Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_name_full 'J.Chem.Soc.,Dalton Trans.' #============================================================================== _journal_coden_Cambridge 0186 # 0. AUDIT DETAILS _audit_creation_date ' 2002' _audit_creation_method SHELX-97 _audit_update_record ? #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry and Biochemistry Baylor University PO Box 97348 Waco TX, 76798-7348 USA ; _publ_contact_author_email Gordon_Stone@baylor.edu _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_category ? _publ_requested_coeditor_name ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and reactivity of icosahedral molybdenum-monocarbaborane complexes containing one or two intramolecular amino bridges ; loop_ _publ_author_name _publ_author_address S.Du ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; J.A.Kautz ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; T.D.McGrath ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; F.G.A.Stone ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #============================================================================== _publ_section_exptl_refinement ; Diffracted intensities were collected on an Enraf-Nonius CAD-4 using graphite-monochromated Mo-K\a 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. Hydrogen atoms were constrained to idealized geometries and assigned isotropic displacement parameters 1.2 times U~iso~ value of the parent atom, except for methyl hydrogens where U~iso~ = 1.5 U~iso~. Data were processed by the SHELXTL program (Bruker, 1995). ; _publ_section_references ; Enraf-Nonius (1989). CAD-4 Software. Version 5. Enraf-Nonius, Delft, The Netherlands. 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 crystal structure refinement. University of G\\"ottingen, Germany. Siemens (1995). SHELXTL-PC. Version 5.03. Bruker Analytical X-ray Instruments Inc. (1995), Madison, Wisconsin, USA. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_3b _database_code_CSD 192675 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H35 B10 Fe Mo N O6' _chemical_formula_weight 669.40 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' N N 0.0061 0.0033 '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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.346(2) _cell_length_b 18.006(3) _cell_length_c 18.339(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.94(2) _cell_angle_gamma 90.00 _cell_volume 3085.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description blocks _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.7538 _exptl_absorpt_correction_T_max 0.9422 _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_% none _diffrn_reflns_number 6443 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.1377 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 20.04 _reflns_number_total 5728 _reflns_number_gt 3974 _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^)+(0.0373P)^2^+2.4519P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.11(5) _refine_ls_number_reflns 5728 _refine_ls_number_parameters 608 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1175 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1375 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.4023(2) -0.37228(9) 0.92057(8) 0.0399(5) Uani 1 d . . C1 C 0.3242(16) -0.3849(10) 1.0422(8) 0.037(5) Uani 1 d . . H1 H 0.4038(16) -0.4199(10) 1.0707(8) 0.045 Uiso 1 calc R . B2 B 0.3601(23) -0.2945(11) 1.0130(11) 0.039(3) Uani 1 d . . B3 B 0.2281(22) -0.2761(12) 0.9352(11) 0.039(3) Uani 1 d . . H3 H 0.2372(22) -0.2353(12) 0.8909(11) 0.046 Uiso 1 calc R . B4 B 0.1407(19) -0.3606(11) 0.9171(10) 0.039(3) Uani 1 d . . H4 H 0.0976(19) -0.3753(11) 0.8629(10) 0.046 Uiso 1 calc R . B5 B 0.2126(21) -0.4296(11) 0.9863(10) 0.039(3) Uani 1 d . . H5 H 0.2178(21) -0.4894(11) 0.9742(10) 0.046 Uiso 1 calc R . B6 B 0.2604(20) -0.3141(11) 1.0889(10) 0.040(6) Uani 1 d . . H6 H 0.3009(20) -0.2988(11) 1.1436(10) 0.047 Uiso 1 calc R . B7 B 0.2002(20) -0.2452(10) 1.0261(10) 0.034(5) Uani 1 d . . H7 H 0.2024(20) -0.1856(10) 1.0393(10) 0.040 Uiso 1 calc R . B8 B 0.0620(22) -0.2906(11) 0.9715(9) 0.035(6) Uani 1 d . . H8 H -0.0324(22) -0.2604(11) 0.9506(9) 0.042 Uiso 1 calc R . B9 B 0.0483(18) -0.3833(11) 1.0009(9) 0.029(5) Uani 1 d . . H9 H -0.0523(18) -0.4149(11) 0.9979(9) 0.034 Uiso 1 calc R . B10 B 0.1635(20) -0.3955(12) 1.0740(10) 0.046(7) Uani 1 d . . H10 H 0.1363(20) -0.4330(12) 1.1191(10) 0.055 Uiso 1 calc R . B11 B 0.0764(20) -0.3090(11) 1.0636(11) 0.042(6) Uani 1 d . . H11 H -0.0064(20) -0.2894(11) 1.1010(11) 0.051 Uiso 1 calc R . C2 C 0.4443(20) -0.3246(13) 0.8289(11) 0.065(6) Uani 1 d . . O2 O 0.4594(17) -0.2920(11) 0.7751(8) 0.113(7) Uani 1 d . . C3 C 0.3477(21) -0.4550(12) 0.8551(11) 0.052(6) Uani 1 d . . O3 O 0.3131(16) -0.5052(9) 0.8184(7) 0.081(5) Uani 1 d . . C4 C 0.5702(22) -0.4375(11) 0.9330(10) 0.051(6) Uani 1 d . . O4 O 0.6650(16) -0.4800(8) 0.9401(8) 0.086(5) Uani 1 d . . N1 N 0.5072(14) -0.2819(7) 0.9912(8) 0.031(4) Uani 1 d . . C11 C 0.6251(17) -0.3075(9) 1.0417(9) 0.046(5) Uani 1 d . . H11A H 0.7125(17) -0.3135(9) 1.0145(9) 0.056 Uiso 1 calc R . H11B H 0.6001(17) -0.3553(9) 1.0623(9) 0.056 Uiso 1 calc R . C12 C 0.6501(21) -0.2520(11) 1.1027(12) 0.080(7) Uani 1 d . . H12A H 0.7273(21) -0.2694(11) 1.1343(12) 0.096 Uiso 1 calc R . H12B H 0.5644(21) -0.2481(11) 1.1316(12) 0.096 Uiso 1 calc R . C13 C 0.6889(22) -0.1741(13) 1.0717(13) 0.083(8) Uani 1 d . . H13A H 0.6971(22) -0.1386(13) 1.1113(13) 0.100 Uiso 1 calc R . H13B H 0.7804(22) -0.1766(13) 1.0476(13) 0.100 Uiso 1 calc R . C14 C 0.5742(23) -0.1488(10) 1.0177(12) 0.076(7) Uani 1 d . . H14A H 0.4858(23) -0.1393(10) 1.0431(12) 0.091 Uiso 1 calc R . H14B H 0.6038(23) -0.1031(10) 0.9944(12) 0.091 Uiso 1 calc R . C15 C 0.5499(20) -0.2081(12) 0.9610(11) 0.073(7) Uani 1 d . . H15A H 0.6371(20) -0.2143(12) 0.9337(11) 0.088 Uiso 1 calc R . H15B H 0.4759(20) -0.1914(12) 0.9272(11) 0.088 Uiso 1 calc R . Fe1 Fe -0.0294(3) -0.55708(14) 1.24956(12) 0.0403(7) Uani 1 d . . C201 C -0.1181(19) -0.6658(9) 1.2486(9) 0.040(2) Uani 1 d . . C202 C -0.2211(18) -0.6077(9) 1.2280(8) 0.040(2) Uani 1 d . . C203 C -0.1797(18) -0.5791(9) 1.1626(8) 0.040(2) Uani 1 d . . C204 C -0.0417(19) -0.6079(10) 1.1475(9) 0.040(2) Uani 1 d . . C205 C -0.0106(19) -0.6599(10) 1.1990(9) 0.040(2) Uani 1 d . . C206 C -0.1363(22) -0.7216(11) 1.3093(10) 0.080(3) Uani 1 d . . H20A H -0.2229(22) -0.7111(11) 1.3348(10) 0.120 Uiso 1 calc R . H20B H -0.0562(22) -0.7184(11) 1.3427(10) 0.120 Uiso 1 calc R . H20C H -0.1412(22) -0.7707(11) 1.2891(10) 0.120 Uiso 1 calc R . C207 C -0.3649(21) -0.5990(12) 1.2650(10) 0.080(3) Uani 1 d . . H20D H -0.3630(21) -0.6254(12) 1.3105(10) 0.120 Uiso 1 calc R . H20E H -0.4393(21) -0.6188(12) 1.2340(10) 0.120 Uiso 1 calc R . H20F H -0.3829(21) -0.5473(12) 1.2739(10) 0.120 Uiso 1 calc R . C208 C -0.2655(21) -0.5227(11) 1.1169(10) 0.080(3) Uani 1 d . . H20G H -0.2142(21) -0.5112(11) 1.0734(10) 0.120 Uiso 1 calc R . H20H H -0.2789(21) -0.4782(11) 1.1448(10) 0.120 Uiso 1 calc R . H20I H -0.3570(21) -0.5435(11) 1.1039(10) 0.120 Uiso 1 calc R . C209 C 0.0352(21) -0.5908(11) 1.0777(10) 0.080(3) Uani 1 d . . H20J H -0.0125(21) -0.5508(11) 1.0527(10) 0.120 Uiso 1 calc R . H20K H 0.0349(21) -0.6341(11) 1.0471(10) 0.120 Uiso 1 calc R . H20L H 0.1322(21) -0.5767(11) 1.0889(10) 0.120 Uiso 1 calc R . C210 C 0.1190(22) -0.7122(12) 1.1985(10) 0.080(3) Uani 1 d . . H21A H 0.1170(22) -0.7438(12) 1.2406(10) 0.120 Uiso 1 calc R . H21B H 0.2055(22) -0.6834(12) 1.1994(10) 0.120 Uiso 1 calc R . H21C H 0.1156(22) -0.7420(12) 1.1551(10) 0.120 Uiso 1 calc R . C211 C -0.0756(20) -0.4591(13) 1.2424(9) 0.051(6) Uani 1 d . . O211 O -0.1074(17) -0.3982(8) 1.2388(8) 0.086(5) Uani 1 d . . C212 C -0.0289(22) -0.5604(11) 1.3471(11) 