122.8(3) . . ? B8 B3 Mo 123.0(3) . . ? B2 B3 Mo 68.4(2) . . ? Cu B3 Mo 164.3(3) . . y B3 B4 B8 60.1(3) . . ? B3 B4 B9 106.7(4) . . ? B8 B4 B9 58.4(3) . . ? B3 B4 B5 105.5(4) . . ? B8 B4 B5 104.8(4) . . ? B9 B4 B5 59.1(3) . . ? B3 B4 Mo 67.5(2) . . ? B8 B4 Mo 122.5(3) . . ? B9 B4 Mo 122.2(3) . . ? B5 B4 Mo 67.4(2) . . ? C1 B5 B10 58.6(3) . . ? C1 B5 B9 104.6(4) . . ? B10 B5 B9 59.3(3) . . ? C1 B5 B4 106.6(4) . . ? B10 B5 B4 107.9(4) . . ? B9 B5 B4 59.8(3) . . ? C1 B5 Mo 70.4(2) . . ? B10 B5 Mo 125.1(3) . . ? B9 B5 Mo 122.8(3) . . ? B4 B5 Mo 67.4(2) . . ? C1 B6 B7 104.3(4) . . ? C1 B6 B10 58.4(3) . . ? B7 B6 B10 107.1(4) . . ? C1 B6 B2 58.0(3) . . ? B7 B6 B2 60.2(3) . . ? B10 B6 B2 106.9(4) . . ? C1 B6 B11 104.6(4) . . ? B7 B6 B11 60.4(3) . . ? B10 B6 B11 59.5(3) . . ? B2 B6 B11 108.4(4) . . ? B6 B7 B2 60.2(3) . . ? B6 B7 B8 108.3(4) . . ? B2 B7 B8 108.6(4) . . ? B6 B7 B11 60.5(3) . . ? B2 B7 B11 108.6(4) . . ? B8 B7 B11 59.5(3) . . ? B6 B7 B3 110.1(4) . . ? B2 B7 B3 61.3(3) . . ? B8 B7 B3 60.4(3) . . ? B11 B7 B3 109.0(4) . . ? B6 B7 Cu 174.5(4) . . ? B2 B7 Cu 114.7(3) . . ? B8 B7 Cu 70.6(3) . . ? B11 B7 Cu 121.6(3) . . ? B3 B7 Cu 64.6(2) . . ? B9 B8 B11 60.9(3) . . ? B9 B8 B7 108.2(4) . . ? B11 B8 B7 60.3(3) . . ? B9 B8 B4 61.0(3) . . ? B11 B8 B4 110.6(4) . . ? B7 B8 B4 108.5(4) . . ? B9 B8 B3 108.4(4) . . ? B11 B8 B3 109.5(4) . . ? B7 B8 B3 60.2(3) . . ? B4 B8 B3 59.7(3) . . ? B9 B8 Cu 169.6(4) . . ? B11 B8 Cu 116.8(3) . . ? B7 B8 Cu 64.2(3) . . ? B4 B8 Cu 113.4(3) . . ? B3 B8 Cu 62.0(2) . . ? B8 B9 B10 107.2(4) . . ? B8 B9 B11 59.7(3) . . ? B10 B9 B11 59.4(3) . . ? B8 B9 B5 108.1(4) . . ? B10 B9 B5 60.0(3) . . ? B11 B9 B5 107.7(4) . . ? B8 B9 B4 60.6(3) . . ? B10 B9 B4 109.6(4) . . ? B11 B9 B4 109.3(4) . . ? B5 B9 B4 61.2(3) . . ? C1 B10 B11 106.1(4) . . ? C1 B10 B9 105.4(4) . . ? B11 B10 B9 60.9(3) . . ? C1 B10 B6 59.1(3) . . ? B11 B10 B6 60.6(3) . . ? B9 B10 B6 109.1(4) . . ? C1 B10 B5 58.1(3) . . ? B11 B10 B5 109.5(4) . . ? B9 B10 B5 60.7(3) . . ? B6 B10 B5 108.1(4) . . ? B10 B11 B8 107.2(4) . . ? B10 B11 B7 106.5(4) . . ? B8 B11 B7 60.2(3) . . ? B10 B11 B6 59.9(3) . . ? B8 B11 B6 107.8(4) . . ? B7 B11 B6 59.1(3) . . ? B10 B11 B9 59.7(3) . . ? B8 B11 B9 59.3(3) . . ? B7 B11 B9 106.9(4) . . ? B6 B11 B9 107.6(4) . . ? H3 Cu H7 96.4(17) . . y H3 Cu H8 91.4(17) . . y H7 Cu H8 88.2(16) . . y H3 Cu P1 136.1(13) . . y H7 Cu P1 116.7(12) . . y H8 Cu P1 116.1(12) . . y H3 Cu B3 31.5(13) . . ? H7 Cu B3 72.7(12) . . ? H8 Cu B3 70.5(12) . . ? P1 Cu B3 167.61(14) . . y H3 Cu B7 76.3(13) . . ? H7 Cu B7 27.8(12) . . ? H8 Cu B7 70.0(12) . . ? P1 Cu B7 143.38(15) . . y B3 Cu B7 47.57(19) . . y H3 Cu B8 73.9(13) . . ? H7 Cu B8 69.2(12) . . ? H8 Cu B8 28.0(11) . . ? P1 Cu B8 142.71(14) . . y B3 Cu B8 46.33(18) . . y B7 Cu B8 45.3(2) . . y C31 P1 C21 105.2(2) . . ? C31 P1 C11 105.0(2) . . ? C21 P1 C11 105.5(2) . . ? C31 P1 Cu 111.28(16) . . ? C21 P1 Cu 112.06(16) . . ? C11 P1 Cu 116.88(17) . . ? C16 C11 C12 119.5(5) . . ? C16 C11 P1 122.2(4) . . ? C12 C11 P1 118.3(4) . . ? C13 C12 C11 120.5(6) . . ? C14 C13 C12 119.9(6) . . ? C13 C14 C15 120.1(6) . . ? C14 C15 C16 119.9(6) . . ? C11 C16 C15 120.0(6) . . ? C26 C21 C22 118.6(5) . . ? C26 C21 P1 123.0(4) . . ? C22 C21 P1 118.4(4) . . ? C21 C22 C23 120.3(6) . . ? C24 C23 C22 120.4(6) . . ? C23 C24 C25 119.6(6) . . ? C24 C25 C26 120.3(6) . . ? C21 C26 C25 120.7(6) . . ? C32 C31 C36 118.6(5) . . ? C32 C31 P1 123.5(4) . . ? C36 C31 P1 117.8(4) . . ? C31 C32 C33 120.2(5) . . ? C34 C33 C32 120.3(6) . . ? C35 C34 C33 119.9(6) . . ? C34 C35 C36 120.4(6) . . ? C35 C36 C31 120.5(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.407 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.071 #===END data_10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H43 Ag B10 Cl2 Mo O3 P2' _chemical_formula_weight 1028.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.146(2) _cell_length_b 14.6174(12) _cell_length_c 16.121(4) _cell_angle_alpha 70.670(11) _cell_angle_beta 84.020(18) _cell_angle_gamma 69.706(10) _cell_volume 2324.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description blocks _exptl_crystal_colour 'clear yellow' _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.68534 _exptl_absorpt_correction_T_max 0.79543 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 16.03 _diffrn_reflns_number 8622 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 24.98 _reflns_number_total 8161 _reflns_number_gt 6766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.2524P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0018(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8161 _refine_ls_number_parameters 561 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.0976 _refine_ls_wR_factor_gt 0.0911 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.058 _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 Mo Mo 0.24132(3) 0.37829(2) 0.255333(19) 0.03857(10) Uani 1 1 d . . . C1 C 0.1961(3) 0.2375(2) 0.3651(2) 0.0404(7) Uani 1 1 d . . . H1 H 0.2770 0.1696 0.3611 0.049 Uiso 1 1 calc R . . B2 B 0.2200(3) 0.3185(3) 0.4118(2) 0.0376(8) Uani 1 1 d . . . H2 H 0.3123 0.3080 0.4387 0.045 Uiso 1 1 calc R . . B3 B 0.1046(3) 0.4433(3) 0.3626(3) 0.0390(8) Uani 1 1 d . . . H3 H 0.117(3) 0.520(3) 0.364(2) 0.047 Uiso 1 1 d . . . B4 B 0.0170(4) 0.4313(3) 0.2815(3) 0.0461(9) Uani 1 1 d . . . H4 H -0.0282 0.4963 0.2235 0.055 Uiso 1 1 calc R . . B5 B 0.0843(4) 0.2971(3) 0.2839(3) 0.0464(9) Uani 1 1 d . . . H5 H 0.0870 0.2719 0.2264 0.056 Uiso 1 1 calc R . . B6 B 0.1366(4) 0.2321(3) 0.4678(3) 0.0446(9) Uani 1 1 d . . . H6 H 0.1757 0.1677 0.5277 0.054 Uiso 1 1 calc R . . B7 B 0.0759(4) 0.3614(3) 0.4667(3) 0.0422(9) Uani 1 1 d . . . H7 H 0.075(3) 0.384(3) 0.524(2) 0.051 Uiso 1 1 d . . . B8 B -0.0491(4) 0.4277(3) 0.3882(3) 0.0480(10) Uani 1 1 d . . . H8 H -0.138(4) 0.491(3) 0.399(2) 0.058 Uiso 1 1 d . . . B9 B -0.0629(4) 0.3416(3) 0.3372(3) 0.0498(10) Uani 1 1 d . . . H9 H -0.1545 0.3490 0.3112 0.060 Uiso 1 1 calc R . . B10 B 0.0504(4) 0.2205(3) 0.3887(3) 0.0488(10) Uani 1 1 d . . . H10 H 0.0325 0.1485 0.3973 0.059 Uiso 1 1 calc R . . B11 B -0.0307(4) 0.3005(3) 0.4525(3) 0.0495(10) Uani 1 1 d . . . H11 H -0.1012 0.2816 0.5023 0.059 Uiso 1 1 calc R . . C2 C 0.1612(4) 0.4265(3) 0.1371(3) 0.0653(11) Uani 1 1 d . . . O2 O 0.1151(4) 0.4547(3) 0.0699(2) 0.0973(12) Uani 1 1 d . . . C3 C 0.3601(4) 0.2855(3) 0.1908(3) 0.0629(11) Uani 1 1 d . . . O3 O 0.4189(4) 0.2319(3) 0.1534(3) 0.1018(12) Uani 1 1 d . . . C4 C 0.2419(3) 0.5216(3) 0.2047(2) 0.0494(9) Uani 1 1 d . . . O4 O 0.2306(3) 0.6072(2) 0.1781(2) 0.0724(8) Uani 1 1 d . . . P2 P 0.46560(8) 0.36464(6) 0.29652(6) 0.0397(2) Uani 1 1 d . . . C41 C 0.4719(3) 0.4681(2) 0.3349(2) 0.0455(8) Uani 1 1 d . . . C42 C 0.3791(4) 0.5027(3) 0.3917(3) 0.0539(9) Uani 1 1 d . . . H42 H 0.3176 0.4710 0.4116 0.065 Uiso 1 1 calc R . . C43 C 0.3758(4) 0.5835(3) 0.4195(3) 0.0695(12) Uani 1 1 d . . . H43 H 0.3127 0.6057 0.4579 0.083 Uiso 1 1 calc R . . C44 C 0.4664(5) 0.6307(3) 0.3900(4) 0.0804(14) Uani 1 1 d . . . H44 H 0.4635 0.6865 0.4068 0.096 Uiso 1 1 calc R . . C45 C 0.5608(5) 0.5954(4) 0.3359(4) 0.0882(16) Uani 1 1 d . . . H45 H 0.6236 0.6261 0.3178 0.106 Uiso 1 1 calc R . . C46 C 0.5650(4) 0.5148(3) 0.3074(3) 0.0721(13) Uani 1 1 d . . . H46 H 0.6296 0.4921 0.2701 0.086 Uiso 1 1 calc R . . C51 C 0.5768(4) 0.3679(3) 0.2039(3) 0.0543(9) Uani 1 1 d . . . C52 C 0.5562(5) 0.4549(4) 0.1323(4) 0.104(2) Uani 1 1 d . . . H52 H 0.4848 0.5124 0.1306 0.125 Uiso 1 1 calc R . . C53 C 0.6405(6) 0.4586(6) 0.0623(4) 0.129(3) Uani 1 1 d . . . H53 H 0.6257 0.5185 0.0147 0.155 Uiso 1 1 calc R . . C54 C 0.7438(6) 0.3755(6) 0.0633(4) 0.112(2) Uani 1 1 d . . . H54 H 0.8001 0.3779 0.0164 0.134 Uiso 1 1 calc R . . C55 C 0.7647(5) 0.2892(5) 0.1325(4) 0.112(2) Uani 1 1 d . . . H55 H 0.8354 0.2317 0.1328 0.134 Uiso 1 1 calc R . . C56 C 0.6826(4) 0.2845(4) 0.2033(3) 0.0781(14) Uani 1 1 d . . . H56 H 0.6994 0.2244 0.2508 0.094 Uiso 1 1 calc R . . C61 C 0.5588(3) 0.2456(2) 0.3785(2) 0.0380(7) Uani 1 1 d . . . C62 C 0.6535(3) 0.2443(3) 0.4277(2) 0.0448(8) Uani 1 1 d . . . H62 H 0.6620 0.3060 0.4261 0.054 Uiso 1 1 calc R . . C63 C 0.7361(4) 0.1523(3) 0.4796(3) 0.0523(9) Uani 1 1 d . . . H63 H 0.7997 0.1524 0.5126 0.063 Uiso 1 1 calc R . . C64 C 0.7243(3) 0.0608(3) 0.4825(3) 0.0526(9) Uani 1 1 d . . . H64 H 0.7813 -0.0011 0.5162 0.063 Uiso 1 1 calc R . . C65 C 0.6284(4) 0.0610(3) 0.4355(3) 0.0546(10) Uani 1 1 d . . . H65 H 0.6189 -0.0009 0.4388 0.066 Uiso 1 1 calc R . . C66 C 0.5458(3) 0.1526(3) 0.3834(3) 0.0488(9) Uani 1 1 d . . . H66 H 0.4812 0.1522 0.3515 0.059 Uiso 1 1 calc R . . Ag Ag -0.06342(3) 0.61888(2) 0.33195(3) 0.07301(13) Uani 1 1 d . . . P1 P -0.13691(9) 0.79182(7) 0.23859(7) 0.0478(2) Uani 1 1 d . . . C11 C -0.0527(3) 0.8690(3) 0.2590(2) 0.0469(8) Uani 1 1 d . . . C12 C -0.1134(4) 0.9621(3) 0.2732(3) 0.0601(10) Uani 1 1 d . . . H12 H -0.2023 0.9895 0.2704 0.072 Uiso 1 1 calc R . . C13 C -0.0439(4) 1.0151(3) 0.2915(3) 0.0688(12) Uani 1 1 d . . . H13 H -0.0860 1.0774 0.3017 0.083 Uiso 1 1 calc R . . C14 C 0.0862(4) 0.9763(4) 0.2945(3) 0.0709(12) Uani 1 1 d . . . H14 H 0.1329 1.0127 0.3061 0.085 Uiso 1 1 calc R . . C15 C 0.1484(4) 0.8839(4) 0.2807(4) 0.0848(15) Uani 1 1 d . . . H15 H 0.2374 0.8579 0.2821 0.102 Uiso 1 1 calc R . . C16 C 0.0788(4) 0.8294(4) 0.2648(3) 0.0751(13) Uani 1 1 d . . . H16 H 0.1212 0.7653 0.2579 0.090 Uiso 1 1 calc R . . C21 C -0.1178(4) 0.8076(3) 0.1222(3) 0.0561(10) Uani 1 1 d . . . C22 C -0.1270(7) 0.7336(4) 0.0918(4) 0.107(2) Uani 1 1 d . . . H22 H -0.1391 0.6746 0.1312 0.128 Uiso 1 1 calc R . . C23 C -0.1185(9) 0.7458(6) 0.0022(5) 0.140(3) Uani 1 1 d . . . H23 H -0.1270 0.6955 -0.0178 0.167 Uiso 1 1 calc R . . C24 C -0.0985(7) 0.8282(7) -0.0551(4) 0.114(2) Uani 1 1 d . . . H24 H -0.0925 0.8348 -0.1146 0.137 Uiso 1 1 calc R . . C25 C -0.0870(8) 0.9017(7) -0.0277(4) 0.127(3) Uani 1 1 d . . . H25 H -0.0728 0.9594 -0.0680 0.153 Uiso 1 1 calc R . . C26 C -0.0962(6) 0.8913(5) 0.0610(3) 0.1020(19) Uani 1 1 d . . . H26 H -0.0876 0.9425 0.0796 0.122 Uiso 1 1 calc R . . C31 C -0.3048(4) 0.8583(3) 0.2527(3) 0.0518(9) Uani 1 1 d . . . C32 C -0.3533(4) 0.8313(3) 0.3371(3) 0.0667(11) Uani 1 1 d . . . H32 H -0.3019 0.7784 0.3824 0.080 Uiso 1 1 calc R . . C33 C -0.4772(5) 0.8830(5) 