Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global # *** Added by check_cif _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bayly, Simon R.' 'Bell, Zoe R.' 'Courric, Stephane' 'de Chair, Helena' 'Gatteschi, Dante' 'Humphrey, Elizabeth R.' 'Jeffery, J.' 'McCleverty, J. A.' 'Paredes, Cecelia G.' 'Screttas, Constantinos G.' 'Steele, Barry' 'Totti, Federico' 'Ward, Mike' _publ_contact_author_name 'Dr Mike Ward' _publ_contact_author_address ; Dr Mike Ward School of Chemistry University of Bristol Cantock's Close Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email 'mike.ward@bristol.ac.uk' _publ_contact_author ; Dr. Mike Ward School of Chemistry Cantock's Close BRISTOL BS8 1TS ; _publ_contact_author_fax '0117 9287655' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'Electronic and magnetic metal-metal interactions...' by S. R. Bayly, et al, submitted to Dalton Transactions for publication. ; #======================================================== data_test1 _database_code_CSD 157071 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 B Cl Mo N7 O2' _chemical_formula_weight 550.69 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.060(5) _cell_length_b 11.916(5) _cell_length_c 11.985(6) _cell_angle_alpha 119.69(2) _cell_angle_beta 114.15(4) _cell_angle_gamma 90.46(4) _cell_volume 1206.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 562 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ? _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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12455 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_av_sigmaI/netI 0.1540 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5481 _reflns_number_gt 2609 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0728P)^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 5481 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1588 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.003 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 0.18682(6) -0.25817(6) -0.58446(6) 0.0455(2) Uani 1 1 d . . . O48 O 0.2481(4) -0.2168(4) -0.3880(4) 0.0390(10) Uani 1 1 d . A . N11 N 0.4707(5) -0.2522(5) -0.5907(5) 0.0378(12) Uani 1 1 d . . . N12 N 0.4088(5) -0.1832(5) -0.5074(5) 0.0365(12) Uani 1 1 d . A . N21 N 0.2623(5) -0.3653(5) -0.8352(5) 0.0384(12) Uani 1 1 d . . . N22 N 0.1617(5) -0.3208(5) -0.7982(5) 0.0359(12) Uani 1 1 d . A . N31 N 0.3347(5) -0.4826(5) -0.7025(5) 0.0380(12) Uani 1 1 d . . . N32 N 0.2527(5) -0.4456(5) -0.6351(5) 0.0376(12) Uani 1 1 d . A . N47 N 0.0535(5) -0.0179(5) 0.0151(6) 0.0455(13) Uani 1 1 d . . . C13 C 0.5052(6) -0.0723(6) -0.3876(6) 0.0360(14) Uani 1 1 d . . . C14 C 0.6253(6) -0.0698(6) -0.3946(7) 0.0417(15) Uani 1 1 d . A . H14A H 0.7076 -0.0032 -0.3255 0.050 Uiso 1 1 calc R . . C15 C 0.6011(6) -0.1849(6) -0.5239(7) 0.0365(14) Uani 1 1 d . A . C16 C 0.4791(6) 0.0298(6) -0.2690(6) 0.0435(16) Uani 1 1 d . A . H16A H 0.3854 0.0026 -0.2929 0.065 Uiso 1 1 calc R . . H16B H 0.4958 0.1146 -0.2586 0.065 Uiso 1 1 calc R . . H16C H 0.5395 0.0383 -0.1790 0.065 Uiso 1 1 calc R . . C17 C 0.6952(6) -0.2360(7) -0.5887(7) 0.0552(19) Uani 1 1 d . . . H17A H 0.6458 -0.3200 -0.6808 0.083 Uiso 1 1 calc R A . H17B H 0.7715 -0.2484 -0.5235 0.083 Uiso 1 1 calc R . . H17C H 0.7285 -0.1722 -0.6032 0.083 Uiso 1 1 calc R . . C23 C 0.0693(6) -0.3125(6) -0.9051(6) 0.0389(15) Uani 1 1 d . . . C24 C 0.1079(7) -0.3513(6) -1.0118(7) 0.0497(17) Uani 1 1 d . A . H24A H 0.0609 -0.3547 -1.0984 0.060 Uiso 1 1 calc R . . C25 C 0.2284(7) -0.3837(6) -0.9652(7) 0.0442(16) Uani 1 1 d . A . C26 C -0.0609(6) -0.2721(6) -0.9083(7) 0.0499(17) Uani 1 1 d . A . H26A H -0.0619 -0.2494 -0.8200 0.075 Uiso 1 1 calc R . . H26B H -0.1393 -0.3453 -0.9906 0.075 Uiso 1 1 calc R . . H26C H -0.0640 -0.1959 -0.9165 0.075 Uiso 1 1 calc R . . C27 C 0.3194(8) -0.4314(7) -1.0391(7) 0.061(2) Uani 1 1 d . . . H27A H 0.3982 -0.4460 -0.9791 0.092 Uiso 1 1 calc R A . H27B H 0.3489 -0.3644 -1.0516 0.092 