# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'N Connelly' _publ_contact_author_email NEIL.CONNELLY@BRISTOL.AC.UK _publ_section_title ; The effect of redox-active cyanomanganese(I) ligands on intramolecular electron transfer to, and alkyne alignment in, M(CO)(RC?CR)Tp' (M = Mo or W) units ; loop_ _publ_author_name 'N Connelly' 'Chris Adams' 'sriwipha onganusorn' # Attachment 'Revised_cifs.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 702894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H32 B N7 O W' _chemical_formula_weight 713.30 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' W W -0.8490 6.8722 '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 17.173(2) _cell_length_b 9.4865(16) _cell_length_c 18.3138(18) _cell_angle_alpha 90.00 _cell_angle_beta 108.157(8) _cell_angle_gamma 90.00 _cell_volume 2834.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 4.113 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.545 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details XPREP _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17821 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0522 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6374 _reflns_number_gt 5299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6374 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0492 _refine_ls_wR_factor_gt 0.0479 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.228302(8) 0.560508(13) 0.262124(7) 0.01139(4) Uani 1 1 d . . . N1 N 0.16175(15) 0.3578(3) 0.36481(15) 0.0119(6) Uani 1 1 d . . . N2 N 0.17885(15) 0.3671(3) 0.29597(15) 0.0129(6) Uani 1 1 d . . . C1 C 0.11808(19) 0.1797(3) 0.44479(18) 0.0159(7) Uani 1 1 d . . . H1A H 0.0762 0.2430 0.4524 0.024 Uiso 1 1 calc R . . H1B H 0.1669 0.1828 0.4902 0.024 Uiso 1 1 calc R . . H1C H 0.0967 0.0832 0.4371 0.024 Uiso 1 1 calc R . . C2 C 0.14020(19) 0.2255(3) 0.37580(18) 0.0136(7) Uani 1 1 d . . . C3 C 0.14236(19) 0.1464(3) 0.31325(18) 0.0157(7) Uani 1 1 d . . . H3A H 0.1301 0.0489 0.3050 0.019 Uiso 1 1 calc R . . C4 C 0.16607(18) 0.2379(3) 0.26462(18) 0.0134(7) Uani 1 1 d . . . C5 C 0.1783(2) 0.2045(3) 0.18889(18) 0.0185(8) Uani 1 1 d . . . H5A H 0.1556 0.2809 0.1524 0.028 Uiso 1 1 calc R . . H5B H 0.1503 0.1160 0.1689 0.028 Uiso 1 1 calc R . . H5C H 0.2370 0.1949 0.1959 0.028 Uiso 1 1 calc R . . N3 N 0.12432(16) 0.6112(3) 0.37386(16) 0.0148(6) Uani 1 1 d . . . N4 N 0.13153(16) 0.6534(3) 0.30415(15) 0.0148(6) Uani 1 1 d . . . C6 C 0.0456(2) 0.6758(4) 0.4631(2) 0.0248(8) Uani 1 1 d . . . H6A H 0.0952 0.6625 0.5070 0.037 Uiso 1 1 calc R . . H6B H 0.0101 0.5931 0.4579 0.037 Uiso 1 1 calc R . . H6C H 0.0164 0.7599 0.4715 0.037 Uiso 1 1 calc R . . C7 C 0.06869(19) 0.6938(3) 0.3915(2) 0.0174(7) Uani 1 1 d . . . C8 C 0.03888(19) 0.7883(3) 0.3328(2) 0.0184(8) Uani 1 1 d . . . H8A H -0.0010 0.8593 0.3298 0.022 Uiso 1 1 calc R . . C9 C 0.07804(19) 0.7604(3) 0.2786(2) 0.0153(7) Uani 1 1 d . . . C10 C 0.0642(2) 0.8336(3) 0.20342(19) 0.0197(8) Uani 1 1 d . . . H10A H 0.1169 0.8648 0.1988 0.030 Uiso 1 1 calc R . . H10B H 0.0286 0.9156 0.2007 0.030 Uiso 1 1 calc R . . H10C H 0.0379 0.7685 0.1614 0.030 Uiso 1 1 calc R . . N5 N 0.26698(16) 0.5269(3) 0.44162(15) 0.0130(6) Uani 1 1 d . . . N6 N 0.29926(15) 0.5747(3) 0.38652(15) 0.0124(6) Uani 1 1 d . . . C11 C 0.3065(2) 0.4892(4) 0.58377(19) 0.0219(8) Uani 1 1 d . . . H11A H 0.2738 0.4026 0.5749 0.033 Uiso 1 1 calc R . . H11B H 0.2759 0.5651 0.5988 0.033 Uiso 1 1 calc R . . H11C H 0.3582 0.4733 0.6249 0.033 Uiso 1 1 calc R . . C12 C 0.3244(2) 0.5298(3) 0.51153(19) 0.0167(8) Uani 1 1 d . . . C13 C 0.3958(2) 0.5789(3) 0.50179(19) 0.0176(7) Uani 1 1 d . . . H13A H 0.4471 0.5903 0.5405 0.021 Uiso 1 1 calc R . . C14 C 0.3779(2) 0.6085(3) 0.42380(19) 0.0155(7) Uani 1 1 d . . . C15 C 0.43449(19) 0.6761(4) 0.38640(19) 0.0189(8) Uani 1 1 d . . . H15A H 0.4322 0.6244 0.3394 0.028 Uiso 1 1 calc R . . H15B H 0.4906 0.6739 0.4218 0.028 Uiso 1 1 calc R . . H15C H 0.4178 0.7740 0.3735 0.028 Uiso 1 1 calc R . . B1 B 0.1759(2) 0.4867(4) 0.4181(2) 0.0148(8) Uani 1 1 d . . . H1 H 0.1597 0.4643 0.4647 0.018 Uiso 1 1 calc R . . C16 C 0.28537(19) 0.5003(3) 0.18451(19) 0.0130(7) Uani 1 1 d . . . C17 C 0.28846(18) 0.4978(3) 0.10522(18) 0.0122(7) Uani 1 1 d . . . C18 C 0.25639(19) 0.6075(3) 0.05367(19) 0.0150(7) Uani 1 1 d . . . H18A H 0.2284 0.6833 0.0684 0.018 Uiso 1 1 calc R . . C19 C 0.2654(2) 0.6058(3) -0.01871(19) 0.0165(7) Uani 1 1 d . . . H19A H 0.2445 0.6817 -0.0531 0.020 Uiso 1 1 calc R . . C20 C 0.3043(2) 0.4952(4) -0.04157(19) 0.0186(8) Uani 1 1 d . . . H20A H 0.3097 0.4944 -0.0917 0.022 Uiso 1 1 calc R . . C21 C 0.33594(19) 0.3845(3) 0.00918(18) 0.0154(7) Uani 1 1 d . . . H21A H 0.3625 0.3076 -0.0065 0.018 Uiso 1 1 calc R . . C22 C 0.32863(19) 0.3865(3) 0.08225(19) 0.0147(7) Uani 1 1 d . . . H22A H 0.3511 0.3118 0.1170 0.018 Uiso 1 1 calc R . . C23 C 0.32653(19) 0.4522(3) 0.25287(18) 0.0136(7) Uani 1 1 d . . . C24 C 0.39639(19) 0.3612(3) 0.29037(18) 0.0138(7) Uani 1 1 d . . . C25 C 0.3898(2) 0.2665(3) 0.34634(18) 0.0167(7) Uani 1 1 d . . . H25A H 0.3422 0.2668 0.3623 0.020 Uiso 1 1 calc R . . C26 C 0.4526(2) 0.1718(4) 0.37878(19) 0.0206(8) Uani 1 1 d . . . H26A H 0.4469 0.1046 0.4152 0.025 Uiso 1 1 calc R . . C27 C 0.5231(2) 0.1749(4) 0.35840(19) 0.0204(8) Uani 1 1 d . . . H27A H 0.5665 0.1112 0.3815 0.024 Uiso 1 1 calc R . . C28 C 0.5309(2) 0.2709(4) 0.30410(19) 0.0187(8) Uani 1 1 d . . . H28A H 0.5799 0.2736 0.2904 0.022 Uiso 1 1 calc R . . C29 C 0.4680(2) 0.3622(3) 0.26993(19) 0.0169(7) Uani 1 1 d . . . H29A H 0.4734 0.4265 0.2320 0.020 Uiso 1 1 calc R . . C30 C 0.14506(19) 0.5655(3) 0.15970(19) 0.0143(7) Uani 1 1 d . . . O1 O 0.09523(14) 0.5605(3) 0.10065(13) 0.0223(5) Uani 1 1 d . . . C31 C 0.26312(19) 0.7745(3) 0.25592(18) 0.0152(7) Uani 1 1 d . . . N7 N 0.28271(17) 0.8909(3) 0.25514(17) 0.0236(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.01012(7) 0.01410(6) 0.01061(7) 0.00016(6) 0.00419(5) 0.00085(6) N1 0.0126(15) 0.0155(14) 0.0099(14) -0.0008(11) 0.0069(12) 0.0009(11) N2 0.0110(15) 0.0192(14) 0.0096(14) 0.0007(11) 0.0049(12) 0.0012(11) C1 0.0120(18) 0.0195(17) 0.0166(18) 0.0014(14) 0.0049(15) -0.0011(14) C2 