0.060(6) Uani 1 d . . O212 O -0.0248(17) -0.5716(9) 1.4090(7) 0.088(5) Uani 1 d . . C213 C 0.1516(24) -0.5428(10) 1.2421(10) 0.052(6) Uani 1 d . . O213 O 0.2759(15) -0.5363(8) 1.2321(8) 0.084(5) Uani 1 d . . Mo2 Mo -0.5124(2) -0.82554(9) 0.62335(8) 0.0464(5) Uani 1 d . . C101 C -0.4175(20) -0.8850(13) 0.5223(10) 0.070(7) Uani 1 d . . H101 H -0.5048(20) -0.9200(13) 0.5005(10) 0.084 Uiso 1 calc R . B102 B -0.4148(26) -0.7875(15) 0.5203(13) 0.054(3) Uani 1 d . . B103 B -0.3090(23) -0.7558(14) 0.5948(12) 0.054(3) Uani 1 d . . H103 H -0.3196(23) -0.7023(14) 0.6231(12) 0.064 Uiso 1 calc R . B104 B -0.2594(21) -0.8312(13) 0.6436(11) 0.054(3) Uani 1 d . . H104 H -0.2413(21) -0.8295(13) 0.7030(11) 0.064 Uiso 1 calc R . B105 B -0.3241(24) -0.9159(14) 0.5976(13) 0.054(3) Uani 1 d . . H105 H -0.3463(24) -0.9688(14) 0.6251(13) 0.064 Uiso 1 calc R . B106 B -0.3051(22) -0.8377(14) 0.4613(12) 0.061(8) Uani 1 d . . H106 H -0.3222(22) -0.8385(14) 0.4018(12) 0.073 Uiso 1 calc R . B107 B -0.2412(22) -0.7578(13) 0.5073(11) 0.052(7) Uani 1 d . . H107 H -0.2179(22) -0.7066(13) 0.4769(11) 0.062 Uiso 1 calc R . B108 B -0.1370(27) -0.7859(16) 0.5823(12) 0.063(8) Uani 1 d . . H108 H -0.0417(27) -0.7545(16) 0.6000(12) 0.075 Uiso 1 calc R . B109 B -0.1503(26) -0.8821(18) 0.5889(12) 0.081(9) Uani 1 d . . H109 H -0.0626(26) -0.9134(18) 0.6152(12) 0.097 Uiso 1 calc R . B110 B -0.2403(28) -0.9178(14) 0.5096(14) 0.067(8) Uani 1 d . . H110 H -0.2116(28) -0.9695(14) 0.4816(14) 0.080 Uiso 1 calc R . B111 B -0.1367(22) -0.8384(13) 0.5047(13) 0.063(8) Uani 1 d . . H111 H -0.0385(22) -0.8411(13) 0.4726(13) 0.076 Uiso 1 calc R . C102 C -0.4998(21) -0.8755(14) 0.7216(11) 0.068(6) Uani 1 d . . O102 O -0.5051(18) -0.9056(8) 0.7768(8) 0.090(5) Uani 1 d . . C103 C -0.6746(21) -0.8946(14) 0.6122(11) 0.073(8) Uani 1 d . . O103 O -0.7577(19) -0.9410(12) 0.6027(9) 0.128(7) Uani 1 d . . C104 C -0.5903(20) -0.7429(12) 0.6835(11) 0.059(6) Uani 1 d . . O104 O -0.6352(16) -0.6942(10) 0.7164(8) 0.097(6) Uani 1 d . . N101 N -0.5614(17) -0.7597(9) 0.5213(8) 0.053(5) Uani 1 d . . C111 C -0.5782(26) -0.6746(14) 0.5285(12) 0.101(9) Uani 1 d . . H11C H -0.6702(26) -0.6641(14) 0.5500(12) 0.122 Uiso 1 calc R . H11D H -0.5046(26) -0.6562(14) 0.5618(12) 0.122 Uiso 1 calc R . C112 C -0.5681(38) -0.6324(17) 0.4566(16) 0.158(15) Uani 1 d . . H11D' H -0.5858(38) -0.5800(17) 0.4648(16) 0.189 Uiso 1 calc R . H11E H -0.4726(38) -0.6377(17) 0.4373(16) 0.189 Uiso 1 calc R . C113 C -0.6775(38) -0.6627(22) 0.4018(18) 0.162(17) Uani 1 d . . H11F H -0.6643(38) -0.6386(22) 0.3551(18) 0.195 Uiso 1 calc R . H11G H -0.7730(38) -0.6509(22) 0.4182(18) 0.195 Uiso 1 calc R . C114 C -0.6644(29) -0.7472(18) 0.3920(11) 0.125(12) Uani 1 d . . H11H H -0.5733(29) -0.7594(18) 0.3704(11) 0.150 Uiso 1 calc R . H11I H -0.7404(29) -0.7653(18) 0.3601(11) 0.150 Uiso 1 calc R . C115 C -0.6758(22) -0.7852(14) 0.4708(12) 0.107(9) Uani 1 d . . H11J H -0.7681(22) -0.7735(14) 0.4913(12) 0.129 Uiso 1 calc R . H11K H -0.6698(22) -0.8387(14) 0.4655(12) 0.129 Uiso 1 calc R . Fe2 Fe -0.0961(3) -0.50956(13) 0.74209(13) 0.0431(7) Uani 1 d . . C301 C -0.2385(19) -0.6008(10) 0.7408(9) 0.045(2) Uani 1 d . . C302 C -0.1013(19) -0.6275(10) 0.7213(10) 0.045(2) Uani 1 d . . C303 C -0.0557(19) -0.5898(10) 0.6605(9) 0.045(2) Uani 1 d . . C304 C -0.1642(19) -0.5405(9) 0.6375(9) 0.045(2) Uani 1 d . . C305 C -0.2757(19) -0.5458(10) 0.6856(8) 0.045(2) Uani 1 d . . C306 C -0.3303(21) -0.6286(11) 0.8006(10) 0.080(3) Uani 1 d . . H30A H -0.4174(21) -0.6005(11) 0.8014(10) 0.120 Uiso 1 calc R . H30B H -0.2803(21) -0.6233(11) 0.8464(10) 0.120 Uiso 1 calc R . H30C H -0.3522(21) -0.6801(11) 0.7924(10) 0.120 Uiso 1 calc R . C307 C -0.0190(22) -0.6860(11) 0.7619(11) 0.080(3) Uani 1 d . . H30D H -0.0742(22) -0.7033(11) 0.8022(11) 0.120 Uiso 1 calc R . H30E H 0.0697(22) -0.6655(11) 0.7798(11) 0.120 Uiso 1 calc R . H30F H 0.0004(22) -0.7267(11) 0.7298(11) 0.120 Uiso 1 calc R . C308 C 0.0827(22) -0.6008(11) 0.6201(11) 0.080(3) Uani 1 d . . H30G H 0.0860(22) -0.5669(11) 0.5797(11) 0.120 Uiso 1 calc R . H30H H 0.0876(22) -0.6509(11) 0.6024(11) 0.120 Uiso 1 calc R . H30I H 0.1623(22) -0.5914(11) 0.6525(11) 0.120 Uiso 1 calc R . C309 C -0.1734(22) -0.4937(11) 0.5659(10) 0.080(3) Uani 1 d . . H30J H -0.0846(22) -0.4974(11) 0.5406(10) 0.120 Uiso 1 calc R . H30K H -0.1916(22) -0.4427(11) 0.5778(10) 0.120 Uiso 1 calc R . H30L H -0.2497(22) -0.5123(11) 0.5354(10) 0.120 Uiso 1 calc R . C310 C -0.4249(20) -0.5121(11) 0.6762(10) 0.080(3) Uani 1 d . . H31A H -0.4816(20) -0.5244(11) 0.7177(10) 0.120 Uiso 1 calc R . H31B H -0.4698(20) -0.5317(11) 0.6328(10) 0.120 Uiso 1 calc R . H31C H -0.4171(20) -0.4591(11) 0.6722(10) 0.120 Uiso 1 calc R . C311 C -0.0374(21) -0.5288(11) 0.8315(13) 0.069(7) Uani 1 d . . O311 O -0.0102(17) -0.5484(8) 0.8908(7) 0.088(5) Uani 1 d . . C312 C 0.0537(23) -0.4582(14) 0.7158(10) 0.073(7) Uani 1 d . . O312 O 0.1528(18) -0.4258(10) 0.6964(9) 0.111(6) Uani 1 d . . C313 C -0.1918(22) -0.4283(12) 0.7646(13) 0.073(7) Uani 1 d . . O313 O -0.2535(17) -0.3766(10) 0.7800(10) 0.124(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0422(10) 0.0448(11) 0.0330(10) 0.0026(10) 0.0051(8) 0.0045(10) C1 0.040(11) 0.033(12) 0.039(11) 0.009(10) 0.003(9) 0.006(10) B2 0.050(7) 0.036(7) 0.030(6) -0.008(6) 0.005(6) 0.010(6) B3 0.050(7) 0.036(7) 0.030(6) -0.008(6) 0.005(6) 0.010(6) B4 0.050(7) 0.036(7) 0.030(6) -0.008(6) 0.005(6) 0.010(6) B5 0.050(7) 0.036(7) 0.030(6) -0.008(6) 0.005(6) 0.010(6) B6 0.038(13) 0.045(15) 0.036(12) -0.015(12) 0.014(10) 0.004(12) B7 0.055(15) 0.006(11) 0.040(13) 0.009(10) 0.004(11) 0.002(10) B8 0.045(14) 0.042(14) 0.020(12) -0.006(10) -0.004(10) -0.003(11) B9 0.023(11) 0.022(13) 0.041(12) -0.004(11) -0.011(9) -0.013(10) B10 0.038(14) 0.065(19) 0.034(13) 0.000(12) 0.008(11) -0.006(12) B11 0.017(12) 0.051(17) 0.059(15) -0.014(13) 0.007(10) -0.001(12) C2 0.065(14) 0.086(16) 0.045(13) -0.011(15) 0.020(12) -0.008(15) O2 0.104(14) 0.169(19) 0.068(12) 0.041(13) 0.019(11) 0.016(12) C3 0.048(14) 0.059(17) 0.051(15) 0.006(12) 0.014(12) 0.020(13) O3 0.097(12) 0.081(12) 0.066(10) -0.024(10) -0.007(9) 0.011(10) C4 0.060(16) 0.051(15) 0.043(13) 0.001(11) -0.003(12) 0.012(12) O4 0.079(11) 0.087(13) 0.090(11) -0.014(10) -0.035(9) 0.027(10) N1 0.016(8) 0.025(9) 0.052(10) 0.007(8) -0.001(7) 0.003(7) C11 0.048(12) 0.030(12) 0.061(12) -0.034(11) 0.010(11) -0.005(10) C12 0.069(16) 0.054(16) 0.116(21) 0.016(15) -0.002(14) 0.006(13) C13 0.062(17) 0.095(21) 0.092(19) -0.041(16) 0.009(15) -0.013(15) C14 0.088(19) 0.038(14) 0.102(19) -0.009(14) 0.014(16) -0.040(13) C15 0.037(13) 0.081(18) 0.101(19) 0.038(16) -0.015(12) -0.026(13) Fe1 0.054(2) 0.036(2) 0.031(2) -0.0051(14) 0.0009(14) -0.0031(15) C201 0.059(6) 0.034(6) 0.025(5) 0.002(4) 0.000(5) -0.009(5) C202 0.059(6) 0.034(6) 0.025(5) 0.002(4) 0.000(5) -0.009(5) C203 0.059(6) 0.034(6) 0.025(5) 0.002(4) 0.000(5) -0.009(5) C204 0.059(6) 0.034(6) 0.025(5) 0.002(4) 0.000(5) -0.009(5) C205 0.059(6) 0.034(6) 0.025(5) 0.002(4) 0.000(5) -0.009(5) C206 0.100(9) 0.080(8) 0.060(7) 0.005(6) -0.006(6) 0.001(7) C207 0.100(9) 0.080(8) 0.060(7) 0.005(6) -0.006(6) 0.001(7) C208 0.100(9) 0.080(8) 0.060(7) 0.005(6) -0.006(6) 0.001(7) C209 0.100(9) 0.080(8) 0.060(7) 0.005(6) -0.006(6) 0.001(7) C210 0.100(9) 0.080(8) 0.060(7) 0.005(6) -0.006(6) 0.001(7) C211 0.054(14) 0.085(18) 0.014(11) -0.008(12) -0.004(9) 0.017(14) O211 0.113(13) 0.041(10) 0.103(13) -0.004(10) 0.004(10) 0.006(10) C212 0.091(17) 0.037(13) 0.054(14) -0.008(13) 0.023(14) -0.005(13) O212 0.125(14) 0.096(13) 0.045(9) -0.005(10) 0.014(10) 0.014(11) C213 0.073(16) 0.030(13) 0.052(13) 0.003(10) -0.016(13) -0.035(12) O213 0.059(10) 0.087(13) 0.104(12) 0.014(9) -0.014(10) -0.024(10) Mo2 0.0450(11) 0.0577(12) 0.0365(10) -0.0032(10) 0.0022(8) -0.0051(10) C101 0.057(14) 0.079(19) 