Uiso 1 1 calc R . . H27C H 0.2678 -0.5135 -1.1327 0.092 Uiso 1 1 calc R . . C33 C 0.2280(7) -0.5428(6) -0.6134(7) 0.0470(17) Uani 1 1 d . . . C34 C 0.2917(7) -0.6391(7) -0.6685(7) 0.0523(18) Uani 1 1 d . A . H34A H 0.2886 -0.7179 -0.6700 0.063 Uiso 1 1 calc R . . C35 C 0.3595(6) -0.5999(6) -0.7199(7) 0.0470(17) Uani 1 1 d . A . C36 C 0.1383(7) -0.5387(7) -0.5462(8) 0.058(2) Uani 1 1 d . A . H36A H 0.1103 -0.4570 -0.5177 0.086 Uiso 1 1 calc R . . H36B H 0.1887 -0.5426 -0.4617 0.086 Uiso 1 1 calc R . . H36C H 0.0585 -0.6139 -0.6159 0.086 Uiso 1 1 calc R . . C37 C 0.4471(7) -0.6678(7) -0.7891(9) 0.068(2) Uani 1 1 d . . . H37A H 0.4814 -0.6140 -0.8139 0.103 Uiso 1 1 calc R A . H37B H 0.3925 -0.7543 -0.8759 0.103 Uiso 1 1 calc R . . H37C H 0.5228 -0.6784 -0.7215 0.103 Uiso 1 1 calc R . . C41 C 0.1975(6) -0.1654(6) -0.2932(6) 0.0362(14) Uani 1 1 d . . . C42 C 0.0802(7) -0.1226(8) -0.3209(7) 0.065(2) Uani 1 1 d . A . H42A H 0.0346 -0.1250 -0.4071 0.078 Uiso 1 1 calc R . . C43 C 0.0282(7) -0.0760(7) -0.2239(7) 0.059(2) Uani 1 1 d . . . H43A H -0.0535 -0.0509 -0.2472 0.071 Uiso 1 1 calc R A . C44 C 0.0950(6) -0.0664(6) -0.0946(7) 0.0388(15) Uani 1 1 d . A . C45 C 0.2154(7) -0.1057(8) -0.0646(8) 0.068(2) Uani 1 1 d . . . H45A H 0.2634 -0.0989 0.0238 0.082 Uiso 1 1 calc R A . C46 C 0.2662(7) -0.1549(8) -0.1627(8) 0.065(2) Uani 1 1 d . A . H46A H 0.3474 -0.1809 -0.1400 0.078 Uiso 1 1 calc R . . B1 B 0.3857(8) -0.3884(8) -0.7355(8) 0.0426(19) Uani 1 1 d . A . H1 H 0.4424 -0.4268 -0.7826 0.051 Uiso 1 1 calc R . . Cl1 Cl 0.1400(7) -0.0625(7) -0.5346(8) 0.0448(15) Uani 0.457(9) 1 d P A 1 O1 O 0.0177(17) -0.362(2) -0.670(2) 0.045(4) Uani 0.457(9) 1 d P A 1 O1' O 0.1696(14) -0.0986(13) -0.5552(15) 0.038(3) Uani 0.543(9) 1 d P A 2 Cl1' Cl -0.0287(6) -0.3545(8) -0.6646(8) 0.0459(14) Uani 0.543(9) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0477(4) 0.0662(4) 0.0409(4) 0.0326(3) 0.0315(3) 0.0322(3) O48 0.044(2) 0.050(3) 0.041(3) 0.028(2) 0.031(2) 0.023(2) N11 0.044(3) 0.043(3) 0.042(3) 0.027(3) 0.027(3) 0.019(3) N12 0.038(3) 0.044(3) 0.033(3) 0.020(3) 0.022(3) 0.016(3) N21 0.048(3) 0.039(3) 0.035(3) 0.018(3) 0.028(3) 0.012(3) N22 0.035(3) 0.036(3) 0.037(3) 0.018(2) 0.019(3) 0.012(2) N31 0.045(3) 0.043(3) 0.045(3) 0.027(3) 0.033(3) 0.025(3) N32 0.039(3) 0.044(3) 0.041(3) 0.025(3) 0.025(3) 0.017(3) N47 0.049(3) 0.061(4) 0.045(3) 0.033(3) 0.031(3) 0.024(3) C13 0.038(4) 0.043(4) 0.031(4) 0.026(3) 0.013(3) 0.010(3) C14 0.036(3) 0.051(4) 0.042(4) 0.030(4) 0.016(3) 0.010(3) C15 0.032(3) 0.050(4) 0.043(4) 0.035(3) 0.019(3) 0.017(3) C16 0.038(4) 0.051(4) 0.035(4) 0.020(3) 0.015(3) 0.013(3) C17 0.043(4) 0.063(5) 0.066(5) 0.036(4) 0.032(4) 0.019(4) C23 0.050(4) 0.035(4) 0.035(4) 0.021(3) 0.020(3) 0.009(3) C24 0.063(5) 0.052(4) 0.038(4) 0.028(4) 0.024(4) 0.013(4) C25 0.061(4) 0.042(4) 0.037(4) 0.023(3) 0.028(4) 0.007(3) C26 0.054(4) 0.045(4) 0.043(4) 0.027(3) 0.014(4) 0.018(4) C27 0.087(6) 0.063(5) 0.052(5) 0.031(4) 0.049(4) 0.024(4) C33 0.062(4) 0.050(4) 0.057(4) 0.040(4) 0.037(4) 0.025(4) C34 0.067(5) 0.057(4) 0.072(5) 0.049(4) 0.047(4) 0.039(4) C35 0.053(4) 0.047(4) 0.061(5) 0.034(4) 0.039(4) 0.026(4) C36 0.076(5) 0.072(5) 0.084(6) 0.062(5) 0.062(5) 0.038(4) C37 0.082(5) 0.072(5) 0.106(6) 0.059(5) 0.075(5) 0.057(5) C41 0.037(3) 0.044(4) 0.038(4) 0.021(3) 0.027(3) 0.018(3) C42 0.071(5) 0.117(7) 0.041(4) 0.052(5) 0.040(4) 0.056(5) C43 0.052(4) 0.092(6) 0.051(5) 0.040(4) 0.038(4) 0.042(4) C44 0.048(4) 0.051(4) 0.040(4) 0.030(3) 0.033(3) 0.024(3) C45 0.058(4) 0.123(7) 0.046(4) 0.052(5) 0.035(4) 0.052(5) C46 0.060(5) 0.125(7) 0.061(5) 0.070(5) 0.046(4) 0.063(5) B1 0.053(5) 0.057(5) 0.048(5) 0.036(4) 0.040(4) 0.030(4) Cl1 0.053(3) 0.041(4) 0.049(3) 0.027(3) 0.029(2) 0.028(2) O1 0.028(10) 0.044(8) 0.053(8) 0.020(6) 0.018(7) 0.011(8) O1' 0.044(7) 0.029(7) 0.051(7) 0.024(6) 0.030(5) 0.020(5) Cl1' 0.042(4) 0.049(3) 0.054(2) 0.028(2) 0.029(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1' 1.782(13) . ? Mo1 O1 