0.3530(5) 0.0935(18) Uani 1 1 d . . . H33 H -0.5093 0.8662 0.4096 0.112 Uiso 1 1 calc R . . C34 C -0.5534(5) 0.9584(5) 0.2870(6) 0.111(3) Uani 1 1 d . . . H34 H -0.6372 0.9931 0.2989 0.133 Uiso 1 1 calc R . . C35 C -0.5086(6) 0.9843(5) 0.2028(6) 0.115(2) Uani 1 1 d . . . H35 H -0.5620 1.0356 0.1577 0.138 Uiso 1 1 calc R . . C36 C -0.3827(5) 0.9333(4) 0.1855(4) 0.0830(14) Uani 1 1 d . . . H36 H -0.3515 0.9499 0.1286 0.100 Uiso 1 1 calc R . . Cl1 Cl 0.5441(8) 0.7626(7) 0.0707(5) 0.441(5) Uani 1 1 d D . . Cl2 Cl 0.3026(8) 0.8473(6) 0.0374(5) 0.475(6) Uani 1 1 d D . . C90 C 0.4194(19) 0.7639(11) 0.1310(13) 0.209(13) Uani 0.59(2) 1 d PD A 1 H90A H 0.4144 0.7962 0.1756 0.251 Uiso 0.59(2) 1 calc PR A 1 H90B H 0.4118 0.6962 0.1576 0.251 Uiso 0.59(2) 1 calc PR A 1 C90A C 0.410(2) 0.7550(16) 0.0388(19) 0.163(13) Uani 0.41(2) 1 d PD A 2 H90C H 0.4217 0.7475 -0.0194 0.196 Uiso 0.41(2) 1 calc PR A 2 H90D H 0.3929 0.6951 0.0791 0.196 Uiso 0.41(2) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.03996(17) 0.03670(16) 0.04098(17) -0.01565(12) -0.00097(12) -0.01147(12) C1 0.0401(18) 0.0324(16) 0.051(2) -0.0185(15) 0.0009(15) -0.0095(14) B2 0.0357(19) 0.0328(18) 0.046(2) -0.0163(16) -0.0007(16) -0.0100(15) B3 0.0365(19) 0.0298(18) 0.053(2) -0.0178(16) -0.0006(16) -0.0088(15) B4 0.039(2) 0.039(2) 0.058(2) -0.0153(19) -0.0096(18) -0.0085(17) B5 0.048(2) 0.039(2) 0.058(3) -0.0221(19) -0.0047(19) -0.0139(18) B6 0.046(2) 0.0329(19) 0.054(2) -0.0149(17) 0.0013(18) -0.0118(17) B7 0.042(2) 0.036(2) 0.054(2) -0.0219(18) 0.0064(18) -0.0131(17) B8 0.034(2) 0.035(2) 0.078(3) -0.024(2) 0.0028(19) -0.0101(16) B9 0.038(2) 0.044(2) 0.074(3) -0.024(2) -0.005(2) -0.0144(18) B10 0.046(2) 0.037(2) 0.070(3) -0.022(2) 0.003(2) -0.0181(18) B11 0.041(2) 0.042(2) 0.072(3) -0.025(2) 0.011(2) -0.0194(18) C2 0.078(3) 0.062(3) 0.060(3) -0.017(2) -0.007(2) -0.028(2) O2 0.135(3) 0.102(3) 0.056(2) -0.0112(18) -0.035(2) -0.044(2) C3 0.070(3) 0.066(3) 0.062(3) -0.032(2) 0.006(2) -0.024(2) O3 0.115(3) 0.105(3) 0.110(3) -0.083(3) 0.035(2) -0.028(2) C4 0.045(2) 0.049(2) 0.049(2) -0.0133(17) -0.0001(16) -0.0117(17) O4 0.085(2) 0.0463(17) 0.076(2) -0.0048(14) -0.0009(16) -0.0234(15) P2 0.0362(4) 0.0347(4) 0.0469(5) -0.0140(4) 0.0042(4) -0.0102(4) C41 0.0372(18) 0.0333(17) 0.064(2) -0.0133(16) -0.0057(16) -0.0091(14) C42 0.047(2) 0.052(2) 0.075(3) -0.032(2) 0.0021(19) -0.0202(18) C43 0.057(2) 0.068(3) 0.099(3) -0.052(3) -0.002(2) -0.015(2) C44 0.076(3) 0.050(2) 0.129(4) -0.039(3) -0.011(3) -0.024(2) C45 0.072(3) 0.065(3) 0.150(5) -0.044(3) 0.014(3) -0.043(3) C46 0.054(2) 0.052(2) 0.117(4) -0.034(3) 0.017(2) -0.022(2) C51 0.046(2) 0.060(2) 0.050(2) -0.0132(18) 0.0083(17) -0.0151(18) C52 0.078(3) 0.085(4) 0.088(4) 0.014(3) 0.033(3) -0.001(3) C53 0.102(5) 0.125(5) 0.085(4) 0.031(4) 0.030(4) -0.016(4) C54 0.085(4) 0.138(6) 0.075(4) -0.011(4) 0.037(3) -0.024(4) C55 0.083(4) 0.122(5) 0.085(4) -0.025(4) 0.036(3) 0.005(3) C56 0.069(3) 0.078(3) 0.063(3) -0.016(2) 0.025(2) -0.007(2) C61 0.0315(16) 0.0336(16) 0.0480(19) -0.0168(14) 0.0079(14) -0.0081(13) C62 0.048(2) 0.0390(18) 0.051(2) -0.0146(16) 0.0044(16) -0.0191(16) C63 0.048(2) 0.049(2) 0.058(2) -0.0103(18) -0.0083(17) -0.0181(17) C64 0.045(2) 0.0356(19) 0.067(2) -0.0111(17) -0.0005(18) -0.0056(16) C65 0.048(2) 0.0339(18) 0.082(3) -0.0221(18) 0.0035(19) -0.0109(16) C66 0.0394(18) 0.0418(19) 0.068(2) -0.0225(18) -0.0009(17) -0.0118(15) Ag 0.0748(2) 0.03497(17) 0.0903(3) -0.00881(16) -0.00371(19) -0.00452(15) P1 0.0478(5) 0.0350(5) 0.0561(6) -0.0153(4) 0.0014(4) -0.0077(4) C11 0.047(2) 0.0427(19) 0.048(2) -0.0161(16) 0.0032(16) -0.0110(16) C12 0.046(2) 0.050(2) 0.084(3) -0.028(2) 0.002(2) -0.0092(18) C13 0.063(3) 0.060(3) 0.096(3) -0.042(2) 0.003(2) -0.018(2) C14 0.067(3) 0.082(3) 0.078(3) -0.037(3) -0.001(2) -0.031(3) C15 0.048(2) 0.096(4) 0.120(4) -0.056(3) -0.005(3) -0.014(2) C16 0.052(2) 0.066(3) 0.114(4) -0.049(3) -0.006(2) -0.006(2) C21 0.057(2) 0.053(2) 0.059(2) -0.0253(19) 0.0000(19) -0.0110(18) C22 0.169(6) 0.077(4) 0.088(4) -0.036(3) -0.016(4) -0.042(4) C23 0.232(10) 0.110(5) 0.105(5) -0.066(5) -0.023(6) -0.052(6) C24 0.115(5) 0.153(7) 0.083(4) -0.068(5) 0.009(4) -0.029(5) C25 0.175(7) 0.181(7) 0.064(4) -0.041(4) 0.031(4) -0.112(6) C26 0.155(6) 0.123(5) 0.064(3) -0.037(3) 0.026(3) -0.090(5) C31 0.047(2) 0.043(2) 0.070(3) -0.0234(18) 0.0044(18) -0.0157(17) C32 0.066(3) 0.067(3) 0.085(3) -0.039(2) 0.017(2) -0.034(2) C33 0.070(3) 0.106(4) 0.146(5) -0.083(4) 0.048(4) -0.052(3) C34 0.044(3) 0.104(5) 0.220(9) -0.103(6) 0.026(4) -0.026(3) C35 0.060(3) 0.082(4) 0.183(7) -0.042(4) -0.022(4) 0.006(3) C36 0.064(3) 0.069(3) 0.093(4) -0.018(3) -0.001(3) -0.001(2) Cl1 0.464(10) 0.657(14) 0.321(7) -0.155(8) -0.007(7) -0.326(11) Cl2 0.436(10) 0.363(9) 0.376(9) 0.020(7) 0.068(8) 0.019(7) C90 0.29(3) 0.097(10) 0.22(2) -0.046(11) 0.16(2) -0.097(13) C90A 0.20(2) 0.131(17) 0.24(3) -0.127(19) 0.10(2) -0.107(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C4 1.983(4) . y Mo C2 1.989(5) . y Mo C3 2.020(4) . y Mo B5 2.365(4) . y Mo B4 2.384(4) . y Mo B2 2.396(4) . y Mo C1 2.397(3) . y Mo B3 2.397(4) . y Mo P2 2.5774(10) . y C1 B5 1.691(5) . ? C1 B2 1.700(5) . ? C1 B6 1.705(5) . ? C1 B10 1.713(5) . ? B2 B7 1.769(5) . ? B2 B6 1.777(5) . ? B2 B3 1.800(5) . ? B3 H3 1.18(3) . y B3 B7 1.782(6) . ? B3 B8 1.795(5) . ? B3 B4 1.797(5) . ? B3 Ag 2.522(4) . y B4 B9 1.784(6) . ? B4 B8 1.791(6) . ? B4 B5 1.830(5) . ? B5 B10 1.777(6) . ? B5 B9 1.786(6) . ? B6 B10 1.757(6) . ? B6 B7 1.768(5) . ? B6 B11 1.782(6) . ? B7 Ag 3.540(4) . y B7 H7 1.08(4) . y B7 B8 1.761(6) . ? B7 B11 1.784(5) . ? B8 H8 1.14(4) . y B8 B11 1.754(6) . ? B8 B9 1.769(6) . ? B8 Ag 2.589(4) . y B9 B10 1.764(6) . ? B9 B11 1.788(7) . ? B10 B11 1.764(6) . ? C2 O2 1.132(5) . y C3 O3 1.132(5) . y C4 O4 1.145(4) . y P2 C61 1.834(3) . y P2 C51 1.837(4) . y P2 C41 1.837(3) . y C41 C42 1.382(5) . ? C41 C46 1.392(5) . ? C42 C43 1.384(5) . ? C43 C44 1.374(6) . ? C44 C45 1.366(7) . ? C45 C46 1.384(6) . ? C51 C52 1.373(6) . ? C51 C56 1.374(6) . ? C52 C53 1.391(7) . ? C53 C54 1.350(8) . ? C54 C55 1.345(8) . ? C55 C56 1.385(6) . ? C61 C62 1.377(5) . ? C61 C66 1.392(5) . ? C62 C63 1.383(5) . ? C63 C64 1.374(5) . ? C64 C65 1.372(5) . ? C65 C66 1.381(5) . ? Ag H3 2.03(3) . y Ag H8 2.21(4) . y Ag B7 3.338(4) 2_566 y Ag H7 2.29(4) 2_566 y Ag H7 3.75(3) . y Ag P1 2.3724(11) . y P1 C21 1.813(4) . y P1 C31 1.815(4) . y P1 C11 1.817(4) . y C11 C16 1.377(5) . ? C11 C12 1.377(5) . ? C12 C13 1.380(6) . ? C13 C14 1.361(6) . ? C14 C15 1.368(6) . ? C15 C16 1.382(6) . ? C21 C22 1.363(6) . ? C21 C26 1.373(6) . ? C22 C23 1.394(9) . ? C23 C24 1.326(9) . ? C24 C25 1.337(9) . ? C25 C26 1.383(7) . ? C31 C36 1.372(6) . ? C31 C32 1.392(6) . ? C32 C33 1.370(7) . ? C33 C34 1.352(9) . ? C34 C35 1.373(10) . ? C35 C36 1.390(7) . ? Cl1 C90 1.609(15) . ? Cl1 C90A 1.68(2) . ? Cl2 C90A 1.457(19) . ? Cl2 C90 1.88(2) . ? 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 C4 Mo C2 76.16(16) . . y C4 Mo C3 111.89(16) . . y C2 Mo C3 75.08(18) . . y C4 Mo B5 135.74(14) . . y C2 Mo B5 78.35(17) . . y C3 Mo B5 95.43(16) . . y C4 Mo B4 93.12(14) . . y C2 Mo B4 75.45(17) . . y C3 Mo B4 134.86(16) . . y B5 Mo B4 45.31(13) . . ? C4 Mo B2 115.71(14) . . y C2 Mo B2 148.10(16) . . y C3 Mo B2 121.10(15) . . y B5 Mo B2 73.10(14) . . ? B4 Mo B2 74.44(14) . . ? C4 Mo C1 154.92(13) . . y C2 Mo C1 117.66(15) . . y C3 Mo C1 92.49(15) . . y B5 Mo C1 41.59(13) . . ? B4 Mo C1 72.22(13) . . ? B2 Mo C1 41.54(11) . . ? C4 Mo B3 83.54(14) . . y C2 Mo B3 114.60(16) . . y C3 Mo B3 163.91(15) . . y B5 Mo B3 75.04(13) . . ? B4 Mo B3 44.14(13) . . ? B2 Mo B3 44.10(12) . . ? C1 Mo B3 71.73(12) . . ? C4 Mo P2 76.71(11) . . y C2 Mo P2 129.26(13) . . y C3 Mo P2 76.53(12) . . y B5 Mo P2 145.65(10) . . ? B4 Mo P2 147.83(10) . . ? B2 Mo P2 82.59(9) . . ? C1 Mo P2 104.69(8) . . ? B3 Mo P2 103.88(9) . . ? B5 C1 B2 113.5(3) . . ? B5 C1 B6 114.3(3) . . ? B2 C1 B6 62.9(2) . . ? B5 C1 B10 63.0(2) . . ? B2 C1 B10 113.5(3) . . ? B6 C1 B10 61.9(2) . . ? B5 C1 Mo 68.21(18) . . ? B2 C1 Mo 69.22(17) . . ? B6 C1 Mo 128.3(2) . . ? B10 C1 Mo 127.2(2) . . ? C1 B2 B7 105.1(3) . . ? C1 B2 B6 58.7(2) . . ? B7 B2 B6 59.8(2) . . ? C1 B2 B3 106.7(3) . . ? B7 B2 B3 59.9(2) . . ? B6 B2 B3 108.5(3) . . ? C1 B2 Mo 69.24(17) . . ? B7 B2 Mo 123.2(2) . . ? B6 B2 Mo 124.4(2) . . ? B3 B2 Mo 67.97(17) . . ? B7 B3 B8 59.0(2) . . ? B7 B3 B4 107.3(3) . . ? B8 B3 B4 59.8(2) . . ? B7 B3 B2 59.2(2) . . ? B8 B3 B2 105.7(3) . . ? B4 B3 B2 107.1(2) . . ? B7 B3 Mo 122.6(2) . . ? B8 B3 Mo 122.2(2) . . ? B4 B3 Mo 67.56(18) . . ? B2 B3 Mo 67.93(17) . . ? B7 B3 Ag 109.5(2) . . ? B8 B3 Ag 71.44(17) . . ? B4 B3 Ag 83.74(19) . . ? B2 B3 Ag 165.9(2) . . ? Mo B3 Ag 125.61(16) . . y B9 B4 B8 59.3(2) . . ? B9 B4 B3 107.6(3) . . ? B8 B4 B3 60.0(2) . . ? B9 B4 B5 59.2(2) . . ? B8 B4 B5 105.6(3) . . ? B3 B4 B5 106.2(3) . . ? B9 B4 Mo 122.1(2) . . ? B8 B4 Mo 123.1(2) . . ? B3 B4 Mo 68.31(17) . . ? B5 B4 Mo 66.79(18) . . ? C1 B5 B10 59.1(2) . . ? C1 B5 B9 105.1(3) . . ? B10 B5 B9 59.3(2) . . ? C1 B5 B4 106.3(3) . . ? B10 B5 B4 107.2(3) . . ? B9 B5 B4 59.1(2) . . ? C1 B5 Mo 70.20(17) . . ? B10 B5 Mo 125.5(2) . . ? B9 B5 Mo 123.0(2) . . ? B4 B5 Mo 67.90(18) . . ? C1 B6 B10 59.3(2) . . ? C1 B6 B7 104.9(3) . . ? B10 B6 B7 107.7(3) . . ? C1 B6 B2 58.4(2) . . ? B10 B6 B2 107.7(3) . . ? B7 B6 B2 59.9(2) . . ? C1 B6 B11 105.7(3) . . ? B10 B6 B11 59.8(2) . . ? B7 B6 B11 60.4(2) . . ? B2 B6 B11 108.3(3) . . ? B8 B7 B6 107.8(3) . . ? B8 B7 B2 108.5(3) . . ? B6 B7 B2 60.3(2) . . ? B8 B7 B3 60.9(2) . . ? B6 B7 B3 109.8(3) . . ? B2 B7 B3 60.9(2) . . ? B8 B7 B11 59.3(2) . . ? B6 B7 B11 60.2(2) . . ? B2 B7 B11 108.6(3) . . ? B3 B7 B11 109.3(3) . . ? B11 B8 B7 61.0(2) . . ? B11 B8 B9 61.0(2) . . ? B7 B8 B9 108.6(3) . . ? B11 B8 B4 110.1(3) . . ? B7 B8 B4 108.5(3) . . ? B9 B8 B4 60.1(2) . . ? B11 B8 B3 110.1(3) . . ? B7 B8 B3 60.1(2) . . ? B9 B8 B3 108.3(3) . . ? B4 B8 B3 60.1(2) . . ? B11 B8 Ag 165.0(3) . . ? B7 B8 Ag 107.4(2) . . ? B9 B8 Ag 134.0(3) . . ? B4 B8 Ag 81.9(2) . . ? B3 B8 Ag 67.47(17) . . ? B10 B9 B8 106.9(3) . . ? B10 B9 B4 109.9(3) . . ? B8 B9 B4 60.5(2) . . ? B10 B9 B5 60.1(2) . . ? B8 B9 B5 108.4(3) . . ? B4 B9 B5 61.7(2) . . ? B10 B9 B11 59.5(2) . . ? B8 B9 B11 59.1(2) . . ? B4 B9 B11 108.9(3) . . ? B5 B9 B11 107.9(3) . . ? C1 B10 B6 