0.0076(17) 0.0178(16) 0.0137(18) 0.0036(13) 0.0010(14) 0.0012(13) C3 0.0158(19) 0.0135(16) 0.0164(18) 0.0004(13) 0.0030(15) 0.0005(13) C4 0.0087(17) 0.0172(16) 0.0129(18) -0.0025(13) 0.0016(14) 0.0032(13) C5 0.023(2) 0.0184(17) 0.0153(18) -0.0051(14) 0.0075(16) -0.0007(15) N3 0.0151(16) 0.0156(13) 0.0170(16) -0.0015(12) 0.0096(13) -0.0027(11) N4 0.0137(15) 0.0184(14) 0.0130(15) 0.0001(11) 0.0054(12) 0.0002(12) C6 0.023(2) 0.0265(19) 0.031(2) -0.0056(17) 0.0180(18) 0.0015(16) C7 0.0126(18) 0.0192(17) 0.024(2) -0.0087(15) 0.0110(16) -0.0032(14) C8 0.0104(18) 0.0181(17) 0.027(2) -0.0058(15) 0.0072(16) -0.0001(14) C9 0.0086(17) 0.0129(16) 0.024(2) -0.0029(14) 0.0047(15) -0.0010(13) C10 0.0143(19) 0.0171(17) 0.025(2) -0.0023(15) 0.0026(16) 0.0020(14) N5 0.0148(15) 0.0154(14) 0.0104(14) 0.0001(11) 0.0061(12) -0.0006(11) N6 0.0113(14) 0.0138(13) 0.0125(14) -0.0007(11) 0.0043(12) 0.0005(11) C11 0.029(2) 0.0213(17) 0.0139(19) -0.0010(14) 0.0039(17) -0.0015(16) C12 0.023(2) 0.0151(17) 0.0118(18) -0.0007(13) 0.0048(16) 0.0020(14) C13 0.0173(19) 0.0183(17) 0.0147(18) -0.0009(14) 0.0012(15) 0.0013(14) C14 0.0140(19) 0.0154(15) 0.0179(19) -0.0007(14) 0.0060(16) 0.0024(13) C15 0.0147(19) 0.0252(18) 0.0166(19) -0.0007(15) 0.0047(15) -0.0003(15) B1 0.018(2) 0.0162(18) 0.013(2) 0.0001(15) 0.0092(18) -0.0027(16) C16 0.0122(18) 0.0144(15) 0.0144(18) 0.0010(13) 0.0069(15) -0.0016(13) C17 0.0078(17) 0.0179(15) 0.0129(17) -0.0008(13) 0.0059(14) -0.0054(13) C18 0.0115(18) 0.0154(15) 0.0188(19) -0.0015(14) 0.0055(15) -0.0015(13) C19 0.0156(19) 0.0206(17) 0.0120(18) 0.0029(13) 0.0022(15) -0.0049(14) C20 0.0157(19) 0.0292(18) 0.0118(18) -0.0030(15) 0.0059(15) -0.0045(15) C21 0.0145(18) 0.0197(16) 0.0147(18) -0.0076(14) 0.0085(15) -0.0004(14) C22 0.0126(18) 0.0170(15) 0.0141(18) 0.0015(13) 0.0037(15) -0.0009(13) C23 0.0109(17) 0.0161(16) 0.0159(17) -0.0049(14) 0.0071(14) -0.0051(14) C24 0.0134(18) 0.0172(16) 0.0093(17) -0.0034(13) 0.0015(14) 0.0019(13) C25 0.0128(18) 0.0226(17) 0.0162(18) 0.0022(14) 0.0068(15) 0.0008(14) C26 0.017(2) 0.0246(18) 0.020(2) 0.0064(15) 0.0058(16) 0.0015(15) C27 0.0151(19) 0.0222(18) 0.020(2) -0.0050(15) -0.0001(16) 0.0069(15) C28 0.0126(19) 0.0273(19) 0.0168(19) -0.0047(15) 0.0054(16) 0.0038(15) C29 0.0155(19) 0.0233(18) 0.0124(18) 0.0003(14) 0.0051(15) -0.0017(14) C30 0.0139(18) 0.0175(15) 0.0156(18) 0.0022(15) 0.0104(15) 0.0035(15) O1 0.0174(13) 0.0307(13) 0.0175(13) 0.0016(12) 0.0037(11) 0.0051(11) C31 0.0105(18) 0.0221(18) 0.0128(18) 0.0026(14) 0.0033(14) 0.0051(14) N7 0.0216(18) 0.0240(16) 0.0274(19) 0.0041(13) 0.0110(15) 0.0013(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 W1 C30 1.973(3) . ? W1 C23 2.027(3) . ? W1 C16 2.043(3) . ? W1 C31 2.129(3) . ? W1 N2 2.191(3) . ? W1 N4 2.220(3) . ? W1 N6 2.228(3) . ? N1 C2 1.341(4) . ? N1 N2 1.384(3) . ? N1 B1 1.535(4) . ? N2 C4 1.342(4) . ? C1 C2 1.493(4) . ? C2 C3 1.380(4) . ? C3 C4 1.392(4) . ? C4 C5 1.500(4) . ? N3 C7 1.350(4) . ? N3 N4 1.380(3) . ? N3 B1 1.545(4) . ? N4 C9 1.351(4) . ? C6 C7 1.494(4) . ? C7 C8 1.370(5) . ? C8 C9 1.386(4) . ? C9 C10 1.494(4) . ? N5 C12 1.351(4) . ? N5 N6 1.371(3) . ? N5 B1 1.536(4) . ? N6 C14 1.349(4) . ? C11 C12 1.499(5) . ? C12 C13 1.374(5) . ? C13 C14 1.393(4) . ? C14 C15 1.496(4) . ? C16 C23 1.313(4) . ? C16 C17 1.470(4) . ? C17 C22 1.396(4) . ? C17 C18 1.397(4) . ? C18 C19 1.381(4) . ? C19 C20 1.378(5) . ? C20 C21 1.396(5) . ? C21 C22 1.383(4) . ? C23 C24 1.464(4) . ? C24 C29 1.393(4) . ? C24 C25 1.394(4) . ? C25 C26 1.388(4) . ? C26 C27 1.374(4) . ? C27 C28 1.385(5) . ? C28 C29 1.373(4) . ? C30 O1 1.152(4) . ? C31 N7 1.156(4) . ? 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 C30 W1 C23 107.94(13) . . ? C30 W1 C16 73.01(13) . . ? C23 W1 C16 37.64(12) . . ? C30 W1 C31 93.37(13) . . ? C23 W1 C31 102.94(12) . . ? C16 W1 C31 91.48(12) . . ? C30 W1 N2 93.39(11) . . ? C23 W1 N2 90.30(11) . . ? C16 W1 N2 105.96(11) . . ? C31 W1 N2 162.47(11) . . ? C30 W1 N4 85.48(11) . . ? C23 W1 N4 164.30(11) . . ? C16 W1 N4 157.71(11) . . ? C31 W1 N4 83.86(11) . . ? N2 W1 N4 80.57(9) . . ? C30 W1 N6 166.94(11) . . ? C23 W1 N6 84.94(11) . . ? C16 W1 N6 120.01(11) . . ? C31 W1 N6 85.63(11) . . ? N2 W1 N6 84.15(9) . . ? N4 W1 N6 81.46(9) . . ? C2 N1 N2 110.1(2) . . ? C2 N1 B1 130.3(3) . . ? N2 N1 B1 119.5(2) . . ? C4 N2 N1 106.2(2) . . ? C4 N2 W1 132.1(2) . . ? N1 N2 W1 121.48(18) . . ? N1 C2 C3 107.7(3) . . ? N1 C2 C1 123.7(3) . . ? C3 C2 C1 128.6(3) . . ? C2 C3 C4 106.3(3) . . ? N2 C4 C3 109.7(3) . . ? N2 C4 C5 122.5(3) . . ? C3 C4 C5 127.8(3) . . ? C7 N3 N4 109.1(3) . . ? C7 N3 B1 130.6(3) . . ? N4 N3 B1 120.3(3) . . ? C9 N4 N3 106.9(3) . . ? C9 N4 W1 132.8(2) . . ? N3 N4 W1 119.89(19) . . ? N3 C7 C8 108.2(3) . . ? N3 C7 C6 123.0(3) . . ? C8 C7 C6 128.9(3) . . ? C7 C8 C9 106.9(3) . . ? N4 C9 C8 108.9(3) . . ? N4 C9 C10 124.3(3) . . ? C8 C9 C10 126.7(3) . . ? C12 N5 N6 110.3(3) . . ? C12 N5 B1 130.5(3) . . ? N6 N5 B1 119.0(2) . . ? C14 N6 N5 106.1(2) . . ? C14 N6 W1 132.4(2) . . ? N5 N6 W1 120.99(19) . . ? N5 C12 C13 107.5(3) . . ? N5 C12 C11 122.8(3) . . ? C13 C12 C11 129.6(3) . . ? C12 C13 C14 106.4(3) . . ? N6 C14 C13 109.7(3) . . ? N6 C14 C15 124.1(3) . . ? C13 C14 C15 126.1(3) . . ? N1 B1 N5 108.8(3) . . ? N1 B1 N3 108.9(3) . . ? N5 B1 N3 108.9(3) . . ? C23 C16 C17 139.7(3) . . ? C23 C16 W1 70.5(2) . . ? C17 C16 W1 149.8(2) . . ? C22 C17 C18 119.2(3) . . ? C22 C17 C16 118.9(3) . . ? C18 C17 C16 121.9(3) . . ? C19 C18 C17 120.1(3) . . ? C20 C19 C18 120.7(3) . . ? C19 C20 C21 119.7(3) . . ? C22 C21 C20 120.0(3) . . ? C21 C22 C17 120.3(3) . . ? C16 C23 C24 140.5(3) . . ? C16 C23 W1 71.9(2) . . ? C24 C23 W1 147.3(2) . . ? C29 C24 C25 118.9(3) . . ? C29 C24 C23 122.2(3) . . ? C25 C24 C23 118.8(3) . . ? C26 C25 C24 120.1(3) . . ? C27 C26 C25 120.2(3) . . ? C26 C27 C28 119.9(3) . . ? C29 C28 C27 120.3(3) . . ? C28 C29 C24 120.5(3) . . ? O1 C30 W1 176.0(3) . . ? N7 C31 W1 177.8(3) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.223 _refine_diff_density_min -1.623 _refine_diff_density_rms 0.114 #===END data_21[PF6].Et2O _database_code_depnum_ccdc_archive 'CCDC 702895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H79 B F6 