0.074(15) -0.013(15) -0.017(12) 0.008(14) B102 0.050(8) 0.061(9) 0.050(8) 0.001(7) 0.004(6) -0.008(7) B103 0.050(8) 0.061(9) 0.050(8) 0.001(7) 0.004(6) -0.008(7) B104 0.050(8) 0.061(9) 0.050(8) 0.001(7) 0.004(6) -0.008(7) B105 0.050(8) 0.061(9) 0.050(8) 0.001(7) 0.004(6) -0.008(7) B106 0.056(16) 0.093(22) 0.034(13) -0.018(15) 0.018(12) -0.018(16) B107 0.046(16) 0.068(19) 0.041(15) 0.010(13) 0.021(12) -0.026(14) B108 0.058(18) 0.094(21) 0.037(15) 0.000(14) 0.012(13) -0.002(15) B109 0.078(20) 0.107(26) 0.056(17) 0.014(19) -0.032(14) 0.021(20) B110 0.093(22) 0.038(17) 0.068(19) -0.010(14) -0.018(17) 0.029(16) B111 0.035(14) 0.053(18) 0.102(21) -0.026(15) 0.014(13) 0.027(14) C102 0.074(15) 0.059(15) 0.071(15) 0.003(16) -0.009(13) -0.028(15) O102 0.134(14) 0.074(12) 0.062(10) 0.030(9) 0.003(11) -0.013(10) C103 0.044(15) 0.120(24) 0.056(14) -0.012(15) 0.000(12) -0.018(14) O103 0.106(15) 0.191(21) 0.086(13) -0.018(13) 0.013(11) -0.079(14) C104 0.040(14) 0.084(18) 0.052(14) 0.021(13) 0.005(11) 0.035(13) O104 0.074(12) 0.128(16) 0.087(12) -0.027(11) -0.002(9) 0.044(11) N101 0.062(12) 0.055(13) 0.043(11) -0.027(9) 0.013(9) 0.004(10) C111 0.119(22) 0.127(25) 0.059(16) 0.002(17) 0.011(15) 0.051(19) C112 0.247(44) 0.120(27) 0.107(25) 0.060(23) 0.040(26) 0.090(29) C113 0.190(38) 0.188(40) 0.108(29) 0.042(28) 0.005(24) 0.112(33) C114 0.130(25) 0.215(37) 0.029(15) 0.026(19) -0.017(15) 0.042(25) C115 0.073(17) 0.161(26) 0.086(18) -0.005(18) -0.044(15) 0.036(17) Fe2 0.048(2) 0.037(2) 0.044(2) 0.0042(14) 0.0019(14) -0.0035(15) C301 0.054(6) 0.042(6) 0.040(6) 0.004(5) -0.002(5) -0.005(5) C302 0.054(6) 0.042(6) 0.040(6) 0.004(5) -0.002(5) -0.005(5) C303 0.054(6) 0.042(6) 0.040(6) 0.004(5) -0.002(5) -0.005(5) C304 0.054(6) 0.042(6) 0.040(6) 0.004(5) -0.002(5) -0.005(5) C305 0.054(6) 0.042(6) 0.040(6) 0.004(5) -0.002(5) -0.005(5) C306 0.098(8) 0.067(8) 0.074(7) 0.014(6) -0.004(6) 0.003(6) C307 0.098(8) 0.067(8) 0.074(7) 0.014(6) -0.004(6) 0.003(6) C308 0.098(8) 0.067(8) 0.074(7) 0.014(6) -0.004(6) 0.003(6) C309 0.098(8) 0.067(8) 0.074(7) 0.014(6) -0.004(6) 0.003(6) C310 0.098(8) 0.067(8) 0.074(7) 0.014(6) -0.004(6) 0.003(6) C311 0.050(14) 0.056(16) 0.102(20) 0.041(15) -0.030(14) -0.020(11) O311 0.136(15) 0.073(11) 0.056(10) 0.013(9) -0.026(10) -0.011(11) C312 0.066(17) 0.121(21) 0.031(13) 0.005(13) -0.007(12) -0.018(16) O312 0.086(13) 0.128(15) 0.118(14) 0.034(11) 0.029(11) -0.045(11) C313 0.052(15) 0.057(17) 0.109(19) -0.014(15) -0.017(14) 0.022(13) O313 0.121(14) 0.053(11) 0.200(18) -0.045(14) 0.050(13) 0.008(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.93(2) . ? Mo1 C4 1.97(2) . ? Mo1 C3 1.98(2) . ? Mo1 B2 2.24(2) . ? Mo1 N1 2.291(13) . ? Mo1 C1 2.370(15) . ? Mo1 B3 2.39(2) . ? Mo1 B5 2.39(2) . ? Mo1 B4 2.45(2) . ? C1 B10 1.63(2) . ? C1 B6 1.65(2) . ? C1 B5 1.66(2) . ? C1 B2 1.75(3) . ? B2 N1 1.46(2) . ? B2 B6 1.72(3) . ? B2 B7 1.76(3) . ? B2 B3 1.90(3) . ? B3 B8 1.72(3) . ? B3 B4 1.76(3) . ? B3 B7 1.78(3) . ? B4 B8 1.78(3) . ? B4 B9 1.82(2) . ? B4 B5 1.89(3) . ? B5 B9 1.77(3) . ? B5 B10 1.79(3) . ? B6 B10 1.74(3) . ? B6 B11 1.78(3) . ? B6 B7 1.78(3) . ? B7 B11 1.78(3) . ? B7 B8 1.82(3) . ? B8 B11 1.72(3) . ? B8 B9 1.76(3) . ? B9 B10 1.72(2) . ? B9 B11 1.78(3) . ? B10 B11 1.77(3) . ? C2 O2 1.16(2) . ? C3 O3 1.17(2) . ? C4 O4 1.18(2) . ? N1 C15 1.50(2) . ? N1 C11 1.50(2) . ? C11 C12 1.51(2) . ? C12 C13 1.56(3) . ? C13 C14 1.52(3) . ? C14 C15 1.50(2) . ? Fe1 C213 1.72(2) . ? Fe1 C212 1.79(2) . ? Fe1 C211 1.82(2) . ? Fe1 C202 2.04(2) . ? Fe1 C205 2.08(2) . ? Fe1 C204 2.08(2) . ? Fe1 C201 2.13(2) . ? Fe1 C203 2.15(2) . ? C201 C205 1.37(2) . ? C201 C202 1.47(2) . ? C201 C206 1.51(2) . ? C202 C203 1.37(2) . ? C202 C207 1.52(2) . ? C203 C204 1.42(2) . ? C203 C208 1.53(2) . ? C204 C205 1.36(2) . ? C204 C209 1.51(2) . ? C205 C210 1.53(2) . ? C211 O211 1.14(2) . ? C212 O212 1.15(2) . ? C213 O213 1.19(2) . ? Mo2 C103 1.97(2) . ? Mo2 C104 2.00(2) . ? Mo2 C102 2.02(2) . ? Mo2 B102 2.22(2) . ? Mo2 N101 2.26(2) . ? Mo2 C101 2.33(2) . ? Mo2 B103 2.34(2) . ? Mo2 B104 2.39(2) . ? Mo2 B105 2.45(2) . ? C101 B105 1.71(3) . ? C101 B102 1.76(3) . ? C101 B106 1.77(3) . ? C101 B110 1.78(3) . ? B102 N101 1.46(3) . ? B102 B107 1.73(3) . ? B102 B106 1.75(3) . ? B102 B103 1.77(3) . ? B103 B104 1.69(3) . ? B103 B108 1.71(3) . ? B103 B107 1.73(3) . ? B104 B109 1.71(3) . ? B104 B108 1.81(3) . ? B104 B105 1.84(3) . ? B105 B109 1.74(3) . ? B105 B110 1.80(3) . ? B106 B111 1.75(3) . ? B106 B107 1.77(3) . ? B106 B110 1.79(3) . ? B107 B111 1.75(3) . ? B107 B108 1.75(3) . ? B108 B111 1.71(3) . ? B108 B109 1.74(4) . ? B109 B111 1.74(3) . ? B109 B110 1.79(3) . ? B110 B111 1.73(3) . ? C102 O102 1.15(2) . ? C103 O103 1.15(2) . ? C104 O104 1.15(2) . ? N101 C115 1.48(2) . ? N101 C111 1.55(2) . ? C111 C112 1.53(3) . ? C112 C113 1.52(4) . ? C113 C114 1.54(4) . ? C114 C115 1.60(3) . ? Fe2 C312 1.75(2) . ? Fe2 C311 1.75(2) . ? Fe2 C313 1.77(2) . ? Fe2 C305 2.06(2) . ? Fe2 C304 2.09(2) . ? Fe2 C301 2.11(2) . ? Fe2 C303 2.12(2) . ? Fe2 C302 2.16(2) . ? C301 C302 1.42(2) . ? C301 C305 1.45(2) . ? C301 C306 1.49(2) . ? C302 C303 1.38(2) . ? C302 C307 1.50(2) . ? C303 C304 1.41(2) . ? C303 C308 1.51(2) . ? C304 C305 1.38(2) . ? C304 C309 1.56(2) . ? C305 C310 1.53(2) . ? C311 O311 1.17(2) . ? C312 O312 1.16(2) . ? C313 O313 1.13(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 C2 Mo1 C4 101.1(8) . . ? C2 Mo1 C3 82.0(8) . . ? C4 Mo1 C3 79.5(8) . . ? C2 Mo1 B2 114.9(9) . . ? C4 Mo1 B2 115.8(8) . . ? C3 Mo1 B2 152.3(8) . . ? C2 Mo1 N1 94.9(7) . . ? C4 Mo1 N1 91.4(6) . . ? C3 Mo1 N1 169.6(6) . . ? B2 Mo1 N1 37.5(6) . . ? C2 Mo1 C1 158.6(8) . . ? C4 Mo1 C1 95.2(7) . . ? C3 Mo1 C1 114.8(7) . . ? B2 Mo1 C1 44.5(7) . . ? N1 Mo1 C1 70.8(5) . . ? C2 Mo1 B3 85.7(8) . . ? C4 Mo1 B3 163.6(7) . . ? C3 Mo1 B3 116.4(7) . . ? B2 Mo1 B3 48.3(7) . . ? N1 Mo1 B3 73.0(6) . . ? C1 Mo1 B3 75.1(6) . . ? C2 Mo1 B5 142.4(7) . . ? C4 Mo1 B5 106.2(7) . . ? C3 Mo1 B5 78.2(7) . . ? B2 Mo1 B5 75.4(7) . . ? N1 Mo1 B5 109.6(6) . . ? C1 Mo1 B5 40.8(6) . . ? B3 Mo1 B5 75.2(7) . . ? C2 Mo1 B4 99.0(7) . . ? C4 Mo1 B4 147.7(7) . . ? C3 Mo1 B4 78.6(7) . . ? B2 Mo1 B4 77.2(7) . . ? N1 Mo1 B4 111.8(5) . . ? C1 Mo1 B4 73.2(6) . . ? B3 Mo1 B4 42.4(7) . . ? B5 Mo1 B4 45.9(6) . . ? B10 C1 B6 64.1(11) . . ? B10 C1 B5 65.8(11) . . ? B6 C1 B5 117.8(13) . . ? B10 C1 B2 113.6(14) . . ? B6 C1 B2 60.9(11) . . ? B5 C1 B2 112.6(13) . . ? B10 C1 Mo1 130.3(11) . . ? B6 C1 Mo1 122.2(11) . . ? B5 C1 Mo1 70.4(8) . . ? B2 C1 Mo1 63.8(7) . . ? N1 B2 B6 141.1(17) . . ? N1 B2 C1 114.6(14) . . ? B6 B2 C1 56.8(11) . . ? N1 B2 B7 140.1(16) . . ? B6 B2 B7 61.4(11) . . ? C1 B2 B7 105.1(14) . . ? N1 B2 B3 111.8(15) . . ? B6 B2 B3 106.8(15) . . ? C1 B2 B3 105.5(14) . . ? B7 B2 B3 58.1(11) . . ? N1 B2 Mo1 73.2(9) . . ? B6 B2 Mo1 126.0(13) . . ? C1 B2 Mo1 71.7(8) . . ? B7 B2 Mo1 125.5(13) . . ? B3 B2 Mo1 70.2(9) . . ? B8 B3 B4 61.4(11) . . ? B8 B3 B7 62.4(10) . . ? B4 B3 B7 111.9(15) . . ? B8 B3 B2 105.2(14) . . ? B4 B3 B2 106.5(15) . . ? B7 B3 B2 56.9(10) . . ? B8 B3 Mo1 123.6(13) . . ? B4 B3 Mo1 70.6(9) . . ? B7 B3 Mo1 116.2(12) . . ? B2 B3 Mo1 61.6(8) . . ? B3 B4 B8 58.3(11) . . ? B3 B4 B9 105.1(13) . . ? B8 B4 B9 58.6(10) . . ? B3 B4 B5 106.5(14) . . ? B8 B4 B5 103.6(12) . . ? B9 B4 B5 57.0(10) . . ? B3 B4 Mo1 67.0(9) . . ? B8 B4 Mo1 117.9(11) . . ? B9 B4 Mo1 116.4(10) . . ? B5 B4 Mo1 65.4(8) . . ? C1 B5 B9 102.5(13) . . ? C1 B5 B10 56.3(10) . . ? B9 B5 B10 57.8(10) . . ? C1 B5 B4 108.0(14) . . ? B9 B5 B4 59.5(10) . . ? B10 B5 B4 106.5(13) . . ? C1 B5 Mo1 68.8(9) . . ? B9 B5 Mo1 121.6(12) . . ? B10 B5 Mo1 120.5(12) . . ? B4 B5 Mo1 68.7(8) . . ? C1 B6 B2 62.3(10) . . ? C1 B6 B10 57.4(11) . . ? B2 B6 B10 109.4(14) . . ? C1 B6 B11 105.1(14) . . ? B2 B6 B11 108.2(15) . . ? B10 B6 B11 60.3(11) . . ? C1 B6 B7 108.4(13) . . ? B2 B6 B7 60.2(11) . . ? B10 B6 B7 