58.8(2) . . ? C1 B10 B11 106.2(3) . . ? B6 B10 B11 60.8(2) . . ? C1 B10 B9 105.1(3) . . ? B6 B10 B9 109.0(3) . . ? B11 B10 B9 60.9(2) . . ? C1 B10 B5 57.9(2) . . ? B6 B10 B5 107.6(3) . . ? B11 B10 B5 109.4(3) . . ? B9 B10 B5 60.6(2) . . ? B8 B11 B10 107.6(3) . . ? B8 B11 B6 107.4(3) . . ? B10 B11 B6 59.4(2) . . ? B8 B11 B7 59.7(2) . . ? B10 B11 B7 106.7(3) . . ? B6 B11 B7 59.4(2) . . ? B8 B11 B9 59.9(2) . . ? B10 B11 B9 59.6(2) . . ? B6 B11 B9 106.8(3) . . ? B7 B11 B9 106.8(3) . . ? O2 C2 Mo 179.5(5) . . y O3 C3 Mo 174.8(4) . . y O4 C4 Mo 173.5(3) . . y C61 P2 C51 100.41(16) . . ? C61 P2 C41 104.74(15) . . ? C51 P2 C41 103.37(18) . . ? C61 P2 Mo 117.57(11) . . ? C51 P2 Mo 113.12(13) . . ? C41 P2 Mo 115.63(11) . . ? C42 C41 C46 118.5(3) . . ? C42 C41 P2 119.0(3) . . ? C46 C41 P2 122.5(3) . . ? C41 C42 C43 121.5(4) . . ? C44 C43 C42 119.4(4) . . ? C45 C44 C43 119.7(4) . . ? C44 C45 C46 121.4(4) . . ? C45 C46 C41 119.5(4) . . ? C52 C51 C56 117.5(4) . . ? C52 C51 P2 120.6(3) . . ? C56 C51 P2 121.9(3) . . ? C51 C52 C53 121.1(5) . . ? C54 C53 C52 120.2(5) . . ? C55 C54 C53 119.5(5) . . ? C54 C55 C56 121.0(5) . . ? C51 C56 C55 120.6(5) . . ? C62 C61 C66 118.8(3) . . ? C62 C61 P2 121.0(2) . . ? C66 C61 P2 119.7(3) . . ? C61 C62 C63 120.7(3) . . ? C64 C63 C62 120.1(3) . . ? C65 C64 C63 119.9(3) . . ? C64 C65 C66 120.3(3) . . ? C65 C66 C61 120.2(3) . . ? H3 Ag H8 89.3(14) . . y H3 Ag P1 130.4(10) . . y H8 Ag P1 139.5(10) . . y H3 Ag B3 27.4(10) . . ? H8 Ag B3 66.3(10) . . ? P1 Ag B3 147.37(10) . . ? H3 Ag B8 66.5(10) . . ? H8 Ag B8 26.0(10) . . ? P1 Ag B8 155.26(10) . . ? B3 Ag B8 41.09(12) . . ? C21 P1 C31 105.81(19) . . ? C21 P1 C11 104.96(18) . . ? C31 P1 C11 104.94(16) . . ? C21 P1 Ag 114.67(13) . . y C31 P1 Ag 113.41(13) . . y C11 P1 Ag 112.18(12) . . y C16 C11 C12 118.4(4) . . ? C16 C11 P1 117.9(3) . . ? C12 C11 P1 123.6(3) . . ? C11 C12 C13 120.7(4) . . ? C14 C13 C12 120.2(4) . . ? C13 C14 C15 120.1(4) . . ? C14 C15 C16 119.8(4) . . ? C11 C16 C15 120.7(4) . . ? C22 C21 C26 116.9(5) . . ? C22 C21 P1 119.1(4) . . ? C26 C21 P1 124.0(3) . . ? C21 C22 C23 120.4(6) . . ? C24 C23 C22 120.9(6) . . ? C23 C24 C25 120.5(6) . . ? C24 C25 C26 119.4(7) . . ? C21 C26 C25 121.9(5) . . ? C36 C31 C32 119.9(4) . . ? C36 C31 P1 123.2(3) . . ? C32 C31 P1 116.9(3) . . ? C33 C32 C31 119.6(5) . . ? C34 C33 C32 120.5(6) . . ? C33 C34 C35 120.9(5) . . ? C34 C35 C36 119.5(6) . . ? C31 C36 C35 119.6(6) . . ? C90 Cl1 C90A 56.3(10) . . ? C90A Cl2 C90 53.5(11) . . ? Cl1 C90 Cl2 94.5(9) . . ? Cl2 C90A Cl1 110.1(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.908 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.061 #===END data_12a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H70 B10 Cl3 Mo O3 P3 Ru' _chemical_formula_weight 1391.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1520(18) _cell_length_b 13.811(3) _cell_length_c 21.962(4) _cell_angle_alpha 105.442(9) _cell_angle_beta 95.010(14) _cell_angle_gamma 93.19(2) _cell_volume 3237.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 177 _cell_measurement_theta_min 5 _cell_measurement_theta_max 50 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.9239 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_special_details ; Unit cell dimensions were determined from reflections taken from four sets of 30 frames (at 0.3\% steps in \w) each at 10 seconds exposure, for which all strong reflections in the complete data set were used. A sphere of reciprocal space was scanned by 0.3\% \w steps at three different \f angles. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analyzing the duplicate reflections; no decay was observed. ; _diffrn_ambient_temperature 173(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 'SMART CCD Detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 60 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33811 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14646 _reflns_number_gt 11870 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995)' _computing_publication_material 'SHELXTL (Siemens, 1995)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14646 _refine_ls_number_parameters 823 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.004 _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 Mo Mo 1.180300(15) -0.698475(12) -0.345008(7) 0.02013(5) Uani 1 1 d . . . C3 C 1.25364(19) -0.62426(16) -0.40194(9) 0.0285(4) Uani 1 1 d . . . O3 O 1.29168(15) -0.57875(13) -0.43342(7) 0.0424(4) Uani 1 1 d . . . C4 C 1.0377(2) -0.65489(16) -0.38891(10) 0.0295(5) Uani 1 1 d . . . O4 O 0.95400(15) -0.63051(13) -0.41252(8) 0.0433(4) Uani 1 1 d . . . C5 C 1.06678(19) -0.82508(16) -0.37933(10) 0.0306(5) Uani 1 1 d . . . O5 O 0.99719(15) -0.89239(12) -0.39651(8) 0.0452(4) Uani 1 1 d . . . P2 P 1.31152(5) -0.82603(4) -0.40951(2) 0.02445(11) Uani 1 1 d . . . C41 C 1.47515(19) -0.80331(16) -0.38737(9) 0.0289(5) Uani 1 1 d . . . C42 C 1.5315(2) -0.70698(18) -0.37683(11) 0.0398(6) Uani 1 1 d . . . H42 H 1.4846 -0.6530 -0.3803 0.048 Uiso 1 1 calc R . . C43 C 1.6556(2) -0.6890(2) -0.36125(13) 0.0485(7) Uani 1 1 d . . . H43 H 1.6928 -0.6228 -0.3538 0.058 Uiso 1 1 calc R . . C44 C 1.7247(2) -0.7663(2) -0.35657(13) 0.0523(7) Uani 1 1 d . . . H44 H 1.8095 -0.7534 -0.3454 0.063 Uiso 1 1 calc R . . C45 C 1.6711(2) -0.8628(2) -0.36811(15) 0.0567(7) Uani 1 1 d . . . H45 H 1.7191 -0.9165 -0.3654 0.068 Uiso 1 1 calc R . . C46 C 1.5466(2) -0.8814(2) -0.38370(13) 0.0456(6) Uani 1 1 d . . . H46 H 1.5101 -0.9481 -0.3919 0.055 Uiso 1 1 calc R . . C51 C 1.28033(19) -0.95600(15) -0.40648(10) 0.0286(4) Uani 1 1 d . . . C52 C 1.2525(3) -1.03485(19) -0.46070(12) 0.0505(7) Uani 1 1 d . . . H52 H 1.2472 -1.0224 -0.5013 0.061 Uiso 1 1 calc R . . C53 C 1.2320(3) -1.1330(2) -0.45565(15) 0.0716(10) Uani 1 1 d . . . H53 H 1.2116 -1.1869 -0.4930 0.086 Uiso 1 1 calc R . . C54 C 1.2411(3) -1.1522(2) -0.39769(15) 0.0610(8) Uani 1 1 d . . . H54 H 1.2283 -1.2194 -0.3948 0.073 Uiso 1 1 calc R . . C55 C 1.2687(2) -1.07435(19) -0.34344(13) 0.0463(6) Uani 1 1 d . . . H55 H 1.2751 -1.0874 -0.3030 0.056 Uiso 1 1 calc R . . C56 C 1.2870(2) -0.97744(17) -0.34804(11) 0.0400(6) Uani 1 1 d . . . H56 H 1.3046 -0.9238 -0.3103 0.048 Uiso 1 1 calc R . . C61 C 1.2940(2) -0.83645(16) -0.49501(10) 0.0313(5) Uani 1 1 d . . . C62 C 1.3931(2) -0.84447(18) -0.53010(11) 0.0422(6) Uani 1 1 d . . . H62 H 1.4723 -0.8421 -0.5097 0.051 Uiso 1 1 calc R . . C63 C 1.3752(3) -0.8559(2) -0.59516(12) 0.0558(8) Uani 1 1 d . . . H63 H 1.4426 -0.8607 -0.6191 0.067 Uiso 1 1 calc R . . C64 C 1.2597(3) -0.8604(2) -0.62547(12) 0.0587(8) Uani 1 1 d . . . H64 H 1.2480 -0.8682 -0.6699 0.070 Uiso 1 1 calc R . . C65 C 1.1623(3) -0.8535(2) -0.59074(12) 0.0572(8) Uani 1 1 d . . . H65 H 1.0830 -0.8577 -0.6115 0.069 Uiso 1 1 calc R . . C66 C 1.1788(2) -0.8407(2) -0.52590(11) 0.0448(6) Uani 1 1 d . . . H66 H 1.1109 -0.8347 -0.5023 0.054 Uiso 1 1 calc R . . C1 C 1.30361(19) -0.71272(15) -0.25206(9) 0.0274(4) Uani 1 1 d . . . H1 H 1.3642 -0.7732 -0.2710 0.033 Uiso 1 1 calc R . . B2 B 1.3304(2) -0.59738(16) -0.26557(10) 0.0213(4) Uani 1 1 d . . . H2 H 1.4053 -0.5763 -0.2916 0.026 Uiso 1 1 calc R . . B3 B 1.18357(19) -0.54772(16) -0.26589(9) 0.0191(4) Uani 1 1 d . . . H3 H 1.1644(18) -0.4750(15) -0.2828(9) 0.023 Uiso 1 1 d . . . B4 B 1.0706(2) -0.63995(16) -0.25584(10) 0.0224(4) Uani 1 1 d . . . H4 H 0.9728 -0.6463 -0.2743 0.027 Uiso 1 1 calc R . . B5 B 1.1543(2) -0.74383(17) -0.24832(10) 0.0246(5) Uani 1 1 d . . . H5 H 1.1127 -0.8234 -0.2640 0.030 Uiso 1 1 calc R . . B6 B 1.3667(2) -0.61677(18) -0.18809(10) 0.0248(5) Uani 1 1 d . . . H6 H 1.4624 -0.6095 -0.1661 0.030 Uiso 1 1 calc R . . B7 B 1.28779(19) -0.51428(16) -0.19615(10) 0.0200(4) Uani 1 1 d . . . H7 H 1.3250(18) -0.4328(16) -0.1805(9) 0.024 Uiso 1 1 d . . . B8 B 1.13640(19) -0.53957(16) -0.19066(10) 0.0198(4) Uani 1 1 d . . . H8 H 1.0805(18) -0.4607(15) -0.1690(9) 0.024 Uiso 1 1 d . . . B9 B 1.1112(2) -0.65951(17) -0.17876(10) 0.0258(5) Uani 1 1 d . . . H9 H 1.0396 -0.6797 -0.1505 0.031 Uiso 1 1 calc R . . B10 B 1.2561(2) -0.70867(18) -0.17878(11) 0.0284(5) Uani 1 1 d . . . H10 H 1.2798 -0.7634 -0.1509 0.034 Uiso 1 1 calc R . . B11 B 1.2444(2) -0.58025(17) -0.14151(10) 0.0242(5) Uani 1 1 d . . . H11 H 1.2595 -0.5481 -0.0887 0.029 Uiso 1 1 calc R . . Ru Ru 1.166830(13) -0.377265(11) -0.197188(7) 0.01722(4) Uani 1 1 d . . . Cl1 Cl 1.29653(4) -0.27188(4) -0.23843(2) 0.02816(11) Uani 1 1 d . . . P1 P 1.18991(5) -0.27262(4) -0.09534(2) 0.02280(11) Uani 1 1 d . . . C11 C 1.05911(19) -0.27436(18) -0.05053(9) 0.0317(5) Uani 1 1 d . . . C12 C 1.0144(2) -0.1859(2) -0.01691(10) 0.0419(6) Uani 1 1 d . . . H12 H 1.0516 -0.1224 -0.0170 0.050 Uiso 1 1 calc R . . C13 C 0.9153(2) -0.1905(3) 0.01683(11) 0.0565(8) Uani 1 1 d . . . H13 H 0.8846 -0.1298 0.0393 0.068 Uiso 1 1 calc R . . C14 C 0.8618(2) -0.2807(3) 0.01805(11) 0.0617(9) Uani 1 1 d . . . H14 H 0.7946 -0.2826 0.0416 0.074 Uiso 1 1 calc R . . C15 C 0.9044(2) -0.3693(3) -0.01468(11) 0.0588(8) Uani 1 1 d . . . H15 H 0.8665 -0.4321 -0.0138 0.071 Uiso 1 1 calc R . . C16 C 1.0037(2) -0.3667(2) -0.04938(10) 0.0439(6) Uani 1 1 d . . . H16 H 1.0331 -0.4278 -0.0720 0.053 Uiso 1 1 calc R . . C21 C 1.24548(19) -0.13885(16) -0.07550(11) 0.0334(5) Uani 1 1 d . . . C22 C 1.2954(3) -0.0908(2) -0.01335(14) 0.0576(8) Uani 1 1 d . . . H22 H 1.2955 -0.1264 0.0181 0.069 Uiso 1 1 calc R . . C23 C 1.3446(3) 0.0079(2) 0.00285(18) 0.0804(12) Uani 1 1 d . . . H23 H 1.3772 0.0399 0.0454 0.096 Uiso 1 1 calc R . . C24 C 1.3465(3) 0.0603(2) -0.0433(2) 0.0751(11) Uani 1 1 d . . . H24 H 1.3827 0.1274 -0.0326 0.090 Uiso 1 1 calc R . . C25 C 1.2963(2) 0.01481(19) -0.10356(16) 0.0560(8) Uani 1 1 d . . . H25 H 1.2957 0.0511 -0.1348 0.067 Uiso 1 1 calc R . . C26 C 1.2455(2) -0.08442(17) -0.12001(13) 0.0398(6) Uani 1 1 d . . . H26 H 1.2106 -0.1150 -0.1623 0.048 Uiso 1 1 calc R . . C31 C 1.30928(19) -0.31514(16) -0.04786(9) 0.0289(5) Uani 1 1 d . . . C32 C 1.4257(2) -0.31033(17) -0.06653(10) 0.0349(5) Uani 1 1 d . . . H32 H 1.4392 -0.2876 -0.1027 0.042 Uiso 1 1 calc R . . C33 C 1.5218(2) -0.33869(19) -0.03230(12) 0.0447(6) Uani 1 1 d . . . H33 H 1.6006 -0.3357 -0.0453 0.054 Uiso 1 1 calc R . . C34 C 1.5030(3) -0.3712(2) 0.02057(12) 0.0554(8) Uani 1 1 d . . . H34 H 1.5690 -0.3898 0.0442 