Mn Mo N7 O7 P4' _chemical_formula_weight 1505.95 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.117(3) _cell_length_b 30.205(6) _cell_length_c 17.119(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.97(3) _cell_angle_gamma 90.00 _cell_volume 7272(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1745 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 18.21 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78104 _diffrn_reflns_av_R_equivalents 0.1711 _diffrn_reflns_av_sigmaI/netI 0.3583 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16195 _reflns_number_gt 6338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16195 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2244 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.05668(5) 0.22471(2) 0.47193(4) 0.00855(17) Uani 1 1 d . . . N1 N 0.8846(4) 0.16834(19) 0.5163(3) 0.0112(15) Uiso 1 1 d . . . N2 N 0.9822(4) 0.17288(19) 0.5318(3) 0.0132(16) Uiso 1 1 d . . . C1 C 0.7563(5) 0.1150(2) 0.5397(4) 0.021(2) Uiso 1 1 d . . . H1A H 0.7178 0.1364 0.5662 0.031 Uiso 1 1 calc R . . H1B H 0.7511 0.0858 0.5637 0.031 Uiso 1 1 calc R . . H1C H 0.7335 0.1135 0.4840 0.031 Uiso 1 1 calc R . . C2 C 0.8577(5) 0.1295(2) 0.5474(4) 0.0104(18) Uiso 1 1 d . . . C3 C 0.9377(5) 0.1082(3) 0.5822(4) 0.016(2) Uiso 1 1 d . . . H3A H 0.9402 0.0801 0.6073 0.019 Uiso 1 1 calc R . . C4 C 1.0125(6) 0.1361(3) 0.5728(4) 0.017(2) Uiso 1 1 d . . . C5 C 1.1158(5) 0.1288(3) 0.5970(5) 0.023(2) Uiso 1 1 d . . . H5A H 1.1229 0.1035 0.6330 0.034 Uiso 1 1 calc R . . H5B H 1.1424 0.1554 0.6234 0.034 Uiso 1 1 calc R . . H5C H 1.1495 0.1227 0.5505 0.034 Uiso 1 1 calc R . . N3 N 0.8476(4) 0.21059(19) 0.3937(3) 0.0126(16) Uiso 1 1 d . . . N4 N 0.9413(4) 0.21895(19) 0.3760(3) 0.0093(15) Uiso 1 1 d . . . C6 C 0.6842(5) 0.2044(3) 0.3261(5) 0.023(2) Uiso 1 1 d . . . H6A H 0.6546 0.2067 0.2723 0.034 Uiso 1 1 calc R . . H6B H 0.6574 0.2271 0.3587 0.034 Uiso 1 1 calc R . . H6C H 0.6719 0.1750 0.3472 0.034 Uiso 1 1 calc R . . C7 C 0.7907(5) 0.2114(2) 0.3263(4) 0.0110(19) Uiso 1 1 d . . . C8 C 0.8436(5) 0.2185(2) 0.2649(5) 0.019(2) Uiso 1 1 d . . . H8A H 0.8212 0.2198 0.2109 0.023 Uiso 1 1 calc R . . C9 C 0.9380(5) 0.2236(2) 0.2969(4) 0.0106(17) Uiso 1 1 d . . . C10 C 1.0219(5) 0.2333(2) 0.2528(4) 0.020(2) Uiso 1 1 d . . . H10A H 1.0799 0.2322 0.2887 0.029 Uiso 1 1 calc R . . H10B H 1.0152 0.2629 0.2294 0.029 Uiso 1 1 calc R . . H10C H 1.0261 0.2113 0.2113 0.029 Uiso 1 1 calc R . . N5 N 0.8539(4) 0.24992(19) 0.5209(3) 0.0120(16) Uiso 1 1 d . . . N6 N 0.9460(5) 0.26588(19) 0.5232(4) 0.0142(15) Uiso 1 1 d . . . C11 C 0.6971(5) 0.2720(3) 0.5666(5) 0.029(2) Uiso 1 1 d . . . H11A H 0.6717 0.2977 0.5928 0.044 Uiso 1 1 calc R . . H11B H 0.6905 0.2456 0.5987 0.044 Uiso 1 1 calc R . . H11C H 0.6618 0.2679 0.5153 0.044 Uiso 1 1 calc R . . C12 C 0.8008(5) 0.2796(3) 0.5559(4) 0.0141(19) Uiso 1 1 d . . . C13 C 0.8555(6) 0.3152(3) 0.5797(5) 0.022(2) Uiso 1 1 d . . . H13A H 0.8353 0.3412 0.6047 0.026 Uiso 1 1 calc R . . C14 C 0.9452(6) 0.3059(2) 0.5604(4) 0.0135(19) Uiso 1 1 d . . . C15 C 1.0324(6) 0.3344(2) 0.5751(5) 0.025(2) Uiso 1 1 d . . . H15A H 1.0842 0.3219 0.5473 0.038 Uiso 1 1 calc R . . H15B H 1.0516 0.3353 0.6314 0.038 Uiso 1 1 calc R . . H15C H 1.0181 0.3644 0.5560 0.038 Uiso 1 1 calc R . . B1 B 0.8273(7) 0.2072(3) 0.4791(5) 0.017(2) Uiso 1 1 d . . . H1 H 0.7579 0.2014 0.4822 0.021 Uiso 1 1 calc R . . C16 C 1.1385(5) 0.2404(2) 0.5661(4) 0.0146(19) Uiso 1 1 d . . . O1 O 1.1868(4) 0.25042(18) 0.6217(3) 0.0292(16) Uiso 1 1 d . . . C17 C 1.1200(5) 0.1779(2) 0.4112(4) 0.0126(19) Uiso 1 1 d . . . C18 C 1.1880(5) 0.1960(2) 0.4576(4) 0.0107(18) Uiso 1 1 d . . . C19 C 1.2913(5) 0.1960(2) 0.4814(4) 0.0117(19) Uiso 1 1 d . . . C20 C 1.3386(6) 0.1554(3) 0.4771(4) 0.021(2) Uiso 1 1 d . . . H20A H 1.3054 0.1290 0.4620 0.025 Uiso 1 1 calc R . . C21 C 1.4365(6) 0.1555(3) 0.4960(5) 0.029(2) Uiso 1 1 d . . . H21A H 1.4704 0.1283 0.4956 0.034 Uiso 1 1 calc R . . C22 C 1.4860(6) 0.1943(3) 0.5154(5) 0.033(3) Uiso 1 1 d . . . H22A H 1.5531 0.1937 0.5270 0.040 Uiso 1 1 calc R . . C23 C 1.4363(6) 0.2343(3) 0.5177(5) 0.031(2) Uiso 1 1 d . . . H23A H 1.4693 0.2609 0.5318 0.037 Uiso 1 1 calc R . . C24 C 1.3383(6) 0.2350(3) 0.4994(4) 0.022(2) Uiso 1 1 d . . . H24A H 1.3043 0.2622 0.4992 0.026 Uiso 1 1 calc R . . C25 C 1.1049(5) 0.1426(2) 0.3536(4) 0.0119(19) Uiso 1 1 d . . . C26 C 1.0181(6) 0.1200(2) 0.3447(4) 0.018(2) Uiso 1 1 d . . . H26A H 0.9683 0.1278 0.3759 0.022 Uiso 1 1 calc R . . C27 C 1.0052(6) 0.0862(3) 0.2903(5) 0.026(2) Uiso 1 1 d . . . H27A H 0.9460 0.0711 0.2841 0.031 Uiso 1 1 calc R . . C28 C 1.0759(6) 0.0743(3) 0.2455(5) 0.025(2) Uiso 1 1 d . . . H28A H 1.0654 0.0508 0.2088 0.030 Uiso 1 1 calc R . . C29 C 1.1640(6) 0.0960(3) 0.2525(5) 0.027(2) Uiso 1 1 d . . . H29A H 1.2125 0.0884 0.2197 0.032 Uiso 1 1 calc R . . C30 C 1.1785(6) 0.1291(3) 0.3088(5) 0.023(2) Uiso 1 1 d . . . H30A H 1.2392 0.1427 0.3171 0.028 Uiso 1 1 calc R . . C31 C 1.0916(5) 0.2842(2) 0.4143(4) 0.0065(17) Uiso 1 1 d . . . N7 N 1.1102(4) 0.31722(19) 0.3845(3) 0.0080(15) Uiso 1 1 d . . . Mn1 Mn 1.13986(8) 0.37360(4) 0.33385(7) 0.0092(3) Uani 1 1 d . . . C32 C 1.1360(5) 0.4011(2) 0.4281(4) 0.0086(18) Uiso 1 1 d . . . O2 O 1.1306(4) 0.41992(17) 0.4855(3) 0.0238(15) Uiso 1 1 d . . . C33 C 1.1353(5) 0.3482(2) 0.2376(4) 0.0109(19) Uiso 1 1 d . . . O3 O 1.1314(4) 0.33226(16) 0.1761(3) 0.0191(14) Uiso 1 1 d . . . P1 P 0.98945(15) 0.39365(7) 0.31169(12) 0.0114(5) Uiso 1 1 d . . . O4 O 0.9469(3) 0.38338(15) 0.2232(3) 0.0143(13) Uiso 1 1 d . . . C34 C 0.8507(5) 0.3934(3) 0.1926(4) 0.020(2) Uiso 1 1 d . . . H34A H 0.8126 0.4015 0.2363 0.024 Uiso 1 1 calc R . . H34B H 0.8217 0.3668 0.1666 0.024 Uiso 1 1 calc R . . C34A C 0.8488(5) 0.4308(2) 0.1348(4) 0.019(2) Uiso 1 1 d . . . H34C H 0.7839 0.4347 0.1105 0.029 Uiso 1 1 calc R . . H34D H 0.8915 0.4241 0.0942 0.029 Uiso 1 1 calc R . . H34E H 0.8698 0.4581 0.1620 0.029 Uiso 1 1 calc R . . O5 O 0.9109(3) 0.37360(16) 0.3638(3) 0.0147(13) Uiso 1 1 d . . . C35 C 0.8682(5) 0.3299(2) 0.3509(4) 0.015(2) Uiso 1 1 d . . . H35A H 0.9004 0.3081 0.3874 0.018 Uiso 1 1 calc R . . H35B H 0.8749 0.3200 0.2965 0.018 Uiso 1 1 calc