Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Daniel Miguel' _publ_contact_author_address ; Dept de Quimica Inorganica Universidad de Valladolid Facultad de Ciencias Prado de la Magdalena s/n Valladolid E47005 SPAIN ; _publ_contact_author_email DMSJ@QI.UVA.ES _publ_section_title ; Pyridine-2-carboxaldehyde as ligand: synthesis and derivatization of carbonyl complexes ; loop_ _publ_author_name 'D Miguel' 'Raul Garcia-Rodriguez' data_Compound_1b_rg106c _database_code_depnum_ccdc_archive 'CCDC 637219' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 Cl Mn N O4' _chemical_formula_weight 281.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 10.767(5) _cell_length_b 8.076(4) _cell_length_c 13.357(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.987(10) _cell_angle_gamma 90.00 _cell_volume 1143.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour DEEP_RED _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.582280 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 4886 _diffrn_reflns_av_R_equivalents 0.0975 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 23.50 _reflns_number_total 1658 _reflns_number_gt 1041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0672P)^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 1658 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn 0.70243(9) 0.80075(14) 0.60317(8) 0.0400(4) Uani 1 1 d . . . Cl1 Cl 0.91157(16) 0.8936(2) 0.66618(14) 0.0515(6) Uani 1 1 d . . . N1 N 0.7819(4) 0.5977(7) 0.5441(4) 0.0331(13) Uani 1 1 d . . . C1 C 0.5464(8) 0.7250(10) 0.5567(6) 0.056(2) Uani 1 1 d . . . O1 O 0.4465(5) 0.6769(8) 0.5242(5) 0.096(2) Uani 1 1 d . . . C2 C 0.6403(7) 0.9709(11) 0.6691(6) 0.060(2) Uani 1 1 d . . . O2 O 0.6032(6) 1.0789(9) 0.7110(5) 0.101(2) Uani 1 1 d . . . C3 C 0.6920(6) 0.9280(9) 0.4941(6) 0.0467(19) Uani 1 1 d . . . O3 O 0.6869(5) 1.0122(8) 0.4225(4) 0.0721(17) Uani 1 1 d . . . O4 O 0.7311(5) 0.6441(7) 0.7276(3) 0.0570(14) Uani 1 1 d . . . C11 C 0.8032(6) 0.5700(9) 0.4505(5) 0.0407(18) Uani 1 1 d . . . H11 H 0.7803 0.6508 0.4012 0.049 Uiso 1 1 calc R . . C12 C 0.8589(6) 0.4243(10) 0.4233(6) 0.047(2) Uani 1 1 d . . . H12 H 0.8738 0.4104 0.3573 0.056 Uiso 1 1 calc R . . C13 C 0.8915(6) 0.3022(10) 0.4938(6) 0.050(2) Uani 1 1 d . . . H13 H 0.9276 0.2041 0.4764 0.060 Uiso 1 1 calc R . . C14 C 0.8697(6) 0.3277(9) 0.5922(5) 0.0421(18) Uani 1 1 d . . . H14 H 0.8914 0.2472 0.6420 0.051 Uiso 1 1 calc R . . C15 C 0.8153(6) 0.4742(9) 0.6145(5) 0.0362(17) Uani 1 1 d . . . C16 C 0.7848(6) 0.5121(10) 0.7129(6) 0.052(2) Uani 1 1 d . . . H16 H 0.8056 0.4370 0.7659 0.062 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 Mn1 0.0436(6) 0.0354(7) 0.0398(7) -0.0039(6) 0.0040(4) 0.0076(5) Cl1 0.0498(11) 0.0442(13) 0.0558(14) -0.0122(10) -0.0039(9) 0.0046(9) N1 0.038(3) 0.030(3) 0.029(4) -0.005(3) 0.001(3) -0.003(3) C1 0.052(5) 0.042(5) 0.076(6) -0.004(4) 0.017(4) 0.016(4) O1 0.048(4) 0.074(5) 0.161(7) -0.029(4) 0.005(4) -0.004(3) C2 0.063(5) 0.064(7) 0.051(6) -0.018(5) 0.001(4) 0.010(5) O2 0.108(5) 0.098(6) 0.092(5) -0.043(4) 0.008(4) 0.043(4) C3 0.056(5) 0.038(5) 0.045(5) -0.016(4) 0.004(4) 0.006(4) O3 0.109(5) 0.055(4) 0.052(4) 0.007(3) 0.012(3) 0.010(3) O4 0.083(4) 0.049(4) 0.044(3) 0.001(3) 0.025(3) 0.010(3) C11 0.046(4) 0.040(5) 0.033(5) -0.006(4) 0.000(3) -0.006(4) C12 0.046(4) 0.044(6) 0.052(5) -0.020(4) 0.009(4) -0.010(4) C13 0.041(4) 0.030(5) 0.080(6) -0.016(5) 0.013(4) -0.001(4) C14 0.048(4) 0.032(5) 0.045(5) 0.001(4) 0.004(3) 0.003(4) C15 0.043(4) 0.037(5) 0.029(4) -0.007(4) 0.005(3) -0.002(3) C16 0.062(5) 0.041(5) 0.053(6) 0.009(4) 0.013(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C3 1.770(9) . ? Mn1 C1 1.794(9) . ? Mn1 C2 1.822(9) . ? Mn1 N1 2.068(5) . ? Mn1 O4 2.069(5) . ? Mn1 Cl1 2.384(2) . ? N1 C11 1.328(8) . ? N1 C15 1.376(8) . ? C1 O1 1.156(8) . ? C2 O2 1.144(9) . ? C3 O3 1.168(8) . ? O4 C16 1.245(8) . ? C11 C12 1.397(9) . ? C12 C13 1.367(10) . ? C13 C14 1.389(9) . ? C14 C15 1.376(9) . ? C15 C16 1.441(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mn1 C1 89.5(3) . . ? C3 Mn1 C2 89.1(3) . . ? C1 Mn1 C2 91.4(3) . . ? C3 Mn1 N1 96.8(3) . . ? C1 Mn1 N1 91.3(3) . . ? C2 Mn1 N1 173.6(3) . . ? C3 Mn1 O4 174.5(3) . . ? C1 Mn1 O4 94.0(3) . . ? C2 Mn1 O4 95.1(3) . . ? N1 Mn1 O4 78.9(2) . . ? C3 Mn1 Cl1 91.7(2) . . ? C1 Mn1 Cl1 178.4(3) . . ? C2 Mn1 Cl1 89.7(3) . . ? N1 Mn1 Cl1 87.50(14) . . ? O4 Mn1 Cl1 84.75(16) . . ? C11 N1 C15 117.0(6) . . ? C11 N1 Mn1 130.0(5) . . ? C15 N1 Mn1 113.0(4) . . ? O1 C1 Mn1 178.2(7) . . ? O2 C2 Mn1 178.8(8) . . ? O3 C3 Mn1 179.0(7) . . ? C16 O4 Mn1 113.9(4) . . ? N1 C11 C12 122.6(7) . . ? C13 C12 C11 119.9(7) . . ? C12 C13 C14 118.7(7) . . ? C15 C14 C13 118.7(6) . . ? N1 C15 C14 123.1(6) . . ? N1 C15 C16 113.3(6) . . ? C14 C15 C16 123.5(7) . . ? O4 C16 C15 120.8(7) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.746 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.099 #===END data_Compound_1c_(rg344dm) _database_code_depnum_ccdc_archive 'CCDC 637220' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 Br N O4 Re' _chemical_formula_weight 457.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 10.693(3) _cell_length_b 8.987(3) _cell_length_c 11.888(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.210(5) _cell_angle_gamma 90.00 _cell_volume 1142.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour RED-BROWN _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.659 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 14.130 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497547 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 4929 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1635 _reflns_number_gt 1403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0258P)^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 1635 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0220 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Re1 Re 0.67254(2) 0.40636(3) 0.77536(2) 0.03007(12) Uani 1 1 d . . . Br1 Br 0.88871(6) 0.41294(7) 0.67268(6) 0.04235(19) Uani 1 1 d . . . N1 N 0.7717(4) 0.5059(5) 0.9175(4) 0.0292(12) Uani 1 1 d . . . C1 C 0.5166(7) 0.4156(6) 0.8505(6) 0.0362(16) Uani 1 1 d . . . O1 O 0.4205(5) 0.4219(5) 0.8944(4) 0.0551(14) Uani 1 1 d . . . C2 C 0.5850(7) 0.3459(8) 0.6419(6) 0.0479(18) Uani 1 1 d . . . O2 O 0.5284(6) 0.3110(7) 0.5635(5) 0.0809(18) Uani 1 1 d . . . C3 C 0.6877(6) 0.2029(8) 0.8170(6) 0.0444(17) Uani 1 1 d . . . O3 O 0.6993(6) 0.0816(5) 0.8445(5) 0.0752(18) Uani 1 1 d . . . O4 O 0.6736(4) 0.6443(5) 0.7427(4) 0.0421(11) Uani 1 1 d . . . C11 C 0.8189(6) 0.4384(7) 1.0081(5) 0.0356(16) Uani 1 1 d . . . H11 H 0.8098 0.3358 1.0140 0.043 Uiso 1 1 calc R . . C12 C 0.8798(6) 0.5121(8) 1.0929(5) 0.0425(17) Uani 1 1 d . . . H12 H 0.9109 0.4606 1.1548 0.051 Uiso 1 1 calc R . . C13 C 0.8943(6) 0.6649(9) 1.0845(6) 0.052(2) Uani 1 1 d . . . H13 H 0.9370 0.7170 1.1403 0.062 Uiso 1 1 calc R . . C14 C 0.8450(6) 0.7391(7) 0.9931(6) 0.0442(18) Uani 1 1 d . . . H14 H 0.8520 0.8419 0.9866 0.053 Uiso 1 1 calc R . . C15 C 0.7849(6) 0.6558(7) 0.9113(5) 0.0348(15) Uani 1 1 d . . . C16 C 0.7283(7) 0.7213(8) 0.8121(6) 0.0445(18) Uani 1 1 d . . . H16 H 0.7336 0.8235 0.8010 0.053 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 Re1 0.03403(18) 0.02596(16) 0.03025(17) -0.00292(12) 0.00316(11) 0.00021(12) Br1 0.0410(4) 0.0454(4) 0.0407(4) -0.0033(3) 0.0100(3) 0.0007(3) N1 0.033(3) 0.025(3) 0.030(3) 0.000(2) 0.004(2) 0.001(2) C1 0.040(5) 0.025(3) 0.043(4) -0.004(3) -0.014(3) 0.001(3) O1 0.037(3) 0.072(4) 0.056(3) -0.007(3) 0.009(3) 0.000(3) C2 0.052(5) 0.052(5) 0.039(4) -0.007(4) 0.007(4) 0.000(4) O2 0.087(4) 0.102(5) 0.054(4) -0.024(3) -0.013(3) -0.016(4) C3 0.048(5) 0.033(4) 0.052(4) -0.009(4) 0.003(3) -0.005(3) O3 0.118(5) 0.024(3) 0.084(4) 0.001(3) 0.009(4) 0.005(3) O4 0.056(3) 0.025(2) 0.045(3) 0.004(2) 0.004(2) 0.005(2) C11 0.035(4) 0.033(4) 0.039(4) 0.000(3) 0.009(3) 0.002(3) C12 0.031(4) 0.063(5) 0.033(4) -0.005(4) -0.001(3) 0.005(4) C13 0.035(4) 0.066(5) 0.054(5) -0.026(4) 0.002(4) -0.006(4) C14 0.046(5) 0.034(4) 0.053(5) -0.015(4) 0.012(4) -0.007(3) C15 0.037(4) 0.031(3) 0.036(4) -0.004(3) 0.012(3) -0.003(3) C16 0.062(5) 0.020(3) 0.051(4) -0.002(4) 0.019(4) 0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.896(8) . ? Re1 C3 1.901(8) . ? Re1 C2 1.918(8) . ? Re1 O4 2.174(4) . ? Re1 N1 2.184(5) . ? Re1 Br1 2.6185(9) . ? N1 C11 1.333(8) . ? N1 C15 1.357(8) . ? C1 O1 1.156(8) . ? C2 O2 1.153(8) . ? C3 O3 1.145(8) . ? O4 C16 1.223(8) . ? C11 C12 1.369(9) . ? C12 C13 1.385(10) . ? C13 C14 1.379(9) . ? C14 C15 1.384(9) . ? C15 C16 1.448(9) . ? 