0.066 Uiso 1 1 calc R . . C35 C 1.3896(3) -0.3766(2) 0.03900(12) 0.0537(7) Uani 1 1 d . . . H35 H 1.3771 -0.4002 0.0750 0.064 Uiso 1 1 calc R . . C36 C 1.2916(2) -0.34773(19) 0.00546(10) 0.0414(6) Uani 1 1 d . . . H36 H 1.2133 -0.3505 0.0192 0.050 Uiso 1 1 calc R . . P3 P 0.99233(4) -0.31961(4) -0.23195(2) 0.02011(10) Uani 1 1 d . . . C71 C 0.96435(18) -0.36043(15) -0.31938(9) 0.0239(4) Uani 1 1 d . . . C72 C 1.0606(2) -0.36084(16) -0.35585(9) 0.0290(5) Uani 1 1 d . . . H72 H 1.1408 -0.3451 -0.3356 0.035 Uiso 1 1 calc R . . C73 C 1.0402(2) -0.38414(16) -0.42180(10) 0.0335(5) Uani 1 1 d . . . H73 H 1.1064 -0.3831 -0.4462 0.040 Uiso 1 1 calc R . . C74 C 0.9245(2) -0.40865(18) -0.45186(10) 0.0375(5) Uani 1 1 d . . . H74 H 0.9107 -0.4240 -0.4968 0.045 Uiso 1 1 calc R . . C75 C 0.8293(2) -0.4108(2) -0.41647(10) 0.0452(6) Uani 1 1 d . . . H75 H 0.7497 -0.4290 -0.4372 0.054 Uiso 1 1 calc R . . C76 C 0.8485(2) -0.38654(19) -0.35046(10) 0.0371(5) Uani 1 1 d . . . H76 H 0.7818 -0.3879 -0.3265 0.045 Uiso 1 1 calc R . . C81 C 0.84773(17) -0.36041(16) -0.20919(9) 0.0242(4) Uani 1 1 d . . . C82 C 0.74807(19) -0.30288(18) -0.20966(10) 0.0356(5) Uani 1 1 d . . . H82 H 0.7578 -0.2385 -0.2174 0.043 Uiso 1 1 calc R . . C83 C 0.6354(2) -0.3390(2) -0.19897(12) 0.0422(6) Uani 1 1 d . . . H83 H 0.5686 -0.2991 -0.1990 0.051 Uiso 1 1 calc R . . C84 C 0.6205(2) -0.4318(2) -0.18841(11) 0.0443(6) Uani 1 1 d . . . H84 H 0.5434 -0.4561 -0.1807 0.053 Uiso 1 1 calc R . . C85 C 0.7169(2) -0.4906(2) -0.18885(12) 0.0425(6) Uani 1 1 d . . . H85 H 0.7058 -0.5556 -0.1822 0.051 Uiso 1 1 calc R . . C86 C 0.83025(19) -0.45458(17) -0.19909(10) 0.0324(5) Uani 1 1 d . . . H86 H 0.8964 -0.4951 -0.1991 0.039 Uiso 1 1 calc R . . C91 C 0.98606(18) -0.18314(15) -0.21509(9) 0.0261(4) Uani 1 1 d . . . C92 C 0.9470(2) -0.12763(17) -0.15830(10) 0.0331(5) Uani 1 1 d . . . H92 H 0.9203 -0.1616 -0.1290 0.040 Uiso 1 1 calc R . . C93 C 0.9470(2) -0.02364(18) -0.14431(12) 0.0441(6) Uani 1 1 d . . . H93 H 0.9189 0.0129 -0.1059 0.053 Uiso 1 1 calc R . . C94 C 0.9873(3) 0.02687(19) -0.18569(13) 0.0486(7) Uani 1 1 d . . . H94 H 0.9884 0.0982 -0.1756 0.058 Uiso 1 1 calc R . . C95 C 1.0266(3) -0.02716(18) -0.24270(12) 0.0448(6) Uani 1 1 d . . . H95 H 1.0538 0.0073 -0.2717 0.054 Uiso 1 1 calc R . . C96 C 1.0258(2) -0.13095(16) -0.25678(10) 0.0335(5) Uani 1 1 d . . . H96 H 1.0529 -0.1673 -0.2956 0.040 Uiso 1 1 calc R . . C7 C 1.4153(9) -0.3563(7) -0.3855(4) 0.068(3) Uani 0.50 1 d PD A 1 H7A H 1.3399 -0.3812 -0.3719 0.082 Uiso 0.50 1 calc PR A 1 H7B H 1.4341 -0.2849 -0.3610 0.082 Uiso 0.50 1 calc PR A 1 Cl4 Cl 1.3916(5) -0.3630(4) -0.46590(15) 0.0840(11) Uani 0.50 1 d PD A 1 Cl5 Cl 1.53223(16) -0.4262(2) -0.36782(11) 0.0824(6) Uani 0.50 1 d PD A 1 C101 C 1.2335(4) -0.2285(4) 0.1792(2) 0.0577(12) Uani 0.750(8) 1 d PD B 1 C102 C 1.3740(6) -0.1952(5) 0.1983(3) 0.108(3) Uani 0.750(8) 1 d PD B 1 C103 C 1.4336(8) -0.1258(7) 0.1790(4) 0.138(3) Uani 0.750(8) 1 d PD B 1 C104 C 1.4263(11) -0.0307(6) 0.2200(4) 0.176(5) Uani 0.750(8) 1 d PD B 1 C105 C 1.4393(8) 0.0801(4) 0.2151(4) 0.096(3) Uani 0.750(8) 1 d PD B 1 C7' C 1.4880(6) -0.4003(6) -0.4459(3) 0.074(2) Uani 0.50 1 d PD C 2 H7'A H 1.5632 -0.3641 -0.4520 0.089 Uiso 0.50 1 calc PR C 2 H7'B H 1.4974 -0.4735 -0.4601 0.089 Uiso 0.50 1 calc PR C 2 Cl4' Cl 1.3700(4) -0.3724(3) -0.49085(14) 0.0706(8) Uani 0.50 1 d PD C 2 Cl5' Cl 1.4664(4) -0.3664(3) -0.36504(15) 0.1189(15) Uani 0.50 1 d PD C 2 C106 C 1.2586(13) -0.1941(12) 0.1693(6) 0.045(3) Uiso 0.250(8) 1 d PD B 2 C107 C 1.331(2) -0.116(2) 0.1760(12) 0.149(10) Uiso 0.250(8) 1 d PD B 2 C108 C 1.4117(17) -0.0782(15) 0.2214(9) 0.073(5) Uiso 0.250(8) 1 d PD B 2 C109 C 1.3974(14) -0.0306(11) 0.1793(8) 0.075(5) Uiso 0.250(8) 1 d PD B 2 C110 C 1.4563(19) 0.0561(14) 0.2173(9) 0.058(5) Uiso 0.250(8) 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.02249(9) 0.01741(9) 0.01988(8) 0.00363(6) 0.00291(6) 0.00258(7) C3 0.0308(11) 0.0266(11) 0.0273(10) 0.0066(9) 0.0013(8) 0.0030(9) O3 0.0468(10) 0.0464(10) 0.0395(9) 0.0241(8) 0.0015(8) -0.0055(8) C4 0.0328(12) 0.0280(11) 0.0275(10) 0.0081(9) 0.0021(9) 0.0011(9) O4 0.0355(9) 0.0493(11) 0.0491(10) 0.0220(8) -0.0038(8) 0.0081(8) C5 0.0272(11) 0.0277(12) 0.0359(11) 0.0054(9) 0.0057(9) 0.0052(9) O5 0.0343(9) 0.0308(9) 0.0626(11) 0.0012(8) 0.0031(8) -0.0060(8) P2 0.0264(3) 0.0204(3) 0.0249(2) 0.0025(2) 0.0058(2) 0.0018(2) C41 0.0273(11) 0.0303(12) 0.0270(10) 0.0025(9) 0.0082(8) 0.0020(9) C42 0.0314(13) 0.0307(13) 0.0546(15) 0.0038(11) 0.0154(11) 0.0023(10) C43 0.0329(13) 0.0400(15) 0.0625(16) -0.0052(12) 0.0173(12) -0.0076(11) C44 0.0265(13) 0.0618(19) 0.0627(17) 0.0075(14) 0.0052(12) -0.0007(13) C45 0.0314(14) 0.0551(18) 0.087(2) 0.0257(16) 0.0035(14) 0.0081(13) C46 0.0341(13) 0.0368(14) 0.0670(17) 0.0173(12) 0.0022(12) 0.0016(11) C51 0.0247(11) 0.0206(10) 0.0397(12) 0.0045(9) 0.0097(9) 0.0027(8) C52 0.072(2) 0.0290(13) 0.0441(14) 0.0028(11) -0.0013(13) -0.0032(13) C53 0.111(3) 0.0277(15) 0.0621(19) -0.0023(13) -0.0067(18) -0.0136(16) C54 0.075(2) 0.0274(14) 0.084(2) 0.0177(14) 0.0207(17) -0.0042(14) C55 0.0592(17) 0.0333(14) 0.0530(15) 0.0179(12) 0.0211(13) 0.0062(12) C56 0.0537(16) 0.0264(12) 0.0401(13) 0.0067(10) 0.0138(11) 0.0024(11) C61 0.0441(13) 0.0215(11) 0.0256(10) 0.0009(8) 0.0063(9) 0.0032(9) C62 0.0540(16) 0.0381(14) 0.0331(12) 0.0063(10) 0.0126(11) -0.0032(12) C63 0.084(2) 0.0503(17) 0.0363(14) 0.0108(12) 0.0265(14) 0.0038(15) C64 0.100(3) 0.0489(17) 0.0279(13) 0.0100(12) 0.0062(14) 0.0172(17) C65 0.076(2) 0.0582(19) 0.0321(13) 0.0029(12) -0.0051(13) 0.0263(16) C66 0.0521(16) 0.0495(16) 0.0291(12) 0.0019(11) 0.0031(11) 0.0167(12) C1 0.0317(11) 0.0259(11) 0.0266(10) 0.0091(8) 0.0038(8) 0.0090(9) B2 0.0215(11) 0.0207(11) 0.0221(10) 0.0056(9) 0.0025(8) 0.0047(9) B3 0.0190(11) 0.0183(11) 0.0198(10) 0.0049(8) 0.0017(8) 0.0021(8) B4 0.0234(11) 0.0203(11) 0.0229(10) 0.0046(9) 0.0048(8) -0.0011(9) B5 0.0318(13) 0.0195(11) 0.0239(11) 0.0076(9) 0.0056(9) 0.0023(9) B6 0.0264(12) 0.0258(12) 0.0228(11) 0.0070(9) 0.0016(9) 0.0071(9) B7 0.0184(10) 0.0199(11) 0.0210(10) 0.0047(8) 0.0010(8) 0.0015(8) B8 0.0187(10) 0.0202(11) 0.0199(10) 0.0044(8) 0.0023(8) 0.0013(8) B9 0.0301(12) 0.0235(12) 0.0250(11) 0.0082(9) 0.0059(9) 0.0003(10) B10 0.0370(14) 0.0256(12) 0.0258(11) 0.0111(10) 0.0053(10) 0.0074(10) B11 0.0266(12) 0.0253(12) 0.0226(11) 0.0088(9) 0.0036(9) 0.0052(9) Ru 0.01536(8) 0.01674(8) 0.01917(8) 0.00375(6) 0.00312(5) 0.00169(6) Cl1 0.0249(2) 0.0250(3) 0.0362(3) 0.0099(2) 0.0088(2) -0.0013(2) P1 0.0187(2) 0.0231(3) 0.0228(2) -0.0002(2) 0.00155(19) 0.0023(2) C11 0.0225(11) 0.0494(14) 0.0183(9) 0.0009(9) 0.0013(8) 0.0039(10) C12 0.0337(13) 0.0597(17) 0.0271(11) 0.0005(11) 0.0037(9) 0.0150(12) C13 0.0370(15) 0.095(3) 0.0320(13) 0.0020(14) 0.0100(11) 0.0262(16) C14 0.0299(14) 0.124(3) 0.0260(12) 0.0088(15) 0.0099(10) 0.0085(17) C15 0.0463(16) 0.095(2) 0.0301(13) 0.0116(14) 0.0092(11) -0.0191(16) C16 0.0385(14) 0.0597(17) 0.0270(11) 0.0009(11) 0.0104(10) -0.0077(12) C21 0.0213(11) 0.0240(11) 0.0455(13) -0.0061(10) -0.0005(9) 0.0048(9) C22 0.0556(18) 0.0354(15) 0.0629(17) -0.0113(13) -0.0231(14) 0.0098(13) C23 0.059(2) 0.0396(18) 0.106(3) -0.0290(18) -0.0392(19) 0.0083(15) C24 0.0355(16) 0.0244(14) 0.144(3) -0.0092(18) -0.0083(18) 0.0019(12) C25 0.0358(15) 0.0277(14) 0.101(2) 0.0078(14) 0.0191(15) 0.0033(11) C26 0.0273(12) 0.0253(12) 0.0627(16) 0.0017(11) 0.0146(11) 0.0028(9) C31 0.0286(11) 0.0275(11) 0.0242(10) -0.0022(8) -0.0039(8) 0.0044(9) C32 0.0287(12) 0.0344(13) 0.0325(11) -0.0046(9) -0.0049(9) 0.0045(10) C33 0.0284(12) 0.0472(15) 0.0454(14) -0.0075(11) -0.0092(10) 0.0102(11) C34 0.0550(18) 0.0545(18) 0.0453(15) 0.0001(13) -0.0238(13) 0.0194(14) C35 0.066(2) 0.0608(19) 0.0333(13) 0.0144(12) -0.0107(12) 0.0128(15) C36 0.0431(14) 0.0495(15) 0.0275(11) 0.0053(10) -0.0024(10) 0.0040(12) P3 0.0191(2) 0.0213(3) 0.0214(2) 0.00720(19) 0.00452(18) 0.00412(19) C71 0.0279(11) 0.0229(10) 0.0223(9) 0.0077(8) 0.0026(8) 0.0064(8) C72 0.0341(12) 0.0261(11) 0.0269(10) 0.0073(8) 0.0046(9) 0.0007(9) C73 0.0460(14) 0.0300(12) 0.0259(10) 0.0074(9) 0.0110(10) 0.0048(10) C74 0.0512(15) 0.0382(13) 0.0230(10) 0.0064(9) 0.0016(10) 0.0148(11) C75 0.0368(14) 0.0652(18) 0.0290(12) 0.0054(11) -0.0055(10) 0.0150(12) C76 0.0302(12) 0.0512(15) 0.0298(11) 0.0087(10) 0.0036(9) 0.0125(11) C81 0.0178(10) 0.0331(11) 0.0218(9) 0.0075(8) 0.0036(7) 0.0019(8) C82 0.0253(11) 0.0411(14) 0.0431(13) 0.0143(11) 0.0070(9) 0.0071(10) C83 0.0215(11) 0.0543(16) 0.0513(14) 0.0119(12) 0.0097(10) 0.0097(11) C84 0.0216(12) 0.0593(18) 0.0491(14) 0.0099(13) 0.0096(10) -0.0055(11) C85 0.0289(12) 0.0448(15) 0.0566(15) 0.0194(12) 0.0081(11) -0.0055(11) C86 0.0221(11) 0.0361(13) 0.0403(12) 0.0129(10) 0.0034(9) 0.0008(9) C91 0.0254(11) 0.0230(10) 0.0303(10) 0.0067(8) 0.0042(8) 0.0071(8) C92 0.0354(12) 0.0327(12) 0.0319(11) 0.0074(9) 0.0068(9) 0.0099(10) C93 0.0489(15) 0.0326(13) 0.0464(14) -0.0003(11) 0.0114(12) 0.0125(11) C94 0.0606(18) 0.0234(12) 0.0611(17) 0.0077(12) 0.0096(14) 0.0128(12) C95 0.0623(17) 0.0267(12) 0.0502(15) 0.0156(11) 0.0126(13) 0.0078(12) C96 0.0443(14) 0.0254(11) 0.0334(11) 0.0101(9) 0.0093(10) 0.0069(10) C7 0.075(6) 0.040(4) 0.083(7) -0.008(4) 0.045(5) 0.004(4) Cl4 0.117(3) 0.0599(14) 0.074(2) 0.0170(18) 0.0143(19) -0.0066(16) Cl5 0.0416(9) 0.1054(18) 0.0911(14) 0.0180(12) -0.0069(9) -0.0073(10) C101 0.039(2) 0.052(3) 0.090(3) 0.025(3) 0.015(2) 0.022(2) C102 0.145(6) 0.087(5) 0.091(4) 0.009(3) 0.025(4) 0.062(4) C103 0.112(6) 0.157(9) 0.148(7) 0.033(6) 0.065(5) 0.002(6) C104 0.341(15) 0.113(7) 0.072(5) 0.050(5) -0.032(6) -0.035(8) C105 0.099(5) 0.034(3) 0.165(7) 0.034(3) 0.033(4) 0.017(3) C7' 0.051(4) 0.069(5) 0.116(6) 0.041(4) 0.032(4) 0.011(3) Cl4' 0.0710(16) 0.0599(16) 0.085(2) 0.0220(19) 0.0176(17) 0.0097(12) Cl5' 0.157(4) 0.119(3) 0.0744(16) 0.0387(16) -0.0171(19) -0.058(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C4 1.992(2) . y Mo C3 2.013(2) . y Mo C5 2.028(2) . y Mo B3 2.326(2) . y Mo B4 2.381(2) . y Mo B2 2.393(2) . y Mo B5 2.404(2) . y Mo C1 2.419(2) . y Mo P2 2.5636(7) . y C3 O3 1.143(2) . y C4 O4 1.139(3) . y C5 O5 1.136(3) . y P2 C51 1.829(2) . ? P2 C41 1.834(2) . ? P2 C61 1.837(2) . ? C41 C46 1.391(3) . ? C41 C42 1.392(3) . ? C42 C43 1.388(3) . ? C43 C44 1.371(4) . ? C44 C45 