R . . C35A C 0.7644(5) 0.3334(3) 0.3650(5) 0.022(2) Uiso 1 1 d . . . H35C H 0.7334 0.3047 0.3547 0.033 Uiso 1 1 calc R . . H35D H 0.7337 0.3558 0.3299 0.033 Uiso 1 1 calc R . . H35E H 0.7586 0.3420 0.4196 0.033 Uiso 1 1 calc R . . O6 O 0.9735(3) 0.44475(15) 0.3260(3) 0.0140(13) Uiso 1 1 d . . . C36 C 0.8846(6) 0.4651(3) 0.3422(5) 0.037(3) Uiso 1 1 d . . . H36A H 0.8467 0.4438 0.3706 0.044 Uiso 1 1 calc R . . H36B H 0.8477 0.4727 0.2922 0.044 Uiso 1 1 calc R . . C36A C 0.9009(7) 0.5051(3) 0.3895(5) 0.043(3) Uiso 1 1 d . . . H36C H 0.8401 0.5162 0.4052 0.065 Uiso 1 1 calc R . . H36D H 0.9305 0.5278 0.3586 0.065 Uiso 1 1 calc R . . H36E H 0.9431 0.4982 0.4364 0.065 Uiso 1 1 calc R . . P2 P 1.21224(15) 0.43490(7) 0.29044(12) 0.0097(5) Uiso 1 1 d . . . C37 C 1.3289(5) 0.4094(2) 0.2868(4) 0.0076(18) Uiso 1 1 d . . . H37A H 1.3809 0.4276 0.3126 0.009 Uiso 1 1 calc R . . H37B H 1.3431 0.4017 0.2329 0.009 Uiso 1 1 calc R . . P3 P 1.30112(15) 0.36077(7) 0.34501(12) 0.0101(5) Uiso 1 1 d . . . C38 C 1.2282(5) 0.4828(2) 0.3570(4) 0.0125(19) Uiso 1 1 d . . . C39 C 1.3048(6) 0.4865(3) 0.4125(4) 0.018(2) Uiso 1 1 d . . . H39A H 1.3537 0.4648 0.4149 0.021 Uiso 1 1 calc R . . C40 C 1.3106(6) 0.5212(2) 0.4643(4) 0.019(2) Uiso 1 1 d . . . H40A H 1.3635 0.5239 0.5022 0.023 Uiso 1 1 calc R . . C41 C 1.2398(6) 0.5516(3) 0.4607(5) 0.021(2) Uiso 1 1 d . . . H41A H 1.2436 0.5754 0.4972 0.025 Uiso 1 1 calc R . . C42 C 1.1622(6) 0.5493(3) 0.4058(4) 0.019(2) Uiso 1 1 d . . . H42A H 1.1136 0.5711 0.4040 0.023 Uiso 1 1 calc R . . C43 C 1.1571(5) 0.5142(2) 0.3532(4) 0.0139(19) Uiso 1 1 d . . . H43A H 1.1047 0.5118 0.3147 0.017 Uiso 1 1 calc R . . C44 C 1.1892(5) 0.4614(2) 0.1949(4) 0.0111(18) Uiso 1 1 d . . . C45 C 1.1061(6) 0.4535(2) 0.1483(4) 0.018(2) Uiso 1 1 d . . . H45A H 1.0589 0.4346 0.1665 0.021 Uiso 1 1 calc R . . C46 C 1.0915(6) 0.4732(3) 0.0749(5) 0.023(2) Uiso 1 1 d . . . H46A H 1.0358 0.4668 0.0417 0.028 Uiso 1 1 calc R . . C47 C 1.1583(6) 0.5022(3) 0.0508(5) 0.024(2) Uiso 1 1 d . . . H47A H 1.1465 0.5168 0.0018 0.028 Uiso 1 1 calc R . . C48 C 1.2411(6) 0.5103(3) 0.0956(5) 0.025(2) Uiso 1 1 d . . . H48A H 1.2876 0.5294 0.0767 0.030 Uiso 1 1 calc R . . C49 C 1.2570(6) 0.4906(2) 0.1691(5) 0.023(2) Uiso 1 1 d . . . H49A H 1.3135 0.4969 0.2015 0.028 Uiso 1 1 calc R . . C50 C 1.3733(5) 0.3636(2) 0.4386(4) 0.0114(19) Uiso 1 1 d . . . C51 C 1.4709(6) 0.3735(2) 0.4408(5) 0.019(2) Uiso 1 1 d . . . H51A H 1.4994 0.3805 0.3941 0.023 Uiso 1 1 calc R . . C52 C 1.5246(7) 0.3728(3) 0.5123(5) 0.036(3) Uiso 1 1 d . . . H52A H 1.5903 0.3800 0.5147 0.043 Uiso 1 1 calc R . . C53 C 1.4848(6) 0.3619(3) 0.5796(5) 0.030(2) Uiso 1 1 d . . . H53A H 1.5233 0.3609 0.6279 0.035 Uiso 1 1 calc R . . C54 C 1.3901(6) 0.3523(3) 0.5783(5) 0.031(2) Uiso 1 1 d . . . H54A H 1.3620 0.3452 0.6252 0.037 Uiso 1 1 calc R . . C55 C 1.3355(6) 0.3532(2) 0.5062(4) 0.017(2) Uiso 1 1 d . . . H55A H 1.2698 0.3462 0.5046 0.021 Uiso 1 1 calc R . . C56 C 1.3526(5) 0.3130(2) 0.3000(4) 0.0104(18) Uiso 1 1 d . . . C57 C 1.3146(6) 0.2720(3) 0.3086(4) 0.024(2) Uiso 1 1 d . . . H57A H 1.2572 0.2687 0.3333 0.028 Uiso 1 1 calc R . . C58 C 1.3597(6) 0.2351(3) 0.2813(5) 0.032(2) Uiso 1 1 d . . . H58A H 1.3329 0.2066 0.2875 0.039 Uiso 1 1 calc R . . C59 C 1.4426(6) 0.2390(3) 0.2454(5) 0.023(2) Uiso 1 1 d . . . H59A H 1.4737 0.2132 0.2285 0.028 Uiso 1 1 calc R . . C60 C 1.4794(6) 0.2789(3) 0.2342(5) 0.028(2) Uiso 1 1 d . . . H60A H 1.5350 0.2819 0.2071 0.034 Uiso 1 1 calc R . . C61 C 1.4358(6) 0.3163(3) 0.2626(5) 0.029(2) Uiso 1 1 d . . . H61A H 1.4635 0.3446 0.2562 0.035 Uiso 1 1 calc R . . P4 P 1.59754(16) 0.46176(7) 0.29100(13) 0.0164(5) Uiso 1 1 d . . . F1 F 1.5197(3) 0.47893(15) 0.2233(3) 0.0338(13) Uiso 1 1 d . . . F2 F 1.5215(3) 0.46784(14) 0.3547(3) 0.0288(13) Uiso 1 1 d . . . F3 F 1.6738(3) 0.44301(14) 0.3570(3) 0.0304(13) Uiso 1 1 d . . . F4 F 1.5594(3) 0.41184(14) 0.2729(3) 0.0257(12) Uiso 1 1 d . . . F5 F 1.6346(3) 0.51081(14) 0.3074(3) 0.0291(13) Uiso 1 1 d . . . F6 F 1.6724(3) 0.45570(14) 0.2264(3) 0.0267(12) Uiso 1 1 d . . . O100 O 0.9136(5) 0.5972(2) 0.2377(4) 0.059(2) Uiso 1 1 d . . . C102 C 0.9676(7) 0.5746(3) 0.1806(6) 0.056(3) Uiso 1 1 d . . . H10D H 0.9398 0.5797 0.1262 0.068 Uiso 1 1 calc R . . H10E H 0.9719 0.5424 0.1908 0.068 Uiso 1 1 calc R . . C101 C 0.8160(8) 0.5803(4) 0.2289(7) 0.077(4) Uiso 1 1 d . . . H10F H 0.8144 0.5477 0.2341 0.093 Uiso 1 1 calc R . . H10G H 0.7829 0.5890 0.1779 0.093 Uiso 1 1 calc R . . C103 C 1.0629(7) 0.5969(3) 0.1959(6) 0.060(3) Uiso 1 1 d . . . H10H H 1.1089 0.5828 0.1641 0.090 Uiso 1 1 calc R . . H10I H 1.0849 0.5941 0.2515 0.090 Uiso 1 1 calc R . . H10J H 1.0568 0.6283 0.1820 0.090 Uiso 1 1 calc R . . C100 C 0.7710(7) 0.6038(3) 0.2993(6) 0.064(3) Uiso 1 1 d . . . H10K H 0.7042 0.5949 0.2997 0.096 Uiso 1 1 calc R . . H10L H 0.7748 0.6360 0.2931 0.096 Uiso 1 1 calc R . . H10M H 0.8059 0.5950 0.3489 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0037(4) 0.0117(4) 0.0098(3) 0.0021(3) -0.0025(3) -0.0010(3) Mn1 0.0065(7) 0.0111(7) 0.0099(6) 0.0009(5) 0.0005(5) -0.0010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C16 1.959(8) . ? Mo1 C17 2.010(8) . ? Mo1 C18 2.080(7) . ? Mo1 C31 2.129(7) . ? Mo1 N2 2.190(6) . ? Mo1 N4 2.217(6) . ? Mo1 N6 2.235(6) . ? N1 C2 1.357(8) . ? N1 N2 1.387(7) . ? N1 B1 1.532(10) . ? N2 C4 1.364(9) . ? C1 C2 1.491(9) . ? C2 C3 1.388(9) . ? C3 C4 1.370(10) . ? C4 C5 1.497(10) . ? N3 C7 1.349(8) . ? N3 N4 1.405(8) . ? N3 B1 1.518(10) . ? N4 C9 1.359(8) . ? C6 C7 1.518(10) . ? C7 C8 1.358(10) . ? C8 C9 1.404(9) . ? C9 C10 1.489(9) . ? N5 C12 1.343(9) . ? N5 N6 1.384(8) . ? N5 B1 1.507(10) . ? N6 C14 1.366(8) . ? C11 C12 1.508(10) . ? C12 C13 1.364(10) . ? C13 C14 1.365(10) . ? C14 C15 1.505(10) . ? C16 O1 1.161(8) . ? C17 C18 1.310(9) . ? C17 C25 1.456(9) . ? C18 C19 1.480(9) . ? C19 C24 1.376(9) . ? C19 C20 1.400(10) . ? C20 C21 1.392(10) . ? C21 C22 1.392(10) . ? C22 C23 1.399(11) . ? C23 C24 1.392(10) . ? C25 C26 1.399(9) . ? C25 C30 1.404(10) . ? C26 C27 1.383(10) . ? C27 C28 1.358(10) . ? C28 C29 1.403(10) . ? C29 C30 1.390(10) . ? C31 N7 1.160(8) . ? N7 Mn1 1.972(6) . ? Mn1 C33 1.813(8) . ? Mn1 C32 1.820(7) . ? Mn1 