1.792(19) . ? Mo1 O48 1.945(4) . ? Mo1 N22 2.172(5) . ? Mo1 Cl1' 2.216(6) . ? Mo1 N32 2.221(5) . ? Mo1 Cl1 2.226(6) . ? Mo1 N12 2.230(5) . ? O48 C41 1.348(6) . ? N11 C15 1.328(7) . ? N11 N12 1.377(6) . ? N11 B1 1.543(9) . ? N12 C13 1.338(7) . ? N21 C25 1.341(7) . ? N21 N22 1.378(6) . ? N21 B1 1.537(8) . ? N22 C23 1.323(7) . ? N31 C35 1.355(7) . ? N31 N32 1.386(5) . ? N31 B1 1.532(8) . ? N32 C33 1.356(7) . ? N47 N47 1.234(9) 2 ? N47 C44 1.421(6) . ? C13 C14 1.366(8) . ? C13 C16 1.487(8) . ? C14 C15 1.380(8) . ? C15 C17 1.504(7) . ? C23 C24 1.377(8) . ? C23 C26 1.513(8) . ? C24 C25 1.361(8) . ? C25 C27 1.536(8) . ? C33 C34 1.376(8) . ? C33 C36 1.501(8) . ? C34 C35 1.348(8) . ? C35 C37 1.513(7) . ? C41 C46 1.367(8) . ? C41 C42 1.372(8) . ? C42 C43 1.379(8) . ? C43 C44 1.358(8) . ? C44 C45 1.381(8) . ? C45 C46 1.380(8) . ? 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 O1' Mo1 O1 107.4(7) . . ? O1' Mo1 O48 99.9(5) . . ? O1 Mo1 O48 98.3(7) . . ? O1' Mo1 N22 88.2(5) . . ? O1 Mo1 N22 89.5(7) . . ? O48 Mo1 N22 166.50(15) . . ? O1' Mo1 Cl1' 99.6(5) . . ? O1 Mo1 Cl1' 9.9(7) . . ? O48 Mo1 Cl1' 93.9(2) . . ? N22 Mo1 Cl1' 95.4(2) . . ? O1' Mo1 N32 164.0(4) . . ? O1 Mo1 N32 85.3(6) . . ? O48 Mo1 N32 87.45(16) . . ? N22 Mo1 N32 82.19(17) . . ? Cl1' Mo1 N32 94.0(2) . . ? O1' Mo1 Cl1 9.9(5) . . ? O1 Mo1 Cl1 100.2(6) . . ? O48 Mo1 Cl1 94.5(2) . . ? N22 Mo1 Cl1 95.0(2) . . ? Cl1' Mo1 Cl1 91.7(3) . . ? N32 Mo1 Cl1 173.9(2) . . ? O1' Mo1 N12 86.9(5) . . ? O1 Mo1 N12 164.3(6) . . ? O48 Mo1 N12 85.03(17) . . ? N22 Mo1 N12 84.59(18) . . ? Cl1' Mo1 N12 173.5(2) . . ? N32 Mo1 N12 79.55(18) . . ? Cl1 Mo1 N12 94.8(2) . . ? C41 O48 Mo1 134.2(3) . . ? C15 N11 N12 109.9(5) . . ? C15 N11 B1 131.5(5) . . ? N12 N11 B1 118.6(5) . . ? C13 N12 N11 106.4(4) . . ? C13 N12 Mo1 132.2(4) . . ? N11 N12 Mo1 121.4(4) . . ? C25 N21 N22 108.1(5) . . ? C25 N21 B1 130.6(5) . . ? N22 N21 B1 121.3(4) . . ? C23 N22 N21 107.4(5) . . ? C23 N22 Mo1 131.9(4) . . ? N21 N22 Mo1 120.2(3) . . ? C35 N31 N32 108.9(4) . . ? C35 N31 B1 132.2(5) . . ? N32 N31 B1 118.9(4) . . ? C33 N32 N31 106.5(4) . . ? C33 N32 Mo1 132.3(4) . . ? N31 N32 Mo1 121.2(3) . . ? N47 N47 C44 114.1(6) 2 . ? N12 C13 C14 109.5(5) . . ? N12 C13 C16 123.2(5) . . ? C14 C13 C16 127.3(6) . . ? C13 C14 C15 106.9(6) . . ? N11 C15 C14 107.4(5) . . ? N11 C15 C17 122.0(5) . . ? C14 C15 C17 130.6(6) . . ? N22 C23 C24 109.6(5) . . ? N22 C23 C26 123.7(5) . . ? C24 C23 C26 126.7(6) . . ? C25 C24 C23 106.2(6) . . ? N21 C25 C24 108.7(5) . . ? N21 C25 C27 122.2(6) . . ? C24 C25 C27 129.1(6) . . ? N32 C33 C34 108.4(5) . . ? N32 C33 C36 121.7(5) . . ? C34 C33 C36 129.9(6) . . ? C35 C34 C33 108.4(6) . . ? C34 C35 N31 107.8(5) . . ? C34 C35 C37 129.7(6) . . ? N31 C35 C37 122.5(5) . . ? O48 C41 C46 118.7(5) . . ? O48 C41 C42 123.1(5) . . ? C46 C41 C42 118.2(5) . . ? C41 C42 C43 121.4(6) . . ? C44 C43 C42 120.8(6) . . ? C43 C44 C45 117.8(5) . . ? C43 C44 N47 126.1(5) . . ? C45 C44 N47 116.1(5) . . ? C46 C45 C44 121.6(6) . . ? C41 C46 C45 120.2(6) . . ? N31 B1 N21 109.7(5) . . ? N31 B1 N11 108.6(5) . . ? N21 B1 N11 108.2(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.495 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.098 #=END data_test2 _database_code_CSD 157072 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H63.60 B2 Cl4 Mo2 N12 O5' _chemical_formula_weight 1244.01 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.059(4) _cell_length_b 19.737(4) _cell_length_c 18.568(2) _cell_angle_alpha 90.000(6) _cell_angle_beta 98.070(9) _cell_angle_gamma 90.000(9) _cell_volume 11996(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour maroon _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5101 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31988 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10552 _reflns_number_gt 6186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1676P)^2^+24.5511P] 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 10552 _refine_ls_number_parameters 688 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0821 _refine_ls_wR_factor_ref 0.2765 _refine_ls_wR_factor_gt 0.2393 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.003 _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 -0.12420(2) -0.35023(4) 0.75032(4) 0.0567(3) Uani 1 1 d . . . Mo2 Mo -0.12927(3) -0.08818(5) 0.17379(4) 0.0684(3) Uani 1 1 d . . . Cl1 Cl -0.1521(2) -0.2505(5) 0.7018(4) 0.076(2) Uani 0.530(15) 1 d P A 1 Cl1' Cl -0.1492(4) -0.4286(7) 0.6628(5) 0.086(3) Uani 0.470(15) 1 d P A 2 Cl2 Cl -0.1690(2) -0.1006(4) 0.2665(5) 0.053(3) Uani 0.362(14) 1 d P B 1 Cl2' Cl -0.0912(3) -0.0248(5) 0.2367(5) 0.094(3) Uani 0.638(14) 1 d P B 2 O1 O -0.1462(7) -0.4110(14) 0.6889(12) 0.070(5) Uani 0.530(15) 1 d P A 1 O1' O -0.1510(7) -0.2835(15) 0.7116(12) 0.083(7) Uani 0.470(15) 1 d PU A 2 O2 O -0.0823(8) -0.0175(13) 0.2323(17) 0.027(5) Uiso 0.362(14) 1 d P B 1 O2' O -0.1692(4) -0.1029(7) 0.2273(12) 0.078(4) Uani 0.638(14) 1 d P B 2 O71 O -0.07226(17) -0.3385(3) 0.7132(3) 0.0531(14) Uani 1 1 d . A . O80 O 0.00782(17) -0.3534(3) 0.4271(3) 0.0542(14) Uani 1 1 d . A . O94 O -0.09810(18) -0.1688(4) 0.1989(3) 0.0686(18) Uani 1 1 d . A . N11 N -0.0942(2) -0.4332(4) 0.8933(3) 0.0506(16) Uani 1 1 d . . . N12 N -0.0928(2) -0.4313(4) 0.8193(3) 0.0509(16) Uani 1 1 d . A . N21 N -0.1648(2) -0.3849(4) 0.8881(3) 0.0585(19) Uani 1 1 d . . . N22 N -0.1736(2) -0.3667(5) 0.8147(4) 0.071(2) Uani 1 1 d . A . N31 N -0.10326(19) -0.3098(3) 0.9158(3) 0.0478(16) Uani 1 1 d . . . N32 N -0.0971(2) -0.2900(4) 0.8463(3) 0.0519(17) Uani 1 1 d . A . N41 N -0.1704(2) -0.1299(4) 0.0169(4) 0.0610(19) Uani 1 1 d . . . N42 N -0.1659(2) -0.1500(4) 0.0880(4) 0.0600(19) Uani 1 1 d . B . N51 N -0.1753(2) -0.0079(4) 0.0436(4) 0.069(2) Uani 1 1 d . . . N52 N -0.1649(2) -0.0065(4) 0.1180(4) 0.0633(19) Uani 1 1 d . B . N61 N -0.1097(2) -0.0576(4) 0.0162(4) 0.064(2) Uani 1 1 d . . . N62 N -0.0916(2) -0.0767(4) 0.0852(4) 0.0595(19) Uani 1 1 d . B . C13 C -0.0664(3) -0.4799(5) 0.8055(5) 0.059(2) Uani 1 1 d . . . C14 C -0.0501(3) -0.5116(5) 0.8700(5) 0.064(2) Uani 1 1 d . A . H14A H -0.0308 -0.5463 0.8755 0.077 Uiso 1 1 calc R . . C15 C -0.0683(3) -0.4810(4) 0.9243(5) 0.056(2) Uani 1 1 d . A . C16 C -0.0626(3) -0.4957(5) 1.0045(5) 0.067(2) Uani 1 1 d . . . H16A H -0.0793 -0.4655 1.0282 0.101 Uiso 1 1 calc R A . H16B H -0.0344 -0.4893 1.0243 0.101 Uiso 1 1 calc R . . H16C H -0.0704 -0.5416 1.0123 0.101 Uiso 1 1 calc R . . C17 C -0.0574(3) -0.4960(5) 0.7301(5) 0.076(3) Uani 1 1 d . A . H17A H -0.0731 -0.4667 0.6956 0.114 Uiso 1 1 calc R . . H17B H -0.0645 -0.5423 0.7186 0.114 Uiso 1 1 calc R . . H17C H -0.0288 -0.4894 0.7280 0.114 Uiso 1 1 calc R . . C23 C -0.2136(3) -0.3705(7) 0.7963(5) 0.087(4) Uani 1 1 d . . . C24 C -0.2310(3) -0.3921(7) 0.8571(6) 0.092(4) Uani 1 1 d . A . H24A H -0.2587 -0.3991 0.8590 0.110 Uiso 1 1 calc R . . C25 C -0.1999(3) -0.4008(6) 0.9130(5) 0.072(3) Uani 1 1 d . A . C26 C -0.2013(3) -0.4233(6) 0.9896(6) 0.082(3) Uani 1 1 d . . . H26A H -0.1742 -0.4232 1.0161 0.122 Uiso 1 1 calc R A . H26B H -0.2124 -0.4683 0.9894 0.122 Uiso 1 1 calc R . . H26C H -0.2183 -0.3930 1.0125 0.122 Uiso 1 1 calc R . . C27 C -0.2335(3) -0.3558(9) 0.7206(6) 0.126(6) Uani 1 1 d . A . H27A H -0.2132 -0.3415 0.6916 0.188 Uiso 1 1 calc R . . H27B H -0.2534 -0.3206 0.7217 0.188 Uiso 1 1 calc R . . H27C H -0.2467 -0.3960 0.6998 0.188 Uiso 1 1 calc R . . C33 C -0.0779(3) -0.2298(5) 0.8533(5) 0.061(2) Uani 1 1 d . . . C34 C -0.0714(3) -0.2121(5) 0.9249(5) 0.067(3) Uani 1 1 d . A . H34A H -0.0582 -0.1733 0.9445 0.080 Uiso 1 1 calc R . . C35 C -0.0881(2) -0.2623(5) 0.9628(4) 0.053(2) Uani 1 1 d . A . C36 C -0.0887(3) -0.2673(6) 1.0426(4) 0.068(3) Uani 1 1 d . . . H36A H -0.1027 -0.3079 1.0532 0.102 Uiso 1 1 calc R A . H36B H -0.1025 -0.2286 1.0589 0.102 Uiso 1 1 calc R . . H36C H -0.0612 -0.2685 1.0673 0.102 Uiso 1 1 calc R . . C37 C -0.0638(4) -0.1921(6) 0.7903(6) 0.086(3) Uani 1 1 d . A . H37A H -0.0725 -0.2162 0.7459 0.129 Uiso 1 1 calc R . . H37B H -0.0346 -0.1886 0.7980 0.129 Uiso 1 1 calc R . . H37C H -0.0755 -0.1475 0.7872 0.129 Uiso 1 1 calc R . . C43 C -0.1832(3) -0.2122(6) 0.0907(7) 0.074(3) Uani 1 1 d . . . C44 C -0.1984(3) -0.2327(7) 0.0216(8) 0.088(3) Uani 1 1 d . B . H44A H -0.2118 -0.2731 0.0083 0.106 Uiso 1 1 calc R . . C45 C -0.1894(3) -0.1801(6) -0.0249(6) 0.082(3) Uani 1 1 d . B . C46 C -0.1951(4) -0.1774(7) -0.1076(6) 0.105(4) Uani 1 1 d . . . H46A H -0.1863 -0.1341 -0.1230 0.158 Uiso 1 1 calc R B . H46B H -0.2235 -0.1837 -0.1261 0.158 Uiso 1 1 calc R . . H46C H -0.1793 -0.2125 -0.1258 0.158 Uiso 1 1 calc R . . C47 C -0.1850(4) -0.2508(6) 0.1571(7) 0.097(4) Uani 1 1 d . B . H47A H -0.1722 -0.2254 0.1982 0.145 Uiso 1 1 calc R . . H47B H -0.1710 -0.2931 0.1544 0.145 Uiso 1 1 calc R . . H47C H -0.2131 -0.2593 0.1623 0.145 Uiso 1 1 calc R . . C53 C -0.1850(3) 0.0460(6) 0.1436(6) 0.081(3) Uani 1 1 d . . . C54 C -0.2078(5) 0.0789(7) 0.0877(7) 0.129(6) Uani 1 1 d . B . H54A H -0.2242 0.1169 0.0905 0.155 Uiso 1 1 calc R . . C55 C -0.2012(4) 0.0428(7) 0.0241(6) 0.094(4) Uani 1 1 d . B . C56 C -0.2187(5) 0.0561(8) -0.0570(6) 0.134(6) Uani 1 1 d . . . H56A H -0.2086 0.0223 -0.0871 0.201 Uiso 1 1 calc R B . H56B H -0.2103 0.1001 -0.0711 0.201 Uiso 1 1 calc R . . H56C H -0.2480 0.0541 -0.0628 0.201 Uiso 1 1 calc R . . C57 C -0.1807(4) 0.0621(7) 0.2219(6) 0.103(4) Uani 1 1 d . B . H57A H -0.1630 0.0295 0.2487 0.155 Uiso 1 1 calc R . . H57B H -0.2070 0.0605 0.2380 0.155 Uiso 1 1 calc R . . H57C H -0.1693 0.1066 0.2301 0.155 Uiso 1 1 calc R . . C63 C -0.0496(3) -0.0766(6) 0.0864(6) 0.077(3) Uani 1 1 d . . . C64 C -0.0442(4) -0.0552(6) 0.0141(6) 0.080(3) Uani 1 1 d . B . H64A H -0.0190 -0.0505 -0.0023 0.096 Uiso 1 1 calc R . . C65 C -0.0805(4) -0.0431(5) -0.0260(6) 0.079(3) Uani 1 1 d . B . C66 C -0.0897(5) -0.0236(6) -0.1036(6) 0.108(4) Uani 1 1 d . . . H66A H -0.1187 -0.0179 -0.1163 0.162 Uiso 1 1 calc R B . H66B H -0.0804 -0.0585 -0.1332 0.162 Uiso 1 1 calc R . . H66C H -0.0761 0.0181 -0.1115 0.162 Uiso 1 1 calc R . . C67 C -0.0214(3) -0.0963(9) 0.1513(7) 0.122(6) Uani 1 1 d . B . H67A H -0.0366 -0.1071 0.1901 0.183 Uiso 1 1 calc R . . H67B H -0.0031 -0.0595 0.1658 0.183 Uiso 1 1 calc R . . H67C H -0.0059 -0.1352 0.1403 0.183 Uiso 1 1 calc R . . C71 C -0.0613(2) -0.3319(4) 0.6463(4) 0.0492(19) Uani 1 1 d . . . C72 C -0.0205(3) -0.3385(4) 0.6380(4) 0.052(2) Uani 1 1 d . A . H72A H -0.0011 -0.3461 0.6786 0.063 Uiso 1 1 calc R . . C73 C -0.0083(2) -0.3341(4) 0.5709(4) 0.0482(19) Uani 1 1 d . . . H73A H 0.0192 -0.3401 0.5665 0.058 Uiso 1 1 calc R A . C74 C -0.0357(2) -0.3210(4) 0.5093(4) 0.0442(18) Uani 1 1 d . A . C75 C -0.0768(2) -0.3138(5) 0.5188(4) 0.054(2) Uani 1 1 d . . . H75A H -0.0959 -0.3042 0.4784 0.064 Uiso 1 1 calc R A . C76 C -0.0897(3) -0.3203(5) 0.5839(4) 0.055(2) Uani 1 1 d . A . H76A H -0.1174 -0.3171 0.5876 0.066 Uiso 1 1 calc R . . C80 C -0.0215(2) -0.3202(4) 0.4374(4) 0.0421(17) Uani 1 1 d . . . C91 C -0.0433(2) -0.2795(4) 0.3761(4) 0.0454(18) Uani 1 1 d . A . C92 C -0.0633(3) -0.2199(5) 0.3869(4) 0.065(3) Uani 1 1 d . . . H92A H -0.0633 -0.2035 0.4339 0.078 Uiso 1 1 calc R A . C93 C -0.0841(3) -0.1833(5) 0.3266(5) 0.075(3) Uani 1 1 d . A . H93A H -0.0999 -0.1458 0.3345 0.090 Uiso 1 1 calc R . . C94 C -0.0810(2) -0.2031(4) 0.2584(4) 0.050(2) Uani 1 1 d . . . C95 C -0.0608(3) -0.2632(5) 0.2469(4) 0.063(2) Uani 1 1 d . A . H95A H -0.0607 -0.2790 0.1997 0.076 Uiso 1 1 calc R . . C96 C -0.0406(3) -0.3003(4) 0.3057(4) 0.055(2) Uani 1 1 d . . . H96A H -0.0254 -0.3385 0.2974 0.066 Uiso 1 1 calc R A . B1 B -0.1203(3) -0.3802(5) 0.9269(5) 0.052(2) Uani 1 1 d . A . H1 H -0.1196 -0.3891 0.9790 0.063 Uiso 1 1 calc R . . B2 B -0.1564(4) -0.0608(6) -0.0023(6) 0.069(3) Uani 1 1 d . B . H2 H -0.1646 -0.0519 -0.0543 0.083 Uiso 1 1 calc R . . C110 C -0.0888(5) 0.1223(8) 0.0939(8) 0.120(5) Uani 1 1 d . . . H11A H -0.0924 0.0769 0.1121 0.144 Uiso 1 1 calc R . . H11B H -0.1000 0.1538 