109.1(14) . . ? B11 B6 B7 60.0(11) . . ? B2 B7 B3 64.9(11) . . ? B2 B7 B11 106.7(13) . . ? B3 B7 B11 105.5(14) . . ? B2 B7 B6 58.3(11) . . ? B3 B7 B6 109.8(13) . . ? B11 B7 B6 60.0(10) . . ? B2 B7 B8 107.2(14) . . ? B3 B7 B8 57.1(11) . . ? B11 B7 B8 57.4(10) . . ? B6 B7 B8 104.9(13) . . ? B3 B8 B11 110.6(14) . . ? B3 B8 B9 109.4(15) . . ? B11 B8 B9 61.5(11) . . ? B3 B8 B4 60.3(11) . . ? B11 B8 B4 112.8(14) . . ? B9 B8 B4 62.0(10) . . ? B3 B8 B7 60.5(11) . . ? B11 B8 B7 60.2(10) . . ? B9 B8 B7 108.3(13) . . ? B4 B8 B7 109.4(14) . . ? B10 B9 B8 108.2(14) . . ? B10 B9 B5 61.6(10) . . ? B8 B9 B5 109.5(14) . . ? B10 B9 B11 60.6(11) . . ? B8 B9 B11 58.3(11) . . ? B5 B9 B11 109.4(12) . . ? B10 B9 B4 112.8(13) . . ? B8 B9 B4 59.4(10) . . ? B5 B9 B4 63.5(10) . . ? B11 B9 B4 108.0(13) . . ? C1 B10 B9 105.9(13) . . ? C1 B10 B6 58.5(11) . . ? B9 B10 B6 109.4(15) . . ? C1 B10 B11 106.5(15) . . ? B9 B10 B11 61.4(11) . . ? B6 B10 B11 60.9(11) . . ? C1 B10 B5 57.8(10) . . ? B9 B10 B5 60.6(11) . . ? B6 B10 B5 106.8(14) . . ? B11 B10 B5 109.3(14) . . ? B8 B11 B10 107.7(14) . . ? B8 B11 B6 109.0(14) . . ? B10 B11 B6 58.9(10) . . ? B8 B11 B7 62.4(11) . . ? B10 B11 B7 108.0(13) . . ? B6 B11 B7 60.1(10) . . ? B8 B11 B9 60.2(11) . . ? B10 B11 B9 58.0(11) . . ? B6 B11 B9 105.1(13) . . ? B7 B11 B9 109.0(13) . . ? O2 C2 Mo1 174.0(20) . . ? O3 C3 Mo1 177.5(18) . . ? O4 C4 Mo1 176.0(18) . . ? B2 N1 C15 120.0(14) . . ? B2 N1 C11 118.0(14) . . ? C15 N1 C11 107.7(13) . . ? B2 N1 Mo1 69.3(9) . . ? C15 N1 Mo1 122.4(11) . . ? C11 N1 Mo1 115.7(9) . . ? N1 C11 C12 110.9(13) . . ? C11 C12 C13 110.9(17) . . ? C14 C13 C12 110.0(17) . . ? C15 C14 C13 109.6(18) . . ? C14 C15 N1 114.3(16) . . ? C213 Fe1 C212 95.7(9) . . ? C213 Fe1 C211 94.7(9) . . ? C212 Fe1 C211 95.8(8) . . ? C213 Fe1 C202 155.9(8) . . ? C212 Fe1 C202 99.6(8) . . ? C211 Fe1 C202 102.2(8) . . ? C213 Fe1 C205 90.4(8) . . ? C212 Fe1 C205 114.7(8) . . ? C211 Fe1 C205 148.5(7) . . ? C202 Fe1 C205 66.2(7) . . ? C213 Fe1 C204 92.0(8) . . ? C212 Fe1 C204 151.9(8) . . ? C211 Fe1 C204 110.6(7) . . ? C202 Fe1 C204 66.1(7) . . ? C205 Fe1 C204 38.1(6) . . ? C213 Fe1 C201 121.4(8) . . ? C212 Fe1 C201 88.4(8) . . ? C211 Fe1 C201 143.1(8) . . ? C202 Fe1 C201 41.2(6) . . ? C205 Fe1 C201 38.0(6) . . ? C204 Fe1 C201 64.7(7) . . ? C213 Fe1 C203 127.0(7) . . ? C212 Fe1 C203 136.7(8) . . ? C211 Fe1 C203 88.5(7) . . ? C202 Fe1 C203 38.0(6) . . ? C205 Fe1 C203 64.1(7) . . ? C204 Fe1 C203 39.2(6) . . ? C201 Fe1 C203 64.7(6) . . ? C205 C201 C202 105.0(15) . . ? C205 C201 C206 129.2(17) . . ? C202 C201 C206 125.6(16) . . ? C205 C201 Fe1 69.2(10) . . ? C202 C201 Fe1 66.4(9) . . ? C206 C201 Fe1 130.9(13) . . ? C203 C202 C201 107.5(15) . . ? C203 C202 C207 128.1(17) . . ? C201 C202 C207 122.5(15) . . ? C203 C202 Fe1 75.1(10) . . ? C201 C202 Fe1 72.4(10) . . ? C207 C202 Fe1 130.2(12) . . ? C202 C203 C204 107.7(16) . . ? C202 C203 C208 125.1(17) . . ? C204 C203 C208 127.1(16) . . ? C202 C203 Fe1 67.0(10) . . ? C204 C203 Fe1 68.1(9) . . ? C208 C203 Fe1 127.9(12) . . ? C205 C204 C203 107.5(16) . . ? C205 C204 C209 129.1(19) . . ? C203 C204 C209 122.4(16) . . ? C205 C204 Fe1 70.8(10) . . ? C203 C204 Fe1 72.7(10) . . ? C209 C204 Fe1 130.7(13) . . ? C204 C205 C201 111.3(18) . . ? C204 C205 C210 125.4(17) . . ? C201 C205 C210 123.0(16) . . ? C204 C205 Fe1 71.1(10) . . ? C201 C205 Fe1 72.8(10) . . ? C210 C205 Fe1 128.4(13) . . ? O211 C211 Fe1 178.4(19) . . ? O212 C212 Fe1 171.6(20) . . ? O213 C213 Fe1 174.7(18) . . ? C103 Mo2 C104 103.9(9) . . ? C103 Mo2 C102 81.0(8) . . ? C104 Mo2 C102 81.6(8) . . ? C103 Mo2 B102 115.6(8) . . ? C104 Mo2 B102 113.5(9) . . ? C102 Mo2 B102 151.7(8) . . ? C103 Mo2 N101 95.7(8) . . ? C104 Mo2 N101 89.8(6) . . ? C102 Mo2 N101 169.8(7) . . ? B102 Mo2 N101 38.0(7) . . ? C103 Mo2 C101 85.9(8) . . ? C104 Mo2 C101 158.4(8) . . ? C102 Mo2 C101 119.3(9) . . ? B102 Mo2 C101 45.4(8) . . ? N101 Mo2 C101 69.9(6) . . ? C103 Mo2 B103 160.2(8) . . ? C104 Mo2 B103 91.7(8) . . ? C102 Mo2 B103 113.8(8) . . ? B102 Mo2 B103 45.5(8) . . ? N101 Mo2 B103 71.8(7) . . ? C101 Mo2 B103 75.4(8) . . ? C103 Mo2 B104 138.4(9) . . ? C104 Mo2 B104 108.4(8) . . ? C102 Mo2 B104 78.4(8) . . ? B102 Mo2 B104 74.1(8) . . ? N101 Mo2 B104 109.8(7) . . ? C101 Mo2 B104 73.4(7) . . ? B103 Mo2 B104 41.7(7) . . ? C103 Mo2 B105 96.6(9) . . ? C104 Mo2 B105 150.7(8) . . ? C102 Mo2 B105 81.1(8) . . ? B102 Mo2 B105 74.6(9) . . ? N101 Mo2 B105 109.0(7) . . ? C101 Mo2 B105 42.0(7) . . ? B103 Mo2 B105 74.0(8) . . ? B104 Mo2 B105 44.7(8) . . ? B105 C101 B102 109.5(17) . . ? B105 C101 B106 111.5(15) . . ? B102 C101 B106 59.7(14) . . ? B105 C101 B110 62.2(12) . . ? B102 C101 B110 108.4(17) . . ? B106 C101 B110 60.8(13) . . ? B105 C101 Mo2 72.8(11) . . ? B102 C101 Mo2 64.1(11) . . ? B106 C101 Mo2 121.4(14) . . ? B110 C101 Mo2 128.6(13) . . ? N101 B102 B107 141.2(21) . . ? N101 B102 B106 138.1(19) . . ? B107 B102 B106 61.0(13) . . ? N101 B102 C101 109.2(18) . . ? B107 B102 C101 109.0(18) . . ? B106 B102 C101 60.4(13) . . ? N101 B102 B103 113.1(18) . . ? B107 B102 B103 59.5(12) . . ? B106 B102 B103 108.5(17) . . ? C101 B102 B103 108.3(17) . . ? N101 B102 Mo2 72.3(12) . . ? B107 B102 Mo2 127.7(15) . . ? B106 B102 Mo2 128.2(17) . . ? C101 B102 Mo2 70.6(11) . . ? B103 B102 Mo2 71.0(11) . . ? B104 B103 B108 64.3(14) . . ? B104 B103 B107 111.9(17) . . ? B108 B103 B107 60.9(12) . . ? B104 B103 B102 107.2(18) . . ? B108 B103 B102 108.0(17) . . ? B107 B103 B102 59.1(13) . . ? B104 B103 Mo2 70.6(10) . . ? B108 B103 Mo2 128.7(16) . . ? B107 B103 Mo2 120.4(14) . . ? B102 B103 Mo2 63.6(10) . . ? B103 B104 B109 106.4(16) . . ? B103 B104 B108 58.6(13) . . ? B109 B104 B108 59.2(13) . . ? B103 B104 B105 109.8(15) . . ? B109 B104 B105 58.8(14) . . ? B108 B104 B105 107.2(15) . . ? B103 B104 Mo2 67.7(10) . . ? B109 B104 Mo2 122.0(14) . . ? B108 B104 Mo2 121.2(13) . . ? B105 B104 Mo2 69.3(10) . . ? C101 B105 B109 106.0(17) . . ? C101 B105 B110 60.6(12) . . ? B109 B105 B110 60.4(13) . . ? C101 B105 B104 105.1(16) . . ? B109 B105 B104 56.9(13) . . ? B110 B105 B104 106.3(16) . . ? C101 B105 Mo2 65.3(10) . . ? B109 B105 Mo2 117.3(16) . . ? B110 B105 Mo2 120.6(13) . . ? B104 B105 Mo2 66.0(10) . . ? B102 B106 B111 104.7(15) . . ? B102 B106 C101 59.9(12) . . ? B111 B106 C101 104.3(16) . . ? B102 B106 B107 58.8(13) . . ? B111 B106 B107 59.7(12) . . ? C101 B106 B107 106.9(14) . . ? B102 B106 B110 107.8(16) . . ? B111 B106 B110 58.4(13) . . ? C101 B106 B110 59.9(13) . . ? B107 B106 B110 108.1(15) . . ? B102 B107 B103 61.4(12) . . ? B102 B107 B111 105.8(17) . . ? B103 B107 B111 104.7(17) . . ? B102 B107 B108 108.3(16) . . ? B103 B107 B108 59.0(12) . . ? B111 B107 B108 58.5(14) . . ? B102 B107 B106 60.2(13) . . ? B103 B107 B106 109.4(15) . . ? B111 B107 B106 59.7(13) . . ? B108 B107 B106 108.6(18) . . ? B111 B108 B103 107.5(18) . . ? B111 B108 B109 60.5(14) . . ? B103 B108 B109 103.7(20) . . ? B111 B108 B107 60.9(13) . . ? B103 B108 B107 60.1(13) . . ? B109 B108 B107 107.7(19) . . ? B111 B108 B104 106.1(19) . . ? B103 B108 B104 57.1(13) . . ? B109 B108 B104 57.5(14) . . ? B107 B108 B104 105.6(16) . . ? B104 B109 B108 63.3(15) . . ? B104 B109 B111 109.3(19) . . ? B108 B109 B111 58.8(14) . . ? B104 B109 B105 64.4(14) . . ? B108 B109 B105 114.9(20) . . ? B111 B109 B105 108.7(16) . . ? B104 B109 B110 113.1(17) . . ? B108 B109 B110 109.5(18) . . ? B111 B109 B110 58.7(12) . . ? B105 B109 B110 61.5(14) . . ? B111 B110 C101 104.9(16) . . ? B111 B110 B109 59.3(14) . . ? C101 B110 B109 101.7(17) . . ? B111 B110 B106 59.7(13) . . ? C101 B110 B106 59.3(12) . . ? B109 B110 B106 105.3(17) . . ? B111 B110 B105 106.4(17) . . ? C101 B110 B105 57.2(12) . . ? B109 B110 B105 58.1(13) . . ? B106 B110 B105 106.2(16) . . ? B108 B111 B110 113.9(19) . . ? B108 B111 B109 60.7(14) . . ? B110 B111 B109 62.0(15) . . ? B108 B111 B107 