P1 2.209(2) . ? Mn1 P2 2.271(2) . ? Mn1 P3 2.301(2) . ? C32 O2 1.144(8) . ? C33 O3 1.156(8) . ? P1 O6 1.582(5) . ? P1 O5 1.601(5) . ? P1 O4 1.610(5) . ? O4 C34 1.445(8) . ? C34 C34A 1.501(9) . ? O5 C35 1.460(8) . ? C35 C35A 1.510(10) . ? O6 C36 1.446(9) . ? C36 C36A 1.463(11) . ? P2 C37 1.825(7) . ? P2 C44 1.825(7) . ? P2 C38 1.844(7) . ? P2 P3 2.694(3) . ? C37 P3 1.836(7) . ? P3 C56 1.816(8) . ? P3 C50 1.824(7) . ? C38 C43 1.377(9) . ? C38 C39 1.381(9) . ? C39 C40 1.371(9) . ? C40 C41 1.356(10) . ? C41 C42 1.383(10) . ? C42 C43 1.389(9) . ? C44 C45 1.381(9) . ? C44 C49 1.400(10) . ? C45 C46 1.391(10) . ? C46 C47 1.376(10) . ? C47 C48 1.363(10) . ? C48 C49 1.394(10) . ? C50 C55 1.354(9) . ? C50 C51 1.407(9) . ? C51 C52 1.382(10) . ? C52 C53 1.366(11) . ? C53 C54 1.366(10) . ? C54 C55 1.397(10) . ? C56 C57 1.363(10) . ? C56 C61 1.390(10) . ? C57 C58 1.387(10) . ? C58 C59 1.373(10) . ? C59 C60 1.335(10) . ? C60 C61 1.393(10) . ? P4 F5 1.588(5) . ? P4 F3 1.596(5) . ? P4 F6 1.605(5) . ? P4 F2 1.606(5) . ? P4 F1 1.612(5) . ? P4 F4 1.622(5) . ? O100 C102 1.460(10) . ? O100 C101 1.465(11) . ? C102 C103 1.508(12) . ? C101 C100 1.578(13) . ? 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 C16 Mo1 C17 109.8(3) . . ? C16 Mo1 C18 74.3(3) . . ? C17 Mo1 C18 37.3(3) . . ? C16 Mo1 C31 91.9(3) . . ? C17 Mo1 C31 102.9(3) . . ? C18 Mo1 C31 93.1(3) . . ? C16 Mo1 N2 93.5(3) . . ? C17 Mo1 N2 89.6(3) . . ? C18 Mo1 N2 103.1(3) . . ? C31 Mo1 N2 163.8(3) . . ? C16 Mo1 N4 166.4(3) . . ? C17 Mo1 N4 83.9(3) . . ? C18 Mo1 N4 119.0(2) . . ? C31 Mo1 N4 84.7(2) . . ? N2 Mo1 N4 86.5(2) . . ? C16 Mo1 N6 85.7(3) . . ? C17 Mo1 N6 162.1(3) . . ? C18 Mo1 N6 159.9(2) . . ? C31 Mo1 N6 84.8(2) . . ? N2 Mo1 N6 80.4(2) . . ? N4 Mo1 N6 80.8(2) . . ? C2 N1 N2 108.5(6) . . ? C2 N1 B1 132.1(7) . . ? N2 N1 B1 118.9(6) . . ? C4 N2 N1 106.3(6) . . ? C4 N2 Mo1 132.9(5) . . ? N1 N2 Mo1 119.4(4) . . ? N1 C2 C3 108.9(7) . . ? N1 C2 C1 121.1(7) . . ? C3 C2 C1 130.0(7) . . ? C4 C3 C2 105.9(7) . . ? N2 C4 C3 110.5(7) . . ? N2 C4 C5 121.2(7) . . ? C3 C4 C5 128.3(7) . . ? C7 N3 N4 108.3(6) . . ? C7 N3 B1 132.6(7) . . ? N4 N3 B1 118.7(6) . . ? C9 N4 N3 106.3(6) . . ? C9 N4 Mo1 133.6(5) . . ? N3 N4 Mo1 120.0(4) . . ? N3 C7 C8 109.8(7) . . ? N3 C7 C6 121.0(7) . . ? C8 C7 C6 129.2(7) . . ? C7 C8 C9 106.4(7) . . ? N4 C9 C8 109.1(7) . . ? N4 C9 C10 124.4(6) . . ? C8 C9 C10 126.4(7) . . ? C12 N5 N6 108.3(6) . . ? C12 N5 B1 131.1(7) . . ? N6 N5 B1 120.5(6) . . ? C14 N6 N5 106.0(6) . . ? C14 N6 Mo1 135.2(5) . . ? N5 N6 Mo1 118.8(4) . . ? N5 C12 C13 109.6(7) . . ? N5 C12 C11 122.6(7) . . ? C13 C12 C11 127.8(8) . . ? C12 C13 C14 106.2(7) . . ? C13 C14 N6 109.9(7) . . ? C13 C14 C15 127.1(7) . . ? N6 C14 C15 123.0(7) . . ? N5 B1 N3 109.8(7) . . ? N5 B1 N1 110.9(6) . . ? N3 B1 N1 108.3(7) . . ? O1 C16 Mo1 178.8(7) . . ? C18 C17 C25 140.6(8) . . ? C18 C17 Mo1 74.3(5) . . ? C25 C17 Mo1 145.1(6) . . ? C17 C18 C19 145.1(7) . . ? C17 C18 Mo1 68.4(5) . . ? C19 C18 Mo1 146.5(5) . . ? C24 C19 C20 122.6(7) . . ? C24 C19 C18 120.4(7) . . ? C20 C19 C18 116.7(7) . . ? C21 C20 C19 117.1(8) . . ? C22 C21 C20 121.7(8) . . ? C21 C22 C23 119.5(9) . . ? C24 C23 C22 119.9(8) . . ? C19 C24 C23 119.2(8) . . ? C26 C25 C30 118.7(7) . . ? C26 C25 C17 120.5(7) . . ? C30 C25 C17 120.7(7) . . ? C27 C26 C25 119.8(8) . . ? C28 C27 C26 121.1(8) . . ? C27 C28 C29 121.1(8) . . ? C30 C29 C28 118.1(8) . . ? C29 C30 C25 121.1(8) . . ? N7 C31 Mo1 178.4(6) . . ? C31 N7 Mn1 179.1(6) . . ? C33 Mn1 C32 175.7(3) . . ? C33 Mn1 N7 92.4(3) . . ? C32 Mn1 N7 88.9(3) . . ? C33 Mn1 P1 90.1(2) . . ? C32 Mn1 P1 85.7(2) . . ? N7 Mn1 P1 94.30(18) . . ? C33 Mn1 P2 91.6(2) . . ? C32 Mn1 P2 88.1(2) . . ? N7 Mn1 P2 165.14(18) . . ? P1 Mn1 P2 99.98(9) . . ? C33 Mn1 P3 87.8(2) . . ? C32 Mn1 P3 96.2(2) . . ? N7 Mn1 P3 93.68(18) . . ? P1 Mn1 P3 171.83(9) . . ? P2 Mn1 P3 72.20(8) . . ? O2 C32 Mn1 176.4(7) . . ? O3 C33 Mn1 179.2(7) . . ? O6 P1 O5 99.6(3) . . ? O6 P1 O4 106.7(3) . . ? O5 P1 O4 103.4(3) . . ? O6 P1 Mn1 112.9(2) . . ? O5 P1 Mn1 120.1(2) . . ? O4 P1 Mn1 112.5(2) . . ? C34 O4 P1 124.3(5) . . ? O4 C34 C34A 111.1(6) . . ? C35 O5 P1 123.7(4) . . ? O5 C35 C35A 107.8(6) . . ? C36 O6 P1 125.6(5) . . ? O6 C36 C36A 111.1(7) . . ? C37 P2 C44 104.2(3) . . ? C37 P2 C38 106.9(3) . . ? C44 P2 C38 102.2(3) . . ? C37 P2 Mn1 95.8(2) . . ? C44 P2 Mn1 126.9(3) . . ? C38 P2 Mn1 118.2(3) . . ? C44 P2 P3 135.8(3) . . ? C38 P2 P3 114.2(2) . . ? Mn1 P2 P3 54.42(7) . . ? P2 C37 P3 94.8(3) . . ? C56 P3 C50 101.3(3) . . ? C56 P3 C37 107.0(3) . . ? C50 P3 C37 108.0(3) . . ? C56 P3 Mn1 121.9(3) . . ? C50 P3 Mn1 122.6(3) . . ? C37 P3 Mn1 94.4(2) . . ? C56 P3 P2 134.8(3) . . ? C50 P3 P2 118.3(2) . . ? Mn1 P3 P2 53.38(7) . . ? C43 C38 C39 120.1(7) . . ? C43 C38 P2 117.5(6) . . ? C39 C38 P2 122.3(6) . . ? C40 C39 C38 120.4(8) . . ? C41 C40 C39 119.1(8) . . ? C40 C41 C42 122.3(8) . . ? C41 C42 C43 118.2(8) . . ? C38 C43 C42 119.9(7) . . ? C45 C44 C49 119.8(7) . . ? C45 C44 P2 121.2(6) . . ? C49 C44 P2 119.0(6) . . ? C44 C45 C46 119.9(8) . . ? C47 C46 C45 119.5(8) . . ? C48 C47 C46 121.5(8) . . ? C47 C48 C49 119.6(8) . . ? C48 C49 C44 119.5(8) . . ? C55 C50 C51 118.9(7) . . ? C55 C50 P3 120.6(6) . . ? C51 C50 P3 120.4(6) . . ? C52 C51 C50 118.8(8) . . ? C53 C52 C51 121.1(9) . . ? C52 C53 C54 120.7(9) . . ? C53 C54 C55 118.4(9) . . ? C50 C55 C54 122.1(8) . . ? C57 C56 C61 118.1(8) . . ? C57 C56 P3 120.0(6) . . ? C61 C56 P3 121.6(6) . . ? C56 C57 C58 119.8(8) . . ? C59 C58 C57 121.1(9) . . ? C60 C59 C58 119.9(9) . . ? C59 C60 C61 119.6(9) . . ? C56 C61 C60 121.3(8) . . ? F5 P4 F3 90.8(2) . . ? F5 P4 F6 90.1(2) . . ? F3 P4 F6 90.1(2) . . ? F5 P4 F2 90.2(3) . . ? F3 P4 F2 90.6(2) . . ? F6 P4 F2 179.2(3) . . ? F5 P4 F1 91.2(2) . . ? F3 P4 F1 178.0(3) . . ? F6 P4 F1 89.5(2) . . ? F2 P4 F1 89.8(3) . . ? F5 P4 F4 179.2(3) . . ? F3 P4 F4 89.9(2) . . ? F6 P4 F4 89.5(2) . . ? F2 P4 F4 90.3(2) . . ? F1 P4 F4 88.1(2) . . ? C102 O100 C101 108.1(8) . . ? O100 C102 C103 100.6(8) . . ? O100 C101 C100 101.7(9) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.983 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.130 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 138.2 