1.379(4) . ? C45 C46 1.394(4) . ? C51 C52 1.381(3) . ? C51 C56 1.389(3) . ? C52 C53 1.397(4) . ? C53 C54 1.364(4) . ? C54 C55 1.374(4) . ? C55 C56 1.374(3) . ? C61 C66 1.390(3) . ? C61 C62 1.395(3) . ? C62 C63 1.390(3) . ? C63 C64 1.388(4) . ? C64 C65 1.374(4) . ? C65 C66 1.382(3) . ? C1 B5 1.711(3) . ? C1 B2 1.711(3) . ? C1 B6 1.720(3) . ? C1 B10 1.726(3) . ? B2 B7 1.767(3) . ? B2 B6 1.807(3) . ? B2 B3 1.810(3) . ? B3 B8 1.755(3) . ? B3 B7 1.778(3) . ? B3 B4 1.810(3) . ? B3 Ru 2.462(2) . y B4 B8 1.776(3) . ? B4 B5 1.790(3) . ? B4 B9 1.807(3) . ? B5 B10 1.760(3) . ? B5 B9 1.779(3) . ? B6 B7 1.748(3) . ? B6 B10 1.784(3) . ? B6 B11 1.791(3) . ? B7 B8 1.726(3) . ? B7 B11 1.772(3) . ? B7 Ru 2.388(2) . y B8 B9 1.756(3) . ? B8 B11 1.761(3) . ? B8 Ru 2.292(2) . y B9 B10 1.788(3) . ? B9 B11 1.790(3) . ? B10 B11 1.762(3) . ? Ru H8 1.73(2) . y Ru H3 2.00(2) . y Ru H7 2.01(2) . y Ru P3 2.2892(6) . y Ru P1 2.3011(7) . y Ru Cl1 2.3931(7) . y P1 C11 1.832(2) . ? P1 C31 1.837(2) . ? P1 C21 1.839(2) . ? C11 C12 1.392(3) . ? C11 C16 1.393(3) . ? C12 C13 1.391(3) . ? C13 C14 1.359(4) . ? C14 C15 1.377(4) . ? C15 C16 1.402(3) . ? C21 C26 1.383(3) . ? C21 C22 1.399(3) . ? C22 C23 1.381(4) . ? C23 C24 1.393(5) . ? C24 C25 1.360(4) . ? C25 C26 1.394(3) . ? C31 C36 1.387(3) . ? C31 C32 1.399(3) . ? C32 C33 1.389(3) . ? C33 C34 1.379(4) . ? C34 C35 1.365(4) . ? C35 C36 1.400(3) . ? P3 C91 1.828(2) . ? P3 C81 1.832(2) . ? P3 C71 1.8442(19) . ? C71 C76 1.389(3) . ? C71 C72 1.394(3) . ? C72 C73 1.393(3) . ? C73 C74 1.378(3) . ? C74 C75 1.373(3) . ? C75 C76 1.392(3) . ? C81 C86 1.383(3) . ? C81 C82 1.403(3) . ? C82 C83 1.388(3) . ? C83 C84 1.367(4) . ? C84 C85 1.382(3) . ? C85 C86 1.391(3) . ? C91 C96 1.394(3) . ? C91 C92 1.398(3) . ? C92 C93 1.386(3) . ? C93 C94 1.374(4) . ? C94 C95 1.397(3) . ? C95 C96 1.383(3) . ? C7 Cl4 1.740(9) . ? C7 Cl5 1.743(9) . ? C101 C102 1.595(8) . ? C102 C103 1.316(8) . ? C103 C104 1.392(10) . ? C104 C105 1.561(8) . ? C7' Cl4' 1.699(8) . ? C7' Cl5' 1.754(8) . ? C106 C107 1.286(16) . ? C107 C108 1.258(17) . ? C107 C109 1.33(2) . ? C108 C109 1.274(16) . ? C108 C110 1.92(3) . ? C109 C110 1.359(16) . ? 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 C4 Mo C3 76.37(9) . . y C4 Mo C5 75.15(9) . . y C3 Mo C5 122.51(8) . . y C4 Mo B3 87.49(8) . . ? C3 Mo B3 90.08(8) . . ? C5 Mo B3 136.56(8) . . ? C4 Mo B4 81.30(8) . . ? C3 Mo B4 130.72(8) . . ? C5 Mo B4 92.29(8) . . ? B3 Mo B4 45.22(7) . . ? C4 Mo B2 128.59(8) . . ? C3 Mo B2 83.97(8) . . ? C5 Mo B2 150.36(8) . . ? B3 Mo B2 45.08(7) . . ? B4 Mo B2 76.66(8) . . ? C4 Mo B5 117.89(8) . . ? C3 Mo B5 157.19(8) . . ? C5 Mo B5 79.75(8) . . ? B3 Mo B5 73.80(8) . . ? B4 Mo B5 43.93(8) . . ? B2 Mo B5 73.22(8) . . ? C4 Mo C1 153.59(8) . . ? C3 Mo C1 118.42(8) . . ? C5 Mo C1 108.90(8) . . ? B3 Mo C1 71.63(7) . . ? B4 Mo C1 72.54(8) . . ? B2 Mo C1 41.66(7) . . ? B5 Mo C1 41.55(8) . . ? C4 Mo P2 119.63(6) . . y C3 Mo P2 76.32(6) . . y C5 Mo P2 76.20(6) . . y B3 Mo P2 144.58(5) . . y B4 Mo P2 151.25(6) . . ? B2 Mo P2 100.35(6) . . ? B5 Mo P2 107.50(6) . . ? C1 Mo P2 86.20(5) . . ? O3 C3 Mo 176.83(19) . . y O4 C4 Mo 177.75(19) . . y O5 C5 Mo 175.29(19) . . y C51 P2 C41 102.85(10) . . ? C51 P2 C61 103.28(10) . . ? C41 P2 C61 103.98(10) . . ? C51 P2 Mo 114.89(7) . . ? C41 P2 Mo 116.42(7) . . ? C61 P2 Mo 113.81(7) . . ? C46 C41 C42 118.4(2) . . ? C46 C41 P2 121.57(17) . . ? C42 C41 P2 119.99(17) . . ? C43 C42 C41 120.7(2) . . ? C44 C43 C42 120.4(2) . . ? C43 C44 C45 119.9(2) . . ? C44 C45 C46 120.0(3) . . ? C41 C46 C45 120.6(2) . . ? C52 C51 C56 118.3(2) . . ? C52 C51 P2 122.22(18) . . ? C56 C51 P2 119.48(16) . . ? C51 C52 C53 119.8(2) . . ? C54 C53 C52 120.7(3) . . ? C53 C54 C55 119.9(3) . . ? C54 C55 C56 119.6(2) . . ? C55 C56 C51 121.6(2) . . ? C66 C61 C62 119.3(2) . . ? C66 C61 P2 119.19(18) . . ? C62 C61 P2 121.48(18) . . ? C63 C62 C61 119.5(3) . . ? C64 C63 C62 120.6(3) . . ? C65 C64 C63 119.6(2) . . ? C64 C65 C66 120.5(3) . . ? C65 C66 C61 120.5(3) . . ? B5 C1 B2 113.45(15) . . ? B5 C1 B6 113.11(16) . . ? B2 C1 B6 63.57(12) . . ? B5 C1 B10 61.62(13) . . ? B2 C1 B10 114.70(16) . . ? B6 C1 B10 62.35(13) . . ? B5 C1 Mo 68.78(10) . . ? B2 C1 Mo 68.37(10) . . ? B6 C1 Mo 127.64(13) . . ? B10 C1 Mo 126.64(14) . . ? C1 B2 B7 102.40(15) . . ? C1 B2 B6 58.44(12) . . ? B7 B2 B6 58.53(12) . . ? C1 B2 B3 104.10(15) . . ? B7 B2 B3 59.61(12) . . ? B6 B2 B3 107.19(15) . . ? C1 B2 Mo 69.97(10) . . ? B7 B2 Mo 120.52(13) . . ? B6 B2 Mo 124.48(13) . . ? B3 B2 Mo 65.49(9) . . ? B8 B3 B7 58.49(12) . . ? B8 B3 B2 106.30(14) . . ? B7 B3 B2 58.99(12) . . ? B8 B3 B4 59.75(12) . . ? B7 B3 B4 107.36(14) . . ? B2 B3 B4 109.74(15) . . ? B8 B3 Mo 123.51(13) . . ? B7 B3 Mo 123.55(13) . . ? B2 B3 Mo 69.43(10) . . ? B4 B3 Mo 69.01(10) . . ? B8 B3 Ru 63.29(9) . . ? B7 B3 Ru 66.30(10) . . ? B2 B3 Ru 117.77(12) . . ? B4 B3 Ru 112.92(12) . . ? Mo B3 Ru 169.59(10) . . y B8 B4 B5 103.14(15) . . ? B8 B4 B9 58.67(12) . . ? B5 B4 B9 59.27(12) . . ? B8 B4 B3 58.56(12) . . ? B5 B4 B3 104.19(15) . . ? B9 B4 B3 106.49(15) . . ? B8 B4 Mo 119.52(13) . . ? B5 B4 Mo 68.73(10) . . ? B9 B4 Mo 123.66(14) . . ? B3 B4 Mo 65.77(9) . . ? C1 B5 B10 59.61(13) . . ? C1 B5 B9 107.15(16) . . ? B10 B5 B9 60.68(13) . . ? C1 B5 B4 108.40(15) . . ? B10 B5 B4 110.47(16) . . ? B9 B5 B4 60.85(12) . . ? C1 B5 Mo 69.67(10) . . ? B10 B5 Mo 125.63(14) . . ? B9 B5 Mo 123.81(13) . . ? B4 B5 Mo 67.34(10) . . ? C1 B6 B7 102.86(15) . . ? C1 B6 B10 58.99(13) . . ? B7 B6 B10 105.88(16) . . ? C1 B6 B11 104.70(16) . . ? B7 B6 B11 60.08(12) . . ? B10 B6 B11 59.07(13) . . ? C1 B6 B2 57.99(12) . . ? B7 B6 B2 59.59(12) . . ? B10 B6 B2 107.40(16) . . ? B11 B6 B2 108.60(15) . . ? B8 B7 B6 109.50(16) . . ? B8 B7 B2 109.49(15) . . ? B6 B7 B2 61.88(12) . . ? B8 B7 B11 60.45(12) . . ? B6 B7 B11 61.17(13) . . ? B2 B7 B11 111.32(16) . . ? B8 B7 B3 60.07(12) . . ? B6 B7 B3 111.30(15) . . ? B2 B7 B3 61.39(12) . . ? B11 B7 B3 110.29(15) . . ? B8 B7 Ru 65.44(10) . . ? B6 B7 Ru 173.16(14) . . ? B2 B7 Ru 123.53(12) . . ? B11 B7 Ru 112.00(13) . . ? B3 B7 Ru 70.71(10) . . ? B7 B8 B3 61.45(12) . . ? B7 B8 B9 110.13(16) . . ? B3 B8 B9 111.32(15) . . ? B7 B8 B11 61.06(12) . . ? B3 B8 B11 111.92(15) . . ? B9 B8 B11 61.19(13) . . ? B7 B8 B4 111.30(15) . . ? B3 B8 B4 61.69(12) . . ? B9 B8 B4 61.55(12) . . ? B11 B8 B4 112.07(16) . . ? B7 B8 Ru 71.34(10) . . ? B3 B8 Ru 73.58(10) . . ? B9 B8 Ru 175.06(14) . . ? B11 B8 Ru 116.91(13) . . ? B4 B8 Ru 122.68(13) . . ? B8 B9 B5 104.45(15) . . ? B8 B9 B10 105.11(16) . . ? B5 B9 B10 59.14(13) . . ? B8 B9 B11 59.56(12) . . ? B5 B9 B11 106.05(16) . . ? B10 B9 B11 59.01(13) . . ? B8 B9 B4 59.79(12) . . ? B5 B9 B4 59.89(12) . . ? B10 B9 B4 108.44(16) . . ? B11 B9 B4 109.30(15) . . ? C1 B10 B5 58.77(12) . . ? C1 B10 B11 105.70(16) . . ? B5 B10 B11 108.10(16) . . ? C1 B10 B6 58.66(13) . . ? B5 B10 B6 107.75(16) . . ? B11 B10 B6 60.67(13) . . ? C1 B10 B9 106.11(16) . . ? B5 B10 B9 60.18(13) . . ? B11 B10 B9 60.56(13) . . ? B6 B10 B9 109.34(16) . . ? B8 B11 B10 105.98(16) . . ? B8 B11 B7 58.49(12) . . ? B10 B11 B7 105.78(16) . . ? B8 B11 B9 59.26(12) . . ? B10 B11 B9 60.43(14) . . ? B7 B11 B9 106.53(15) . . ? B8 B11 B6 105.99(15) . . ? B10 B11 B6 60.26(13) . . ? B7 B11 B6 58.75(12) . . ? B9 B11 B6 108.92(16) . . ? H8 Ru H3 92.8(9) . . y H8 Ru H7 95.6(9) . . y H3 Ru H7 83.3(8) . . y H8 Ru P3 88.9(7) . . y H3 Ru P3 89.1(6) . . y H7 Ru P3 171.3(5) . . y H8 Ru B8 33.7(7) . . ? H3 Ru B8 69.4(6) . . ? H7 Ru B8 69.4(6) . . ? P3 Ru B8 111.77(6) . . y H8 Ru P1 87.3(6) . . y H3 Ru P1 173.3(6) . . y H7 Ru P1 90.0(5) . . y P3 Ru P1 97.59(3) . . y B8 Ru P1 107.70(5) . . y H8 Ru B7 74.1(7) . . ? H3 Ru B7 67.1(6) . . ? H7 Ru B7 28.1(6) . . ? P3 Ru B7 149.49(5) . . y B8 Ru B7 43.22(7) . . y P1 Ru B7 106.53(5) . . y H8 Ru Cl1 175.6(7) . . y H3 Ru Cl1 84.6(6) . . y H7 Ru Cl1 80.5(6) . . y P3 Ru Cl1 94.61(2) . . y B8 Ru Cl1 141.88(6) . . y P1 Ru Cl1 94.88(3) . . y B7 Ru Cl1 101.53(6) . . y H8 Ru B3 72.6(7) . . ? H3 Ru B3 28.4(6) . . ? H7 Ru B3 66.5(6) . . ? P3 Ru B3 108.11(5) . . y B8 Ru B3 43.13(7) . . y P1 Ru B3 146.62(5) . . y B7 Ru B3 42.99(7) . . y Cl1 Ru B3 103.67(5) . . y C11 P1 C31 103.20(10) . . ? C11 P1 C21 104.57(11) . . ? C31 P1 C21 98.07(10) . . ? C11 P1 Ru 115.39(7) . . ? C31 P1 Ru 109.24(7) . . ? C21 P1 Ru 123.37(8) . . ? C12 C11 C16 119.0(2) . . ? C12 C11 P1 121.82(19) . . ? C16 C11 P1 119.14(17) . . ? C13 C12 C11 120.0(3) . . ? C14 C13 C12 120.8(3) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 C16 120.0(3) . . ? C11 C16 C15 119.8(3) . . ? C26 C21 C22 118.1(2) . . ? C26 C21 P1 122.96(17) . . ? C22 C21 P1 118.9(2) . . ? C23 C22 C21 120.9(3) . . ? C22 C23 C24 119.9(3) . . ? C25 C24 C23 119.6(3) . . ? C24 C25 C26 120.7(3) . . ? C21 C26 C25 120.8(3) . . ? C36 C31 C32 119.1(2) . . ? C36 C31 P1 124.39(17) . . ? C32 C31 P1 116.50(16) . . ? C33 C32 C31 120.2(2) . . ? C34 C33 C32 120.2(2) . . ? C35 C34 C33 120.1(2) . . ? C34 C35 C36 120.8(3) . . ? C31 C36 C35 119.7(2) . . ? C91 P3 C81 102.71(10) . . ? C91 P3 C71 102.05(9) . . ? C81 P3 C71 101.42(9) . . ? C91 P3 Ru 117.38(7) . . ? C81 P3 Ru 119.65(7) . . ? C71 P3 Ru 111.14(7) . . ? C76 C71 C72 118.44(18) . . ? C76 C71 P3 121.76(16) . . ? C72 C71 P3 119.73(15) . . ? C73 C72 C71 120.5(2) . . ? C74 C73 C72 120.3(2) . . ? C75 C74 C73 119.6(2) . . ? C74 C75 C76 120.6(2) . . ? C71 C76 C75 120.5(2) . . ? C86 C81 C82 118.32(19) . . ? C86 C81 P3 120.38(16) . . ? C82 C81 P3 120.79(16) . . ? C83 C82 C81 120.7(2) . . ? C84 C83 C82 120.0(2) . . ? C83 C84 C85 120.3(2) . . ? C84 C85 C86 120.0(2) . . ? C81 C86 C85 120.7(2) . . ? C96 C91 C92 118.2(2) . . ? C96 C91 P3 121.03(16) . . ? C92 C91 P3 120.73(16) . . ? C93 C92 C91 120.8(2) . . ? C94 C93 C92 120.4(2) . . ? C93 C94 C95 119.7(2) . . ? C96 C95 C94 119.8(2) . . ? C95 C96 C91 121.1(2) . . ? Cl4 C7 Cl5 112.9(5) . . ? C103 C102 C101 124.3(7) . . ? C102 C103 C104 110.5(8) . . ? C103 C104 C105 135.7(9) . . ? Cl4' C7' Cl5' 111.5(4) . . ? C108 C107 C106 127(2) . . ? C108 C107 C109 58.9(11) . . ? C106 C107 C109 174(3) . . ? C107 C108 C109 63.5(16) . . ? C107 C108 C110 106.6(17) . . ? C109 C108 C110 44.9(9) . . ? C108 C109 C107 57.7(10) . . ? C108 C109 C110 93.7(17) . . ? C107 C109 C110 146.9(19) . . ? C109 C110 C108 41.4(9) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.776 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.065 #===END data_14 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H41 B10 Fe Mo O5 P' _chemical_formula_weight 820.