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 C1 Re1 C3 89.6(3) . . ? C1 Re1 C2 88.5(3) . . ? C3 Re1 C2 89.1(3) . . ? C1 Re1 O4 92.6(2) . . ? C3 Re1 O4 172.9(2) . . ? C2 Re1 O4 97.7(3) . . ? C1 Re1 N1 92.5(2) . . ? C3 Re1 N1 98.7(2) . . ? C2 Re1 N1 172.2(2) . . ? O4 Re1 N1 74.47(18) . . ? C1 Re1 Br1 176.18(17) . . ? C3 Re1 Br1 93.9(2) . . ? C2 Re1 Br1 92.9(2) . . ? O4 Re1 Br1 83.64(12) . . ? N1 Re1 Br1 85.67(12) . . ? C11 N1 C15 117.2(5) . . ? C11 N1 Re1 128.3(4) . . ? C15 N1 Re1 114.5(4) . . ? O1 C1 Re1 178.7(6) . . ? O2 C2 Re1 177.6(6) . . ? O3 C3 Re1 178.0(7) . . ? C16 O4 Re1 116.0(4) . . ? N1 C11 C12 123.5(6) . . ? C11 C12 C13 118.7(7) . . ? C14 C13 C12 119.6(6) . . ? C13 C14 C15 117.9(6) . . ? N1 C15 C14 123.1(6) . . ? N1 C15 C16 113.9(6) . . ? C14 C15 C16 123.0(6) . . ? O4 C16 C15 121.1(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.760 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.130 #===END data_compound_1d_el6c _database_code_depnum_ccdc_archive 'CCDC 637221' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H12 Cl Mo N O3' _chemical_formula_weight 349.62 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' 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 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 14.421(9) _cell_length_b 9.983(6) _cell_length_c 9.449(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.949(11) _cell_angle_gamma 90.00 _cell_volume 1314.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.199 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.353906 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 5792 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 23.31 _reflns_number_total 1889 _reflns_number_gt 1636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1309P)^2^+1.9405P] 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 1889 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.1773 _refine_ls_wR_factor_gt 0.1651 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.26747(3) 1.00703(4) 0.10341(5) 0.0353(3) Uani 1 1 d . . . Cl1 Cl 0.18532(11) 0.78568(15) 0.09256(17) 0.0518(5) Uani 1 1 d . . . N1 N 0.1552(3) 1.0601(5) 0.2107(5) 0.0381(11) Uani 1 1 d . . . C1 C 0.1998(5) 1.0650(6) -0.0873(7) 0.0486(15) Uani 1 1 d . . . O1 O 0.1602(4) 1.1058(6) -0.1997(5) 0.0714(14) Uani 1 1 d . . . C2 C 0.3009(4) 1.1936(7) 0.1217(7) 0.0505(15) Uani 1 1 d . . . O2 O 0.3185(4) 1.3046(5) 0.1252(6) 0.0753(15) Uani 1 1 d . . . O3 O 0.3209(3) 0.9555(5) 0.3384(4) 0.0466(10) Uani 1 1 d . . . C3 C 0.4257(5) 1.0384(8) 0.1270(10) 0.0590(19) Uani 1 1 d . . . H3A H 0.4430 1.1042 0.0627 0.071 Uiso 1 1 calc R . . H3B H 0.4669 1.0400 0.2260 0.071 Uiso 1 1 calc R . . C4 C 0.3979(4) 0.9143(6) 0.0678(7) 0.0489(15) Uani 1 1 d . . . C5 C 0.3348(5) 0.9176(7) -0.0714(7) 0.0583(17) Uani 1 1 d . . . H5A H 0.3095 0.8324 -0.1136 0.070 Uiso 1 1 calc R . . H5B H 0.3498 0.9795 -0.1414 0.070 Uiso 1 1 calc R . . C6 C 0.4299(5) 0.7867(7) 0.1500(9) 0.0678(19) Uani 1 1 d . . . H6A H 0.4918 0.7617 0.1385 0.102 Uiso 1 1 calc R . . H6B H 0.3845 0.7169 0.1120 0.102 Uiso 1 1 calc R . . H6C H 0.4339 0.8000 0.2520 0.102 Uiso 1 1 calc R . . C11 C 0.0708(4) 1.1122(6) 0.1486(7) 0.0472(15) Uani 1 1 d . . . H11 H 0.0554 1.1288 0.0484 0.057 Uiso 1 1 calc R . . C12 C 0.0050(4) 1.1428(6) 0.2234(7) 0.0512(15) Uani 1 1 d . . . H12 H -0.0538 1.1798 0.1750 0.061 Uiso 1 1 calc R . . C13 C 0.0257(5) 1.1192(6) 0.3693(8) 0.0545(16) Uani 1 1 d . . . H13 H -0.0181 1.1403 0.4229 0.065 Uiso 1 1 calc R . . C14 C 0.1123(5) 1.0635(7) 0.4358(7) 0.0501(15) Uani 1 1 d . . . H14 H 0.1287 1.0456 0.5358 0.060 Uiso 1 1 calc R . . C15 C 0.1736(4) 1.0350(7) 0.3540(7) 0.0391(13) Uani 1 1 d . . . C16 C 0.2662(6) 0.9763(6) 0.4134(8) 0.0433(16) Uani 1 1 d . . . H16 H 0.2846 0.9538 0.5122 0.052 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 0.0431(5) 0.0227(5) 0.0416(5) 0.00065(16) 0.0133(3) -0.00034(16) Cl1 0.0608(10) 0.0304(9) 0.0637(10) -0.0019(6) 0.0149(8) -0.0102(6) N1 0.045(3) 0.023(3) 0.046(3) 0.000(2) 0.012(2) -0.001(2) C1 0.066(4) 0.033(4) 0.048(4) 0.002(3) 0.017(3) 0.001(3) O1 0.091(4) 0.069(4) 0.050(3) 0.008(2) 0.013(3) 0.009(3) C2 0.050(4) 0.033(4) 0.070(4) 0.004(3) 0.017(3) 0.000(3) O2 0.085(4) 0.027(3) 0.109(4) 0.000(3) 0.017(3) -0.003(2) O3 0.055(3) 0.032(2) 0.049(2) -0.001(2) 0.007(2) 0.003(2) C3 0.051(4) 0.038(4) 0.096(6) -0.007(4) 0.033(4) -0.004(3) C4 0.050(4) 0.034(3) 0.070(4) -0.003(3) 0.029(3) 0.004(3) C5 0.075(4) 0.047(4) 0.064(4) -0.004(3) 0.037(4) 0.005(3) C6 0.062(4) 0.044(4) 0.099(6) -0.001(4) 0.023(4) 0.003(3) C11 0.049(3) 0.040(4) 0.052(3) -0.004(3) 0.010(3) 0.002(3) C12 0.047(3) 0.042(4) 0.062(4) -0.002(3) 0.011(3) -0.001(3) C13 0.059(4) 0.042(4) 0.070(4) -0.011(3) 0.032(3) -0.007(3) C14 0.064(4) 0.040(4) 0.048(3) 0.001(3) 0.019(3) -0.006(3) C15 0.050(4) 0.029(3) 0.040(3) -0.001(3) 0.014(3) -0.002(3) C16 0.061(4) 0.033(3) 0.034(3) 0.000(2) 0.009(3) -0.002(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 C1 1.905(7) . ? Mo1 C2 1.920(7) . ? Mo1 N1 2.186(5) . ? Mo1 C4 2.199(6) . ? Mo1 O3 2.215(4) . ? Mo1 C3 2.257(7) . ? Mo1 C5 2.301(6) . ? Mo1 Cl1 2.4968(19) . ? N1 C11 1.314(8) . ? N1 C15 1.335(8) . ? C1 O1 1.143(8) . ? C2 O2 1.136(8) . ? O3 C16 1.206(8) . ? C3 C4 1.376(10) . ? C4 C5 1.393(10) . ? C4 C6 1.502(10) . ? C11 C12 1.356(8) . ? C12 C13 1.354(10) . ? C13 C14 1.363(10) . ? C14 C15 1.346(9) . ? C15 C16 1.433(11) . ? 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 C1 Mo1 C2 81.1(3) . . ? C1 Mo1 N1 96.0(2) . . ? C2 Mo1 N1 85.5(2) . . ? C1 Mo1 C4 103.4(3) . . ? C2 Mo1 C4 102.5(3) . . ? N1 Mo1 C4 159.8(2) . . ? C1 Mo1 O3 168.5(2) . . ? C2 Mo1 O3 96.9(2) . . ? N1 Mo1 O3 72.49(17) . . ? C4 Mo1 O3 88.0(2) . . ? C1 Mo1 C3 108.0(3) . . ? C2 Mo1 C3 68.4(3) . . ? N1 Mo1 C3 140.5(2) . . ? C4 Mo1 C3 35.9(3) . . ? O3 Mo1 C3 81.5(3) . . ? C1 Mo1 C5 69.3(3) . . ? C2 Mo1 C5 107.4(3) . . ? N1 Mo1 C5 158.0(2) . . ? C4 Mo1 C5 36.0(2) . . ? O3 Mo1 C5 121.8(2) . . ? C3 Mo1 C5 61.4(3) . . ? C1 Mo1 Cl1 96.2(2) . . ? C2 Mo1 Cl1 165.34(19) . . ? N1 Mo1 Cl1 80.40(13) . . ? C4 Mo1 Cl1 92.12(18) . . ? O3 Mo1 Cl1 82.77(13) . . ? C3 Mo1 Cl1 125.7(2) . . ? C5 Mo1 Cl1 84.87(19) . . ? C11 N1 C15 116.5(5) . . ? C11 N1 Mo1 126.9(4) . . ? C15 N1 Mo1 116.6(4) . . ? O1 C1 Mo1 176.8(6) . . ? O2 C2 Mo1 176.5(6) . . ? C16 O3 Mo1 116.0(4) . . ? C4 C3 Mo1 69.7(4) . . ? C3 C4 C5 114.5(7) . . ? C3 C4 C6 122.3(7) . . ? C5 C4 C6 123.2(6) . . ? C3 C4 Mo1 74.3(4) . . ? C5 C4 Mo1 76.0(4) . . ? C6 C4 Mo1 116.0(4) . . ? C4 C5 Mo1 68.0(3) . . ? N1 C11 C12 123.2(6) . . ? C13 C12 C11 119.4(6) . . ? C12 C13 C14 118.4(6) . . ? C15 C14 C13 118.7(6) . . ? N1 C15 C14 123.7(6) . . ? N1 C15 C16 113.3(6) . . ? C14 C15 C16 123.0(6) . . ? O3 C16 C15 121.6(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.867 _refine_diff_density_min -1.730 _refine_diff_density_rms 0.193 #===END data_Compound_2a_rg612am _database_code_depnum_ccdc_archive 'CCDC 637222' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 Br Mn N2 O5' _chemical_formula_weight 411.