48.5 2 0.042 0.218 0.905 7.3 0.5 3 0.069 0.955 0.940 7.2 0.2 4 0.500 0.500 1.000 138.2 48.3 5 0.430 0.455 0.560 7.2 0.7 6 0.458 0.718 0.595 7.3 1.0 7 0.542 0.282 0.405 7.3 0.7 8 0.569 0.545 0.440 7.2 0.3 9 0.930 0.045 0.060 7.2 0.7 10 0.958 0.782 0.095 7.4 1.0 _platon_squeeze_details ; ; #===END data_21[BF4]2.0.65DCM _database_code_depnum_ccdc_archive 'CCDC 702896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64.66 H70.31 B3 Cl1.31 F8 Mn Mo N7 O6 P3' _chemical_formula_weight 1516.11 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 23.922(5) _cell_length_b 12.909(3) _cell_length_c 24.742(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.82(3) _cell_angle_gamma 90.00 _cell_volume 6989(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 610 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 14.99 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3106 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 48601 _diffrn_reflns_av_R_equivalents 0.2350 _diffrn_reflns_av_sigmaI/netI 0.5357 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16012 _reflns_number_gt 3988 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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. The ethyl group containing the carbon atoms C36 and C36A apparently has some disorder in the orientation of the ethyl groups; however, the data were not of sufficiently good quality to model these. ; _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^)+(0.0279P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16012 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2821 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2044 _refine_ls_wR_factor_gt 0.1593 _refine_ls_goodness_of_fit_ref 0.765 _refine_ls_restrained_S_all 0.765 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.25638(4) 0.65785(7) 0.61955(4) 0.0189(2) Uani 1 1 d . . . N1 N 0.1561(3) 0.6137(6) 0.6654(4) 0.020(2) Uiso 1 1 d . . . N2 N 0.2156(3) 0.6019(5) 0.6783(4) 0.018(2) Uiso 1 1 d . . . C1 C 0.0728(5) 0.5594(8) 0.6953(5) 0.051(4) Uiso 1 1 d . . . H1A H 0.0567 0.6302 0.6879 0.077 Uiso 1 1 calc R . . H1B H 0.0716 0.5336 0.7321 0.077 Uiso 1 1 calc R . . H1C H 0.0478 0.5146 0.6625 0.077 Uiso 1 1 calc R . . C2 C 0.1367(5) 0.5590(7) 0.7006(5) 0.024(3) Uiso 1 1 d . . . C3 C 0.1873(5) 0.5089(8) 0.7398(5) 0.032(3) Uiso 1 1 d . . . H3A H 0.1889 0.4656 0.7715 0.039 Uiso 1 1 calc R . . C4 C 0.2354(5) 0.5329(8) 0.7247(5) 0.029(3) Uiso 1 1 d . . . C5 C 0.3020(4) 0.4997(7) 0.7550(5) 0.030(3) Uiso 1 1 d . . . H5A H 0.3285 0.5588 0.7572 0.045 Uiso 1 1 calc R . . H5B H 0.3100 0.4437 0.7324 0.045 Uiso 1 1 calc R . . H5C H 0.3102 0.4753 0.7950 0.045 Uiso 1 1 calc R . . N3 N 0.1136(3) 0.6463(6) 0.5557(4) 0.019(2) Uiso 1 1 d . . . N4 N 0.1664(3) 0.6261(5) 0.5465(4) 0.0144(19) Uiso 1 1 d . . . C6 C 0.0011(4) 0.6430(8) 0.4987(5) 0.032(3) Uiso 1 1 d . . . H6A H -0.0027 0.7112 0.5143 0.048 Uiso 1 1 calc R . . H6B H -0.0099 0.5891 0.5206 0.048 Uiso 1 1 calc R . . H6C H -0.0264 0.6391 0.4568 0.048 Uiso 1 1 calc R . . C7 C 0.0645(4) 0.6272(7) 0.5055(5) 0.024(3) Uiso 1 1 d . . . C8 C 0.0845(5) 0.5919(7) 0.4639(5) 0.029(3) Uiso 1 1 d . . . H8A H 0.0599 0.5700 0.4248 0.035 Uiso 1 1 calc R . . C9 C 0.1460(4) 0.5949(7) 0.4900(5) 0.021(3) Uiso 1 1 d . . . C10 C 0.1894(4) 0.5631(7) 0.4631(4) 0.023(3) Uiso 1 1 d . . . H10A H 0.2313 0.5638 0.4934 0.034 Uiso 1 1 calc R . . H10B H 0.1861 0.6116 0.4315 0.034 Uiso 1 1 calc R . . H10C H 0.1791 0.4931 0.4467 0.034 Uiso 1 1 calc R . . N5 N 0.1524(3) 0.7950(6) 0.6251(4) 0.020(2) Uiso 1 1 d . . . N6 N 0.2082(3) 0.8025(5) 0.6263(4) 0.018(2) Uiso 1 1 d . . . C11 C 0.0691(5) 0.9084(8) 0.6307(6) 0.052(4) Uiso 1 1 d . . . H11A H 0.0644 0.8682 0.6622 0.078 Uiso 1 1 calc R . . H11B H 0.0379 0.8871 0.5923 0.078 Uiso 1 1 calc R . . H11C H 0.0644 0.9823 0.6368 0.078 Uiso 1 1 calc R . . C12 C 0.1298(5) 0.8900(8) 0.6316(5) 0.028(3) Uiso 1 1 d . . . C13 C 0.1786(4) 0.9578(8) 0.6402(5) 0.027(3) Uiso 1 1 d . . . H13A H 0.1777 1.0301 0.6468 0.033 Uiso 1 1 calc R . . C14 C 0.2277(4) 0.9063(7) 0.6379(5) 0.019(2) Uiso 1 1 d . . . C15 C 0.2859(4) 0.9435(7) 0.6439(5) 0.029(3) Uiso 1 1 d . . . H15A H 0.2808 1.0085 0.6219 0.044 Uiso 1 1 calc R . . H15B H 0.3054 0.8919 0.6281 0.044 Uiso 1 1 calc R . . H15C H 0.3115 0.9556 0.6857 0.044 Uiso 1 1 calc R . . B1 B 0.1160(5) 0.6909(8) 0.6139(5) 0.020(3) Uiso 1 1 d . . . H1 H 0.0742 0.7010 0.6131 0.025 Uiso 1 1 calc R . . C16 C 0.3278(4) 0.7154(7) 0.6845(5) 0.022(3) Uiso 1 1 d . . . O1 O 0.3687(3) 0.7483(5) 0.7244(3) 0.036(2) Uiso 1 1 d . . . C17 C 0.2756(4) 0.5095(7) 0.6050(4) 0.015(2) Uiso 1 1 d . . . C18 C 0.3260(4) 0.5577(7) 0.6309(4) 0.017(2) Uiso 1 1 d . . . C19 C 0.3909(5) 0.5373(8) 0.6529(5) 0.026(3) Uiso 1 1 d . . . C20 C 0.4113(4) 0.4340(7) 0.6585(5) 0.026(3) Uiso 1 1 d . . . H20A H 0.3823 0.3794 0.6484 0.031 Uiso 1 1 calc R . . C21 C 0.4727(5) 0.4102(8) 0.6785(5) 0.035(3) Uiso 1 1 d . . . H21A H 0.4856 0.3400 0.6841 0.041 Uiso 1 1 calc R . . C22 C 0.5150(6) 0.4878(9) 0.6901(6) 0.053(4) Uiso 1 1 d . . . H22A H 0.5571 0.4711 0.7035 0.064 Uiso 1 1 calc R . . C23 C 0.4970(5) 0.5887(8) 0.6826(5) 0.038(3) Uiso 1 1 d . . . H23A H 0.5267 0.6420 0.6907 0.046 Uiso 1 1 calc R . . C24 C 0.4361(4) 0.6140(8) 0.6633(5) 0.029(3) Uiso 1 1 d . . . H24A H 0.4243 0.6847 0.6568 0.035 Uiso 1 1 calc R . . C25 C 0.2458(3) 0.4132(4) 0.5775(3) 0.017(2) Uiso 1 1 d G . . C26 C 0.1931(3) 0.3793(4) 0.5828(3) 0.021(3) Uiso 1 1 d G . . H26A H 0.1745 0.4212 0.6025 0.025 Uiso 1 1 calc R . . C27 C 0.1676(2) 0.2842(5) 0.5593(3) 0.038(3) Uiso 1 1 d G . . H27A H 0.1316 0.2610 0.5629 0.045 Uiso 1 1 calc R . . C28 C 0.1948(3) 0.2229(4) 0.5305(3) 0.045(3) Uiso 1 1 d G . . H28A H 0.1774 0.1578 0.5144 0.055 Uiso 1 1 calc R . . C29 C 0.2475(3) 0.2567(5) 0.5252(3) 0.045(4) Uiso 1 1 d G . . H29A H 0.2661 0.2149 0.5055 0.054 Uiso 1 1 calc R . . C30 C 0.2730(2) 0.3519(5) 0.5487(3) 0.029(3) Uiso 1 1 d G . . H30A H 0.3090 0.3750 0.5450 0.034 Uiso 1 1 calc R . . C31 C 0.2740(4) 0.7385(7) 0.5519(5) 0.019(3) Uiso 1 1 d . . . N7 N 0.2795(3) 0.7740(5) 0.5113(4) 0.015(2) Uiso 1 1 d . . . Mn1 Mn 0.29027(7) 0.84232(12) 0.44611(7) 0.0230(4) Uani 1 1 d . . . C32 C 0.2922(5) 0.9666(8) 