0.1260 0.144 Uiso 1 1 calc R . . Cl13 Cl -0.03797(15) 0.1375(2) 0.0986(3) 0.1430(15) Uani 1 1 d . . . Cl12 Cl -0.11559(15) 0.1290(2) 0.0108(3) 0.1448(16) Uani 1 1 d . . . C201 C -0.3075(11) 0.1494(19) 0.010(2) 0.147(12) Uiso 0.50 1 d P . . C202 C -0.3065(9) 0.2251(17) 0.0399(17) 0.125(10) Uiso 0.50 1 d P . . C203 C -0.2553(9) 0.2526(16) 0.0252(14) 0.112(9) Uiso 0.50 1 d P . . C204 C -0.1711(10) -0.4401(19) 0.3009(19) 0.137(11) Uiso 0.50 1 d P . . C205 C -0.1648(8) -0.4210(14) 0.3876(15) 0.103(8) Uiso 0.50 1 d P . . C206 C -0.1416(7) -0.3748(12) 0.3082(12) 0.084(6) Uiso 0.50 1 d P . . C207 C -0.2109(4) -0.4256(9) 0.2316(12) 0.177(10) 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 Mo1 0.0526(4) 0.0837(6) 0.0323(4) -0.0017(3) 0.0008(3) 0.0067(4) Mo2 0.0713(6) 0.0956(7) 0.0420(4) 0.0282(4) 0.0207(4) 0.0370(5) Cl1 0.086(4) 0.077(5) 0.063(3) -0.007(3) 0.002(3) 0.023(4) Cl1' 0.077(4) 0.137(8) 0.041(5) -0.018(4) -0.001(4) -0.019(5) Cl2 0.040(3) 0.086(5) 0.035(4) 0.001(4) 0.014(3) -0.001(3) Cl2' 0.084(6) 0.130(6) 0.070(4) -0.025(3) 0.011(4) -0.016(4) O1 0.045(8) 0.114(16) 0.048(12) -0.003(10) -0.002(9) 0.010(9) O1' 0.092(10) 0.087(11) 0.069(9) -0.003(8) 0.012(7) 0.014(9) O2' 0.069(8) 0.089(9) 0.080(11) 0.018(9) 0.027(8) 0.004(6) O71 0.064(3) 0.063(4) 0.031(3) 0.002(2) 0.004(2) 0.008(3) O80 0.053(3) 0.066(4) 0.042(3) 0.006(3) 0.002(2) 0.008(3) O94 0.065(4) 0.098(5) 0.044(3) 0.028(3) 0.012(3) 0.036(3) N11 0.051(4) 0.059(4) 0.040(4) 0.006(3) -0.001(3) -0.006(3) N12 0.051(4) 0.061(5) 0.041(4) -0.004(3) 0.007(3) 0.002(3) N21 0.047(4) 0.093(6) 0.034(4) -0.003(3) 0.003(3) -0.007(4) N22 0.055(4) 0.118(7) 0.038(4) -0.005(4) -0.002(3) 0.002(4) N31 0.048(4) 0.058(4) 0.037(3) -0.005(3) 0.002(3) 0.008(3) N32 0.056(4) 0.062(5) 0.039(4) 0.000(3) 0.011(3) 0.003(3) N41 0.064(4) 0.057(5) 0.056(4) 0.009(4) -0.014(4) 0.004(4) N42 0.041(4) 0.067(5) 0.071(5) 0.016(4) 0.005(3) 0.000(3) N51 0.083(5) 0.063(5) 0.054(4) 0.020(4) -0.015(4) 0.013(4) N52 0.071(5) 0.061(5) 0.054(4) 0.010(4) -0.006(4) 0.007(4) N61 0.088(6) 0.058(5) 0.048(4) 0.002(3) 0.015(4) -0.009(4) N62 0.053(4) 0.080(5) 0.046(4) 0.005(4) 0.010(3) -0.010(4) C13 0.066(5) 0.053(5) 0.060(5) 0.002(4) 0.009(4) 0.000(4) C14 0.067(6) 0.053(6) 0.069(6) -0.004(5) -0.003(5) -0.004(4) C15 0.058(5) 0.051(5) 0.056(5) 0.005(4) 0.000(4) -0.012(4) C16 0.083(6) 0.050(6) 0.063(6) 0.008(4) -0.007(5) -0.004(5) C17 0.088(7) 0.069(7) 0.074(7) -0.006(5) 0.024(5) 0.007(6) C23 0.052(6) 0.155(11) 0.050(6) -0.022(6) -0.003(4) 0.004(6) C24 0.048(5) 0.152(12) 0.072(7) -0.031(7) -0.002(5) -0.008(6) C25 0.052(5) 0.106(8) 0.057(6) -0.014(5) 0.007(4) -0.009(5) C26 0.070(6) 0.107(9) 0.074(7) 0.001(6) 0.033(5) -0.015(6) C27 0.056(6) 0.252(19) 0.060(7) -0.024(9) -0.023(5) 0.012(9) C33 0.071(6) 0.053(6) 0.062(6) 0.002(4) 0.014(5) 0.007(5) C34 0.081(6) 0.058(6) 0.065(6) -0.018(5) 0.021(5) -0.004(5) C35 0.043(4) 0.070(6) 0.044(4) -0.015(4) 0.000(4) 0.014(4) C36 0.052(5) 0.101(8) 0.047(5) -0.024(5) -0.008(4) 0.013(5) C37 0.106(8) 0.079(8) 0.072(7) 0.007(6) 0.013(6) -0.001(6) C43 0.043(5) 0.074(7) 0.108(9) 0.005(6) 0.017(5) -0.002(5) C44 0.038(5) 0.091(9) 0.133(11) 0.001(8) 0.004(6) -0.013(5) C45 0.057(6) 0.081(7) 0.093(8) -0.012(6) -0.040(6) 0.014(5) C46 0.110(9) 0.110(10) 0.081(8) -0.022(7) -0.040(7) 0.019(8) C47 0.095(8) 0.074(8) 0.134(11) 0.020(7) 0.057(8) -0.014(6) C53 0.094(8) 0.079(8) 0.067(6) 0.006(5) -0.005(6) 0.022(6) C54 0.168(14) 0.110(11) 0.095(9) 0.004(8) -0.026(9) 0.087(10) C55 0.103(9) 0.103(9) 0.071(7) 0.020(7) -0.011(6) 0.026(7) C56 0.172(14) 0.134(12) 0.078(8) 0.021(8) -0.042(9) 0.065(11) C57 0.101(9) 0.113(10) 0.091(9) -0.017(7) -0.005(7) 0.042(8) C63 0.054(6) 0.090(8) 0.091(8) -0.032(6) 0.032(5) -0.026(5) C64 0.095(8) 0.074(7) 0.086(7) -0.025(6) 0.060(7) -0.042(6) C65 0.116(9) 0.056(6) 0.071(7) -0.002(5) 0.041(7) -0.015(6) C66 0.187(14) 0.081(8) 0.065(7) 0.019(6) 0.049(8) -0.010(8) C67 0.037(5) 0.240(19) 0.088(8) -0.026(10) 0.005(5) -0.007(8) C71 0.060(5) 0.051(5) 