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 6.9586(17) _cell_length_b 7.8730(19) _cell_length_c 15.422(4) _cell_angle_alpha 94.524(5) _cell_angle_beta 102.427(5) _cell_angle_gamma 97.655(5) _cell_volume 812.7(3) _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 NEEDDLE _exptl_crystal_colour ORANGE_RED _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 3.292 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.556271 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 3717 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 23.30 _reflns_number_total 2334 _reflns_number_gt 1400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0848P)^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 2334 _refine_ls_number_parameters 200 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1550 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _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 Mn1 Mn -0.15894(18) 0.28165(15) 0.71545(8) 0.0422(4) Uani 1 1 d . . . Br1 Br -0.36535(16) -0.00998(13) 0.66769(8) 0.0763(5) Uani 1 1 d . . . N1 N -0.0972(10) 0.2719(8) 0.5894(4) 0.0401(17) Uani 1 1 d . . . N2 N 0.0830(10) 0.1559(8) 0.7323(5) 0.0424(17) Uani 1 1 d . . . C1 C -0.0060(15) 0.4894(13) 0.7530(6) 0.052(2) Uani 1 1 d . . . O1 O 0.0842(11) 0.6227(9) 0.7778(5) 0.075(2) Uani 1 1 d . . . C2 C -0.3702(16) 0.3913(12) 0.6865(6) 0.055(3) Uani 1 1 d . . . O2 O -0.5011(11) 0.4627(9) 0.6697(5) 0.077(2) Uani 1 1 d . . . C3 C -0.1994(16) 0.2650(12) 0.8254(8) 0.065(3) Uani 1 1 d . . . O3 O -0.2257(14) 0.2554(12) 0.8954(6) 0.100(3) Uani 1 1 d . . . C4 C 0.1669(14) 0.0781(11) 0.8125(6) 0.052(2) Uani 1 1 d . . . H4A H 0.2607 0.0051 0.7989 0.062 Uiso 1 1 calc R . . H4B H 0.0608 0.0060 0.8302 0.062 Uiso 1 1 calc R . . C5 C 0.2702(15) 0.2112(15) 0.8883(7) 0.062(3) Uani 1 1 d . . . O5 O 0.3051(14) 0.1399(10) 0.9620(5) 0.099(3) Uani 1 1 d . . . O6 O 0.3161(14) 0.3585(11) 0.8814(5) 0.107(3) Uani 1 1 d . . . C6 C 0.425(3) 0.251(2) 1.0420(9) 0.134(6) Uani 1 1 d . . . H6A H 0.5482 0.2081 1.0636 0.161 Uiso 1 1 calc R . . H6B H 0.4567 0.3676 1.0270 0.161 Uiso 1 1 calc R . . C7 C 0.326(4) 0.254(3) 1.1026(12) 0.240(15) Uani 1 1 d . . . H7A H 0.2544 0.1403 1.1024 0.361 Uiso 1 1 calc R . . H7B H 0.2328 0.3335 1.0913 0.361 Uiso 1 1 calc R . . H7C H 0.4152 0.2883 1.1598 0.361 Uiso 1 1 calc R . . C11 C -0.2042(14) 0.3172(11) 0.5154(7) 0.051(2) Uani 1 1 d . . . H11 H -0.3215 0.3601 0.5174 0.061 Uiso 1 1 calc R . . C12 C -0.1465(17) 0.3025(11) 0.4349(6) 0.059(3) Uani 1 1 d . . . H12 H -0.2266 0.3309 0.3832 0.071 Uiso 1 1 calc R . . C13 C 0.0285(16) 0.2461(11) 0.4325(7) 0.055(3) Uani 1 1 d . . . H13 H 0.0729 0.2407 0.3798 0.066 Uiso 1 1 calc R . . C14 C 0.1380(14) 0.1978(10) 0.5075(6) 0.049(2) Uani 1 1 d . . . H14 H 0.2573 0.1575 0.5065 0.058 Uiso 1 1 calc R . . C15 C 0.0714(12) 0.2088(10) 0.5857(6) 0.040(2) Uani 1 1 d . . . C16 C 0.1624(13) 0.1432(10) 0.6667(6) 0.043(2) Uani 1 1 d . . . H16 H 0.2770 0.0928 0.6703 0.052 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 Mn1 0.0387(8) 0.0372(8) 0.0520(9) -0.0043(6) 0.0150(6) 0.0082(6) Br1 0.0564(8) 0.0616(8) 0.1108(10) -0.0094(6) 0.0276(7) 0.0053(5) N1 0.038(4) 0.036(4) 0.043(4) -0.002(3) 0.006(4) 0.002(3) N2 0.038(4) 0.036(4) 0.050(4) -0.005(3) 0.008(4) 0.003(3) C1 0.061(7) 0.056(6) 0.045(5) -0.001(5) 0.019(5) 0.026(5) O1 0.089(6) 0.045(4) 0.081(5) -0.012(4) 0.015(4) -0.005(4) C2 0.056(7) 0.049(6) 0.060(6) -0.012(5) 0.025(5) 0.004(5) O2 0.051(5) 0.069(5) 0.109(6) -0.006(4) 0.011(4) 0.021(4) C3 0.063(7) 0.053(6) 0.078(8) -0.010(6) 0.018(6) 0.019(5) O3 0.127(8) 0.118(7) 0.078(6) 0.020(5) 0.056(6) 0.034(5) C4 0.051(6) 0.049(5) 0.057(6) 0.008(5) 0.005(5) 0.020(4) C5 0.052(7) 0.061(7) 0.070(8) -0.008(6) 0.011(6) 0.008(5) O5 0.147(8) 0.086(6) 0.047(4) 0.009(4) 0.000(5) -0.001(5) O6 0.129(8) 0.071(6) 0.085(6) 0.001(5) -0.033(5) -0.017(5) C6 0.186(19) 0.141(14) 0.060(9) -0.008(9) 0.009(10) 0.011(12) C7 0.39(4) 0.19(2) 0.132(16) -0.062(15) 0.16(2) -0.08(2) C11 0.041(6) 0.041(5) 0.064(7) -0.007(5) 0.008(5) -0.001(4) C12 0.081(8) 0.038(5) 0.049(6) 0.001(4) 0.004(6) -0.002(5) C13 0.072(8) 0.034(5) 0.061(7) -0.004(5) 0.025(6) 0.006(5) C14 0.049(6) 0.035(5) 0.064(6) -0.006(4) 0.022(5) 0.003(4) C15 0.033(5) 0.033(5) 0.054(6) -0.008(4) 0.012(4) 0.006(4) C16 0.033(5) 0.035(5) 0.057(6) -0.005(4) 0.006(5) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C3 1.789(12) . ? Mn1 C2 1.795(11) . ? Mn1 C1 1.807(11) . ? Mn1 N2 2.044(7) . ? Mn1 N1 2.076(7) . ? Mn1 Br1 2.5053(16) . ? N1 C11 1.325(11) . ? N1 C15 1.344(10) . ? N2 C16 1.257(10) . ? N2 C4 1.466(10) . ? C1 O1 1.140(11) . ? C2 O2 1.128(11) . ? C3 O3 1.140(11) . ? C4 C5 1.491(13) . ? C5 O6 1.180(12) . ? C5 O5 1.298(12) . ? O5 C6 1.476(14) . ? C6 C7 1.27(2) . ? C11 C12 1.385(13) . ? C12 C13 1.358(14) . ? C13 C14 1.353(12) . ? C14 C15 1.382(11) . ? C15 C16 1.441(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mn1 C2 91.1(4) . . ? C3 Mn1 C1 90.3(4) . . ? C2 Mn1 C1 88.4(4) . . ? C3 Mn1 N2 95.9(4) . . ? C2 Mn1 N2 173.0(4) . . ? C1 Mn1 N2 92.5(3) . . ? C3 Mn1 N1 172.7(4) . . ? C2 Mn1 N1 95.2(4) . . ? C1 Mn1 N1 93.5(3) . . ? N2 Mn1 N1 77.8(3) . . ? C3 Mn1 Br1 88.4(3) . . ? C2 Mn1 Br1 92.9(3) . . ? C1 Mn1 Br1 178.2(3) . . ? N2 Mn1 Br1 86.35(18) . . ? N1 Mn1 Br1 87.60(18) . . ? C11 N1 C15 118.6(7) . . ? C11 N1 Mn1 127.8(6) . . ? C15 N1 Mn1 113.5(6) . . ? C16 N2 C4 118.3(7) . . ? C16 N2 Mn1 115.8(6) . . ? C4 N2 Mn1 125.8(6) . . ? O1 C1 Mn1 177.2(8) . . ? O2 C2 Mn1 178.6(9) . . ? O3 C3 Mn1 179.5(10) . . ? N2 C4 C5 111.9(8) . . ? O6 C5 O5 125.5(10) . . ? O6 C5 C4 124.8(10) . . ? O5 C5 C4 109.8(9) . . ? C5 O5 C6 116.4(10) . . ? C7 C6 O5 109.4(17) . . ? N1 C11 C12 122.0(9) . . ? C13 C12 C11 119.0(9) . . ? C14 C13 C12 119.5(9) . . ? C13 C14 C15 119.5(9) . . ? N1 C15 C14 121.2(8) . . ? N1 C15 C16 114.0(8) . . ? C14 C15 C16 124.6(8) . . ? N2 C16 C15 118.3(8) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.769 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.146 #===END data_Compound_2b_esmngam _database_code_depnum_ccdc_archive 'CCDC 637223' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 Cl Mn N2 O5' _chemical_formula_weight 366.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mn Mn 0.3368 0.7283 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 18.262(7) _cell_length_b 10.629(4) _cell_length_c 16.641(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.685(8) _cell_angle_gamma 90.00 _cell_volume 3230(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour ORANGE_RED _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.860366 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6928 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2309 _reflns_number_gt 1859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0800P)^2^+127.0308P] 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 2309 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0966 _refine_ls_wR_factor_ref 0.2833 _refine_ls_wR_factor_gt 0.2774 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.33769(9) 0.23121(16) 0.67031(11) 0.0354(6) Uani 1 1 d . . . Cl1 Cl 0.20910(16) 0.2023(3) 0.6831(2) 0.0495(9) Uani 1 1 d . . . N1 N 0.3391(5) 0.2710(9) 0.7918(6) 0.036(2) Uani 1 1 d . . . N2 N 0.3507(6) 0.0551(9) 0.7201(6) 0.042(2) Uani 1 1 d . . . C1 C 0.4334(8) 0.2598(13) 0.6621(8) 0.055(3) Uani 1 1 d . . . O1 O 0.4952(5) 0.2846(12) 0.6522(8) 0.083(4) Uani 1 1 d . . . C2 C 0.3213(8) 0.3908(14) 0.6342(8) 0.052(3) Uani 1 1 d . . . O2 O 0.3116(7) 0.4897(10) 0.6093(7) 0.077(3) Uani 1 1 d . . . C3 C 0.3299(7) 0.1744(13) 0.5690(9) 0.049(3) Uani 1 1 d . . . O3 O 0.3257(7) 0.1354(11) 0.5046(7) 0.080(3) Uani 1 1 d . . . C4 C 0.3613(7) -0.0647(11) 0.6767(9) 0.049(3) Uani 1 1 d . . . H4A H 0.3491 -0.1337 0.7123 0.058 Uiso 1 1 calc R . . H4B H 0.3275 -0.0675 0.6313 0.058 Uiso 1 1 calc R . . C5 C 0.4352(9) -0.0835(17) 0.6476(13) 0.090(6) Uani 1 1 d . . . O5 O 0.4437(6) -0.1930(11) 0.6188(9) 0.095(4) Uani 1 1 d . . . C6 C 0.5147(12) -0.226(3) 0.578(2) 0.177(16) Uani 1 1 d . . . H6A H 0.5175 -0.1840 0.5264 0.212 Uiso 1 1 calc R . . H6B H 0.5561 -0.1993 0.6110 0.212 Uiso 1 1 calc R . . C7 C 0.5156(13) -0.359(2) 0.568(2) 0.179(16) Uani 1 1 d . . . H7A H 0.5055 -0.3991 0.6181 0.269 Uiso 1 1 calc R . . H7B H 0.5629 -0.3847 0.5494 0.269 Uiso 1 1 calc R . . H7C H 0.4789 -0.3826 0.5288 0.269 Uiso 1 1 calc R . . C11 C 0.3325(6) 0.3834(11) 0.8271(7) 0.040(3) Uani 1 1 d . . . H11 H 0.3287 0.4548 0.7951 0.048 Uiso 1 1 calc R . . C12 C 0.3313(7) 0.3964(12) 0.9093(8) 0.049(3) Uani 1 1 d . . . H12 H 0.3284 0.4760 0.9322 0.058 Uiso 1 1 calc R . . C13 C 0.3345(7) 0.2902(14) 0.9581(9) 0.056(4) Uani 1 1 d . . . H13 H 0.3318 0.2972 1.0137 0.067 Uiso 1 1 calc R . . C14 C 0.3416(7) 0.1783(14) 0.9231(8) 0.053(3) Uani 1 1 d . . . H14 H 0.3461 0.1060 0.9543 0.063 Uiso 1 1 calc R . . C15 C 0.3421(6) 0.1702(11) 0.8394(7) 0.038(3) Uani 1 1 d . . . C16 C 0.3505(7) 0.0530(11) 0.7966(8) 0.044(3) Uani 1 1 d . . . H16 H 0.3558 -0.0224 0.8244 0.053 Uiso 1 1 calc R . . O4A O 0.4821(13) 0.006(2) 0.636(2) 0.121(11) Uani 0.60 1 d P . . O4B O 0.4902(17) -0.058(3) 0.699(2) 0.093(11) Uani 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0356(10) 0.0316(10) 0.0392(10) 0.0022(8) 0.0003(7) 0.0009(8) Cl1 0.0384(16) 0.0393(17) 0.071(2) -0.0042(15) -0.0049(15) 0.0002(13) N1 0.036(5) 0.030(5) 0.042(5) 0.002(5) 0.003(4) 0.002(4) N2 0.047(6) 0.033(5) 0.045(7) 0.002(5) 0.002(5) 0.009(5) C1 0.058(9) 0.052(8) 0.055(8) 0.001(7) 0.011(7) 0.001(7) O1 0.036(6) 0.100(9) 0.111(10) -0.006(7) 0.001(6) 0.000(6) C2 0.059(9) 0.053(9) 0.044(8) 0.000(7) 0.007(6) -0.007(7) O2 0.112(9) 0.045(6) 0.073(7) 0.027(5) -0.001(6) 0.008(6) C3 0.049(8) 0.054(8) 0.043(8) 0.011(7) 0.000(6) 0.005(6) O3 0.110(9) 0.074(8) 0.057(7) -0.011(6) -0.012(6) 0.006(7) C4 0.045(8) 0.033(7) 0.067(9) -0.007(6) -0.006(7) 0.005(6) C5 0.063(11) 0.067(12) 0.138(17) -0.058(12) -0.013(11) 0.002(9) O5 0.066(7) 0.082(8) 0.137(12) -0.051(8) 0.013(7) 0.009(6) C6 0.077(15) 0.19(3) 0.26(4) -0.14(3) 0.057(19) 0.011(17) C7 0.084(16) 0.078(15) 0.38(5) -0.05(2) 0.01(2) 0.038(13) C11 0.041(7) 0.033(7) 0.046(7) -0.004(5) -0.008(6) 0.000(5) C12 0.055(8) 0.040(7) 0.050(8) -0.014(6) -0.003(6) 0.007(6) C13 0.047(8) 0.074(10) 0.047(8) -0.020(8) 0.002(6) -0.009(7) C14 0.057(8) 0.060(9) 0.041(8) 0.012(7) 0.003(6) -0.008(7) C15 0.038(7) 0.034(6) 0.042(7) 0.004(5) -0.006(5) 0.002(5) C16 0.045(7) 0.032(7) 0.055(9) 0.008(6) 0.005(6) 0.001(5) O4A 0.074(15) 0.051(13) 0.24(4) -0.028(17) 0.052(19) -0.007(12) O4B 0.06(2) 0.08(2) 0.14(3) -0.03(2) -0.01(2) 0.015(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 C1 1.780(15) . ? Mn1 C3 1.795(15) . ? Mn1 C2 1.823(15) . ? Mn1 N2 2.060(10) . ? Mn1 N1 2.066(10) . ? Mn1 Cl1 2.381(4) . ? N1 C15 1.334(15) . ? N1 C11 1.336(15) . ? N2 C16 1.274(16) . ? N2 C4 1.478(15) . ? C1 O1 1.173(16) . ? C2 O2 1.143(16) . ? C3 O3 1.151(16) . ? C4 C5 1.45(2) . ? C5 O5 1.269(18) . ? C5 O4A 1.29(3) . ? C5 O4B 1.34(4) . ? O5 C6 1.51(2) . ? C6 C7 1.42(3) . ? C11 C12 1.375(18) . ? C12 C13 1.39(2) . ? C13 C14 1.331(19) . ? C14 C15 1.396(18) . ? C15 C16 1.443(17) . ? O4A O4B 1.25(4) . ? O4B O4B 1.74(8) 2_656 ? 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 C1 Mn1 C3 93.0(6) . . ? C1 Mn1 C2 88.5(6) . . ? C3 Mn1 C2 89.6(6) . . ? C1 Mn1 N2 94.4(5) . . ? C3 Mn1 N2 94.5(5) . . ? C2 Mn1 N2 174.8(5) . . ? C1 Mn1 N1 92.3(5) . . ? C3 Mn1 N1 171.2(5) . . ? C2 Mn1 N1 97.6(5) . . ? N2 Mn1 N1 78.0(4) . . ? C1 Mn1 Cl1 177.5(5) . . ? C3 Mn1 Cl1 88.5(4) . . ? C2 Mn1 Cl1 89.5(4) . . ? N2 Mn1 Cl1 87.5(3) . . ? N1 Mn1 Cl1 86.5(3) . . ? C15 N1 C11 117.4(10) . . ? C15 N1 Mn1 114.6(8) . . ? C11 N1 Mn1 127.8(8) . . ? C16 N2 C4 118.4(11) . . ? C16 N2 Mn1 114.6(8) . . ? C4 N2 Mn1 127.0(8) . . ? O1 C1 Mn1 175.1(13) . . ? O2 C2 Mn1 177.9(13) . . ? O3 C3 Mn1 178.4(13) . . ? C5 C4 N2 114.2(11) . . ? O5 C5 O4A 122.2(19) . . ? O5 C5 O4B 109(2) . . ? O4A C5 O4B 57(2) . . ? O5 C5 C4 111.7(15) . . ? O4A C5 C4 124.6(16) . . ? O4B C5 C4 117(2) . . ? C5 O5 C6 119.3(17) . . ? C7 C6 O5 107(2) . . ? N1 C11 C12 122.0(11) . . ? C11 C12 C13 119.9(12) . . ? C14 C13 C12 118.2(13) . . ? C13 C14 C15 119.6(13) . . ? N1 C15 C14 122.8(11) . . ? N1 C15 C16 113.8(10) . . ? C14 C15 C16 123.2(11) . . ? N2 C16 C15 118.7(11) . . ? O4B O4A C5 63(2) . . ? O4A O4B C5 60(2) . . ? O4A O4B O4B 147(2) . 2_656 ? C5 O4B O4B 140(4) . 2_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.993 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.143 #===END data_Compound_2d_rg227am _database_code_depnum_ccdc_archive 'CCDC 637224' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H19 Cl Mo N2 O4' _chemical_formula_weight 434.72 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' 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 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 10.372(5) _cell_length_b 9.448(5) _cell_length_c 18.500(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.479(9) _cell_angle_gamma 90.00 _cell_volume 1793.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description NEEDDLE _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747483 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 7809 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.31 _reflns_number_total 2589 _reflns_number_gt 1953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0792P)^2^+3.4359P] 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 2589 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1570 _refine_ls_wR_factor_gt 0.1479 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _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 0.19904(7) 0.18488(7) 0.41440(4) 0.0317(3) Uani 1 1 d . . . Cl1 Cl 0.1596(2) 0.2188(2) 0.54358(11) 0.0424(6) Uani 1 1 d . . . N1 N -0.0122(6) 0.2359(7) 0.3925(3) 0.0319(16) Uani 1 1 d . . . N2 N 0.1807(7) 0.4212(7) 0.4177(3) 0.0379(17) Uani 1 1 d . . . C1 C 0.1987(9) -0.0225(9) 0.4334(4) 0.043(2) Uani 1 1 d . . . O1 O 0.2004(7) -0.1395(7) 0.4455(4) 0.069(2) Uani 1 1 d . . . C2 C 0.3862(10) 0.1634(9) 0.4511(5) 0.044(2) Uani 1 1 d . . . O2 O 0.4968(7) 0.1542(8) 0.4725(4) 0.076(2) Uani 1 1 d . . . C3 C 0.1523(10) 0.0578(10) 0.3065(5) 0.055(3) Uani 1 1 d . . . H3A H 0.2106 -0.0196 0.2995 0.066 Uiso 1 1 calc R . . H3B H 0.0612 0.0372 0.2897 0.066 Uiso 1 1 calc R . . C4 C 0.1958(10) 0.1955(9) 0.2931(4) 0.044(2) Uani 1 1 d . . . C5 C 0.3235(9) 0.2271(9) 0.3235(4) 0.044(2) Uani 1 1 d . . . H5A H 0.3522 0.3238 0.3183 0.053 Uiso 1 1 calc R . . H5B H 0.3892 0.1569 0.3172 0.053 Uiso 1 1 calc R . . C6 C 0.1052(11) 0.2978(11) 0.2475(5) 0.062(3) Uani 1 1 d . . . H6A H 0.1218 0.3922 0.2657 0.093 Uiso 1 1 calc R . . H6B H 0.0164 0.2728 0.2504 0.093 Uiso 1 1 calc R . . H6C H 0.1200 0.2933 0.1975 0.093 Uiso 1 1 calc R . . C7 C 0.3376(10) 0.5830(9) 0.3723(5) 0.046(2) Uani 1 1 d . . . O3 O 0.2701(8) 0.6077(8) 0.3158(4) 0.081(2) Uani 1 1 d . . . O4 O 0.4644(6) 0.6135(7) 0.3872(4) 0.0557(17) Uani 1 1 d . . . C8 C 0.5220(11) 0.6850(11) 0.3317(6) 0.070(3) Uani 1 1 d . . . H8A H 0.4843 0.6486 0.2843 0.085 Uiso 1 1 calc R . . H8B H 0.6147 0.6651 0.3385 0.085 Uiso 1 1 calc R . . C9 C 0.5022(11) 0.8400(10) 0.3330(6) 0.066(3) Uani 1 1 d . . . H9A H 0.4106 0.8606 0.3233 0.099 Uiso 1 1 calc R . . H9B H 0.5453 0.8835 0.2962 0.099 Uiso 1 1 calc R . . H9C