60.7(13) . . ? B110 B111 B107 111.8(15) . . ? B109 B111 B107 107.6(17) . . ? B108 B111 B106 111.1(15) . . ? B110 B111 B106 62.0(13) . . ? B109 B111 B106 109.2(17) . . ? B107 B111 B106 60.6(13) . . ? O102 C102 Mo2 174.0(18) . . ? O103 C103 Mo2 171.8(21) . . ? O104 C104 Mo2 178.1(18) . . ? B102 N101 C115 123.7(17) . . ? B102 N101 C111 115.9(18) . . ? C115 N101 C111 106.8(18) . . ? B102 N101 Mo2 69.7(12) . . ? C115 N101 Mo2 119.5(13) . . ? C111 N101 Mo2 118.0(12) . . ? C112 C111 N101 114.3(19) . . ? C113 C112 C111 109.9(29) . . ? C112 C113 C114 112.2(26) . . ? C113 C114 C115 108.1(23) . . ? N101 C115 C114 112.0(19) . . ? C312 Fe2 C311 97.1(9) . . ? C312 Fe2 C313 92.1(11) . . ? C311 Fe2 C313 95.5(10) . . ? C312 Fe2 C305 132.5(8) . . ? C311 Fe2 C305 130.2(8) . . ? C313 Fe2 C305 88.2(8) . . ? C312 Fe2 C304 96.9(8) . . ? C311 Fe2 C304 153.2(8) . . ? C313 Fe2 C304 106.7(9) . . ? C305 Fe2 C304 38.9(6) . . ? C312 Fe2 C301 155.9(9) . . ? C311 Fe2 C301 92.5(8) . . ? C313 Fe2 C301 109.0(8) . . ? C305 Fe2 C301 40.7(6) . . ? C304 Fe2 C301 66.4(6) . . ? C312 Fe2 C303 90.8(9) . . ? C311 Fe2 C303 118.0(9) . . ? C313 Fe2 C303 145.7(9) . . ? C305 Fe2 C303 65.3(7) . . ? C304 Fe2 C303 39.1(6) . . ? C301 Fe2 C303 65.3(7) . . ? C312 Fe2 C302 119.1(9) . . ? C311 Fe2 C302 88.7(8) . . ? C313 Fe2 C302 147.8(9) . . ? C305 Fe2 C302 65.4(7) . . ? C304 Fe2 C302 64.5(7) . . ? C301 Fe2 C302 38.8(6) . . ? C303 Fe2 C302 37.6(6) . . ? C302 C301 C305 105.2(15) . . ? C302 C301 C306 127.1(17) . . ? C305 C301 C306 127.4(17) . . ? C302 C301 Fe2 72.2(10) . . ? C305 C301 Fe2 67.8(10) . . ? C306 C301 Fe2 128.6(13) . . ? C303 C302 C301 109.2(17) . . ? C303 C302 C307 125.9(18) . . ? C301 C302 C307 124.9(17) . . ? C303 C302 Fe2 69.7(10) . . ? C301 C302 Fe2 68.9(10) . . ? C307 C302 Fe2 126.5(13) . . ? C302 C303 C304 108.8(17) . . ? C302 C303 C308 127.6(18) . . ? C304 C303 C308 123.5(17) . . ? C302 C303 Fe2 72.7(11) . . ? C304 C303 Fe2 69.2(10) . . ? C308 C303 Fe2 126.7(13) . . ? C305 C304 C303 108.1(16) . . ? C305 C304 C309 123.0(17) . . ? C303 C304 C309 128.5(16) . . ? C305 C304 Fe2 69.7(9) . . ? C303 C304 Fe2 71.7(10) . . ? C309 C304 Fe2 129.9(12) . . ? C304 C305 C301 108.6(16) . . ? C304 C305 C310 126.6(16) . . ? C301 C305 C310 123.8(16) . . ? C304 C305 Fe2 71.5(10) . . ? C301 C305 Fe2 71.5(10) . . ? C310 C305 Fe2 131.6(13) . . ? O311 C311 Fe2 171.9(18) . . ? O312 C312 Fe2 177.7(22) . . ? O313 C313 Fe2 179.0(23) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.04 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.328 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.081 #============================================================================== #===END #============================================================================== data_6 _database_code_CSD 192676 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 B10 Cl2 Cu Mo N O3 P' _chemical_formula_weight 805.04 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' N N 0.0061 0.0033 '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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.827(2) _cell_length_b 15.0408(13) _cell_length_c 18.274(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.015(10) _cell_angle_gamma 90.00 _cell_volume 3634.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 16 _exptl_crystal_description plates _exptl_crystal_colour purple _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.598 _exptl_absorpt_correction_T_max 0.697 _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_% 37 _diffrn_reflns_number 6588 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.1069 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4745 _reflns_number_gt 2784 _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^)+(0.0250P)^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 'H3 & H4 located, the rest calculated' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4745 _refine_ls_number_parameters 470 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1214 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.0982 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.41126(5) 0.69487(5) 0.02311(3) 0.0406(2) Uani 1 d . . . C1 C 0.5683(5) 0.6564(5) 0.0079(4) 0.041(2) Uani 1 d . . . H1 H 0.6028 0.6112 0.0558 0.049 Uiso 1 calc R . . B2 B 0.5475(6) 0.7689(6) 0.0189(5) 0.042(2) Uani 1 d . . . B3 B 0.4444(7) 0.8050(6) -0.0618(4) 0.041(2) Uani 1 d . . . H3 H 0.395(5) 0.865(4) -0.066(3) 0.050 Uiso 1 d . . . B4 B 0.4002(7) 0.7068(7) -0.1134(5) 0.045(2) Uani 1 d . . . H4 H 0.328(5) 0.698(5) -0.145(3) 0.054 Uiso 1 d . . . B5 B 0.4777(6) 0.6137(6) -0.0644(4) 0.040(2) Uani 1 d . . . H5 H 0.4484 0.5455 -0.0661 0.048 Uiso 1 calc R . . B6 B 0.6474(7) 0.7299(6) -0.0148(5) 0.051(3) Uani 1 d . . . H6 H 0.7274 0.7375 0.0184 0.061 Uiso 1 calc R . . B7 B 0.5707(7) 0.8228(6) -0.0591(5) 0.051(3) Uani 1 d . . . H7 H 0.6016 0.8907 -0.0543 0.061 Uiso 1 calc R . . B8 B 0.4814(7) 0.7825(6) -0.1441(5) 0.045(3) Uani 1 d . . . H8 H 0.4551 0.8229 -0.1964 0.054 Uiso 1 calc R . . B9 B 0.4979(6) 0.6674(6) -0.1472(5) 0.043(2) Uani 1 d . . . H9 H 0.4792 0.6326 -0.2025 0.052 Uiso 1 calc R . . B10 B 0.6041(7) 0.6348(6) -0.0710(5) 0.045(3) Uani 1 d . . . H10 H 0.6552 0.5810 -0.0767 0.055 Uiso 1 calc R . . B11 B 0.6044(7) 0.7390(6) -0.1156(5) 0.055(3) Uani 1 d . . . H11 H 0.6570 0.7526 -0.1492 0.066 Uiso 1 calc R . . C2 C 0.3006(7) 0.6056(6) -0.0176(4) 0.053(2) Uani 1 d . . . O2 O 0.2369(5) 0.5543(4) -0.0377(3) 0.075(2) Uani 1 d . . . C3 C 0.4344(6) 0.6170(5) 0.1171(4) 0.049(2) Uani 1 d . . . O3 O 0.4464(5) 0.5720(4) 0.1685(3) 0.0672(18) Uani 1 d . . . C4 C 0.3028(6) 0.7642(5) 0.0481(4) 0.056(2) Uani 1 d . . . O4 O 0.2445(5) 0.8037(4) 0.0683(3) 0.090(2) Uani 1 d . . . N N 0.5346(4) 0.7889(4) 0.0939(3) 0.0431(16) Uani 1 d . . . C12 C 0.6080(6) 0.7532(5) 0.1653(4) 0.050(2) Uani 1 d . . . H12A H 0.6272 0.6932 0.1561 0.060 Uiso 1 calc R . . H12B H 0.5757 0.7508 0.2058 0.060 Uiso 1 calc R . . C13 C 0.7017(6) 0.8104(6) 0.1909(4) 0.067(3) Uani 1 d . . . H13A H 0.7364 0.8099 0.1518 0.081 Uiso 1 calc R . . H13B H 0.7472 0.7858 0.2374 0.081 Uiso 1 calc R . . C14 C 0.6757(7) 0.9063(6) 0.2057(5) 0.077(3) Uani 1 d . . . H14A H 0.6512 0.9085 0.2503 0.093 Uiso 1 calc R . . H14B H 0.7358 0.9431 0.2157 0.093 Uiso 1 calc R . . C15 C 0.5946(7) 0.9417(5) 0.1359(5) 0.069(3) Uani 1 d . . . H15A H 0.5715 0.9992 0.1480 0.083 Uiso 1 calc R . . H15B H 0.6237 0.9498 0.0941 0.083 Uiso 1 calc R . . C16 C 0.5063(6) 0.8800(5) 0.1110(4) 0.057(2) Uani 1 d . . . H16A H 0.4733 0.8768 0.1510 0.068 Uiso 1 calc R . . H16B H 0.4581 0.9042 0.0656 0.068 Uiso 1 calc R . . Cu Cu 0.28021(7) 0.78971(7) -0.09472(5) 0.0574(3) Uani 1 d . . . P P 0.12881(16) 0.84000(14) -0.15089(11) 0.0455(6) Uani 1 d . . . C21 C 0.1015(6) 0.9493(5) -0.1220(4) 0.043(2) Uani 1 d . . . C22 C 0.1579(8) 0.9831(6) -0.0548(5) 0.089(3) Uani 1 d . . . H22A H 0.2104 0.9488 -0.0244 0.107 Uiso 1 calc R . . C23 C 0.1414(9) 1.0655(8) -0.0292(6) 0.117(4) Uani 1 d . . . H23A H 0.1817 1.0861 0.0178 0.141 Uiso 1 calc R . . C24 C 0.0659(8) 1.1168(6) -0.0728(6) 0.082(3) Uani 1 d . . . H24A H 0.0528 1.1722 -0.0552 0.098 Uiso 1 calc R . . C25 C 0.0104(9) 1.0875(7) -0.1411(6) 0.105(4) Uani 1 d . . . H25A H -0.0402 1.1233 -0.1719 0.126 Uiso 1 calc R . . C26 C 0.0279(9) 1.0047(7) -0.1658(6) 0.104(4) Uani 1 d . . . H26A H -0.0111 0.9853 -0.2136 0.125 Uiso 1 calc R . . C31 C 0.0329(5) 0.7668(5) -0.1375(4) 0.043(2) Uani 1 d . . . C32 C -0.0450(6) 0.7927(6) -0.1101(4) 0.058(2) Uani 1 d . . . H32A H -0.0519 0.8523 -0.0992 0.070 Uiso 1 calc R . . C33 C -0.1134(7) 0.7317(8) -0.0986(5) 0.075(3) Uani 1 d . . . H33A H -0.1641 0.7509 -0.0783 0.091 Uiso 1 calc R . . C34 C -0.1087(7) 0.6450(7) -0.1159(5) 0.074(3) Uani 1 d . . . H34A H -0.1570 0.6050 -0.1097 0.088 Uiso 1 calc R . . C35 C -0.0301(8) 0.6172(6) -0.1430(5) 