0.037(4) 0.003(3) 0.007(4) 0.002(4) C72 0.058(5) 0.063(6) 0.033(4) 0.008(4) -0.003(3) -0.001(4) C73 0.051(4) 0.050(5) 0.040(4) 0.006(3) -0.003(3) 0.001(4) C74 0.051(4) 0.044(4) 0.037(4) 0.004(3) 0.003(3) 0.004(4) C75 0.053(5) 0.071(6) 0.034(4) 0.000(4) -0.005(3) 0.005(4) C76 0.054(5) 0.069(6) 0.040(4) 0.009(4) 0.002(4) 0.012(4) C80 0.047(4) 0.039(4) 0.039(4) 0.000(3) 0.003(3) -0.004(4) C91 0.047(4) 0.058(5) 0.031(4) 0.003(3) 0.007(3) 0.002(4) C92 0.103(7) 0.064(6) 0.030(4) 0.001(4) 0.014(4) 0.018(5) C93 0.104(8) 0.077(7) 0.052(5) 0.026(5) 0.035(5) 0.048(6) C94 0.049(4) 0.064(6) 0.036(4) 0.012(4) 0.001(3) 0.011(4) C95 0.094(7) 0.068(6) 0.027(4) 0.006(4) 0.005(4) 0.005(5) C96 0.070(5) 0.057(5) 0.040(4) 0.009(4) 0.013(4) 0.015(4) B1 0.051(5) 0.070(7) 0.036(5) -0.007(4) 0.005(4) 0.002(5) B2 0.077(7) 0.085(8) 0.040(5) 0.010(5) -0.010(5) 0.001(6) C110 0.138(12) 0.101(10) 0.122(12) -0.007(9) 0.018(10) -0.042(9) Cl13 0.138(3) 0.140(4) 0.155(4) -0.017(3) 0.032(3) -0.010(3) Cl12 0.165(4) 0.119(3) 0.156(4) -0.007(3) 0.044(3) -0.053(3) C207 0.069(8) 0.144(14) 0.30(2) 0.156(16) -0.028(11) 0.000(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 O1' 1.69(3) . ? Mo1 O1 1.74(3) . ? Mo1 O71 1.952(6) . ? Mo1 N22 2.179(8) . ? Mo1 N12 2.216(7) . ? Mo1 N32 2.223(7) . ? Mo1 Cl1 2.303(9) . ? Mo1 Cl1' 2.311(10) . ? Mo2 O2' 1.785(17) . ? Mo2 O94 1.917(6) . ? Mo2 Cl2' 2.026(10) . ? Mo2 N52 2.171(7) . ? Mo2 N62 2.209(7) . ? Mo2 N42 2.227(8) . ? Mo2 O2 2.25(3) . ? Mo2 Cl2 2.320(8) . ? O71 C71 1.348(9) . ? O80 C80 1.208(9) . ? O94 C94 1.351(9) . ? N11 C15 1.349(11) . ? N11 N12 1.381(9) . ? N11 B1 1.543(12) . ? N12 C13 1.346(11) . ? N21 C25 1.343(11) . ? N21 N22 1.400(9) . ? N21 B1 1.548(11) . ? N22 C23 1.320(11) . ? N31 C35 1.330(10) . ? N31 N32 1.389(9) . ? N31 B1 1.524(13) . ? N32 C33 1.346(11) . ? N41 C45 1.357(12) . ? N41 N42 1.366(9) . ? N41 B2 1.499(14) . ? N42 C43 1.356(12) . ? N51 C55 1.335(13) . ? N51 N52 1.375(10) . ? N51 B2 1.536(15) . ? N52 C53 1.354(13) . ? N61 C65 1.359(12) . ? N61 N62 1.388(10) . ? N61 B2 1.534(14) . ? N62 C63 1.386(11) . ? C13 C14 1.392(12) . ? C13 C17 1.505(12) . ? C14 C15 1.384(13) . ? C15 C16 1.503(12) . ? C23 C24 1.405(15) . ? C23 C27 1.495(14) . ? C24 C25 1.367(13) . ? C25 C26 1.498(13) . ? C33 C34 1.361(12) . ? C33 C37 1.514(14) . ? C34 C35 1.374(13) . ? C35 C36 1.489(11) . ? C43 C44 1.371(15) . ? C43 C47 1.458(15) . ? C44 C45 1.408(16) . ? C45 C46 1.521(16) . ? C53 C54 1.359(14) . ? C53 C57 1.476(15) . ? C54 C55 1.422(17) . ? C55 C56 1.558(14) . ? C63 C64 1.442(15) . ? C63 C67 1.469(16) . ? C64 C65 1.343(15) . ? C65 C66 1.480(15) . ? C71 C72 1.387(11) . ? C71 C76 1.405(11) . ? C72 C73 1.365(11) . ? C73 C74 1.381(10) . ? C74 C75 1.402(11) . ? C74 C80 1.476(10) . ? C75 C76 1.344(11) . ? C80 C91 1.493(10) . ? C91 C92 1.380(12) . ? C91 C96 1.384(11) . ? C92 C93 1.425(12) . ? C93 C94 1.344(12) . ? C94 C95 1.393(12) . ? C95 C96 1.403(11) . ? C110 Cl12 1.674(15) . ? C110 Cl13 1.696(15) . ? C201 C202 1.59(5) . ? C202 C203 1.83(4) . ? C203 C203 1.05(5) 7_455 ? C204 C206 1.61(4) . ? C204 C205 1.64(4) . ? C204 C207 1.73(4) . ? C205 C206 1.98(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 O1' Mo1 O1 96.4(11) . . ? O1' Mo1 O71 101.1(8) . . ? O1 Mo1 O71 99.1(8) . . ? O1' Mo1 N22 87.8(8) . . ? O1 Mo1 N22 88.9(8) . . ? O71 Mo1 N22 167.3(2) . . ? O1' Mo1 N12 169.7(8) . . ? O1 Mo1 N12 90.0(8) . . ? O71 Mo1 N12 85.7(2) . . ? N22 Mo1 N12 84.4(3) . . ? O1' Mo1 N32 93.0(8) . . ? O1 Mo1 N32 167.7(8) . . ? O71 Mo1 N32 86.8(2) . . ? N22 Mo1 N32 83.5(3) . . ? N12 Mo1 N32 79.6(2) . . ? O1' Mo1 Cl1 8.3(9) . . ? O1 Mo1 Cl1 103.0(8) . . ? O71 Mo1 Cl1 94.9(3) . . ? N22 Mo1 Cl1 92.9(3) . . ? N12 Mo1 Cl1 166.7(2) . . ? N32 Mo1 Cl1 87.2(3) . . ? O1' Mo1 Cl1' 96.2(9) . . ? O1 Mo1 Cl1' 4.9(10) . . ? O71 Mo1 Cl1' 94.4(4) . . ? N22 Mo1 Cl1' 93.7(4) . . ? N12 Mo1 Cl1' 90.9(4) . . ? N32 Mo1 Cl1' 170.3(4) . . ? Cl1 Mo1 Cl1' 102.3(4) . . ? O2' Mo2 O94 98.3(5) . . ? O2' Mo2 Cl2' 103.2(7) . . ? O94 Mo2 Cl2' 