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' 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 20.0653(15) _cell_length_b 16.9217(17) _cell_length_c 11.7368(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3985.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 25 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.757 _exptl_absorpt_correction_type 'Semi-empirical (Bruker, 1995)' _exptl_absorpt_correction_T_min 0.55475 _exptl_absorpt_correction_T_max 0.58253 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 3901 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 24.94 _reflns_number_total 3676 _reflns_number_gt 2728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+4.6118P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00056(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(5) _refine_ls_number_reflns 3676 _refine_ls_number_parameters 486 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.0890 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.049 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.77156(3) 0.87599(4) 0.49677(6) 0.03439(18) Uani 1 d . . . C3 C 0.8315(4) 0.7805(6) 0.4842(10) 0.051(3) Uani 1 d . . . O3 O 0.8615(3) 0.7251(4) 0.4680(7) 0.076(3) Uani 1 d . . . C4 C 0.8139(5) 0.8882(7) 0.3482(10) 0.057(3) Uani 1 d . . . O4 O 0.8356(4) 0.8939(6) 0.2576(7) 0.078(3) Uani 1 d . . . C5 C 0.8069(4) 0.9869(5) 0.4927(12) 0.049(2) Uani 1 d . . . O5 O 0.8266(4) 1.0492(4) 0.4784(8) 0.079(2) Uani 1 d . . . P P 0.83664(12) 0.88273(13) 0.6819(2) 0.0348(6) Uani 1 d . . . C11 C 0.9211(4) 0.9212(4) 0.6724(9) 0.040(2) Uani 1 d . . . C12 C 0.9530(5) 0.9553(6) 0.7651(10) 0.062(3) Uani 1 d . . . H12A H 0.9302 0.9628 0.8333 0.074 Uiso 1 calc R . . C13 C 1.0192(5) 0.9781(8) 0.7552(12) 0.086(5) Uani 1 d . . . H13A H 1.0399 1.0018 0.8174 0.104 Uiso 1 calc R . . C14 C 1.0548(5) 0.9673(7) 0.6587(12) 0.078(4) Uani 1 d . . . H14A H 1.0995 0.9816 0.6559 0.094 Uiso 1 calc R . . C15 C 1.0246(5) 0.9354(6) 0.5657(10) 0.068(3) Uani 1 d . . . H15A H 1.0480 0.9286 0.4980 0.081 Uiso 1 calc R . . C16 C 0.9573(5) 0.9127(6) 0.5738(10) 0.062(3) Uani 1 d . . . H16A H 0.9366 0.8913 0.5101 0.074 Uiso 1 calc R . . C21 C 0.8486(4) 0.7853(5) 0.7449(8) 0.043(2) Uani 1 d . . . C22 C 0.9086(5) 0.7451(6) 0.7364(9) 0.058(3) Uani 1 d . . . H22A H 0.9448 0.7691 0.7010 0.069 Uiso 1 calc R . . C23 C 0.9149(6) 0.6702(6) 0.7797(12) 0.085(4) Uani 1 d . . . H23A H 0.9549 0.6431 0.7713 0.102 Uiso 1 calc R . . C24 C 0.8624(7) 0.6350(7) 0.8355(12) 0.087(4) Uani 1 d . . . H24A H 0.8680 0.5853 0.8679 0.104 Uiso 1 calc R . . C25 C 0.8029(6) 0.6719(7) 0.8434(11) 0.078(4) Uani 1 d . . . H25A H 0.7668 0.6470 0.8779 0.093 Uiso 1 calc R . . C26 C 0.7965(5) 0.7474(6) 0.7994(9) 0.062(3) Uani 1 d . . . H26A H 0.7559 0.7734 0.8066 0.074 Uiso 1 calc R . . C31 C 0.8008(4) 0.9420(5) 0.7964(8) 0.040(2) Uani 1 d . . . C32 C 0.8059(5) 0.9227(6) 0.9100(8) 0.048(2) Uani 1 d . . . H32A H 0.8257 0.8751 0.9305 0.058 Uiso 1 calc R . . C33 C 0.7822(5) 0.9725(6) 0.9946(13) 0.070(3) Uani 1 d . . . H33A H 0.7859 0.9578 1.0707 0.084 Uiso 1 calc R . . C34 C 0.7538(5) 1.0426(7) 0.9666(9) 0.068(3) Uani 1 d . . . H34A H 0.7392 1.0766 1.0237 0.082 Uiso 1 calc R . . C35 C 0.7464(6) 1.0636(6) 0.8545(11) 0.073(3) Uani 1 d . . . H35A H 0.7255 1.1107 0.8351 0.088 Uiso 1 calc R . . C36 C 0.7704(5) 1.0138(5) 0.7707(9) 0.059(3) Uani 1 d . . . H36A H 0.7663 1.0288 0.6948 0.071 Uiso 1 calc R . . C1 C 0.6750(4) 0.8576(5) 0.6155(8) 0.040(2) Uani 1 d . . . H1 H 0.6936 0.8652 0.7030 0.048 Uiso 1 calc R . . B2 B 0.6947(6) 0.7751(6) 0.5423(9) 0.040(3) Uani 1 d . . . H2 H 0.7258 0.7275 0.5777 0.049 Uiso 1 calc R . . B3 B 0.6945(6) 0.7984(6) 0.3928(9) 0.040(3) Uani 1 d . . . H3 H 0.7227 0.7662 0.3273 0.049 Uiso 1 calc R . . B4 B 0.6766(5) 0.9046(6) 0.3851(9) 0.036(2) Uani 1 d . . . H4 H 0.6934 0.9423 0.3143 0.043 Uiso 1 calc R . . B5 B 0.6666(5) 0.9396(5) 0.5305(8) 0.036(3) Uani 1 d . . . H5 H 0.6783 1.0005 0.5565 0.044 Uiso 1 calc R . . B6 B 0.6139(6) 0.7891(8) 0.5985(10) 0.049(3) Uani 1 d . . . H6 H 0.5941 0.7515 0.6671 0.059 Uiso 1 calc R . . B7 B 0.6239(5) 0.7534(6) 0.4590(9) 0.043(3) Uani 1 d . . . H7 H 0.6102 0.6926 0.4360 0.052 Uiso 1 calc R . . B8 B 0.6120(5) 0.8330(6) 0.3684(10) 0.040(3) Uani 1 d . . . H8 H 0.5893 0.8242 0.2840 0.048 Uiso 1 calc R . . B9 B 0.5944(6) 0.9182(7) 0.4468(10) 0.045(3) Uani 1 d . . . H9 H 0.5614 0.9654 0.4154 0.054 Uiso 1 calc R . . B10 B 0.5964(6) 0.8906(7) 0.5920(10) 0.047(3) Uani 1 d . . . H10 H 0.5655 0.9199 0.6568 0.056 Uiso 1 calc R . . B11 B 0.5624(5) 0.8265(6) 0.4900(13) 0.049(2) Uani 1 d . . . H11 H 0.5086 0.8139 0.4867 0.059 Uiso 1 calc R . . Fe Fe 0.56370(10) 0.78353(9) 0.17348(16) 0.0801(6) Uani 1 d D . . C40 C 0.4764(7) 0.7814(8) 0.0848(12) 0.082(4) Uani 1 d . . . C41 C 0.4834(5) 0.8553(7) 0.1377(10) 0.066(3) Uani 1 d . . . C42 C 0.5409(5) 0.8911(7) 0.0925(9) 0.060(3) Uani 1 d . . . C43 C 0.5686(5) 0.8386(7) 0.0136(11) 0.065(3) Uani 1 d . . . C44 C 0.5304(7) 0.7687(7) 0.0106(12) 0.081(3) Uani 1 d . . . C45 C 0.4156(8) 0.7279(10) 0.0984(17) 0.164(9) Uani 1 d . . . H44A H 0.3863 0.7496 0.1550 0.197 Uiso 1 calc R . . H44B H 0.4298 0.6761 0.1217 0.197 Uiso 1 calc R . . H44C H 0.3924 0.7242 0.0270 0.197 Uiso 1 calc R . . C46 C 0.4383(7) 0.8939(8) 0.2231(12) 0.117(6) Uani 1 d . . . H46A H 0.4563 0.9445 0.2441 0.140 Uiso 1 calc R . . H46B H 0.4350 0.8611 0.2896 0.140 Uiso 1 calc R . . H46C H 0.3949 0.9009 0.1904 0.140 Uiso 1 calc R . . C47 C 0.5658(6) 0.9719(6) 0.1160(11) 0.088(4) Uani 1 d . . . H47A H 0.5392 0.9958 0.1745 0.106 Uiso 1 calc R . . H47B H 0.5631 1.0031 0.0478 0.106 Uiso 1 calc R . . H47C H 0.6114 0.9692 0.1408 0.106 Uiso 1 calc R . . C49 C 0.5394(9) 0.6958(9) -0.0631(13) 0.153(8) Uani 1 d . . . H49A H 0.5798 0.7007 -0.1064 0.184 Uiso 1 calc R . . H49B H 0.5023 0.6909 -0.1141 0.184 Uiso 1 calc R . . H49C H 0.5419 0.6498 -0.0155 0.184 Uiso 1 calc R . . C48 C 0.6254(8) 0.8533(11) -0.0656(15) 0.154(7) Uani 1 d . . . H48A H 0.6330 0.8071 -0.1112 0.184 Uiso 1 calc R . . H48B H 0.6648 0.8651 -0.0223 0.184 Uiso 1 calc R . . H48C H 0.6150 0.8973 -0.1142 0.184 Uiso 1 calc R . . C7 C 0.5157(10) 0.7160(10) 0.2691(15) 0.102(9) Uani 0.702(10) d PD A 1 O7 O 0.4839(7) 0.6729(8) 0.3250(12) 0.117(6) Uani 0.702(10) d PD A 1 C8 C 0.6275(9) 0.7128(11) 0.1619(15) 0.094(7) Uani 0.702(10) d PD A 1 O8 O 0.6764(8) 0.6844(12) 0.1342(15) 0.195(12) Uani 0.702(10) d PD A 1 C9 C 0.5779(19) 0.6873(18) 0.235(4) 0.158 Uiso 0.298(10) d PD A 2 O9 O 0.5969(17) 0.6249(17) 0.213(3) 0.120(13) Uiso 0.298(10) d PD A 2 C10 C 0.6544(12) 0.787(3) 0.138(6) 0.16(3) Uiso 0.298(10) d PD A 2 O10 O 0.7113(11) 0.8000(19) 0.111(3) 0.111(12) Uiso 0.298(10) d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.0276(3) 0.0390(3) 0.0365(3) 0.0001(5) -0.0042(5) 0.0011(3) C3 0.043(5) 0.058(6) 0.053(7) -0.029(6) -0.014(6) 0.003(4) O3 0.060(4) 0.077(5) 0.091(7) -0.038(5) -0.016(4) 0.030(4) C4 0.028(5) 0.082(8) 0.060(8) -0.008(7) -0.002(5) 0.008(6) O4 0.064(5) 0.120(8) 0.052(5) 0.011(5) 0.026(4) 0.006(5) C5 0.042(4) 0.050(5) 0.054(5) 0.002(7) -0.004(7) -0.001(4) O5 0.094(5) 0.052(4) 0.091(7) 0.018(5) -0.001(6) -0.020(4) P 0.0316(13) 0.0347(12) 0.0381(13) 0.0042(13) -0.0064(12) 0.0002(11) C11 0.032(5) 0.033(4) 0.054(6) -0.003(5) -0.009(5) -0.004(4) C12 0.041(6) 0.081(8) 0.064(7) -0.010(6) -0.004(5) -0.016(5) C13 0.057(9) 0.109(12) 0.093(10) -0.042(9) -0.005(8) -0.040(8) C14 0.035(6) 0.101(9) 0.099(11) -0.011(8) 0.007(7) -0.019(6) C15 0.040(6) 0.091(9) 0.073(8) -0.014(7) 0.005(6) -0.016(6) C16 0.040(6) 0.081(8) 0.065(8) -0.008(6) -0.008(6) -0.005(5) C21 0.043(5) 0.035(5) 0.051(6) 0.012(4) -0.009(5) -0.003(4) C22 0.055(6) 0.043(6) 0.074(7) 0.011(5) -0.014(6) 0.010(5) C23 0.084(9) 0.051(7) 0.119(12) 0.001(8) -0.020(9) 0.036(7) C24 0.104(10) 0.051(7) 0.105(11) 0.018(7) -0.019(9) -0.005(8) C25 0.072(8) 0.067(7) 0.094(10) 0.043(7) -0.007(8) -0.007(7) C26 0.054(6) 0.064(7) 0.068(7) 0.008(6) 0.002(6) -0.002(5) C31 0.040(5) 0.034(5) 0.045(6) -0.002(4) -0.004(5) -0.005(4) C32 0.050(6) 0.058(6) 0.038(6) 0.001(5) -0.001(5) -0.001(5) C33 0.071(7) 0.098(8) 0.039(5) 0.002(9) -0.009(8) -0.015(6) C34 0.077(8) 0.072(7) 0.056(9) -0.021(6) 0.009(6) 0.002(6) C35 0.094(9) 0.048(6) 0.079(9) -0.020(6) -0.014(7) 0.015(6) C36 0.079(7) 0.043(5) 0.055(6) -0.012(5) -0.001(6) 0.009(6) C1 0.035(5) 0.051(6) 0.033(5) 0.003(5) 0.002(4) -0.005(5) B2 0.043(6) 0.036(6) 0.043(6) 0.003(5) -0.010(5) -0.003(5) B3 0.045(6) 0.041(6) 0.036(6) 0.003(5) -0.006(5) 0.001(5) B4 0.030(6) 0.040(6) 0.037(6) 0.004(5) -0.002(5) -0.004(5) B5 0.036(5) 0.029(5) 0.044(7) -0.005(4) -0.002(5) 0.001(4) B6 0.042(7) 0.068(8) 0.039(7) 0.002(6) -0.002(6) -0.014(7) B7 0.040(6) 0.044(6) 0.045(7) 0.003(5) -0.010(5) -0.011(5) B8 0.033(6) 0.045(6) 0.041(6) 0.000(5) -0.010(5) 0.004(5) B9 0.033(6) 0.049(7) 0.052(7) 0.002(6) 0.001(5) 0.009(5) B10 0.036(6) 0.062(8) 0.042(7) -0.005(6) 0.000(5) 0.002(6) B11 0.035(5) 0.055(6) 0.056(7) -0.003(7) -0.008(8) -0.002(4) Fe 0.1149(15) 0.0630(10) 0.0624(10) -0.0120(10) -0.0520(11) 0.0220(10) C40 0.079(9) 0.093(9) 0.075(9) 0.030(8) -0.039(8) -0.033(8) C41 0.058(7) 0.086(9) 0.056(7) 0.028(6) 0.001(6) 0.005(6) C42 0.053(6) 0.083(8) 0.045(6) 0.015(6) -0.017(5) -0.001(6) C43 0.060(6) 0.086(7) 0.048(8) 0.001(7) 0.001(7) -0.001(6) C44 0.097(9) 0.096(9) 0.049(8) -0.008(8) -0.027(9) 0.007(7) C45 0.124(14) 0.172(16) 0.20(2) 0.076(16) -0.041(14) -0.097(13) C46 0.112(12) 0.128(13) 0.110(12) 0.050(10) 0.033(10) 0.048(10) C47 0.085(9) 0.069(8) 0.110(11) 0.009(8) -0.034(8) -0.008(7) C49 0.25(2) 0.127(14) 0.083(11) -0.033(10) -0.087(13) 0.037(14) C48 0.147(16) 0.197(18) 0.117(14) -0.012(14) 0.065(12) 0.002(14) C7 0.142(19) 0.058(11) 0.107(16) 0.046(11) -0.086(15) -0.055(12) O7 0.143(12) 0.108(10) 0.100(10) 0.042(9) -0.065(10) -0.066(9) C8 0.131(17) 0.088(13) 0.061(12) -0.046(11) -0.065(13) 0.056(13) O8 0.193(19) 0.24(2) 0.153(18) -0.138(16) -0.095(15) 0.155(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C4 1.951(12) . ? Mo C5 2.007(9) . ? Mo C3 2.019(9) . ? Mo B2 2.361(11) . ? Mo B4 2.362(10) . ? Mo B3 2.367(11) . ? Mo B5 2.398(9) . ? Mo C1 2.407(9) . ? Mo P 2.538(3) . ? C3 O3 1.131(9) . ? C4 O4 1.153(12) . ? C5 O5 1.138(9) . ? P C11 1.818(8) . ? P C21 1.822(8) . ? P C31 1.825(9) . ? C11 C16 1.374(14) . ? C11 C12 1.388(13) . ? C12 C13 1.389(14) . ? C13 C14 1.351(17) . ? C14 C15 1.360(15) . ? C15 C16 1.407(13) . ? C21 C26 1.383(13) . ? C21 C22 1.387(12) . ? C22 C23 1.371(14) . ? C23 C24 1.376(16) . ? C24 C25 1.351(15) . ? C25 C26 1.385(13) . ? C31 C32 1.376(12) . ? C31 C36 1.393(12) . ? C32 C33 1.387(15) . ? C33 C34 1.357(14) . ? C34 C35 1.371(15) . ? C35 C36 1.381(13) . ? C1 B2 1.687(14) . ? C1 B10 1.695(14) . ? C1 B6 1.699(14) . ? C1 B5 1.717(13) . ? B2 B7 1.764(14) . ? B2 B6 1.767(16) . ? B2 B3 1.798(16) . ? B3 B8 1.779(15) . ? B3 B7 1.785(14) . ? B3 B4 1.833(14) . ? B4 B8 1.785(14) . ? B4 B9 1.816(15) . ? B4 B5 1.818(14) . ? B5 B10 1.786(14) . ? B5 B9 1.787(15) . ? B6 B10 1.756(16) . ? B6 B7 1.756(16) . ? B6 B11 1.758(17) . ? B7 B8 1.732(15) . ? B7 B11 1.785(14) . ? B8 B11 1.744(18) . ? B8 B9 1.747(15) . ? B9 B11 1.756(16) . ? B9 B10 1.767(16) . ? B10 B11 1.754(17) . ? Fe H8 1.5559 . ? Fe C8 1.757(14) . ? Fe C9 1.81(2) . ? Fe C10 1.87(2) . ? Fe C7 1.869(15) . ? Fe C40 2.037(11) . ? Fe C44 2.040(13) . ? Fe C41 2.060(11) . ? Fe C43 2.097(12) . ? Fe C42 2.103(10) . ? C40 C41 1.403(16) . ? C40 C44 1.406(18) . ? C40 C45 1.529(15) . ? C41 C42 1.406(14) . ? C41 C46 1.502(16) . ? C42 C43 1.397(15) . ? C42 C47 1.483(13) . ? C43 C44 1.410(15) . ? C43 C48 1.492(17) . ? C44 C49 1.518(17) . ? C7 O7 1.170(15) . ? C8 O8 1.141(16) . ? C9 O9 1.15(2) . ? C10 O10 1.21(2) . ? 