H 0.5378 0.8764 0.3801 0.099 Uiso 1 1 calc R . . C11 C -0.1092(9) 0.1422(9) 0.3835(4) 0.042(2) Uani 1 1 d . . . H11 H -0.0893 0.0463 0.3836 0.050 Uiso 1 1 calc R . . C12 C -0.2396(9) 0.1832(11) 0.3740(5) 0.056(3) Uani 1 1 d . . . H12 H -0.3053 0.1154 0.3682 0.067 Uiso 1 1 calc R . . C13 C -0.2701(10) 0.3227(11) 0.3733(5) 0.058(3) Uani 1 1 d . . . H13 H -0.3566 0.3521 0.3657 0.069 Uiso 1 1 calc R . . C14 C -0.1714(9) 0.4186(10) 0.3839(5) 0.047(2) Uani 1 1 d . . . H14 H -0.1899 0.5150 0.3840 0.057 Uiso 1 1 calc R . . C15 C -0.0478(8) 0.3741(8) 0.3942(4) 0.0324(19) Uani 1 1 d . . . C16 C 0.0634(9) 0.4701(8) 0.4084(4) 0.039(2) Uani 1 1 d . . . H16 H 0.0495 0.5671 0.4108 0.047 Uiso 1 1 calc R . . C17 C 0.2881(9) 0.5197(9) 0.4378(4) 0.042(2) Uani 1 1 d . . . H17A H 0.3590 0.4705 0.4675 0.050 Uiso 1 1 calc R . . H17B H 0.2593 0.5953 0.4671 0.050 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 0.0381(5) 0.0273(4) 0.0313(4) -0.0001(3) 0.0104(3) 0.0044(4) Cl1 0.0603(15) 0.0382(12) 0.0310(11) 0.0010(9) 0.0140(10) 0.0003(10) N1 0.028(4) 0.030(4) 0.037(4) 0.000(3) 0.003(3) 0.002(3) N2 0.046(5) 0.037(4) 0.034(4) 0.005(3) 0.020(3) -0.001(4) C1 0.053(6) 0.034(5) 0.044(5) 0.010(4) 0.013(5) 0.009(4) O1 0.092(6) 0.030(4) 0.086(5) 0.007(4) 0.014(4) 0.011(4) C2 0.049(6) 0.043(5) 0.043(5) -0.001(4) 0.013(5) 0.013(5) O2 0.039(4) 0.099(6) 0.088(5) -0.007(4) 0.002(4) 0.020(4) C3 0.063(7) 0.057(6) 0.045(5) -0.016(5) 0.012(5) 0.013(5) C4 0.068(7) 0.047(5) 0.020(4) -0.006(4) 0.015(4) 0.003(5) C5 0.052(6) 0.051(6) 0.036(5) 0.001(4) 0.028(5) 0.008(5) C6 0.080(8) 0.076(7) 0.030(5) 0.006(5) 0.011(5) 0.024(6) C7 0.057(7) 0.033(5) 0.048(6) -0.005(4) 0.012(5) -0.011(5) O3 0.089(6) 0.093(6) 0.056(4) 0.030(4) -0.004(4) -0.041(5) O4 0.050(4) 0.050(4) 0.071(4) 0.005(3) 0.021(4) -0.006(3) C8 0.067(7) 0.062(7) 0.092(8) -0.006(6) 0.045(6) -0.016(6) C9 0.084(8) 0.049(6) 0.070(7) 0.017(5) 0.030(6) 0.010(6) C11 0.055(6) 0.033(5) 0.040(5) -0.002(4) 0.013(4) 0.000(4) C12 0.045(6) 0.065(7) 0.058(6) -0.006(5) 0.008(5) -0.021(6) C13 0.042(6) 0.074(8) 0.054(6) -0.010(6) -0.001(5) 0.018(6) C14 0.053(6) 0.042(5) 0.048(5) -0.008(4) 0.009(5) 0.011(5) C15 0.033(5) 0.027(4) 0.038(4) -0.002(4) 0.008(4) 0.005(4) C16 0.058(6) 0.025(4) 0.039(5) 0.005(4) 0.017(5) 0.011(4) C17 0.053(6) 0.035(5) 0.041(5) -0.002(4) 0.016(4) -0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.970(10) . ? Mo1 C1 1.991(9) . ? Mo1 N1 2.221(7) . ? Mo1 C4 2.242(7) . ? Mo1 N2 2.243(7) . ? Mo1 C5 2.301(8) . ? Mo1 C3 2.319(8) . ? Mo1 Cl1 2.504(2) . ? N1 C11 1.333(10) . ? N1 C15 1.359(10) . ? N2 C16 1.289(10) . ? N2 C17 1.456(10) . ? C1 O1 1.128(10) . ? C2 O2 1.161(10) . ? C3 C4 1.411(12) . ? C4 C5 1.393(13) . ? C4 C6 1.515(12) . ? C7 O3 1.192(10) . ? C7 O4 1.335(11) . ? C7 C17 1.506(12) . ? O4 C8 1.431(11) . ? C8 C9 1.479(13) . ? C11 C12 1.393(13) . ? C12 C13 1.354(13) . ? C13 C14 1.360(13) . ? C14 C15 1.336(11) . ? C15 C16 1.460(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 82.2(4) . . ? C2 Mo1 N1 168.6(3) . . ? C1 Mo1 N1 102.6(3) . . ? C2 Mo1 C4 102.6(4) . . ? C1 Mo1 C4 102.7(3) . . ? N1 Mo1 C4 86.5(3) . . ? C2 Mo1 N2 100.2(3) . . ? C1 Mo1 N2 166.6(3) . . ? N1 Mo1 N2 72.7(2) . . ? C4 Mo1 N2 89.6(3) . . ? C2 Mo1 C5 68.9(3) . . ? C1 Mo1 C5 108.4(3) . . ? N1 Mo1 C5 118.3(3) . . ? C4 Mo1 C5 35.7(3) . . ? N2 Mo1 C5 84.6(3) . . ? C2 Mo1 C3 108.3(3) . . ? C1 Mo1 C3 68.7(3) . . ? N1 Mo1 C3 83.1(3) . . ? C4 Mo1 C3 36.0(3) . . ? N2 Mo1 C3 122.1(3) . . ? C5 Mo1 C3 61.9(3) . . ? C2 Mo1 Cl1 88.6(2) . . ? C1 Mo1 Cl1 87.3(2) . . ? N1 Mo1 Cl1 81.39(17) . . ? C4 Mo1 Cl1 165.8(2) . . ? N2 Mo1 Cl1 79.65(16) . . ? C5 Mo1 Cl1 149.7(2) . . ? C3 Mo1 Cl1 147.7(3) . . ? C11 N1 C15 116.0(7) . . ? C11 N1 Mo1 125.8(6) . . ? C15 N1 Mo1 118.0(5) . . ? C16 N2 C17 118.5(7) . . ? C16 N2 Mo1 115.8(6) . . ? C17 N2 Mo1 125.3(6) . . ? O1 C1 Mo1 178.5(9) . . ? O2 C2 Mo1 178.3(8) . . ? C4 C3 Mo1 69.0(5) . . ? C5 C4 C3 115.9(8) . . ? C5 C4 C6 124.3(9) . . ? C3 C4 C6 119.9(9) . . ? C5 C4 Mo1 74.5(5) . . ? C3 C4 Mo1 75.0(5) . . ? C6 C4 Mo1 120.2(6) . . ? C4 C5 Mo1 69.8(5) . . ? O3 C7 O4 124.9(9) . . ? O3 C7 C17 123.8(9) . . ? O4 C7 C17 111.2(8) . . ? C7 O4 C8 117.2(8) . . ? O4 C8 C9 112.5(8) . . ? N1 C11 C12 122.2(8) . . ? C13 C12 C11 119.5(9) . . ? C12 C13 C14 118.5(9) . . ? C15 C14 C13 119.8(9) . . ? C14 C15 N1 123.9(8) . . ? C14 C15 C16 123.1(8) . . ? N1 C15 C16 113.0(7) . . ? N2 C16 C15 120.4(7) . . ? N2 C17 C7 112.8(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.040 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.119 #===END data_Compound_3a_rg263am _database_code_depnum_ccdc_archive 'CCDC 637225' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H5 Cl Mn N O8' _chemical_formula_weight 345.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Mn Mn 0.3368 0.7283 '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 11.206(5) _cell_length_b 7.084(3) _cell_length_c 16.026(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.857(8) _cell_angle_gamma 90.00 _cell_volume 1257.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour 'DARK RED' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 1.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747138 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5364 _diffrn_reflns_av_R_equivalents 0.0184 _diffrn_reflns_av_sigmaI/netI 0.0139 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 23.27 _reflns_number_total 1809 _reflns_number_gt 1678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0371P)^2^+0.9701P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1809 _refine_ls_number_parameters 182 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Mn1 Mn 0.33980(3) 0.31963(6) 0.57825(2) 0.04579(19) Uani 1 1 d . . . N1 N 0.23950(17) 0.1271(3) 0.50322(12) 0.0384(5) Uani 1 1 d . . . C1 C 0.4794(3) 0.2123(5) 0.56578(19) 0.0581(8) Uani 1 1 d . . . O1 O 0.5692(2) 0.1432(4) 0.56113(17) 0.0826(8) Uani 1 1 d . . . C2 C 0.4237(3) 0.5172(6) 0.6285(2) 0.0732(10) Uani 1 1 d . . . O2 O 0.4806(3) 0.6400(5) 0.6565(2) 0.1201(13) Uani 1 1 d . . . C3 C 0.3488(3) 0.1947(6) 0.6761(2) 0.0650(9) Uani 1 1 d . . . O3 O 0.3581(2) 0.1104(5) 0.73695(16) 0.1042(10) Uani 1 1 d . . . O4 O 0.32010(17) 0.4505(3) 0.46394(12) 0.0508(5) Uani 1 1 d . . . C11 C 0.1958(2) -0.0365(4) 0.52315(18) 0.0505(7) Uani 1 1 d . . . H11 H 0.2107 -0.0761 0.5791 0.061 Uiso 1 1 calc R . . C12 C 0.1295(3) -0.1505(4) 0.4647(2) 0.0605(8) Uani 1 1 d . . . H12 H 0.0997 -0.2648 0.4813 0.073 Uiso 1 1 calc R . . C13 C 0.1070(3) -0.0971(4) 0.3826(2) 0.0600(8) Uani 1 1 d . . . H13 H 0.0629 -0.1744 0.3422 0.072 Uiso 1 1 calc R . . C14 C 0.1503(2) 0.0721(4) 0.36059(17) 0.0507(7) Uani 1 1 d . . . H14 H 0.1363 0.1130 0.3048 0.061 Uiso 1 1 calc R . . C15 C 0.2146(2) 0.1804(4) 0.42182(15) 0.0385(6) Uani 1 1 d . . . C16 C 0.2622(2) 0.3633(4) 0.40661(18) 0.0473(7) Uani 1 1 d . . . H16 H 0.2484 0.4148 0.3526 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.12558(6) 0.50816(9) 0.65456(4) 0.0452(2) Uani 1 1 d . . . O11 O 0.17301(16) 0.4378(3) 0.58061(11) 0.0508(5) Uani 1 1 d . . . O12 O 0.1350(2) 0.3683(3) 0.71679(15) 0.0766(7) Uani 1 1 d . . . O13 O 0.1946(3) 0.6646(3) 0.68614(16) 0.0840(8) Uani 1 1 d . . . O14 O 0.0048(2) 0.5568(4) 0.62692(16) 0.0799(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 Mn1 0.0356(3) 0.0643(3) 0.0377(3) -0.00821(19) 0.00648(17) 0.00386(19) N1 0.0362(11) 0.0436(13) 0.0371(11) 0.0023(10) 0.0108(9) 0.0103(9) C1 0.0433(17) 0.077(2) 0.0537(17) -0.0112(16) 0.0067(13) 0.0005(16) O1 0.0437(13) 0.105(2) 0.1006(19) -0.0204(15) 0.0153(11) 0.0160(13) C2 0.0490(18) 0.113(3) 0.060(2) -0.034(2) 0.0138(15) -0.007(2) O2 0.0859(19) 0.163(3) 0.116(2) -0.083(2) 0.0302(17) -0.056(2) C3 0.0426(16) 0.106(3) 