95.9(4) . . ? O2' Mo2 N52 89.6(5) . . ? O94 Mo2 N52 165.6(3) . . ? Cl2' Mo2 N52 93.9(4) . . ? O2' Mo2 N62 165.8(7) . . ? O94 Mo2 N62 85.8(3) . . ? Cl2' Mo2 N62 89.8(3) . . ? N52 Mo2 N62 83.8(3) . . ? O2' Mo2 N42 86.4(7) . . ? O94 Mo2 N42 86.5(3) . . ? Cl2' Mo2 N42 169.5(3) . . ? N52 Mo2 N42 82.0(3) . . ? N62 Mo2 N42 80.2(3) . . ? O2' Mo2 O2 110.3(10) . . ? O94 Mo2 O2 94.9(7) . . ? Cl2' Mo2 O2 7.1(9) . . ? N52 Mo2 O2 93.5(7) . . ? N62 Mo2 O2 82.7(8) . . ? N42 Mo2 O2 162.8(8) . . ? O2' Mo2 Cl2 13.9(6) . . ? O94 Mo2 Cl2 94.2(3) . . ? Cl2' Mo2 Cl2 90.5(3) . . ? N52 Mo2 Cl2 96.2(3) . . ? N62 Mo2 Cl2 179.7(3) . . ? N42 Mo2 Cl2 99.5(3) . . ? O2 Mo2 Cl2 97.5(8) . . ? C71 O71 Mo1 134.5(5) . . ? C94 O94 Mo2 139.8(6) . . ? C15 N11 N12 109.6(7) . . ? C15 N11 B1 131.2(7) . . ? N12 N11 B1 119.0(6) . . ? C13 N12 N11 106.6(7) . . ? C13 N12 Mo1 131.9(6) . . ? N11 N12 Mo1 121.0(5) . . ? C25 N21 N22 109.0(7) . . ? C25 N21 B1 131.5(7) . . ? N22 N21 B1 119.4(7) . . ? C23 N22 N21 107.5(8) . . ? C23 N22 Mo1 131.8(6) . . ? N21 N22 Mo1 120.3(5) . . ? C35 N31 N32 108.7(7) . . ? C35 N31 B1 131.8(7) . . ? N32 N31 B1 119.2(6) . . ? C33 N32 N31 106.7(6) . . ? C33 N32 Mo1 132.9(6) . . ? N31 N32 Mo1 120.0(5) . . ? C45 N41 N42 108.6(8) . . ? C45 N41 B2 131.4(9) . . ? N42 N41 B2 120.0(7) . . ? C43 N42 N41 108.1(8) . . ? C43 N42 Mo2 131.2(7) . . ? N41 N42 Mo2 120.4(5) . . ? C55 N51 N52 108.5(9) . . ? C55 N51 B2 130.9(8) . . ? N52 N51 B2 120.5(7) . . ? C53 N52 N51 107.6(7) . . ? C53 N52 Mo2 131.3(6) . . ? N51 N52 Mo2 120.5(6) . . ? C65 N61 N62 109.9(8) . . ? C65 N61 B2 130.8(9) . . ? N62 N61 B2 119.1(7) . . ? C63 N62 N61 108.4(7) . . ? C63 N62 Mo2 131.0(6) . . ? N61 N62 Mo2 120.0(5) . . ? N12 C13 C14 109.8(8) . . ? N12 C13 C17 123.1(8) . . ? C14 C13 C17 127.1(9) . . ? C15 C14 C13 106.0(9) . . ? N11 C15 C14 108.0(8) . . ? N11 C15 C16 122.8(8) . . ? C14 C15 C16 129.1(9) . . ? N22 C23 C24 108.6(9) . . ? N22 C23 C27 121.7(10) . . ? C24 C23 C27 129.7(9) . . ? C25 C24 C23 107.3(9) . . ? N21 C25 C24 107.7(9) . . ? N21 C25 C26 122.7(8) . . ? C24 C25 C26 129.6(10) . . ? N32 C33 C34 109.2(8) . . ? N32 C33 C37 123.5(8) . . ? C34 C33 C37 127.2(9) . . ? C33 C34 C35 107.2(8) . . ? N31 C35 C34 108.3(7) . . ? N31 C35 C36 123.4(9) . . ? C34 C35 C36 128.3(8) . . ? N42 C43 C44 109.5(10) . . ? N42 C43 C47 124.9(11) . . ? C44 C43 C47 125.6(11) . . ? C43 C44 C45 106.0(10) . . ? N41 C45 C44 107.9(10) . . ? N41 C45 C46 122.2(11) . . ? C44 C45 C46 129.7(11) . . ? N52 C53 C54 110.2(10) . . ? N52 C53 C57 121.8(9) . . ? C54 C53 C57 128.0(11) . . ? C53 C54 C55 105.2(10) . . ? N51 C55 C54 108.5(9) . . ? N51 C55 C56 121.7(11) . . ? C54 C55 C56 129.8(11) . . ? N62 C63 C64 104.0(10) . . ? N62 C63 C67 122.2(9) . . ? C64 C63 C67 133.8(10) . . ? C65 C64 C63 110.5(9) . . ? C64 C65 N61 107.1(9) . . ? C64 C65 C66 129.3(11) . . ? N61 C65 C66 123.3(12) . . ? O71 C71 C72 119.0(7) . . ? O71 C71 C76 122.7(7) . . ? C72 C71 C76 118.2(7) . . ? C73 C72 C71 120.9(7) . . ? C72 C73 C74 121.6(8) . . ? C73 C74 C75 116.8(7) . . ? C73 C74 C80 119.7(7) . . ? C75 C74 C80 123.4(7) . . ? C76 C75 C74 122.7(7) . . ? C75 C76 C71 119.8(8) . . ? O80 C80 C74 120.1(7) . . ? O80 C80 C91 118.9(7) . . ? C74 C80 C91 121.0(7) . . ? C92 C91 C96 119.1(7) . . ? C92 C91 C80 122.5(7) . . ? C96 C91 C80 118.2(7) . . ? C91 C92 C93 120.4(8) . . ? C94 C93 C92 120.1(8) . . ? C93 C94 O94 123.1(8) . . ? C93 C94 C95 119.6(7) . . ? O94 C94 C95 117.2(7) . . ? C94 C95 C96 120.7(8) . . ? C91 C96 C95 119.6(8) . . ? N31 B1 N11 108.9(7) . . ? N31 B1 N21 109.7(7) . . ? N11 B1 N21 108.6(7) . . ? N41 B2 N61 108.7(8) . . ? N41 B2 N51 108.8(9) . . ? N61 B2 N51 108.7(8) . . ? Cl12 C110 Cl13 115.2(9) . . ? C201 C202 C203 102(2) . . ? C203 C203 C202 122(4) 7_455 . ? C206 C204 C205 75(2) . . ? C206 C204 C207 109(2) . . ? C205 C204 C207 132(3) . . ? C204 C205 C206 51.9(16) . . ? C204 C206 C205 53.1(15) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.564 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.133 #=END