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 C4 Mo C5 74.1(5) . . ? C4 Mo C3 76.1(5) . . ? C5 Mo C3 122.4(4) . . ? C4 Mo B2 124.3(4) . . ? C5 Mo B2 155.8(4) . . ? C3 Mo B2 80.0(4) . . ? C4 Mo B4 80.4(4) . . ? C5 Mo B4 94.6(4) . . ? C3 Mo B4 127.1(4) . . ? B2 Mo B4 75.4(4) . . ? C4 Mo B3 83.3(4) . . ? C5 Mo B3 137.5(4) . . ? C3 Mo B3 84.7(4) . . ? B2 Mo B3 44.7(4) . . ? B4 Mo B3 45.6(3) . . ? C4 Mo B5 118.9(4) . . ? C5 Mo B5 83.9(3) . . ? C3 Mo B5 153.4(3) . . ? B2 Mo B5 73.4(4) . . ? B4 Mo B5 44.9(3) . . ? B3 Mo B5 76.1(4) . . ? C4 Mo C1 151.9(4) . . ? C5 Mo C1 114.8(4) . . ? C3 Mo C1 114.7(4) . . ? B2 Mo C1 41.4(3) . . ? B4 Mo C1 72.5(3) . . ? B3 Mo C1 72.6(4) . . ? B5 Mo C1 41.9(3) . . ? C4 Mo P 122.4(3) . . ? C5 Mo P 78.3(4) . . ? C3 Mo P 78.0(3) . . ? B2 Mo P 100.1(3) . . ? B4 Mo P 151.7(3) . . ? B3 Mo P 143.4(3) . . ? B5 Mo P 106.9(2) . . ? C1 Mo P 85.6(2) . . ? O3 C3 Mo 173.2(9) . . ? O4 C4 Mo 176.0(9) . . ? O5 C5 Mo 172.9(12) . . ? C11 P C21 103.1(4) . . ? C11 P C31 102.5(4) . . ? C21 P C31 104.5(4) . . ? C11 P Mo 116.3(4) . . ? C21 P Mo 112.0(3) . . ? C31 P Mo 116.9(3) . . ? C16 C11 C12 117.3(8) . . ? C16 C11 P 120.5(7) . . ? C12 C11 P 122.1(8) . . ? C11 C12 C13 119.5(11) . . ? C14 C13 C12 122.5(11) . . ? C13 C14 C15 119.4(9) . . ? C14 C15 C16 118.7(11) . . ? C11 C16 C15 122.5(10) . . ? C26 C21 C22 117.5(9) . . ? C26 C21 P 120.5(7) . . ? C22 C21 P 121.9(7) . . ? C23 C22 C21 120.4(10) . . ? C22 C23 C24 120.5(11) . . ? C25 C24 C23 120.6(11) . . ? C24 C25 C26 118.9(11) . . ? C21 C26 C25 122.1(10) . . ? C32 C31 C36 116.7(9) . . ? C32 C31 P 123.6(7) . . ? C36 C31 P 119.5(7) . . ? C31 C32 C33 121.6(10) . . ? C34 C33 C32 120.2(13) . . ? C33 C34 C35 120.2(11) . . ? C34 C35 C36 119.3(10) . . ? C35 C36 C31 122.0(10) . . ? B2 C1 B10 114.1(8) . . ? B2 C1 B6 62.9(6) . . ? B10 C1 B6 62.3(6) . . ? B2 C1 B5 113.3(7) . . ? B10 C1 B5 63.1(6) . . ? B6 C1 B5 114.3(7) . . ? B2 C1 Mo 67.8(5) . . ? B10 C1 Mo 127.7(6) . . ? B6 C1 Mo 126.9(6) . . ? B5 C1 Mo 68.8(4) . . ? C1 B2 B7 105.4(8) . . ? C1 B2 B6 58.9(6) . . ? B7 B2 B6 59.7(6) . . ? C1 B2 B3 108.4(8) . . ? B7 B2 B3 60.2(6) . . ? B6 B2 B3 109.4(8) . . ? C1 B2 Mo 70.8(5) . . ? B7 B2 Mo 123.4(6) . . ? B6 B2 Mo 125.9(7) . . ? B3 B2 Mo 67.8(5) . . ? B8 B3 B7 58.2(6) . . ? B8 B3 B2 103.4(8) . . ? B7 B3 B2 59.0(6) . . ? B8 B3 B4 59.2(6) . . ? B7 B3 B4 106.5(8) . . ? B2 B3 B4 105.3(8) . . ? B8 B3 Mo 120.6(7) . . ? B7 B3 Mo 122.0(6) . . ? B2 B3 Mo 67.5(5) . . ? B4 B3 Mo 67.1(5) . . ? B8 B4 B9 58.0(6) . . ? B8 B4 B5 104.1(7) . . ? B9 B4 B5 58.9(6) . . ? B8 B4 B3 58.9(6) . . ? B9 B4 B3 106.4(7) . . ? B5 B4 B3 107.1(7) . . ? B8 B4 Mo 120.5(6) . . ? B9 B4 Mo 122.5(6) . . ? B5 B4 Mo 68.6(5) . . ? B3 B4 Mo 67.3(5) . . ? C1 B5 B10 57.8(6) . . ? C1 B5 B9 103.7(7) . . ? B10 B5 B9 59.3(6) . . ? C1 B5 B4 105.8(7) . . ? B10 B5 B4 108.4(7) . . ? B9 B5 B4 60.5(6) . . ? C1 B5 Mo 69.3(4) . . ? B10 B5 Mo 123.4(6) . . ? B9 B5 Mo 122.0(6) . . ? B4 B5 Mo 66.5(4) . . ? C1 B6 B10 58.7(6) . . ? C1 B6 B7 105.2(8) . . ? B10 B6 B7 108.6(8) . . ? C1 B6 B11 105.3(8) . . ? B10 B6 B11 59.9(7) . . ? B7 B6 B11 61.0(7) . . ? C1 B6 B2 58.2(6) . . ? B10 B6 B2 107.4(8) . . ? B7 B6 B2 60.1(6) . . ? B11 B6 B2 108.5(8) . . ? B8 B7 B6 106.8(8) . . ? B8 B7 B2 106.9(7) . . ? B6 B7 B2 60.2(6) . . ? B8 B7 B11 59.4(7) . . ? B6 B7 B11 59.5(7) . . ? B2 B7 B11 107.5(8) . . ? B8 B7 B3 60.8(6) . . ? B6 B7 B3 110.5(8) . . ? B2 B7 B3 60.9(6) . . ? B11 B7 B3 110.0(7) . . ? B7 B8 B11 61.8(6) . . ? B7 B8 B9 110.3(8) . . ? B11 B8 B9 60.4(6) . . ? B7 B8 B3 61.1(6) . . ? B11 B8 B3 112.2(8) . . ? B9 B8 B3 112.0(8) . . ? B7 B8 B4 111.1(7) . . ? B11 B8 B4 111.6(8) . . ? B9 B8 B4 61.9(6) . . ? B3 B8 B4 61.9(6) . . ? B8 B9 B11 59.7(7) . . ? B8 B9 B10 106.6(9) . . ? B11 B9 B10 59.7(7) . . ? B8 B9 B5 107.0(8) . . ? B11 B9 B5 108.5(8) . . ? B10 B9 B5 60.3(6) . . ? B8 B9 B4 60.1(6) . . ? B11 B9 B4 109.6(8) . . ? B10 B9 B4 109.3(9) . . ? B5 B9 B4 60.6(6) . . ? C1 B10 B11 105.6(8) . . ? C1 B10 B6 59.0(6) . . ? B11 B10 B6 60.1(6) . . ? C1 B10 B9 105.4(9) . . ? B11 B10 B9 59.8(7) . . ? B6 B10 B9 107.8(9) . . ? C1 B10 B5 59.0(6) . . ? B11 B10 B5 108.6(8) . . ? B6 B10 B5 108.3(8) . . ? B9 B10 B5 60.4(6) . . ? B8 B11 B10 107.3(7) . . ? B8 B11 B9 59.9(6) . . ? B10 B11 B9 60.5(6) . . ? B8 B11 B6 106.3(7) . . ? B10 B11 B6 60.0(7) . . ? B9 B11 B6 108.2(8) . . ? B8 B11 B7 58.8(6) . . ? B10 B11 B7 107.4(7) . . ? B9 B11 B7 107.5(7) . . ? B6 B11 B7 59.4(6) . . ? H8 Fe C8 97.2 . . ? H8 Fe C9 90.7 . . ? C8 Fe C9 45.7(6) . . ? H8 Fe C10 81.5 . . ? C8 Fe C10 45.0(8) . . ? C9 Fe C10 87.9(15) . . ? H8 Fe C7 86.6 . . ? C8 Fe C7 90.3(10) . . ? C9 Fe C7 44.6(6) . . ? C10 Fe C7 130.9(17) . . ? H8 Fe C40 135.9 . . ? C8 Fe C40 125.1(7) . . ? C9 Fe C40 109.0(19) . . ? C10 Fe C40 136(2) . . ? C7 Fe C40 81.6(6) . . ? H8 Fe C44 160.7 . . ? C8 Fe C44 94.7(6) . . ? C9 Fe C44 109(2) . . ? C10 Fe C44 96(2) . . ? C7 Fe C44 108.6(7) . . ? C40 Fe C44 40.3(5) . . ? H8 Fe C41 99.6 . . ? C8 Fe C41 162.7(6) . . ? C9 Fe C41 137.4(11) . . ? C10 Fe C41 134.3(15) . . ? C7 Fe C41 94.6(7) . . ? C40 Fe C41 40.0(5) . . ? C44 Fe C41 68.0(5) . . ? H8 Fe C43 122.3 . . ? C8 Fe C43 101.5(7) . . ? C9 Fe C43 138.9(16) . . ? C10 Fe C43 75(2) . . ? C7 Fe C43 146.4(6) . . ? C40 Fe C43 65.9(5) . . ? C44 Fe C43 39.8(4) . . ? C41 Fe C43 65.9(4) . . ? H8 Fe C42 93.8 . . ? C8 Fe C42 135.4(8) . . ? C9 Fe C42 175(2) . . ? C10 Fe C42 94.9(15) . . ? C7 Fe C42 133.5(7) . . ? C40 Fe C42 66.3(4) . . ? C44 Fe C42 67.1(5) . . ? C41 Fe C42 39.5(4) . . ? C43 Fe C42 38.9(4) . . ? C41 C40 C44 109.4(11) . . ? C41 C40 C45 124.2(15) . . ? C44 C40 C45 126.1(15) . . ? C41 C40 Fe 70.8(6) . . ? C44 C40 Fe 69.9(7) . . ? C45 C40 Fe 130.1(9) . . ? C40 C41 C42 107.4(11) . . ? C40 C41 C46 128.6(12) . . ? C42 C41 C46 124.0(12) . . ? C40 C41 Fe 69.1(7) . . ? C42 C41 Fe 71.9(6) . . ? C46 C41 Fe 126.3(8) . . ? C43 C42 C41 107.6(10) . . ? C43 C42 C47 125.1(11) . . ? C41 C42 C47 127.1(11) . . ? C43 C42 Fe 70.3(6) . . ? C41 C42 Fe 68.6(6) . . ? C47 C42 Fe 129.9(7) . . ? C42 C43 C44 109.5(11) . . ? C42 C43 C48 127.6(12) . . ? C44 C43 C48 122.7(13) . . ? C42 C43 Fe 70.8(7) . . ? C44 C43 Fe 67.9(7) . . ? C48 C43 Fe 131.9(10) . . ? C40 C44 C43 106.0(11) . . ? C40 C44 C49 124.7(14) . . ? C43 C44 C49 129.1(15) . . ? C40 C44 Fe 69.7(7) . . ? C43 C44 Fe 72.3(7) . . ? C49 C44 Fe 126.5(9) . . ? O7 C7 Fe 177.1(15) . . ? O8 C8 Fe 159(2) . . ? O9 C9 Fe 142(4) . . ? O10 C10 Fe 171(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.552 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.074 #===END data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 B10 Cu Fe O3 P' _chemical_formula_weight 596.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5862(10) _cell_length_b 12.7603(10) _cell_length_c 17.5809(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.795(10) _cell_angle_gamma 90.00 _cell_volume 2790.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 5 _exptl_crystal_description blocks _exptl_crystal_colour yellow _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 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 1.364 _exptl_absorpt_correction_type 'None Applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? _diffrn_reflns_number 2689 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.2001 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 19.99 _reflns_number_total 2533 _reflns_number_gt 1241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4 (1989)' _computing_cell_refinement 'Enraf-Nonius CAD4 (1989)' _computing_data_reduction 'XCAD4 Siemens Software (Harms, 1993)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-PC (Bruker, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2533 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2183 _refine_ls_R_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.2616 _refine_ls_wR_factor_gt 0.2186 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _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 Fe Fe -0.1601(2) -0.1609(2) 0.36249(15) 0.0487(10) Uani 1 1 d . . . C3 C -0.139(2) -0.076(2) 0.4421(14) 0.093(10) Uani 1 1 d . . . O3 O -0.1256(14) -0.0235(16) 0.4940(9) 0.109(7) Uani 1 1 d . . . C4 C -0.2719(16) -0.228(2) 0.3963(12) 0.068(8) Uani 1 1 d . . . O4 O -0.3386(13) -0.2671(16) 0.4189(9) 0.112(7) Uani 1 1 d . . . C5 C -0.071(3) -0.246(2) 0.4043(17) 0.127(14) Uani 1 1 d . . . O5 O -0.0086(17) -0.3092(18) 0.4353(11) 0.131(8) Uani 1 1 d . . . C1 C -0.1846(13) -0.2132(15) 0.2461(9) 0.046(5) Uiso 1 1 d . . . H1 H -0.2022 -0.2976 0.2468 0.055 Uiso 1 1 calc R . . B2 B -0.0533(19) -0.1748(19) 0.2781(13) 0.055(7) Uiso 1 1 d . . . H2 H 0.0155 -0.2260 0.2985 0.066 Uiso 1 1 calc R . . B3 B -0.0697(19) -0.0409(19) 0.3145(13) 0.044(7) Uiso 1 1 d . . . H3 H 0.003(12) -0.018(12) 0.323(8) 