0.4833(5) 0.029(3) Uiso 1 1 d . . . O2 O 0.2878(3) 1.0367(5) 0.5088(3) 0.034(2) Uiso 1 1 d . . . C33 C 0.2809(4) 0.7168(7) 0.4066(5) 0.021(3) Uiso 1 1 d . . . O3 O 0.2738(3) 0.6417(5) 0.3809(3) 0.0281(18) Uiso 1 1 d . . . P1 P 0.18823(13) 0.8763(2) 0.39194(14) 0.0273(8) Uiso 1 1 d . . . O4 O 0.1544(3) 0.7707(5) 0.3654(3) 0.038(2) Uiso 1 1 d . . . O5 O 0.1511(3) 0.9277(5) 0.4246(3) 0.0316(19) Uiso 1 1 d . . . O6 O 0.1797(3) 0.9556(5) 0.3405(3) 0.038(2) Uiso 1 1 d . . . C34 C 0.0901(5) 0.7560(8) 0.3362(6) 0.050(4) Uiso 1 1 d . . . H34A H 0.0722 0.8074 0.3040 0.060 Uiso 1 1 calc R . . H34B H 0.0707 0.7646 0.3644 0.060 Uiso 1 1 calc R . . C34A C 0.0795(5) 0.6448(9) 0.3105(5) 0.054(4) Uiso 1 1 d . . . H34C H 0.0357 0.6291 0.2940 0.082 Uiso 1 1 calc R . . H34D H 0.1013 0.5952 0.3421 0.082 Uiso 1 1 calc R . . H34E H 0.0948 0.6396 0.2794 0.082 Uiso 1 1 calc R . . C35 C 0.1403(5) 0.8860(8) 0.4729(5) 0.042(3) Uiso 1 1 d D . . H35A H 0.1730 0.9088 0.5106 0.050 Uiso 1 1 calc R . . H35B H 0.1408 0.8094 0.4715 0.050 Uiso 1 1 calc R . . C35A C 0.0795(4) 0.9228(8) 0.4691(5) 0.043(3) Uiso 1 1 d D . . H35C H 0.0734 0.8989 0.5040 0.064 Uiso 1 1 calc R . . H35D H 0.0471 0.8948 0.4334 0.064 Uiso 1 1 calc R . . H35E H 0.0783 0.9986 0.4677 0.064 Uiso 1 1 calc R . . C36 C 0.1142(8) 1.0044(14) 0.3001(9) 0.133(8) Uiso 1 1 d . . . H36A H 0.0995 0.9826 0.2583 0.159 Uiso 1 1 calc R . . H36E H 0.0828 0.9895 0.3156 0.159 Uiso 1 1 calc R . . C36A C 0.1316(12) 1.097(2) 0.3077(13) 0.308(18) Uiso 1 1 d . . . H36B H 0.1033 1.1393 0.2754 0.461 Uiso 1 1 calc R . . H36C H 0.1727 1.1016 0.3083 0.461 Uiso 1 1 calc R . . H36D H 0.1324 1.1217 0.3454 0.461 Uiso 1 1 calc R . . P2 P 0.32913(13) 0.9208(2) 0.38289(14) 0.0230(7) Uiso 1 1 d . . . C37 C 0.4074(4) 0.9073(7) 0.4337(4) 0.019(2) Uiso 1 1 d . . . H37A H 0.4253 0.9738 0.4530 0.023 Uiso 1 1 calc R . . H37B H 0.4331 0.8772 0.4148 0.023 Uiso 1 1 calc R . . P3 P 0.39519(12) 0.81537(19) 0.48571(13) 0.0184(7) Uiso 1 1 d . . . C38 C 0.3143(5) 1.0572(8) 0.3645(5) 0.028(3) Uiso 1 1 d . . . C39 C 0.2811(4) 1.0895(8) 0.3051(5) 0.026(3) Uiso 1 1 d . . . H39A H 0.2692 1.0404 0.2738 0.032 Uiso 1 1 calc R . . C40 C 0.2661(4) 1.1946(7) 0.2931(5) 0.031(3) Uiso 1 1 d . . . H40A H 0.2426 1.2180 0.2540 0.037 Uiso 1 1 calc R . . C41 C 0.2870(5) 1.2639(8) 0.3408(5) 0.037(3) Uiso 1 1 d . . . H41A H 0.2773 1.3352 0.3328 0.045 Uiso 1 1 calc R . . C42 C 0.3197(5) 1.2362(8) 0.3967(5) 0.035(3) Uiso 1 1 d . . . H42A H 0.3336 1.2870 0.4270 0.042 Uiso 1 1 calc R . . C43 C 0.3334(4) 1.1309(7) 0.4102(5) 0.033(3) Uiso 1 1 d . . . H43A H 0.3554 1.1097 0.4500 0.040 Uiso 1 1 calc R . . C44 C 0.3207(3) 0.8598(4) 0.3138(2) 0.018(2) Uiso 1 1 d G . . C45 C 0.3687(2) 0.8624(4) 0.2957(3) 0.022(3) Uiso 1 1 d G . . H45A H 0.4071 0.8905 0.3211 0.027 Uiso 1 1 calc R . . C46 C 0.3605(2) 0.8240(4) 0.2406(3) 0.023(3) Uiso 1 1 d G . . H46A H 0.3933 0.8258 0.2282 0.028 Uiso 1 1 calc R . . C47 C 0.3044(3) 0.7829(5) 0.2035(2) 0.028(3) Uiso 1 1 d G . . H47A H 0.2988 0.7566 0.1658 0.033 Uiso 1 1 calc R . . C48 C 0.2564(2) 0.7802(5) 0.2215(3) 0.031(3) Uiso 1 1 d G . . H48A H 0.2180 0.7521 0.1961 0.037 Uiso 1 1 calc R . . C49 C 0.2646(2) 0.8187(5) 0.2767(3) 0.028(3) Uiso 1 1 d G . . H49A H 0.2318 0.8168 0.2890 0.033 Uiso 1 1 calc R . . C50 C 0.4460(4) 0.8465(8) 0.5616(4) 0.022(2) Uiso 1 1 d . . . C51 C 0.4258(5) 0.8955(7) 0.5998(5) 0.027(3) Uiso 1 1 d . . . H51A H 0.3838 0.9133 0.5862 0.033 Uiso 1 1 calc R . . C52 C 0.4643(5) 0.9194(8) 0.6573(5) 0.034(3) Uiso 1 1 d . . . H52A H 0.4493 0.9524 0.6831 0.041 Uiso 1 1 calc R . . C53 C 0.5255(4) 0.8940(7) 0.6762(5) 0.027(3) Uiso 1 1 d . . . H53A H 0.5526 0.9098 0.7156 0.033 Uiso 1 1 calc R . . C54 C 0.5477(4) 0.8476(8) 0.6405(5) 0.028(3) Uiso 1 1 d . . . H54A H 0.5900 0.8321 0.6549 0.034 Uiso 1 1 calc R . . C55 C 0.5087(4) 0.8214(7) 0.5817(5) 0.025(3) Uiso 1 1 d . . . H55A H 0.5243 0.7879 0.5565 0.030 Uiso 1 1 calc R . . C56 C 0.4144(4) 0.6835(6) 0.4752(4) 0.013(2) Uiso 1 1 d . . . C57 C 0.4289(4) 0.6501(8) 0.4289(5) 0.028(3) Uiso 1 1 d . . . H57A H 0.4359 0.6984 0.4034 0.034 Uiso 1 1 calc R . . C58 C 0.4329(5) 0.5423(8) 0.4210(6) 0.043(3) Uiso 1 1 d . . . H58A H 0.4415 0.5174 0.3890 0.052 Uiso 1 1 calc R . . C59 C 0.4244(4) 0.4731(8) 0.4595(5) 0.033(3) Uiso 1 1 d . . . H59A H 0.4284 0.4011 0.4538 0.040 Uiso 1 1 calc R . . C60 C 0.4103(4) 0.5040(8) 0.5063(5) 0.031(3) Uiso 1 1 d . . . H60A H 0.4058 0.4552 0.5330 0.037 Uiso 1 1 calc R . . C61 C 0.4028(4) 0.6112(7) 0.5123(5) 0.022(3) Uiso 1 1 d . . . H61A H 0.3899 0.6351 0.5417 0.026 Uiso 1 1 calc R . . B2 B 0.5680(5) 0.8239(8) 0.4209(5) 0.016(3) Uiso 1 1 d . . . F1 F 0.5656(3) 0.9058(5) 0.4591(3) 0.058(2) Uiso 1 1 d . . . F2 F 0.5897(3) 0.7352(5) 0.4547(3) 0.062(2) Uiso 1 1 d . . . F3 F 0.5093(3) 0.8086(4) 0.3801(3) 0.0506(19) Uiso 1 1 d . . . F4 F 0.6051(3) 0.8512(5) 0.3951(3) 0.064(2) Uiso 1 1 d . . . B3 B 0.0716(6) 0.2216(10) 0.6638(6) 0.029(3) Uiso 1 1 d . . . F5 F 0.1244(4) 0.2257(6) 0.7151(4) 0.109(3) Uiso 1 1 d . . . F6 F 0.0419(3) 0.3073(6) 0.6505(4) 0.087(3) Uiso 1 1 d . . . F7 F 0.0821(3) 0.1751(6) 0.6204(4) 0.087(3) Uiso 1 1 d . . . F8 F 0.0333(3) 0.1469(5) 0.6788(3) 0.062(2) Uiso 1 1 d . . . Cl2 Cl 0.0631(3) 1.2233(5) 0.3889(3) 0.084(3) Uiso 0.655(7) 1 d P . . Cl1 Cl 0.1395(3) 1.3423(7) 0.3476(4) 0.139(4) Uiso 0.655(7) 1 d P . . C100 C 0.0940(9) 1.3430(17) 0.3837(10) 0.088(8) Uiso 0.655(7) 1 d P . . H10D H 0.0600 1.3920 0.3637 0.106 Uiso 0.655(7) 1 calc PR . . H10E H 0.1174 1.3696 0.4241 0.106 Uiso 0.655(7) 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0257(5) 0.0081(4) 0.0213(6) -0.0020(5) 0.0077(4) -0.0012(5) Mn1 0.0309(10) 0.0112(8) 0.0255(11) 0.0035(8) 0.0100(9) 0.0005(8) _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 C16 1.958(11) . ? Mo1 C17 2.035(9) . ? Mo1 C18 2.036(9) . ? Mo1 C31 2.152(10) . ? Mo1 N2 2.175(8) . ? Mo1 N4 2.219(8) . ? Mo1 N6 2.236(7) . ? N1 N2 1.335(9) . ? N1 C2 1.340(11) . ? N1 B1 1.597(13) . ? N2 C4 1.377(12) . ? C1 C2 1.481(12) . ? C2 C3 1.369(13) . ? C3 C4 1.382(13) . ? C4 C5 1.522(13) . ? N3 C7 1.342(12) . ? N3 N4 1.395(9) . ? N3 B1 1.532(13) . ? N4 C9 1.342(12) . ? C6 C7 1.473(11) . ? C7 C8 1.376(13) . ? C8 C9 