0.0443(18) -0.0016(18) 0.0012(13) 0.0197(17) O3 0.0809(17) 0.174(3) 0.0559(15) 0.0364(18) 0.0037(12) 0.0360(19) O4 0.0544(11) 0.0501(11) 0.0501(11) -0.0047(10) 0.0152(9) -0.0079(9) C11 0.0549(16) 0.0489(17) 0.0492(16) 0.0112(14) 0.0130(13) 0.0094(14) C12 0.0693(19) 0.0405(16) 0.074(2) 0.0036(16) 0.0170(16) -0.0025(15) C13 0.0679(19) 0.0508(18) 0.0593(19) -0.0098(15) 0.0037(15) -0.0057(15) C14 0.0556(16) 0.0563(18) 0.0390(15) -0.0023(13) 0.0032(12) 0.0035(14) C15 0.0377(13) 0.0422(15) 0.0366(14) 0.0002(11) 0.0093(10) 0.0085(11) C16 0.0497(16) 0.0514(17) 0.0427(15) 0.0050(14) 0.0137(13) 0.0025(13) Cl1 0.0478(4) 0.0469(4) 0.0438(4) -0.0027(3) 0.0163(3) 0.0033(3) O11 0.0460(10) 0.0692(13) 0.0372(9) -0.0118(9) 0.0057(8) 0.0141(9) O12 0.0800(15) 0.0791(16) 0.0801(16) 0.0321(13) 0.0419(12) 0.0178(13) O13 0.111(2) 0.0704(16) 0.0752(16) -0.0313(13) 0.0290(14) -0.0265(14) O14 0.0571(13) 0.0987(18) 0.0865(16) -0.0017(14) 0.0188(12) 0.0341(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 Mn1 C1 1.778(3) . ? Mn1 C3 1.790(4) . ? Mn1 C2 1.805(4) . ? Mn1 O4 2.035(2) . ? Mn1 N1 2.038(2) . ? Mn1 O11 2.0536(19) . ? N1 C11 1.317(4) . ? N1 C15 1.345(3) . ? C1 O1 1.131(4) . ? C2 O2 1.130(4) . ? C3 O3 1.134(4) . ? O4 C16 1.210(3) . ? C11 C12 1.367(4) . ? C12 C13 1.355(4) . ? C13 C14 1.360(4) . ? C14 C15 1.361(4) . ? C15 C16 1.436(4) . ? Cl1 O12 1.398(2) . ? Cl1 O13 1.401(2) . ? Cl1 O14 1.401(2) . ? Cl1 O11 1.4593(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 C1 Mn1 C3 87.43(14) . . ? C1 Mn1 C2 88.58(15) . . ? C3 Mn1 C2 92.11(17) . . ? C1 Mn1 O4 93.96(12) . . ? C3 Mn1 O4 176.20(12) . . ? C2 Mn1 O4 91.46(14) . . ? C1 Mn1 N1 93.57(12) . . ? C3 Mn1 N1 97.93(13) . . ? C2 Mn1 N1 169.81(14) . . ? O4 Mn1 N1 78.47(8) . . ? C1 Mn1 O11 174.47(11) . . ? C3 Mn1 O11 96.55(11) . . ? C2 Mn1 O11 95.09(12) . . ? O4 Mn1 O11 81.83(8) . . ? N1 Mn1 O11 82.11(8) . . ? C11 N1 C15 116.9(2) . . ? C11 N1 Mn1 129.63(19) . . ? C15 N1 Mn1 113.43(17) . . ? O1 C1 Mn1 177.3(3) . . ? O2 C2 Mn1 175.9(3) . . ? O3 C3 Mn1 177.0(3) . . ? C16 O4 Mn1 114.97(18) . . ? N1 C11 C12 122.5(3) . . ? C13 C12 C11 120.1(3) . . ? C12 C13 C14 118.5(3) . . ? C13 C14 C15 118.7(3) . . ? N1 C15 C14 123.3(2) . . ? N1 C15 C16 113.0(2) . . ? C14 C15 C16 123.7(2) . . ? O4 C16 C15 120.1(3) . . ? O12 Cl1 O13 109.03(17) . . ? O12 Cl1 O14 111.30(16) . . ? O13 Cl1 O14 111.88(17) . . ? O12 Cl1 O11 109.89(14) . . ? O13 Cl1 O11 108.28(14) . . ? O14 Cl1 O11 106.39(13) . . ? Cl1 O11 Mn1 126.90(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.289 _refine_diff_density_min -0.250 _refine_diff_density_rms 0.045 #===END data_Compound_3c_rg412am _database_code_depnum_ccdc_archive 'CCDC 637226' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H5 F3 N O7 Re S' _chemical_formula_weight 526.41 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 8.547(7) _cell_length_b 8.892(7) _cell_length_c 10.399(9) _cell_angle_alpha 70.449(14) _cell_angle_beta 72.368(15) _cell_angle_gamma 74.795(16) _cell_volume 698.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 8.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.453241 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 3158 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 23.52 _reflns_number_total 2008 _reflns_number_gt 1694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1794P)^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 2008 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2266 _refine_ls_wR_factor_gt 0.2182 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _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 Re1 Re 0.74210(9) 0.76032(10) 0.84825(7) 0.0307(5) Uani 1 1 d . . . N1 N 0.662(2) 0.741(2) 0.6755(19) 0.034(4) Uani 1 1 d . . . C1 C 0.697(3) 0.556(3) 0.965(2) 0.036(5) Uani 1 1 d . . . O1 O 0.668(3) 0.432(2) 1.042(2) 0.063(6) Uani 1 1 d . . . C2 C 0.780(3) 0.792(3) 1.005(3) 0.045(6) Uani 1 1 d . . . O2 O 0.792(3) 0.803(2) 1.112(2) 0.065(6) Uani 1 1 d . . . C3 C 0.975(3) 0.656(3) 0.808(2) 0.038(6) Uani 1 1 d . . . O3 O 1.102(2) 0.593(2) 0.780(2) 0.057(5) Uani 1 1 d . . . O4 O 0.4845(16) 0.8835(18) 0.8705(14) 0.031(3) Uani 1 1 d . . . C11 C 0.750(3) 0.675(3) 0.574(2) 0.034(5) Uani 1 1 d . . . H11 H 0.8614 0.6306 0.5727 0.041 Uiso 1 1 calc R . . C12 C 0.690(4) 0.668(4) 0.473(3) 0.079(11) Uani 1 1 d . . . H12 H 0.7602 0.6250 0.4017 0.095 Uiso 1 1 calc R . . C13 C 0.520(3) 0.727(3) 0.475(2) 0.046(6) Uani 1 1 d . . . H13 H 0.4732 0.7143 0.4100 0.055 Uiso 1 1 calc R . . C14 C 0.428(3) 0.802(3) 0.575(2) 0.040(5) Uani 1 1 d . . . H14 H 0.3166 0.8486 0.5768 0.048 Uiso 1 1 calc R . . C15 C 0.500(3) 0.809(3) 0.672(2) 0.032(5) Uani 1 1 d . . . C16 C 0.413(3) 0.885(3) 0.787(2) 0.036(5) Uani 1 1 d . . . H16 H 0.3012 0.9348 0.7941 0.043 Uiso 1 1 calc R . . C10 C 0.823(3) 1.221(3) 0.788(3) 0.050(6) Uani 1 1 d . . . O11 O 0.7690(19) 1.0004(19) 0.7092(17) 0.040(4) Uani 1 1 d . . . O12 O 1.0550(19) 1.016(2) 0.6851(16) 0.053(5) Uani 1 1 d . . . O13 O 0.889(2) 1.219(2) 0.5330(17) 0.057(5) Uani 1 1 d . . . S1 S 0.8969(7) 1.1027(7) 0.6638(5) 0.0339(13) Uani 1 1 d . . . F1 F 0.669(2) 1.294(2) 0.796(2) 0.074(5) Uani 1 1 d . . . F2 F 0.838(2) 1.1270(19) 0.9175(14) 0.058(4) Uani 1 1 d . . . F3 F 0.9162(19) 1.3357(18) 0.7516(16) 0.059(4) 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 Re1 0.0403(6) 0.0417(7) 0.0110(6) -0.0035(4) -0.0074(4) -0.0121(4) N1 0.027(9) 0.039(11) 0.026(10) -0.002(8) 0.000(7) -0.003(8) C1 0.048(12) 0.048(14) 0.005(10) 0.004(9) -0.010(9) -0.005(10) O1 0.091(14) 0.054(12) 0.043(11) 0.016(10) -0.032(10) -0.030(10) C2 0.074(17) 0.037(13) 0.033(14) -0.001(10) -0.030(12) -0.013(12) O2 0.121(17) 0.047(11) 0.034(10) 0.001(8) -0.040(11) -0.018(11) C3 0.024(11) 0.046(14) 0.026(12) 0.008(10) -0.004(9) -0.003(10) O3 0.044(11) 0.070(13) 0.056(12) -0.020(10) -0.017(9) 0.001(9) O4 0.024(7) 0.045(9) 0.014(7) -0.002(6) -0.003(6) -0.002(6) C11 0.045(12) 0.038(13) 0.016(11) -0.007(9) -0.001(9) -0.007(10) C12 0.09(2) 0.07(2) 0.06(2) -0.032(16) -0.041(18) 0.051(18) C13 0.047(13) 0.061(16) 0.036(14) -0.016(12) -0.016(11) -0.008(12) C14 0.041(12) 0.053(15) 0.028(13) -0.011(11) -0.014(10) -0.004(11) C15 0.042(12) 0.041(12) 0.011(10) -0.001(8) -0.004(9) -0.014(10) C16 0.046(12) 0.034(13) 0.030(12) -0.015(10) -0.013(10) 0.000(10) C10 0.060(16) 0.056(16) 0.031(14) -0.008(11) -0.008(11) -0.016(13) O11 0.042(8) 0.043(9) 0.032(9) -0.004(7) -0.012(7) -0.009(7) O12 0.044(9) 0.087(13) 0.024(9) -0.016(8) -0.007(7) -0.004(9) O13 0.079(12) 0.066(12) 0.021(9) 0.014(8) -0.016(8) -0.031(10) S1 0.040(3) 0.047(3) 0.015(3) -0.007(2) -0.002(2) -0.015(2) F1 0.054(9) 0.085(13) 0.093(14) -0.056(11) -0.012(9) 0.004(9) F2 0.089(11) 0.069(10) 0.019(7) -0.018(7) -0.004(7) -0.022(8) F3 0.077(10) 0.057(10) 0.055(10) -0.020(8) -0.020(8) -0.021(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 Re1 C2 1.88(2) . ? Re1 C1 1.88(2) . ? Re1 C3 1.95(2) . ? Re1 O11 2.166(15) . ? Re1 O4 2.167(13) . ? Re1 N1 2.18(2) . ? N1 C11 1.31(3) . ? N1 C15 1.36(3) . ? C1 O1 1.16(3) . ? C2 O2 1.19(3) . ? C3 O3 1.08(3) . ? O4 C16 1.20(3) . ? C11 C12 1.32(4) . ? C12 C13 1.40(4) . ? C13 C14 1.36(4) . ? C14 C15 1.36(3) . ? C15 C16 1.47(3) . ? C10 F1 1.30(3) . ? C10 F3 1.34(3) . ? C10 F2 1.35(3) . ? C10 S1 1.80(3) . ? O11 S1 1.472(16) . ? O12 S1 1.410(17) . ? O13 S1 1.414(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C1 86.7(10) . . ? C2 Re1 C3 87.6(11) . . ? C1 Re1 C3 86.7(9) . . ? C2 Re1 O11 96.8(8) . . ? C1 Re1 O11 174.0(7) . . ? C3 Re1 O11 98.3(7) . . ? C2 Re1 O4 97.6(9) . . ? C1 Re1 O4 96.4(8) . . ? C3 Re1 O4 174.1(7) . . ? O11 Re1 O4 78.4(5) . . ? C2 Re1 N1 171.9(9) . . ? C1 Re1 N1 93.8(8) . . ? C3 Re1 N1 100.5(9) . . ? O11 Re1 N1 82.1(6) . . ? O4 Re1 N1 74.3(6) . . ? C11 N1 C15 116.4(19) . . ? C11 N1 Re1 128.7(14) . . ? C15 N1 Re1 114.9(14) . . ? O1 C1 Re1 177(2) . . ? O2 C2 Re1 174(2) . . ? O3 C3 Re1 175(2) . . ? C16 O4 Re1 117.4(14) . . ? N1 C11 C12 124(2) . . ? C11 C12 C13 120(3) . . ? C14 C13 C12 117(2) . . ? C13 C14 C15 119(2) . . ? C14 C15 N1 123(2) . . ? C14 C15 C16 124(2) . . ? N1 C15 C16 113.1(18) . . ? O4 C16 C15 120.3(19) . . ? F1 C10 F3 108(2) . . ? F1 C10 F2 109(2) . . ? F3 C10 F2 107(2) . . ? F1 C10 S1 113.2(18) . . ? F3 C10 S1 109.7(17) . . ? F2 C10 S1 110.5(17) . . ? S1 O11 Re1 135.0(9) . . ? O12 S1 O13 118.1(11) . . ? O12 S1 O11 114.0(10) . . ? O13 S1 O11 111.7(10) . . ? O12 S1 C10 104.7(11) . . ? O13 S1 C10 104.0(12) . . ? O11 S1 C10 102.0(11) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 23.52 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 7.012 _refine_diff_density_min -5.296 _refine_diff_density_rms 0.636 #===END data_Compound_3d_rg281am _database_code_depnum_ccdc_archive 'CCDC 637227' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H12 F3 Mo N O6 S' _chemical_formula_weight 463.