0.052 Uiso 1 1 d . . . B4 B -0.2120(16) -0.0154(18) 0.3054(12) 0.042(6) Uiso 1 1 d . . . H4 H -0.2459 0.0389 0.3440 0.050 Uiso 1 1 calc R . . B5 B -0.2759(18) -0.1287(16) 0.2642(11) 0.039(6) Uiso 1 1 d . . . H5 H -0.3549 -0.1524 0.2779 0.046 Uiso 1 1 calc R . . B6 B -0.1159(18) -0.1740(19) 0.1767(13) 0.057(7) Uiso 1 1 d . . . H6 H -0.0872 -0.2260 0.1342 0.068 Uiso 1 1 calc R . . B7 B -0.0408(18) -0.0610(17) 0.2184(12) 0.036(6) Uiso 1 1 d . . . H7 H 0.041(11) -0.036(11) 0.234(8) 0.043 Uiso 1 1 d . . . B8 B -0.1377(18) 0.030(2) 0.2347(12) 0.045(7) Uiso 1 1 d . . . H8 H -0.117(11) 0.120(12) 0.230(8) 0.054 Uiso 1 1 d . . . B9 B -0.2688(19) -0.0211(19) 0.2051(12) 0.054(7) Uiso 1 1 d . . . H9 H -0.3388 0.0268 0.1814 0.064 Uiso 1 1 calc R . . B10 B -0.2487(18) -0.1455(18) 0.1732(12) 0.048(7) Uiso 1 1 d . . . H10 H -0.3081 -0.1800 0.1278 0.057 Uiso 1 1 calc R . . B11 B -0.1625(18) -0.0487(19) 0.1532(14) 0.060(8) Uiso 1 1 d . . . H11 H -0.1622 -0.0172 0.0950 0.071 Uiso 1 1 calc R . . Cu Cu 0.0322(2) 0.0856(2) 0.28116(15) 0.0646(10) Uani 1 1 d . . . P P 0.1674(4) 0.1920(4) 0.2822(3) 0.0467(17) Uani 1 1 d . . . C31 C 0.1771(14) 0.2386(14) 0.1849(10) 0.036(5) Uiso 1 1 d . . . C32 C 0.2507(15) 0.3157(15) 0.1723(11) 0.057(6) Uiso 1 1 d . . . H32 H 0.2937 0.3468 0.2139 0.069 Uiso 1 1 calc R . . C33 C 0.2601(18) 0.3464(18) 0.0977(12) 0.078(7) Uiso 1 1 d . . . H33 H 0.3103 0.3967 0.0889 0.094 Uiso 1 1 calc R . . C34 C 0.1957(17) 0.3023(16) 0.0388(13) 0.071(7) Uiso 1 1 d . . . H34 H 0.2046 0.3197 -0.0112 0.085 Uiso 1 1 calc R . . C35 C 0.1171(17) 0.2325(17) 0.0498(12) 0.077(7) Uiso 1 1 d . . . H35 H 0.0687 0.2076 0.0085 0.093 Uiso 1 1 calc R . . C36 C 0.1113(17) 0.1992(17) 0.1255(12) 0.066(7) Uiso 1 1 d . . . H36 H 0.0608 0.1490 0.1340 0.079 Uiso 1 1 calc R . . C41 C 0.2936(14) 0.1284(14) 0.3149(10) 0.046(6) Uiso 1 1 d . . . C42 C 0.3293(16) 0.1225(15) 0.3922(11) 0.059(6) Uiso 1 1 d . . . H42 H 0.2900 0.1527 0.4272 0.071 Uiso 1 1 calc R . . C43 C 0.4255(18) 0.0707(17) 0.4176(13) 0.084(7) Uiso 1 1 d . . . H43 H 0.4499 0.0657 0.4702 0.100 Uiso 1 1 calc R . . C44 C 0.4854(18) 0.0265(18) 0.3663(12) 0.079(7) Uiso 1 1 d . . . H44 H 0.5471 -0.0118 0.3840 0.094 Uiso 1 1 calc R . . C45 C 0.4526(16) 0.0400(15) 0.2888(11) 0.063(6) Uiso 1 1 d . . . H45 H 0.4942 0.0146 0.2535 0.076 Uiso 1 1 calc R . . C46 C 0.3574(15) 0.0916(15) 0.2640(11) 0.052(6) Uiso 1 1 d . . . H46 H 0.3359 0.1017 0.2115 0.062 Uiso 1 1 calc R . . C51 C 0.1675(14) 0.3071(14) 0.3429(10) 0.043(5) Uiso 1 1 d . . . C52 C 0.0737(16) 0.3408(16) 0.3664(11) 0.057(6) Uiso 1 1 d . . . H52 H 0.0104 0.3037 0.3515 0.068 Uiso 1 1 calc R . . C53 C 0.0727(17) 0.4299(16) 0.4121(11) 0.068(7) Uiso 1 1 d . . . H53 H 0.0079 0.4562 0.4233 0.082 Uiso 1 1 calc R . . C54 C 0.1658(18) 0.4779(19) 0.4402(12) 0.082(7) Uiso 1 1 d . . . H54 H 0.1656 0.5329 0.4749 0.098 Uiso 1 1 calc R . . C55 C 0.2608(16) 0.4469(15) 0.4184(10) 0.057(6) Uiso 1 1 d . . . H55 H 0.3235 0.4847 0.4339 0.069 Uiso 1 1 calc R . . C56 C 0.2623(16) 0.3576(16) 0.3724(11) 0.059(6) Uiso 1 1 d . . . H56 H 0.3275 0.3320 0.3616 0.070 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 Fe 0.047(2) 0.065(2) 0.0366(18) 0.0016(18) 0.0148(14) -0.0037(19) C3 0.09(2) 0.12(2) 0.072(19) -0.050(18) 0.034(16) -0.077(18) O3 0.109(14) 0.17(2) 0.054(11) -0.041(13) 0.042(10) -0.034(14) C4 0.025(15) 0.12(2) 0.061(16) -0.023(15) 0.004(12) -0.013(14) O4 0.070(14) 0.19(2) 0.089(13) -0.002(13) 0.049(10) -0.046(13) C5 0.22(4) 0.08(2) 0.11(3) 0.06(2) 0.12(3) 0.06(2) O5 0.17(2) 0.14(2) 0.109(16) 0.052(14) 0.078(15) 0.037(16) Cu 0.0478(18) 0.088(2) 0.0593(18) 0.0040(18) 0.0126(14) -0.0222(17) P 0.033(3) 0.067(5) 0.041(3) 0.004(3) 0.008(3) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe C5 1.65(3) . ? Fe C3 1.76(2) . ? Fe C4 1.82(2) . ? Fe B5 2.12(2) . ? Fe C1 2.130(17) . ? Fe B3 2.15(2) . ? Fe B2 2.16(2) . ? Fe B4 2.16(2) . ? C3 O3 1.12(2) . ? C4 O4 1.10(2) . ? C5 O5 1.20(3) . ? C1 B5 1.64(3) . ? C1 B10 1.65(3) . ? C1 B6 1.68(3) . ? C1 B2 1.73(3) . ? B2 B7 1.81(3) . ? B2 B6 1.84(3) . ? B2 B3 1.85(3) . ? B3 B8 1.77(3) . ? B3 B7 1.80(3) . ? B3 B4 1.80(3) . ? B3 Cu 2.20(2) . ? B4 B5 1.76(3) . ? B4 B8 1.76(3) . ? B4 B9 1.80(3) . ? B5 B10 1.70(3) . ? B5 B9 1.73(3) . ? B6 B10 1.70(3) . ? B6 B11 1.73(3) . ? B6 B7 1.82(3) . ? B7 B8 1.73(3) . ? B7 B11 1.77(3) . ? B7 Cu 2.29(2) . ? B8 B11 1.74(3) . ? B8 B9 1.77(3) . ? B8 Cu 2.28(2) . ? B9 B10 1.71(3) . ? B9 B11 1.77(3) . ? B10 B11 1.72(3) . ? Cu H3 1.59(16) . ? Cu H7 1.77(14) . ? Cu H8 2.00(14) . ? Cu P 2.175(6) . ? P C41 1.797(19) . ? P C51 1.815(18) . ? P C31 1.834(17) . ? C31 C36 1.33(2) . ? C31 C32 1.39(2) . ? C32 C33 1.39(2) . ? C33 C34 1.34(3) . ? C34 C35 1.37(2) . ? C35 C36 1.41(3) . ? C41 C42 1.37(2) . ? C41 C46 1.37(2) . ? C42 C43 1.39(3) . ? C43 C44 1.38(3) . ? C44 C45 1.37(2) . ? C45 C46 1.38(2) . ? C51 C52 1.38(2) . ? C51 C56 1.38(2) . ? C52 C53 1.39(2) . ? C53 C54 1.35(3) . ? C54 C55 1.37(2) . ? C55 C56 1.40(2) . ? 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 C5 Fe C3 92.5(15) . . ? C5 Fe C4 92.9(13) . . ? C3 Fe C4 93.4(10) . . ? C5 Fe B5 145.5(13) . . ? C3 Fe B5 121.9(11) . . ? C4 Fe B5 83.5(9) . . ? C5 Fe C1 102.2(12) . . ? C3 Fe C1 160.0(10) . . ? C4 Fe C1 99.3(8) . . ? B5 Fe C1 45.4(7) . . ? C5 Fe B3 106.3(12) . . ? C3 Fe B3 81.2(10) . . ? C4 Fe B3 160.2(10) . . ? B5 Fe B3 83.2(9) . . ? C1 Fe B3 81.6(8) . . ? C5 Fe B2 78.6(11) . . ? C3 Fe B2 124.4(9) . . ? C4 Fe B2 141.2(9) . . ? B5 Fe B2 83.0(9) . . ? C1 Fe B2 47.7(7) . . ? B3 Fe B2 50.8(8) . . ? C5 Fe B4 155.3(13) . . ? C3 Fe B4 80.6(11) . . ? C4 Fe B4 111.1(9) . . ? B5 Fe B4 48.3(8) . . ? C1 Fe B4 80.4(8) . . ? B3 Fe B4 49.4(8) . . ? B2 Fe B4 85.9(9) . . ? O3 C3 Fe 178(3) . . ? O4 C4 Fe 178(2) . . ? O5 C5 Fe 179(3) . . ? B5 C1 B10 62.2(12) . . ? B5 C1 B6 113.5(16) . . ? B10 C1 B6 61.5(12) . . ? B5 C1 B2 114.4(16) . . ? B10 C1 B2 115.6(16) . . ? B6 C1 B2 65.1(12) . . ? B5 C1 Fe 67.1(9) . . ? B10 C1 Fe 124.3(13) . . ? B6 C1 Fe 126.2(13) . . ? B2 C1 Fe 66.9(9) . . ? C1 B2 B7 101.6(16) . . ? C1 B2 B6 55.9(11) . . ? B7 B2 B6 59.7(12) . . ? C1 B2 B3 102.8(16) . . ? B7 B2 B3 58.9(12) . . ? B6 B2 B3 106.0(17) . . ? C1 B2 Fe 65.4(9) . . ? B7 B2 Fe 116.8(14) . . ? B6 B2 Fe 116.6(14) . . ? B3 B2 Fe 64.6(10) . . ? B8 B3 B7 58.1(12) . . ? B8 B3 B4 59.0(12) . . ? B7 B3 B4 106.4(15) . . ? B8 B3 B2 105.1(16) . . ? B7 B3 B2 59.6(12) . . ? B4 B3 B2 107.4(16) . . ? B8 B3 Fe 116.8(14) . . ? B7 B3 Fe 117.4(14) . . ? B4 B3 Fe 65.6(10) . . ? B2 B3 Fe 64.7(10) . . ? B8 B3 Cu 69.3(11) . . ? B7 B3 Cu 69.2(10) . . ? B4 B3 Cu 117.1(14) . . ? B2 B3 Cu 119.1(13) . . ? Fe B3 Cu 172.5(12) . . ? B5 B4 B8 103.6(15) . . ? B5 B4 B9 58.3(12) . . ? B8 B4 B9 59.7(12) . . ? B5 B4 B3 105.9(16) . . ? B8 B4 B3 59.6(12) . . ? B9 B4 B3 108.7(15) . . ? B5 B4 Fe 64.7(10) . . ? B8 B4 Fe 116.8(14) . . ? B9 B4 Fe 117.8(14) . . ? B3 B4 Fe 65.1(10) . . ? C1 B5 B10 59.1(11) . . ? C1 B5 B9 107.6(15) . . ? B10 B5 B9 59.9(12) . . ? C1 B5 B4 109.3(15) . . ? B10 B5 B4 110.3(16) . . ? B9 B5 B4 62.1(12) . . ? C1 B5 Fe 67.5(9) . . ? B10 B5 Fe 121.9(14) . . ? B9 B5 Fe 123.3(14) . . ? B4 B5 Fe 67.0(9) . . ? C1 B6 B10 58.5(12) . . ? C1 B6 B11 104.9(17) . . ? B10 B6 B11 60.0(13) . . ? C1 B6 B7 103.8(16) . . ? B10 B6 B7 107.0(17) . . ? B11 B6 B7 60.0(13) . . ? C1 B6 B2 58.9(12) . . ? B10 B6 B2 108.0(17) . . ? B11 B6 B2 108.5(17) . . ? B7 B6 B2 59.5(12) . . ? B8 B7 B11 59.3(12) . . ? B8 B7 B3 60.2(12) . . ? B11 B7 B3 108.4(16) . . ? B8 B7 B2 108.3(15) . . ? B11 B7 B2 107.6(16) . . ? B3 B7 B2 61.5(12) . . ? B8 B7 B6 105.1(15) . . ? B11 B7 B6 57.6(12) . . ? B3 B7 B6 109.0(16) . . ? B2 B7 B6 60.8(12) . . ? B8 B7 Cu 67.5(10) . . ? B11 B7 Cu 118.8(13) . . ? B3 B7 Cu 63.6(10) . . ? B2 B7 Cu 116.0(12) . . ? B6 B7 Cu 171.2(14) . . ? B7 B8 B11 61.5(13) . . ? B7 B8 B4 111.2(17) . . ? B11 B8 B4 110.3(17) . . ? B7 B8 B3 61.8(13) . . ? B11 B8 B3 111.5(17) . . ? B4 B8 B3 61.3(12) . . ? B7 B8 B9 110.8(17) . . ? B11 B8 B9 60.4(12) . . ? B4 B8 B9 61.2(12) . . ? B3 B8 B9 111.2(17) . . ? B7 B8 Cu 68.0(10) . . ? B11 B8 Cu 121.1(13) . . ? B4 B8 Cu 114.7(13) . . ? B3 B8 Cu 64.1(10) . . ? B9 B8 Cu 175.3(15) . . ? B10 B9 B5 59.1(12) . . ? B10 B9 B11 59.0(13) . . ? B5 B9 B11 105.3(17) . . ? B10 B9 B8 104.8(17) . . ? B5 B9 B8 104.1(16) . . ? B11 B9 B8 58.7(12) . . ? B10 B9 B4 107.5(17) . . ? B5 B9 B4 59.6(12) . . ? B11 B9 B4 107.2(16) . . ? B8 B9 B4 59.1(12) . . ? C1 B10 B5 58.7(12) . . ? C1 B10 B6 60.0(12) . . ? B5 B10 B6 109.4(17) . . ? C1 B10 B9 108.1(16) . . ? B5 B10 B9 61.0(12) . . ? B6 B10 B9 112.3(18) . . ? C1 B10 B11 106.7(16) . . ? B5 B10 B11 109.1(17) . . ? B6 B10 B11 60.8(13) . . ? B9 B10 B11 62.0(13) . . ? B10 B11 B6 59.2(13) . . ? B10 B11 B8 106.5(17) . . ? B6 B11 B8 108.8(17) . . ? B10 B11 B9 59.0(13) . . ? B6 B11 B9 108.5(17) . . ? B8 B11 B9 60.9(13) . . ? B10 B11 B7 108.3(17) . . ? B6 B11 B7 62.4(13) . . ? B8 B11 B7 59.2(12) . . ? B9 B11 B7 109.3(17) . . ? H3 Cu H7 61(6) . . ? H3 Cu H8 97(7) . . ? H7 Cu H8 96(6) . . ? H3 Cu P 139(5) . . ? H7 Cu P 117(5) . . ? H8 Cu P 123(4) . . ? H3 Cu B3 22(5) . . ? H7 Cu B3 64(4) . . ? H8 Cu B3 75(4) . . ? P Cu B3 160.8(6) . . ? H3 Cu B8 69(5) . . ? H7 Cu B8 71(5) . . ? H8 Cu B8 31(4) . . ? P Cu B8 152.5(6) . . ? B3 Cu B8 46.6(8) . . ? H3 Cu B7 56(5) . . ? H7 Cu B7 27(4) . . ? H8 Cu B7 71(4) . . ? P Cu B7 140.3(6) . . ? B3 Cu B7 47.2(7) . . ? B8 Cu B7 44.5(8) . . ? C41 P C51 104.9(8) . . ? C41 P C31 105.2(8) . . ? C51 P C31 107.0(8) . . ? C41 P Cu 111.9(6) . . ? C51 P Cu 116.1(6) . . ? C31 P Cu 111.0(6) . . ? C36 C31 C32 119.6(19) . . ? C36 C31 P 119.2(15) . . ? C32 C31 P 121.2(14) . . ? C31 C32 C33 120(2) . . ? C34 C33 C32 119(2) . . ? C33 C34 C35 122(2) . . ? C34 C35 C36 118(2) . . ? C31 C36 C35 121(2) . . ? C42 C41 C46 119.6(18) . . ? C42 C41 P 118.8(15) . . ? C46 C41 P 121.5(15) . . ? C41 C42 C43 119(2) . . ? C44 C43 C42 121(2) . . ? C45 C44 C43 119(2) . . ? C44 C45 C46 119(2) . . ? C41 C46 C45 121.6(18) . . ? C52 C51 C56 118.1(18) . . ? C52 C51 P 120.3(15) . . ? C56 C51 P 121.3(14) . . ? C51 C52 C53 121(2) . . ? C54 C53 C52 120(2) . . ? C53 C54 C55 121(2) . . ? C54 C55 C56 119(2) . . ? C51 C56 C55 120.6(19) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 19.99 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.889 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.142