1.348(12) . ? C9 C10 1.500(12) . ? N5 N6 1.328(9) . ? N5 C12 1.375(11) . ? N5 B1 1.563(12) . ? N6 C14 1.409(10) . ? C11 C12 1.462(12) . ? C12 C13 1.405(12) . ? C13 C14 1.369(12) . ? C14 C15 1.423(11) . ? C16 O1 1.155(11) . ? C17 C18 1.275(12) . ? C17 C25 1.458(10) . ? C18 C19 1.447(12) . ? C19 C20 1.408(12) . ? C19 C24 1.411(12) . ? C20 C21 1.381(12) . ? C21 C22 1.368(13) . ? C22 C23 1.361(14) . ? C23 C24 1.376(12) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 N7 1.159(11) . ? N7 Mn1 1.945(8) . ? Mn1 C32 1.841(11) . ? Mn1 C33 1.859(10) . ? Mn1 P1 2.303(3) . ? Mn1 P3 2.323(3) . ? Mn1 P2 2.348(3) . ? C32 O2 1.132(11) . ? C33 O3 1.134(10) . ? P1 O5 1.569(7) . ? P1 O6 1.581(8) . ? P1 O4 1.586(7) . ? O4 C34 1.423(11) . ? O5 C35 1.425(11) . ? O6 C36 1.607(18) . ? C34 C34A 1.549(14) . ? C35 C35A 1.497(10) . ? C36 C36A 1.25(3) . ? P2 C37 1.794(9) . ? P2 C38 1.817(10) . ? P2 C44 1.819(5) . ? C37 P3 1.858(9) . ? P3 C56 1.809(9) . ? P3 C50 1.822(10) . ? C38 C43 1.405(13) . ? C38 C39 1.423(14) . ? C39 C40 1.405(12) . ? C40 C41 1.402(14) . ? C41 C42 1.334(15) . ? C42 C43 1.406(13) . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? C50 C51 1.378(12) . ? C50 C55 1.415(11) . ? C51 C52 1.381(14) . ? C52 C53 1.385(12) . ? C53 C54 1.340(12) . ? C54 C55 1.416(13) . ? C56 C57 1.391(12) . ? C56 C61 1.413(12) . ? C57 C58 1.414(13) . ? C58 C59 1.379(14) . ? C59 C60 1.390(13) . ? C60 C61 1.411(12) . ? B2 F4 1.334(11) . ? B2 F3 1.374(12) . ? B2 F2 1.389(12) . ? B2 F1 1.433(12) . ? B3 F6 1.284(13) . ? B3 F7 1.337(14) . ? B3 F5 1.383(15) . ? B3 F8 1.478(13) . ? Cl2 C100 1.74(2) . ? Cl1 C100 1.665(19) . ? 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 C16 Mo1 C17 108.5(4) . . ? C16 Mo1 C18 74.5(4) . . ? C17 Mo1 C18 36.5(3) . . ? C16 Mo1 C31 94.3(4) . . ? C17 Mo1 C31 100.8(4) . . ? C18 Mo1 C31 90.5(4) . . ? C16 Mo1 N2 93.2(4) . . ? C17 Mo1 N2 90.0(3) . . ? C18 Mo1 N2 105.0(3) . . ? C31 Mo1 N2 164.1(3) . . ? C16 Mo1 N4 167.4(3) . . ? C17 Mo1 N4 84.1(3) . . ? C18 Mo1 N4 117.7(3) . . ? C31 Mo1 N4 83.5(3) . . ? N2 Mo1 N4 86.2(3) . . ? C16 Mo1 N6 85.8(3) . . ? C17 Mo1 N6 163.6(3) . . ? C18 Mo1 N6 159.6(3) . . ? C31 Mo1 N6 85.6(3) . . ? N2 Mo1 N6 81.0(3) . . ? N4 Mo1 N6 81.7(3) . . ? N2 N1 C2 113.6(8) . . ? N2 N1 B1 120.0(8) . . ? C2 N1 B1 126.3(8) . . ? N1 N2 C4 104.3(7) . . ? N1 N2 Mo1 121.7(6) . . ? C4 N2 Mo1 132.5(7) . . ? N1 C2 C3 105.7(9) . . ? N1 C2 C1 123.9(10) . . ? C3 C2 C1 130.4(10) . . ? C2 C3 C4 107.2(10) . . ? N2 C4 C3 109.1(9) . . ? N2 C4 C5 122.1(9) . . ? C3 C4 C5 128.6(10) . . ? C7 N3 N4 109.1(8) . . ? C7 N3 B1 128.7(8) . . ? N4 N3 B1 122.1(8) . . ? C9 N4 N3 104.6(7) . . ? C9 N4 Mo1 136.8(6) . . ? N3 N4 Mo1 118.5(6) . . ? N3 C7 C8 108.3(9) . . ? N3 C7 C6 123.8(9) . . ? C8 C7 C6 127.9(10) . . ? C9 C8 C7 105.8(10) . . ? N4 C9 C8 112.1(9) . . ? N4 C9 C10 121.3(9) . . ? C8 C9 C10 126.6(10) . . ? N6 N5 C12 111.8(8) . . ? N6 N5 B1 123.3(8) . . ? C12 N5 B1 124.8(8) . . ? N5 N6 C14 108.7(7) . . ? N5 N6 Mo1 118.8(6) . . ? C14 N6 Mo1 132.2(6) . . ? N5 C12 C13 103.4(8) . . ? N5 C12 C11 125.3(9) . . ? C13 C12 C11 131.3(10) . . ? C14 C13 C12 111.4(9) . . ? C13 C14 N6 104.6(8) . . ? C13 C14 C15 130.6(9) . . ? N6 C14 C15 124.8(9) . . ? N3 B1 N5 107.2(8) . . ? N3 B1 N1 107.3(8) . . ? N5 B1 N1 106.5(8) . . ? O1 C16 Mo1 177.1(9) . . ? C18 C17 C25 146.7(9) . . ? C18 C17 Mo1 71.8(6) . . ? C25 C17 Mo1 141.5(6) . . ? C17 C18 C19 138.8(9) . . ? C17 C18 Mo1 71.7(6) . . ? C19 C18 Mo1 149.5(7) . . ? C20 C19 C24 115.9(9) . . ? C20 C19 C18 119.1(9) . . ? C24 C19 C18 124.6(9) . . ? C21 C20 C19 121.5(9) . . ? C22 C21 C20 120.1(11) . . ? C23 C22 C21 120.3(12) . . ? C22 C23 C24 120.5(11) . . ? C23 C24 C19 121.5(10) . . ? C26 C25 C30 120.0 . . ? C26 C25 C17 121.0(5) . . ? C30 C25 C17 118.9(5) . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? N7 C31 Mo1 172.6(8) . . ? C31 N7 Mn1 176.1(8) . . ? C32 Mn1 C33 175.0(4) . . ? C32 Mn1 N7 88.1(4) . . ? C33 Mn1 N7 90.7(4) . . ? C32 Mn1 P1 86.1(3) . . ? C33 Mn1 P1 89.2(3) . . ? N7 Mn1 P1 96.0(2) . . ? C32 Mn1 P3 96.6(3) . . ? C33 Mn1 P3 88.4(3) . . ? N7 Mn1 P3 93.7(2) . . ? P1 Mn1 P3 169.99(13) . . ? C32 Mn1 P2 91.1(3) . . ? C33 Mn1 P2 91.3(3) . . ? N7 Mn1 P2 165.7(2) . . ? P1 Mn1 P2 98.16(12) . . ? P3 Mn1 P2 72.21(11) . . ? O2 C32 Mn1 170.3(9) . . ? O3 C33 Mn1 177.7(10) . . ? O5 P1 O6 102.9(4) . . ? O5 P1 O4 106.1(4) . . ? O6 P1 O4 110.2(4) . . ? O5 P1 Mn1 117.9(3) . . ? O6 P1 Mn1 110.7(3) . . ? O4 P1 Mn1 108.7(3) . . ? C34 O4 P1 126.2(6) . . ? C35 O5 P1 127.1(6) . . ? P1 O6 C36 122.1(8) . . ? O4 C34 C34A 107.2(8) . . ? O5 C35 C35A 109.2(9) . . ? C36A C36 O6 95.6(19) . . ? C37 P2 C38 108.2(4) . . ? C37 P2 C44 107.8(4) . . ? C38 P2 C44 104.4(4) . . ? C37 P2 Mn1 94.2(3) . . ? C38 P2 Mn1 119.6(3) . . ? C44 P2 Mn1 121.1(2) . . ? P2 C37 P3 97.8(4) . . ? C56 P3 C50 104.7(4) . . ? C56 P3 C37 112.4(4) . . ? C50 P3 C37 110.2(4) . . ? C56 P3 Mn1 112.0(3) . . ? C50 P3 Mn1 124.0(3) . . ? C37 P3 Mn1 93.3(3) . . ? C43 C38 C39 119.9(10) . . ? C43 C38 P2 119.2(9) . . ? C39 C38 P2 120.8(8) . . ? C40 C39 C38 119.3(10) . . ? C41 C40 C39 117.7(11) . . ? C42 C41 C40 124.2(11) . . ? C41 C42 C43 119.3(12) . . ? C38 C43 C42 119.6(11) . . ? C45 C44 C49 120.0 . . ? C45 C44 P2 119.9(4) . . ? C49 C44 P2 119.8(4) . . ? C44 C45 C46 120.0 . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? C51 C50 C55 118.7(10) . . ? C51 C50 P3 122.4(8) . . ? C55 C50 P3 118.9(8) . . ? C50 C51 C52 122.4(10) . . ? C51 C52 C53 118.0(11) . . ? C54 C53 C52 121.9(11) . . ? C53 C54 C55 120.8(10) . . ? C50 C55 C54 118.1(9) . . ? C57 C56 C61 120.6(9) . . ? C57 C56 P3 124.9(8) . . ? C61 C56 P3 113.6(7) . . ? C56 C57 C58 118.2(10) . . ? C59 C58 C57 120.3(11) . . ? C58 C59 C60 122.9(11) . . ? C59 C60 C61 116.9(10) . . ? C60 C61 C56 120.9(9) . . ? F4 B2 F3 111.5(10) . . ? F4 B2 F2 110.3(9) . . ? F3 B2 F2 110.2(8) . . ? F4 B2 F1 109.4(8) . . ? F3 B2 F1 106.8(8) . . ? F2 B2 F1 108.5(9) . . ? F6 B3 F7 116.5(13) . . ? F6 B3 F5 114.1(12) . . ? F7 B3 F5 110.8(11) . . ? F6 B3 F8 106.9(10) . . ? F7 B3 F8 104.2(10) . . ? F5 B3 F8 102.9(10) . . ? Cl1 C100 Cl2 115.1(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.401 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.122