0.079(3) Uani 1 d . . . H35A H -0.0246 0.5576 -0.1547 0.095 Uiso 1 calc R . . C36 C 0.0394(7) 0.6771(6) -0.1525(5) 0.071(3) Uani 1 d . . . H36A H 0.0927 0.6572 -0.1695 0.085 Uiso 1 calc R . . C41 C 0.1015(6) 0.8505(5) -0.2551(4) 0.045(2) Uani 1 d . . . C42 C 0.0051(7) 0.8414(5) -0.3038(5) 0.062(3) Uani 1 d . . . H42A H -0.0483 0.8259 -0.2851 0.074 Uiso 1 calc R . . C43 C -0.0105(7) 0.8557(5) -0.3806(5) 0.072(3) Uani 1 d . . . H43A H -0.0756 0.8504 -0.4139 0.087 Uiso 1 calc R . . C44 C 0.0671(9) 0.8775(6) -0.4094(5) 0.081(3) Uani 1 d . . . H44A H 0.0548 0.8863 -0.4617 0.097 Uiso 1 calc R . . C45 C 0.1606(9) 0.8861(6) -0.3622(6) 0.079(3) Uani 1 d . . . H45A H 0.2133 0.9020 -0.3815 0.095 Uiso 1 calc R . . C46 C 0.1796(6) 0.8712(5) -0.2839(5) 0.060(2) Uani 1 d . . . H46A H 0.2452 0.8752 -0.2514 0.072 Uiso 1 calc R . . C100 C 0.2752(19) 0.5314(10) -0.2656(12) 0.183(10) Uani 0.50 d PD A 1 H10A H 0.2185 0.5704 -0.2885 0.220 Uiso 0.50 calc PR A 1 H10B H 0.3329 0.5677 -0.2396 0.220 Uiso 0.50 calc PR A 1 Cl1 Cl 0.2441(18) 0.4580(12) -0.1989(12) 0.106(6) Uani 0.50 d PD A 1 Cl2 Cl 0.3022(15) 0.4707(12) -0.3330(8) 0.189(9) Uani 0.50 d PD A 1 C101 C 0.2752(19) 0.5314(10) -0.2656(12) 0.183(10) Uani 0.25 d PD B 2 H10C H 0.2250 0.5679 -0.3011 0.220 Uiso 0.25 calc PR B 2 H10D H 0.3281 0.5685 -0.2334 0.220 Uiso 0.25 calc PR B 2 Cl1A Cl 0.222(4) 0.459(4) -0.212(2) 0.22(3) Uani 0.25 d PD B 2 Cl2A Cl 0.3217(19) 0.449(2) -0.3107(15) 0.126(10) Uani 0.25 d PD B 2 C102 C 0.309(4) 0.468(4) -0.258(2) 0.183(10) Uani 0.25 d PD C 3 H10E H 0.3784 0.4804 -0.2291 0.220 Uiso 0.25 calc PR C 3 H10F H 0.3019 0.4064 -0.2734 0.220 Uiso 0.25 calc PR C 3 Cl1B Cl 0.223(3) 0.499(2) -0.2065(17) 0.091(9) Uani 0.25 d PD C 3 Cl2B Cl 0.2666(12) 0.5389(11) -0.3348(9) 0.100(5) Uani 0.25 d PD C 3 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 0.0407(4) 0.0477(4) 0.0357(4) 0.0037(4) 0.0148(3) 0.0009(5) C1 0.043(5) 0.049(5) 0.033(4) 0.001(4) 0.012(4) 0.003(4) B2 0.028(5) 0.054(7) 0.041(5) 0.010(4) 0.006(5) 0.002(5) B3 0.042(6) 0.046(6) 0.037(5) 0.006(5) 0.012(4) 0.013(6) B4 0.040(6) 0.061(7) 0.038(5) -0.005(5) 0.016(5) -0.012(6) B5 0.030(6) 0.052(6) 0.037(5) 0.006(4) 0.006(5) 0.009(5) B6 0.037(6) 0.070(7) 0.041(5) 0.007(5) 0.006(5) 0.012(6) B7 0.052(7) 0.053(7) 0.046(5) -0.001(5) 0.013(5) -0.003(6) B8 0.041(6) 0.056(7) 0.041(5) 0.016(5) 0.017(5) 0.007(5) B9 0.038(6) 0.055(7) 0.032(5) -0.006(4) 0.004(5) 0.001(5) B10 0.033(6) 0.062(7) 0.039(5) -0.006(5) 0.007(5) 0.019(5) B11 0.059(7) 0.077(8) 0.033(5) -0.002(5) 0.021(5) 0.005(6) C2 0.053(6) 0.067(7) 0.043(5) 0.012(5) 0.020(5) 0.005(5) O2 0.069(5) 0.077(5) 0.077(4) 0.004(4) 0.016(4) -0.026(4) C3 0.064(6) 0.051(6) 0.034(5) -0.006(4) 0.019(5) -0.015(5) O3 0.100(5) 0.056(4) 0.046(4) 0.013(3) 0.022(4) 0.001(4) C4 0.053(6) 0.056(6) 0.065(6) 0.011(4) 0.025(5) -0.002(5) O4 0.098(5) 0.089(5) 0.105(5) 0.025(4) 0.064(4) 0.030(5) N 0.045(4) 0.047(4) 0.038(3) 0.002(3) 0.013(3) 0.001(4) C12 0.059(6) 0.050(5) 0.040(5) 0.005(4) 0.013(5) 0.000(5) C13 0.060(7) 0.088(8) 0.047(5) 0.004(5) 0.006(5) -0.002(7) C14 0.086(8) 0.077(8) 0.065(7) -0.024(6) 0.016(6) -0.029(7) C15 0.099(8) 0.045(6) 0.072(7) -0.009(5) 0.039(6) -0.009(6) C16 0.073(7) 0.050(6) 0.054(5) 0.004(4) 0.028(5) 0.008(6) Cu 0.0373(7) 0.0707(8) 0.0627(7) 0.0101(6) 0.0121(5) 0.0103(6) P 0.0369(14) 0.0509(14) 0.0472(13) -0.0026(10) 0.0101(11) 0.0049(12) C21 0.043(5) 0.048(6) 0.030(4) -0.007(4) 0.001(4) -0.001(5) C22 0.101(9) 0.074(8) 0.073(7) -0.013(6) -0.004(7) 0.040(7) C23 0.146(12) 0.092(9) 0.077(8) -0.036(7) -0.027(8) 0.034(9) C24 0.107(10) 0.058(7) 0.072(7) -0.018(6) 0.014(7) 0.009(7) C25 0.132(11) 0.075(8) 0.080(8) -0.006(6) -0.015(8) 0.050(8) C26 0.133(11) 0.079(9) 0.068(7) -0.020(6) -0.023(7) 0.035(8) C31 0.029(5) 0.055(6) 0.040(5) -0.001(4) 0.005(4) 0.005(4) C32 0.043(5) 0.062(6) 0.069(6) -0.006(5) 0.015(5) -0.006(5) C33 0.040(6) 0.121(10) 0.064(6) -0.023(6) 0.013(5) -0.025(7) C34 0.064(8) 0.094(9) 0.059(6) -0.001(6) 0.013(6) -0.040(7) C35 0.092(9) 0.057(7) 0.093(8) 0.002(6) 0.034(7) -0.007(7) C36 0.075(8) 0.065(8) 0.082(7) -0.005(5) 0.035(6) 0.000(6) C41 0.041(5) 0.050(5) 0.043(5) 0.000(4) 0.010(5) 0.009(5) C42 0.062(7) 0.058(6) 0.067(6) -0.008(5) 0.023(6) 0.002(5) C43 0.081(8) 0.076(7) 0.046(6) -0.005(5) -0.004(6) 0.002(6) C44 0.121(10) 0.082(8) 0.045(6) -0.011(6) 0.031(7) 0.005(8) C45 0.100(9) 0.087(8) 0.065(7) -0.006(6) 0.046(7) -0.005(8) C46 0.050(6) 0.071(7) 0.059(6) -0.006(5) 0.015(5) 0.018(5) C100 0.19(2) 0.16(2) 0.26(2) -0.12(2) 0.14(2) -0.061(19) Cl1 0.094(11) 0.135(16) 0.074(6) 0.016(8) 0.001(6) 0.016(10) Cl2 0.27(2) 0.208(19) 0.139(11) -0.091(13) 0.132(13) -0.050(14) C101 0.19(2) 0.16(2) 0.26(2) -0.12(2) 0.14(2) -0.061(19) Cl1A 0.11(3) 0.33(6) 0.19(4) 0.09(3) 0.01(2) -0.09(3) Cl2A 0.076(12) 0.121(16) 0.16(2) 0.005(13) -0.006(12) 0.071(12) C102 0.19(2) 0.16(2) 0.26(2) -0.12(2) 0.14(2) -0.061(19) Cl1B 0.09(2) 0.14(2) 0.063(13) -0.010(13) 0.047(15) 0.017(14) Cl2B 0.094(10) 0.134(14) 0.073(9) 0.039(10) 0.027(9) 0.034(11) _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 1.987(9) . y Mo C2 2.007(9) . y Mo C3 2.026(8) . y Mo B2 2.209(8) . y Mo N 2.300(6) . y Mo C1 2.341(7) . y Mo B5 2.399(8) . y Mo B3 2.403(8) . y Mo B4 2.460(8) . y Mo Cu 2.7697(12) . y C1 B5 1.661(10) . ? C1 B10 1.688(9) . ? C1 B6 1.690(11) . ? C1 B2 1.738(11) . ? B2 N 1.464(9) . y B2 B7 1.750(11) . ? B2 B6 1.771(11) . ? B2 B3 1.808(11) . ? B3 H3 1.12(6) . y B3 B7 1.755(12) . ? B3 B8 1.758(10) . ? B3 B4 1.763(13) . ? B3 Cu 2.183(9) . y B4 H4 1.01(6) . y B4 B9 1.746(11) . ? B4 B8 1.801(11) . ? B4 B5 1.830(13) . ? B4 Cu 2.181(9) . y B5 B9 1.807(11) . ? B5 B10 1.814(11) . ? B6 B10 1.760(12) . ? B6 B11 1.767(11) . ? B6 B7 1.798(12) . ? B7 B11 1.776(11) . ? B7 B8 1.783(12) . ? B8 B9 1.749(12) . ? B8 B11 1.754(12) . ? B9 B10 1.771(12) . ? B9 B11 1.778(12) . ? B10 B11 1.766(12) . ? C2 O2 1.148(9) . ? C3 O3 1.129(8) . ? C4 O4 1.146(8) . ? N C16 1.482(8) . ? N C12 1.499(8) . ? C12 C13 1.511(10) . ? C13 C14 1.529(11) . ? C14 C15 1.527(11) . ? C15 C16 1.493(10) . ? Cu H4 1.88(6) . y Cu H3 1.90(6) . y Cu P 2.180(2) . y P C31 1.795(7) . ? P C21 1.800(8) . ? P C41 1.836(7) . ? C21 C22 1.348(10) . ? C21 C26 1.375(11) . ? C22 C23 1.367(11) . ? C23 C24 1.355(12) . ? C24 C25 1.334(12) . ? C25 C26 1.371(11) . ? C31 C32 1.370(9) . ? C31 C36 1.384(10) . ? C32 C33 1.376(11) . ? C33 C34 1.348(11) . ? C34 C35 1.385(11) . ? C35 C36 1.365(11) . ? C41 C46 1.368(9) . ? C41 C42 1.376(10) . ? C42 C43 1.374(10) . ? C43 C44 1.365(11) . ? C44 C45 1.335(12) . ? C45 C46 1.395(10) . ? C100 Cl2 1.661(14) . ? C100 Cl1 1.788(17) . ? C102 Cl2B 1.72(2) . ? C102 Cl1B 1.78(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 83.8(3) . . y C4 Mo C3 92.9(3) . . y C2 Mo C3 80.9(3) . . y C4 Mo B2 116.9(3) . . y C2 Mo B2 152.8(3) . . y C3 Mo B2 113.4(3) . . y C4 Mo N 91.9(3) . . y C2 Mo N 168.2(2) . . y C3 Mo N 88.4(3) . . y B2 Mo N 37.8(2) . . y C4 Mo C1 161.0(3) . . y C2 Mo C1 115.1(3) . . y C3 Mo C1 92.1(3) . . y B2 Mo C1 44.8(3) . . ? N Mo C1 70.0(2) . . y C4 Mo B5 152.0(3) . . y C2 Mo B5 79.2(3) . . y C3 Mo B5 106.0(3) . . y B2 Mo B5 74.7(3) . . ? N Mo B5 108.8(3) . . y C1 Mo B5 41.0(2) . . ? C4 Mo B3 94.9(3) . . y C2 Mo B3 119.4(3) . . y C3 Mo B3 159.0(3) . . y B2 Mo B3 45.9(3) . . ? N Mo B3 71.9(2) . . y C1 Mo B3 74.7(3) . . ? B5 Mo B3 74.8(3) . . ? C4 Mo B4 111.6(3) . . y C2 Mo B4 81.9(3) . . y C3 Mo B4 148.1(3) . . y B2 Mo B4 74.3(3) . . ? N Mo B4 110.0(2) . . y C1 Mo B4 71.5(3) . . ? B5 Mo B4 44.2(3) . . ? B3 Mo B4 42.5(3) . . ? C4 Mo Cu 62.8(2) . . y C2 Mo Cu 78.6(2) . . y C3 Mo Cu 149.5(2) . . y B2 Mo Cu 94.8(2) . . y N Mo Cu 109.22(15) . . y C1 Mo Cu 116.98(17) . . y B5 Mo Cu 92.0(2) . . y B3 Mo Cu 49.3(2) . . y B4 Mo Cu 48.8(2) . . y B3 H3 Cu 88(4) . . y B4 H4 Cu 93(4) . . y B5 C1 B10 65.6(5) . . ? B5 C1 B6 116.6(6) . . ? B10 C1 