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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' _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 7.834(4) _cell_length_b 9.046(5) _cell_length_c 14.035(8) _cell_angle_alpha 100.666(10) _cell_angle_beta 99.137(10) _cell_angle_gamma 112.880(11) _cell_volume 870.8(8) _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 PLATE _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.808560 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3921 _diffrn_reflns_av_R_equivalents 0.0236 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 23.35 _reflns_number_total 2491 _reflns_number_gt 1956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0505P)^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 2491 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0515 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28090(7) 1.09255(5) 0.26786(3) 0.03883(17) Uani 1 1 d . . . S1 S -0.0283(2) 0.72467(17) 0.28332(10) 0.0480(4) Uani 1 1 d . . . N1 N 0.3063(6) 0.9107(5) 0.1470(3) 0.0425(10) Uani 1 1 d . . . C1 C 0.0396(9) 1.0804(6) 0.1986(4) 0.0492(14) Uani 1 1 d . . . O1 O -0.1011(7) 1.0765(6) 0.1538(3) 0.0765(13) Uani 1 1 d . . . C2 C 0.3649(9) 1.2577(8) 0.1950(5) 0.0620(17) Uani 1 1 d . . . O2 O 0.4007(8) 1.3521(6) 0.1474(4) 0.0988(17) Uani 1 1 d . . . O3 O 0.5531(5) 1.0699(4) 0.3238(2) 0.0486(9) Uani 1 1 d . . . O11 O 0.1671(5) 0.8573(4) 0.3160(2) 0.0422(8) Uani 1 1 d . . . O12 O -0.1562(7) 0.7521(6) 0.3382(4) 0.0949(16) Uani 1 1 d . . . O13 O -0.1035(7) 0.6667(5) 0.1780(3) 0.0831(14) Uani 1 1 d . . . C3 C 0.1357(9) 1.1819(7) 0.3854(4) 0.0556(16) Uani 1 1 d . . . H3A H 0.0919 1.2652 0.3738 0.067 Uiso 1 1 calc R . . H3B H 0.0498 1.0972 0.4107 0.067 Uiso 1 1 calc R . . C4 C 0.3316(9) 1.2379(6) 0.4255(4) 0.0486(14) Uani 1 1 d . . . C5 C 0.4515(9) 1.3521(7) 0.3800(4) 0.0637(17) Uani 1 1 d . . . H5A H 0.5885 1.3888 0.4036 0.076 Uiso 1 1 calc R . . H5B H 0.4165 1.4397 0.3673 0.076 Uiso 1 1 calc R . . C6 C 0.4098(10) 1.1740(8) 0.5050(4) 0.0631(17) Uani 1 1 d . . . H6A H 0.3227 1.0606 0.4975 0.095 Uiso 1 1 calc R . . H6B H 0.4247 1.2414 0.5700 0.095 Uiso 1 1 calc R . . H6C H 0.5319 1.1792 0.4984 0.095 Uiso 1 1 calc R . . C9 C 0.0086(11) 0.5582(8) 0.3204(7) 0.079(2) Uani 1 1 d . . . C11 C 0.1827(9) 0.8284(7) 0.0575(4) 0.0558(15) Uani 1 1 d . . . H11 H 0.0857 0.8596 0.0376 0.067 Uiso 1 1 calc R . . C12 C 0.1933(10) 0.6989(8) -0.0067(4) 0.0703(19) Uani 1 1 d . . . H12 H 0.1038 0.6438 -0.0684 0.084 Uiso 1 1 calc R . . C13 C 0.3349(10) 0.6520(8) 0.0204(4) 0.0692(18) Uani 1 1 d . . . H13 H 0.3433 0.5648 -0.0223 0.083 Uiso 1 1 calc R . . C14 C 0.4668(9) 0.7364(7) 0.1129(4) 0.0593(16) Uani 1 1 d . . . H14 H 0.5654 0.7071 0.1330 0.071 Uiso 1 1 calc R . . C15 C 0.4491(8) 0.8633(6) 0.1738(4) 0.0419(12) Uani 1 1 d . . . C16 C 0.5773(8) 0.9593(7) 0.2723(4) 0.0466(13) Uani 1 1 d . . . H16 H 0.6790 0.9360 0.2963 0.056 Uiso 1 1 calc R . . F1 F -0.1505(6) 0.4181(5) 0.2908(4) 0.1114(16) Uani 1 1 d . . . F2 F 0.0738(8) 0.5900(6) 0.4159(4) 0.134(2) Uani 1 1 d . . . F3 F 0.1377(7) 0.5285(5) 0.2770(4) 0.1186(17) 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 0.0497(3) 0.0318(3) 0.0406(3) 0.01120(18) 0.0142(2) 0.0216(2) S1 0.0491(10) 0.0414(8) 0.0547(8) 0.0156(6) 0.0119(7) 0.0201(7) N1 0.054(3) 0.043(3) 0.037(2) 0.0127(19) 0.015(2) 0.024(2) C1 0.063(4) 0.043(3) 0.053(3) 0.020(3) 0.022(3) 0.028(3) O1 0.072(3) 0.099(4) 0.081(3) 0.043(3) 0.011(3) 0.054(3) C2 0.075(5) 0.058(4) 0.073(4) 0.034(3) 0.038(4) 0.035(3) O2 0.137(5) 0.088(4) 0.118(4) 0.073(3) 0.075(4) 0.059(3) O3 0.045(2) 0.048(2) 0.048(2) 0.0047(17) 0.0086(17) 0.0195(19) O11 0.051(2) 0.035(2) 0.0413(19) 0.0129(15) 0.0071(17) 0.0189(18) O12 0.072(4) 0.082(3) 0.153(5) 0.025(3) 0.063(3) 0.045(3) O13 0.075(3) 0.080(3) 0.061(3) 0.015(2) -0.007(2) 0.010(3) C3 0.072(5) 0.049(4) 0.064(4) 0.012(3) 0.029(3) 0.041(3) C4 0.064(4) 0.038(3) 0.047(3) 0.002(2) 0.018(3) 0.028(3) C5 0.069(5) 0.044(4) 0.068(4) 0.000(3) 0.014(3) 0.022(3) C6 0.081(5) 0.064(4) 0.041(3) -0.002(3) 0.008(3) 0.039(4) C9 0.063(5) 0.059(5) 0.126(7) 0.050(4) 0.032(5) 0.025(4) C11 0.071(5) 0.065(4) 0.037(3) 0.009(3) 0.011(3) 0.039(3) C12 0.095(6) 0.071(5) 0.038(3) -0.001(3) 0.005(3) 0.041(4) C13 0.089(5) 0.059(4) 0.057(4) -0.006(3) 0.020(4) 0.039(4) C14 0.059(4) 0.060(4) 0.067(4) 0.008(3) 0.018(3) 0.037(3) C15 0.043(3) 0.047(3) 0.043(3) 0.016(2) 0.016(3) 0.023(3) C16 0.042(4) 0.051(3) 0.052(3) 0.012(3) 0.014(3) 0.026(3) F1 0.078(3) 0.051(3) 0.201(5) 0.058(3) 0.035(3) 0.014(2) F2 0.171(5) 0.121(4) 0.110(4) 0.081(3) 0.008(3) 0.051(4) F3 0.091(3) 0.074(3) 0.229(5) 0.054(3) 0.066(4) 0.058(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.930(6) . ? Mo1 C1 1.935(6) . ? Mo1 N1 2.226(4) . ? Mo1 C4 2.241(5) . ? Mo1 O11 2.242(3) . ? Mo1 O3 2.253(4) . ? Mo1 C5 2.302(6) . ? Mo1 C3 2.342(5) . ? S1 O13 1.415(4) . ? S1 O12 1.424(4) . ? S1 O11 1.462(4) . ? S1 C9 1.789(6) . ? N1 C11 1.332(6) . ? N1 C15 1.370(6) . ? C1 O1 1.163(6) . ? C2 O2 1.156(6) . ? O3 C16 1.218(5) . ? C3 C4 1.394(8) . ? C4 C5 1.427(8) . ? C4 C6 1.501(7) . ? C9 F2 1.292(8) . ? C9 F1 1.321(8) . ? C9 F3 1.346(8) . ? C11 C12 1.378(7) . ? C12 C13 1.359(8) . ? C13 C14 1.389(8) . ? C14 C15 1.365(7) . ? C15 C16 1.453(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 78.3(2) . . ? C2 Mo1 N1 88.9(2) . . ? C1 Mo1 N1 97.41(19) . . ? C2 Mo1 C4 105.2(2) . . ? C1 Mo1 C4 104.1(2) . . ? N1 Mo1 C4 156.19(17) . . ? C2 Mo1 O11 166.01(19) . . ? C1 Mo1 O11 98.53(18) . . ? N1 Mo1 O11 77.89(13) . . ? C4 Mo1 O11 88.80(16) . . ? C2 Mo1 O3 101.7(2) . . ? C1 Mo1 O3 169.58(17) . . ? N1 Mo1 O3 72.20(14) . . ? C4 Mo1 O3 86.01(17) . . ? O11 Mo1 O3 78.86(13) . . ? C2 Mo1 C5 70.8(2) . . ? C1 Mo1 C5 108.3(2) . . ? N1 Mo1 C5 142.5(2) . . ? C4 Mo1 C5 36.6(2) . . ? O11 Mo1 C5 122.83(17) . . ? O3 Mo1 C5 81.30(18) . . ? C2 Mo1 C3 108.5(2) . . ? C1 Mo1 C3 70.6(2) . . ? N1 Mo1 C3 155.60(19) . . ? C4 Mo1 C3 35.34(19) . . ? O11 Mo1 C3 82.86(16) . . ? O3 Mo1 C3 118.63(17) . . ? C5 Mo1 C3 61.5(2) . . ? O13 S1 O12 114.8(3) . . ? O13 S1 O11 114.2(2) . . ? O12 S1 O11 114.7(3) . . ? O13 S1 C9 105.6(3) . . ? O12 S1 C9 104.5(3) . . ? O11 S1 C9 101.0(3) . . ? C11 N1 C15 117.5(4) . . ? C11 N1 Mo1 126.5(3) . . ? C15 N1 Mo1 115.4(3) . . ? O1 C1 Mo1 176.8(5) . . ? O2 C2 Mo1 174.8(6) . . ? C16 O3 Mo1 116.5(3) . . ? S1 O11 Mo1 127.46(18) . . ? C4 C3 Mo1 68.4(3) . . ? C3 C4 C5 114.6(5) . . ? C3 C4 C6 122.6(5) . . ? C5 C4 C6 122.6(6) . . ? C3 C4 Mo1 76.3(3) . . ? C5 C4 Mo1 74.1(3) . . ? C6 C4 Mo1 114.7(3) . . ? C4 C5 Mo1 69.3(3) . . ? F2 C9 F1 108.1(6) . . ? F2 C9 F3 106.9(6) . . ? F1 C9 F3 106.9(6) . . ? F2 C9 S1 113.5(5) . . ? F1 