B6 62.8(5) . . ? B5 C1 B2 110.9(6) . . ? B10 C1 B2 112.7(5) . . ? B6 C1 B2 62.2(4) . . ? B5 C1 Mo 71.4(4) . . ? B10 C1 Mo 131.5(5) . . ? B6 C1 Mo 123.9(5) . . ? B2 C1 Mo 63.6(4) . . ? N B2 C1 112.2(6) . . y N B2 B7 140.3(7) . . y C1 B2 B7 106.3(5) . . ? N B2 B6 135.7(7) . . y C1 B2 B6 57.6(4) . . ? B7 B2 B6 61.4(5) . . ? N B2 B3 114.8(6) . . y C1 B2 B3 108.4(6) . . ? B7 B2 B3 59.1(5) . . ? B6 B2 B3 109.0(5) . . ? N B2 Mo 74.5(4) . . y C1 B2 Mo 71.6(4) . . ? B7 B2 Mo 128.6(6) . . ? B6 B2 Mo 127.2(6) . . ? B3 B2 Mo 72.7(4) . . ? H3 B3 B7 117(3) . . ? H3 B3 B8 115(3) . . ? B7 B3 B8 61.0(5) . . ? H3 B3 B4 122(3) . . ? B7 B3 B4 109.2(6) . . ? B8 B3 B4 61.5(5) . . ? H3 B3 B2 128(3) . . ? B7 B3 B2 58.8(5) . . ? B8 B3 B2 106.4(6) . . ? B4 B3 B2 104.6(7) . . ? H3 B3 Cu 60(3) . . ? B7 B3 Cu 166.0(5) . . ? B8 B3 Cu 106.5(5) . . ? B4 B3 Cu 66.1(4) . . ? B2 B3 Cu 134.5(5) . . ? H3 B3 Mo 112(3) . . ? B7 B3 Mo 117.6(5) . . ? B8 B3 Mo 125.3(6) . . ? B4 B3 Mo 70.5(4) . . ? B2 B3 Mo 61.3(4) . . ? Cu B3 Mo 74.1(3) . . y H4 B4 B9 119(3) . . ? H4 B4 B3 123(4) . . ? B9 B4 B3 106.9(6) . . ? H4 B4 B8 121(4) . . ? B9 B4 B8 59.1(5) . . ? B3 B4 B8 59.1(5) . . ? H4 B4 B5 121(4) . . ? B9 B4 B5 60.7(5) . . ? B3 B4 B5 108.5(6) . . ? B8 B4 B5 107.9(6) . . ? H4 B4 Cu 60(4) . . ? B9 B4 Cu 162.3(6) . . ? B3 B4 Cu 66.3(4) . . ? B8 B4 Cu 105.0(6) . . ? B5 B4 Cu 136.5(5) . . ? H4 B4 Mo 109(3) . . ? B9 B4 Mo 120.6(5) . . ? B3 B4 Mo 67.0(4) . . ? B8 B4 Mo 120.2(5) . . ? B5 B4 Mo 66.1(3) . . ? Cu B4 Mo 73.0(2) . . y C1 B5 B9 103.2(6) . . ? C1 B5 B10 57.9(4) . . ? B9 B5 B10 58.6(4) . . ? C1 B5 B4 106.9(6) . . ? B9 B5 B4 57.4(4) . . ? B10 B5 B4 105.8(6) . . ? C1 B5 Mo 67.6(3) . . ? B9 B5 Mo 120.9(5) . . ? B10 B5 Mo 121.3(5) . . ? B4 B5 Mo 69.7(3) . . ? C1 B6 B10 58.5(4) . . ? C1 B6 B11 105.2(6) . . ? B10 B6 B11 60.1(5) . . ? C1 B6 B2 60.2(4) . . ? B10 B6 B2 107.8(6) . . ? B11 B6 B2 106.1(6) . . ? C1 B6 B7 106.3(6) . . ? B10 B6 B7 108.3(6) . . ? B11 B6 B7 59.7(5) . . ? B2 B6 B7 58.7(4) . . ? B2 B7 B3 62.1(5) . . ? B2 B7 B11 106.6(6) . . ? B3 B7 B11 107.7(7) . . ? B2 B7 B8 107.8(6) . . ? B3 B7 B8 59.6(5) . . ? B11 B7 B8 59.0(5) . . ? B2 B7 B6 59.8(5) . . ? B3 B7 B6 110.2(6) . . ? B11 B7 B6 59.3(5) . . ? B8 B7 B6 107.1(6) . . ? B9 B8 B11 61.0(5) . . ? B9 B8 B3 107.0(6) . . ? B11 B8 B3 108.5(6) . . ? B9 B8 B7 107.5(6) . . ? B11 B8 B7 60.3(5) . . ? B3 B8 B7 59.4(5) . . ? B9 B8 B4 58.9(5) . . ? B11 B8 B4 108.1(6) . . ? B3 B8 B4 59.4(5) . . ? B7 B8 B4 106.3(5) . . ? B4 B9 B8 62.0(5) . . ? B4 B9 B10 111.4(6) . . ? B8 B9 B10 109.5(6) . . ? B4 B9 B11 109.4(6) . . ? B8 B9 B11 59.6(5) . . ? B10 B9 B11 59.7(5) . . ? B4 B9 B5 62.0(5) . . ? B8 B9 B5 111.2(6) . . ? B10 B9 B5 60.9(4) . . ? B11 B9 B5 108.3(6) . . ? C1 B10 B6 58.7(4) . . ? C1 B10 B11 105.3(6) . . ? B6 B10 B11 60.1(5) . . ? C1 B10 B9 103.7(6) . . ? B6 B10 B9 107.2(6) . . ? B11 B10 B9 60.4(5) . . ? C1 B10 B5 56.5(4) . . ? B6 B10 B5 105.9(6) . . ? B11 B10 B5 108.6(6) . . ? B9 B10 B5 60.5(4) . . ? B8 B11 B10 109.6(6) . . ? B8 B11 B6 109.9(6) . . ? B10 B11 B6 59.8(5) . . ? B8 B11 B7 60.7(5) . . ? B10 B11 B7 109.0(5) . . ? B6 B11 B7 61.0(5) . . ? B8 B11 B9 59.4(5) . . ? B10 B11 B9 60.0(5) . . ? B6 B11 B9 106.6(6) . . ? B7 B11 B9 106.6(6) . . ? O2 C2 Mo 177.0(7) . . y O3 C3 Mo 178.5(7) . . y O4 C4 Mo 174.8(7) . . y B2 N C16 119.9(6) . . ? B2 N C12 120.3(6) . . ? C16 N C12 107.5(5) . . ? B2 N Mo 67.7(4) . . y C16 N Mo 119.3(5) . . ? C12 N Mo 118.1(4) . . ? N C12 C13 111.5(6) . . ? C12 C13 C14 111.5(7) . . ? C15 C14 C13 109.5(7) . . ? C16 C15 C14 111.9(7) . . ? N C16 C15 113.3(7) . . ? H4 Cu H3 101(3) . . y H4 Cu P 116.6(19) . . y H3 Cu P 122.3(18) . . y H4 Cu B4 27.6(18) . . ? H3 Cu B4 76.7(18) . . ? P Cu B4 142.6(2) . . ? H4 Cu B3 74.3(19) . . ? H3 Cu B3 30.8(18) . . ? P Cu B3 150.6(3) . . ? B4 Cu B3 47.7(3) . . ? H4 Cu Mo 76.2(18) . . y H3 Cu Mo 77.8(18) . . y P Cu Mo 149.83(6) . . ? B4 Cu Mo 58.2(2) . . ? B3 Cu Mo 56.6(2) . . ? C31 P C21 107.1(3) . . ? C31 P C41 105.0(3) . . ? C21 P C41 103.2(3) . . ? C31 P Cu 111.7(3) . . ? C21 P Cu 115.7(3) . . ? C41 P Cu 113.3(3) . . ? C22 C21 C26 115.7(8) . . ? C22 C21 P 119.8(7) . . ? C26 C21 P 124.5(7) . . ? C21 C22 C23 122.9(10) . . ? C24 C23 C22 119.5(10) . . ? C25 C24 C23 119.7(10) . . ? C24 C25 C26 119.9(10) . . ? C25 C26 C21 122.1(9) . . ? C32 C31 C36 116.9(8) . . ? C32 C31 P 124.5(7) . . ? C36 C31 P 118.5(6) . . ? C31 C32 C33 121.0(9) . . ? C34 C33 C32 121.8(9) . . ? C33 C34 C35 118.2(9) . . ? C36 C35 C34 120.1(9) . . ? C35 C36 C31 121.9(8) . . ? C46 C41 C42 119.8(7) . . ? C46 C41 P 118.2(6) . . ? C42 C41 P 121.9(6) . . ? C43 C42 C41 118.6(8) . . ? C44 C43 C42 121.6(9) . . ? C45 C44 C43 119.8(9) . . ? C44 C45 C46 120.2(9) . . ? C41 C46 C45 119.9(8) . . ? Cl2 C100 Cl1 108.6(14) . . ? Cl2B C102 Cl1B 98.9(18) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.328 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.079 #============================================================================== data_9 _database_code_CSD 192677 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H21 B10 I Mo N2 O2' _chemical_formula_weight 508.21 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' N N 0.0061 0.0033 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.322(2) _cell_length_b 14.112(5) _cell_length_c 16.893(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3652.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 16 _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.3671 _exptl_absorpt_correction_T_max 0.9097 _exptl_special_details ; ? ; _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 '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_% none _diffrn_reflns_number 3930 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0883 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.07 _reflns_number_total 3226 _reflns_number_gt 1952 _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^)+(0.0420P)^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 3226 _refine_ls_number_parameters 223 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _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 0.04322(5) 0.64133(5) 0.87981(5) 0.0153(2) Uani 1 d . . . C1 C 0.1825(5) 0.6294(6) 0.8833(6) 0.0166(19) Uani 1 d . . . B2 B 0.1407(7) 0.6634(7) 0.7854(6) 0.017(2) Uani 1 d . . . B3 B 0.0929(7) 0.7773(8) 0.8071(6) 0.017(2) Uani 1 d . . . H3 H 0.0373 0.8108 0.7744 0.021 Uiso 1 calc R . . B4 B 0.1006(8) 0.8006(8) 0.9086(6) 0.023(3) Uani 1 d . . . H4 H 0.0510 0.8454 0.9399 0.028 Uiso 1 calc R . . B5 B 0.1587(7) 0.7051(8) 0.9566(7) 0.022(3) Uani 1 d . . . H5 H 0.1467 0.6899 1.0208 0.026 Uiso 1 calc R . . B6 B 0.1989(8) 0.7650(8) 0.7634(7) 0.025(3) Uani 1 d . . . H6 H 0.2121 0.7856 0.7005 0.030 Uiso 1 calc R . . B7 B 0.2542(7) 0.6636(9) 0.8112(7) 0.025(3) Uani 1 d . . . H7 H 0.3014 0.6154 0.7806 0.030 Uiso 1 calc R . . B8 B 0.2651(7) 0.6950(8) 0.9144(6) 0.019(3) Uani 1 d . . . H8 H 0.3221 0.6690 0.9497 0.023 Uiso 1 calc R . . B9 B 0.2172(7) 0.8076(9) 0.9312(7) 0.024(3) Uani 1 d . . . H9 H 0.2424 0.8569 0.9779 0.029 Uiso 1 calc R . . B10 B 0.1778(7) 0.8498(9) 0.8377(8) 0.029(3) Uani 1 d . . . H10 H 0.1787 0.9273 0.8234 0.035 Uiso 1 calc R . . B11 B 0.2772(7) 0.7836(9) 0.8406(7) 0.026(3) Uani 1 d . . . H11 H 0.3422 0.8163 0.8276 0.031 Uiso 1 calc R . . I I -0.08837(4) 0.50838(4) 0.87804(4) 0.02465(19) Uani 1 d . . . C2 C -0.0615(6) 0.7246(7) 0.8512(5) 0.022(2) Uani 1 d . . . O2 O -0.1200(4) 0.7717(5) 0.8406(5) 0.0347(19) Uani 1 d . . . C3 C -0.0063(6) 0.6658(7) 0.9916(7) 0.024(2) Uani 1 d . . . O3 O -0.0359(4) 0.6832(5) 1.0504(4) 0.0303(18) Uani 1 d . . . N1 N 0.1506(5) 0.5376(6) 0.9071(5) 0.0205(19) Uani 1 d D . . H1A H 0.167(6) 0.493(5) 0.871(4) 0.025 Uiso 1 d D . . H1B H 0.174(5) 0.526(6) 0.955(3) 0.025 Uiso 1 d D . . N2 N 0.0839(4) 0.5914(5) 0.7539(4) 0.0134(16) Uani 1 d . . . C4 C 0.0137(5) 0.6158(7) 0.6952(5) 0.022(2) Uani 1 d . . . H4A H -0.0100 0.6792 0.7080 0.027 Uiso 1 calc R . . H4B H -0.0345 0.5694 0.7003 0.027 Uiso 1 calc R . . C5 C 0.0462(6) 0.6160(6) 0.6088(5) 0.022(2) Uani 1 d . . . H5A H -0.0035 0.6279 0.5727 0.027 Uiso 1 calc R . . H5B H 0.0893 0.6676 0.6015 0.027 Uiso 1 calc R . . C6 C 0.0882(7) 0.5218(7) 0.5881(6) 0.029(2) Uani 1 d . . . H6A H 0.0435 0.4711 0.5879 0.035 Uiso 1 calc R . . H6B H 0.1145 0.5252 0.5347 0.035 Uiso 1 calc R . . C7 C 0.1580(6) 0.4992(7) 0.6488(5) 0.021(2) Uani 1 d . . . H7A H 0.1839 0.4367 0.6363 0.025 Uiso 1 calc R . . H7B H 0.2049 0.5473 0.6451 0.025 Uiso 1 calc R . . C8 C 0.1232(6) 0.4975(6) 0.7326(5) 0.020(2) Uani 1 d . . . H8A H 0.0784 0.4473 0.7375 0.024 Uiso 1 calc R . . H8B H 0.1712 0.4826 0.7697 0.024 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 0.0116(3) 0.0183(4) 0.0160(4) 0.0038(4) 0.0003(4) 0.0009(3) C1 0.015(4) 0.012(4) 0.023(5) 0.003(5) -0.006(5) -0.007(4) B2 0.023(6) 0.014(6) 0.014(5) -0.004(5) 0.004(5) 0.002(5) B3 0.007(5) 0.021(6) 0.024(6) -0.003(5) 0.005(5) 0.004(5) B4 0.035(7) 0.023(6) 0.011(5) -0.001(5) 0.001(5) 0.006(5) B5 0.023(6) 0.018(6) 0.024(6) -0.007(5) 0.002(5) 0.001(5) B6 0.028(7) 0.027(6) 0.020(7) 0.014(6) -0.004(6) -0.002(6) B7 0.018(6) 0.033(7) 0.026(7) 0.003(6) 0.005(5) 0.004(5) B8 0.014(6) 0.025(7) 0.018(6) 0.003(5) -0.002(5) -0.001(5) B9 0.020(6) 0.030(7) 0.023(6) 0.012(6) -0.003(5) 0.001(5) B10 0.020(6) 0.024(7) 0.043(8) -0.002(6) 0.001(6) -0.007(5) B11 0.014(6) 0.031(7) 0.032(7) 0.002(6) 0.001(5) 0.004(5) I 0.0188(3) 0.0289(4) 0.0262(3) 0.0066(4) -0.0003(3) -0.0065(3) C2 0.025(6) 0.024(5) 0.015(5) -0.001(4) 0.002(4) -0.004(4) O2 0.018(4) 0.034(4) 0.052(5) 0.005(4) 0.007(4) 0.006(3) C3 0.012(5) 0.018(5) 0.041(7) 0.014(5) 0.000(5) -0.003(4) O3 0.032(4) 0.042(5) 0.016(4) 0.003(3) 0.012(3) 0.006(4) N1 0.019(4) 0.026(5) 0.016(4) 0.006(4) -0.008(4) -0.001(4) N2 0.009(3) 0.020(4) 0.011(4) -0.001(3) -0.005(3) 0.008(3) C4 0.012(5) 0.030(5) 0.026(5) 0.005(5) 0.004(4) -0.001(4) C5 0.030(5) 0.022(5) 0.014(5) 0.003(4) 0.002(5) -0.001(4) C6 0.034(6) 0.033(6) 0.021(5) -0.007(5) 0.006(5) -0.006(5) C7 0.025(5) 0.020(5) 0.019(5) -0.002(5) 0.004(4) 0.006(4) C8 0.019(5) 0.014(5) 0.028(5) 0.004(5) -0.001(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C2 2.047(10) . ? Mo C3 2.065(12) . ? Mo C1 2.141(8) . ? Mo B2 2.207(11) . ? Mo N1 2.249(8) . ? Mo N2 2.326(7) . ? Mo B5 2.372(11) . ? Mo B3 2.402(11) . ? Mo B4 2.462(12) . ? Mo I 2.7542(10) . ? C1 N1 1.441(11) . ? C1 B8 1.655(13) . ? C1 B5 1.677(14) . ? C1 B7 1.711(14) . ? C1 B2 1.838(14) . ? B2 N2 1.440(13) . ? B2 B6 1.729(15) . ? B2 B7 1.793(16) . ? B2 B3 1.803(14) . ? B3 B10 1.735(15) . ? B3 B4 1.751(15) . ? B3 B6 1.792(15) . ? B4 B5 1.807(15) . ? B4 B10 1.822(16) . ? B4 B9 1.831(16) . ? B5 B9 1.755(16) . ? B5 B8 1.787(15) . ? B6 B10 1.764(17) . ? B6 B11 1.791(16) . ? B6 B7 1.849(16) . ? B7 B11 1.798(16) . ? B7 B8 1.806(16) . ? B8 B9 1.773(16) . ? B8 B11 1.774(16) . ? B9 B10 1.792(17) . ? B9 B11 1.818(16) . ? B10 B11 1.787(16) . ? C2 O2 1.130(11) . ? C3 O3 1.118(12) . ? N1 H1B 0.90(2) . ? N1 H1A 0.91(2) . ? N2 C8 1.500(10) . ? N2 C4 1.503(10) . ? C4 C5 1.542(12) . ? C5 C6 1.518(12) . ? C6 C7 1.515(13) . ? C7 C8 1.513(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo C3 80.3(4) . . ? C2 Mo C1 146.4(3) . . ? C3 Mo C1 110.8(4) . . ? C2 Mo B2 106.2(4) . . ? C3 Mo B2 152.4(4) . . ? C1 Mo B2 50.0(4) . . ? C2 Mo N1 174.4(3) . . ? C3 Mo N1 101.0(3) . . ? C1 Mo N1 38.2(3) . . ? B2 Mo N1 75.2(3) . . ? C2 Mo N2 99.7(3) . . ? C3 Mo N2 170.3(3) . . ? C1 Mo N2 74.6(3) . . ? B2 Mo N2 36.9(3) . . ? N1 Mo N2 78.1(3) . . ? C2 Mo B5 119.7(4) . . ? C3 Mo B5 73.2(4) . . ? C1 Mo B5 43.2(3) . . ? B2 Mo B5 80.6(4) . . ? N1 Mo B5 65.8(3) . . ? N2 Mo B5 114.6(3) . . ? C2 Mo B3 70.7(4) . . ? C3 Mo B3 116.8(4) . . ? C1 Mo B3 76.2(3) . . ? B2 Mo B3 45.8(3) . . ? N1 Mo B3 113.1(3) . . ? N2 Mo B3 71.9(3) . . ? B5 Mo B3 74.9(4) . . ? C2 Mo B4 78.6(4) . . ? C3 Mo B4 78.3(4) . . ? C1 Mo B4 73.2(4) . . ? B2 Mo B4 76.9(4) . . ? N1 Mo B4 107.0(3) . . ? N2 Mo B4 111.2(3) . . ? B5 Mo B4 43.9(4) . . ? B3 Mo B4 42.2(4) . . ? C2 Mo I 79.3(3) . . ? C3 Mo I 81.6(3) . . ? C1 Mo I 132.5(2) . . ? B2 Mo I 125.7(3) . . ? N1 Mo I 95.4(2) . . ? N2 Mo I 88.84(17) . . ? B5 Mo I 144.2(3) . . ? B3 Mo I 140.4(3) . . ? B4 Mo I 152.3(3) . . ? N1 C1 B8 132.4(8) . . ? N1 C1 B5 107.1(8) . . ? B8 C1 B5 64.8(6) . . ? N1 C1 B7 132.1(8) . . ? B8 C1 B7 64.9(6) . . ? B5 C1 B7 119.0(7) . . ? N1 C1 B2 111.6(7) . . ? B8 C1 B2 113.9(7) . . ? B5 C1 B2 115.0(7) . . ? B7 C1 B2 60.6(6) . . ? N1 C1 Mo 75.0(4) . . ? B8 C1 Mo 136.7(6) . . ? B5 C1 Mo 75.7(5) . . ? B7 C1 Mo 126.8(6) . . ? B2 C1 Mo 66.9(4) . . ? N2 B2 B6 144.9(9) . . ? N2 B2 B7 132.6(8) . . ? B6 B2 B7 63.3(7) . . ? N2 B2 B3 117.3(8) . . ? B6 B2 B3 60.9(6) . . ? B7 B2 B3 110.0(8) . . ? N2 B2 C1 111.0(7) . . ? B6 B2 C1 103.3(7) . . ? B7 B2 C1 56.2(5) . . ? B3 B2 C1 101.0(7) . . ? N2 B2 Mo 76.0(5) . . ? B6 B2 Mo 128.4(7) . . ? B7 B2 Mo 118.7(7) . . ? B3 B2 Mo 72.8(5) . . ? C1 B2 Mo 63.1(4) . . ? B10 B3 B4 63.0(7) . . ? B10 B3 B6 60.0(6) . . ? B4 B3 B6 111.2(8) . . ? B10 B3 B2 106.4(7) . . ? B4 B3 B2 109.9(8) . . ? B6 B3 B2 57.5(6) . . ? B10 B3 Mo 123.8(7) . . ? B4 B3 Mo 70.7(5) . . ? B6 B3 Mo 114.9(6) . . ? B2 B3 Mo 61.4(5) . . ? B3 B4 B5 109.4(8) . . ? B3 B4 B10 58.0(6) . . ? B5 B4 B10 105.0(8) . . ? B3 B4 B9 106.2(8) . . ? B5 B4 B9 57.7(6) . . ? B10 B4 B9 58.8(6) . . ? B3 B4 Mo 67.1(5) . . ? B5 B4 Mo 65.4(5) . . ? B10 B4 Mo 116.7(6) . . ? B9 B4 Mo 116.1(7) . . ? C1 B5 B9 103.5(8) . . ? C1 B5 B8 57.0(6) . . ? B9 B5 B8 60.1(6) . . ? C1 B5 B4 104.6(8) . . ? B9 B5 B4 61.8(6) . . ? B8 B5 B4 109.3(8) . . ? C1 B5 Mo 61.0(4) . . ? B9 B5 Mo 124.1(7) . . ? B8 B5 Mo 115.6(6) . . ? B4 B5 Mo 70.7(5) . . ? B2 B6 B10 108.4(8) . . ? B2 B6 B11 108.1(8) . . ? B10 B6 B11 60.4(7) . . ? B2 B6 B3 61.6(6) . . ? B10 B6 B3 58.4(6) . . ? B11 B6 B3 107.1(8) . . ? B2 B6 B7 60.1(6) . . ? B10 B6 B7 107.3(8) . . ? B11 B6 B7 59.2(6) . . ? B3 B6 B7 108.1(8) . . ? C1 B7 B2 63.2(6) . . ? C1 B7 B11 101.3(8) . . ? B2 B7 B11 105.0(8) . . ? C1 B7 B8 56.1(6) . . ? B2 B7 B8 109.0(8) . . ? B11 B7 B8 59.0(6) . . ? C1 B7 B6 103.6(7) . . ? B2 B7 B6 56.7(6) . . ? B11 B7 B6 58.8(6) . . ? B8 B7 B6 105.9(8) . . ? C1 B8 B9 103.6(8) . . ? C1 B8 B11 104.6(8) . . ? B9 B8 B11 61.7(6) . . ? C1 B8 B5 58.2(6) . . ? B9 B8 B5 59.1(6) . . ? B11 B8 B5 108.6(8) . . ? C1 B8 B7 59.0(6) . . ? B9 B8 B7 109.7(8) . . ? B11 B8 B7 60.3(6) . . ? B5 B8 B7 108.7(8) . . ? B5 B9 B8 60.8(6) . . ? B5 B9 B10 108.5(8) . . ? B8 B9 B10 107.2(8) . . ? B5 B9 B11 108.1(9) . . ? B8 B9 B11 59.2(6) . . ? B10 B9 B11 59.3(6) . . ? B5 B9 B4 60.5(6) . . ? B8 B9 B4 108.8(8) . . ? B10 B9 B4 60.4(6) . . ? B11 B9 B4 107.9(8) . . ? B3 B10 B6 61.6(6) . . ? B3 B10 B11 109.8(8) . . ? B6 B10 B11 60.6(7) . . ? B3 B10 B9 108.6(8) . . ? B6 B10 B9 109.9(8) . . ? B11 B10 B9 61.0(7) . . ? B3 B10 B4 58.9(6) . . ? B6 B10 B4 109.2(8) . . ? B11 B10 B4 109.7(9) . . ? B9 B10 B4 60.8(6) . . ? B8 B11 B10 107.4(9) . . ? B8 B11 B6 109.8(9) . . ? B10 B11 B6 59.1(7) . . ? B8 B11 B7 60.7(7) . . ? B10 B11 B7 108.5(8) . . ? B6 B11 B7 62.0(7) . . ? B8 B11 B9 59.2(6) . . ? B10 B11 B9 59.6(7) . . ? B6 B11 B9 107.6(8) . . ? B7 B11 B9 108.0(9) . . ? O2 C2 Mo 175.5(9) . . ? O3 C3 Mo 176.0(8) . . ? H1B N1 H1A 111(8) . . ? H1B N1 C1 106(6) . . ? H1A N1 C1 110(6) . . ? H1B N1 Mo 126(6) . . ? H1A N1 Mo 121(6) . . ? C1 N1 Mo 66.8(4) . . ? B2 N2 C8 118.0(7) . . ? B2 N2 C4 121.0(7) . . ? C8 N2 C4 109.3(7) . . ? B2 N2 Mo 67.0(5) . . ? C8 N2 Mo 126.5(5) . . ? C4 N2 Mo 110.0(5) . . ? N2 C4 C5 113.2(7) . . ? C6 C5 C4 110.7(8) . . ? C7 C6 C5 109.1(8) . . ? C8 C7 C6 112.8(7) . . ? N2 C8 C7 110.6(7) . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 1.561 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.179 #===END