C9 S1 111.7(5) . . ? F3 C9 S1 109.5(5) . . ? N1 C11 C12 122.5(5) . . ? C13 C12 C11 119.8(6) . . ? C12 C13 C14 119.0(5) . . ? C15 C14 C13 118.8(5) . . ? C14 C15 N1 122.4(5) . . ? C14 C15 C16 123.7(5) . . ? N1 C15 C16 113.9(4) . . ? O3 C16 C15 120.8(5) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.604 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.083 #===END data_Compound_4c_rg415am _database_code_depnum_ccdc_archive 'CCDC 637228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 F3 N O7 P Re S' _chemical_formula_weight 788.68 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 8.480(6) _cell_length_b 12.703(9) _cell_length_c 15.187(10) _cell_angle_alpha 71.046(14) _cell_angle_beta 81.004(12) _cell_angle_gamma 74.722(13) _cell_volume 1488.2(17) _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 PRISM _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 4.271 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.547299 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 6701 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.33 _reflns_number_total 4247 _reflns_number_gt 3695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4247 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 Re1 Re 0.83149(3) 0.08862(3) 0.83540(2) 0.03160(18) Uani 1 1 d . . . P1 P 0.6194(2) 0.27150(18) 0.79501(15) 0.0326(5) Uani 1 1 d . . . N1 N 0.7073(8) 0.0091(6) 0.7679(5) 0.0389(17) Uani 1 1 d . . . C1 C 1.0116(11) -0.0495(8) 0.8664(6) 0.042(2) Uani 1 1 d . . . O1 O 1.1154(9) -0.1259(7) 0.8902(5) 0.072(2) Uani 1 1 d . . . C2 C 0.9559(10) 0.1632(8) 0.8783(6) 0.041(2) Uani 1 1 d . . . O2 O 1.0271(9) 0.2123(7) 0.9056(5) 0.068(2) Uani 1 1 d . . . C3 C 0.7337(10) 0.0376(7) 0.9581(7) 0.038(2) Uani 1 1 d . . . O3 O 0.6698(8) 0.0062(6) 1.0314(4) 0.0594(19) Uani 1 1 d . . . O4 O 0.9114(6) 0.1414(5) 0.6889(4) 0.0345(13) Uani 1 1 d . . . C11 C 0.6062(11) -0.0622(7) 0.8072(7) 0.045(2) Uani 1 1 d . . . H11 H 0.5880 -0.0858 0.8719 0.054 Uiso 1 1 calc R . . C12 C 0.5281(11) -0.1019(7) 0.7550(7) 0.049(2) Uani 1 1 d . . . H12 H 0.4563 -0.1491 0.7847 0.059 Uiso 1 1 calc R . . C13 C 0.5557(12) -0.0725(8) 0.6623(8) 0.057(3) Uani 1 1 d . . . H13 H 0.5020 -0.0980 0.6270 0.068 Uiso 1 1 calc R . . C14 C 0.6643(11) -0.0043(8) 0.6193(6) 0.049(2) Uani 1 1 d . . . H14 H 0.6875 0.0152 0.5549 0.059 Uiso 1 1 calc R . . C15 C 0.7380(10) 0.0345(7) 0.6732(6) 0.039(2) Uani 1 1 d . . . C16 C 0.8544(10) 0.1066(8) 0.6347(6) 0.042(2) Uani 1 1 d . . . H16 H 0.8863 0.1266 0.5711 0.050 Uiso 1 1 calc R . . C21 C 0.4884(10) 0.3092(7) 0.8923(6) 0.039(2) Uani 1 1 d . . . C22 C 0.5644(12) 0.3148(8) 0.9653(7) 0.053(2) Uani 1 1 d . . . H22 H 0.6781 0.2936 0.9648 0.063 Uiso 1 1 calc R . . C23 C 0.4748(15) 0.3508(9) 1.0375(7) 0.062(3) Uani 1 1 d . . . H23 H 0.5275 0.3570 1.0843 0.074 Uiso 1 1 calc R . . C24 C 0.3058(15) 0.3779(11) 1.0405(9) 0.075(3) Uani 1 1 d . . . H24 H 0.2444 0.3991 1.0908 0.090 Uiso 1 1 calc R . . C25 C 0.2287(15) 0.3738(12) 0.9698(10) 0.086(4) Uani 1 1 d . . . H25 H 0.1148 0.3937 0.9715 0.103 Uiso 1 1 calc R . . C26 C 0.3197(12) 0.3399(10) 0.8952(8) 0.065(3) Uani 1 1 d . . . H26 H 0.2664 0.3379 0.8469 0.079 Uiso 1 1 calc R . . C31 C 0.4854(9) 0.2718(7) 0.7129(6) 0.0339(19) Uani 1 1 d . . . C32 C 0.3785(10) 0.1990(8) 0.7412(6) 0.041(2) Uani 1 1 d . . . H32 H 0.3675 0.1564 0.8036 0.049 Uiso 1 1 calc R . . C33 C 0.2871(11) 0.1897(9) 0.6761(8) 0.054(3) Uani 1 1 d . . . H33 H 0.2161 0.1404 0.6950 0.065 Uiso 1 1 calc R . . C34 C 0.3022(14) 0.2524(11) 0.5856(8) 0.073(3) Uani 1 1 d . . . H34 H 0.2408 0.2461 0.5426 0.088 Uiso 1 1 calc R . . C35 C 0.4073(18) 0.3253(11) 0.5562(8) 0.086(4) Uani 1 1 d . . . H35 H 0.4168 0.3680 0.4938 0.103 Uiso 1 1 calc R . . C36 C 0.4978(13) 0.3347(9) 0.6192(7) 0.060(3) Uani 1 1 d . . . H36 H 0.5688 0.3839 0.5990 0.072 Uiso 1 1 calc R . . C41 C 0.7050(10) 0.3984(7) 0.7394(6) 0.039(2) Uani 1 1 d . . . C42 C 0.6039(13) 0.5055(8) 0.7374(7) 0.058(3) Uani 1 1 d . . . H42 H 0.4960 0.5116 0.7628 0.069 Uiso 1 1 calc R . . C43 C 0.6660(16) 0.6034(9) 0.6968(8) 0.071(3) Uani 1 1 d . . . H43 H 0.5998 0.6745 0.6971 0.085 Uiso 1 1 calc R . . C44 C 0.8218(16) 0.5961(9) 0.6568(8) 0.064(3) Uani 1 1 d . . . H44 H 0.8617 0.6617 0.6287 0.077 Uiso 1 1 calc R . . C45 C 0.9198(14) 0.4907(10) 0.6584(9) 0.069(3) Uani 1 1 d . . . H45 H 1.0271 0.4852 0.6319 0.083 Uiso 1 1 calc R . . C46 C 0.8606(12) 0.3921(8) 0.6991(7) 0.056(3) Uani 1 1 d . . . H46 H 0.9279 0.3213 0.6988 0.067 Uiso 1 1 calc R . . S1 S 0.8550(3) 0.1720(2) 0.36431(17) 0.0501(6) Uani 1 1 d . . . O11 O 0.6931(9) 0.1966(8) 0.4080(6) 0.082(3) Uani 1 1 d . . . O12 O 0.9826(9) 0.1724(7) 0.4158(5) 0.072(2) Uani 1 1 d . . . O13 O 0.8871(11) 0.0790(6) 0.3262(5) 0.074(2) Uani 1 1 d . . . C10 C 0.8569(14) 0.2956(10) 0.2633(8) 0.067(3) Uani 1 1 d . . . F1 F 0.8272(11) 0.3910(6) 0.2840(6) 0.105(3) Uani 1 1 d . . . F2 F 0.7415(9) 0.3071(6) 0.2067(5) 0.089(2) Uani 1 1 d . . . F3 F 1.0006(9) 0.2840(8) 0.2135(5) 0.109(3) 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 Re1 0.0298(2) 0.0353(2) 0.0302(2) -0.01157(15) -0.00130(13) -0.00654(14) P1 0.0315(11) 0.0342(11) 0.0336(12) -0.0106(9) -0.0009(8) -0.0105(9) N1 0.028(3) 0.038(4) 0.046(5) -0.006(3) -0.003(3) -0.008(3) C1 0.045(5) 0.047(5) 0.037(5) -0.023(4) -0.004(4) -0.003(4) O1 0.064(4) 0.077(5) 0.059(5) -0.026(4) -0.018(4) 0.024(4) C2 0.034(5) 0.051(5) 0.045(5) -0.035(5) -0.001(4) 0.001(4) O2 0.064(5) 0.086(5) 0.071(5) -0.030(4) -0.010(4) -0.033(4) C3 0.038(5) 0.028(4) 0.049(6) -0.013(4) -0.011(4) -0.002(4) O3 0.063(4) 0.080(5) 0.025(4) -0.006(3) 0.010(3) -0.018(4) O4 0.039(3) 0.040(3) 0.028(3) -0.011(3) 0.000(2) -0.016(2) C11 0.050(5) 0.041(5) 0.048(6) -0.015(4) 0.009(4) -0.020(4) C12 0.046(5) 0.035(5) 0.073(7) -0.019(5) -0.003(5) -0.017(4) C13 0.060(6) 0.051(6) 0.071(8) -0.021(5) -0.016(5) -0.023(5) C14 0.061(6) 0.058(6) 0.036(5) -0.017(5) -0.009(4) -0.019(5) C15 0.037(5) 0.039(5) 0.041(5) -0.016(4) 0.000(4) -0.004(4) C16 0.049(5) 0.052(5) 0.024(4) -0.013(4) 0.002(4) -0.011(4) C21 0.046(5) 0.033(4) 0.038(5) -0.013(4) 0.003(4) -0.010(4) C22 0.057(6) 0.054(6) 0.049(6) -0.021(5) -0.008(5) -0.006(5) C23 0.090(8) 0.058(6) 0.045(6) -0.026(5) -0.006(5) -0.016(6) C24 0.076(8) 0.089(9) 0.068(8) -0.045(7) 0.024(6) -0.020(7) C25 0.055(7) 0.117(11) 0.112(11) -0.081(9) 0.023(7) -0.022(7) C26 0.043(6) 0.099(9) 0.069(7) -0.053(7) 0.007(5) -0.011(5) C31 0.028(4) 0.040(5) 0.036(5) -0.019(4) -0.005(3) 0.000(3) C32 0.032(4) 0.048(5) 0.049(5) -0.025(4) 0.002(4) -0.009(4) C33 0.037(5) 0.066(6) 0.074(8) -0.036(6) -0.005(5) -0.016(4) C34 0.075(8) 0.098(9) 0.056(8) -0.025(7) -0.034(6) -0.015(7) C35 0.125(11) 0.088(9) 0.050(7) 0.001(6) -0.038(7) -0.042(8) C36 0.075(7) 0.058(6) 0.046(6) -0.008(5) -0.011(5) -0.021(5) C41 0.043(5) 0.031(4) 0.043(5) -0.012(4) 0.001(4) -0.010(4) C42 0.061(6) 0.043(5) 0.066(7) -0.014(5) -0.002(5) -0.010(5) C43 0.094(9) 0.045(6) 0.078(8) -0.017(6) -0.012(7) -0.023(6) C44 0.093(9) 0.046(6) 0.061(7) -0.001(5) -0.022(6) -0.039(6) C45 0.060(7) 0.068(8) 0.086(9) -0.014(6) -0.001(6) -0.038(6) C46 0.054(6) 0.040(5) 0.078(7) -0.017(5) 0.001(5) -0.023(4) S1 0.0498(14) 0.0567(15) 0.0450(14) -0.0186(12) 0.0039(11) -0.0140(11) O11 0.054(4) 0.114(7) 0.082(6) -0.041(5) 0.024(4) -0.027(4) O12 0.067(5) 0.091(6) 0.054(5) -0.008(4) -0.012(4) -0.023(4) O13 0.109(6) 0.060(5) 0.062(5) -0.036(4) -0.005(4) -0.010(4) C10 0.060(7) 0.071(8) 0.076(8) -0.016(6) -0.027(6) -0.022(6) F1 0.143(7) 0.054(4) 0.134(7) -0.023(4) -0.065(6) -0.025(4) F2 0.101(5) 0.079(5) 0.088(5) -0.017(4) -0.047(4) -0.011(4) F3 0.083(5) 0.149(7) 0.073(5) 0.012(5) 0.007(4) -0.053(5) _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 Re1 C2 1.892(9) . ? Re1 C3 1.896(10) . ? Re1 C1 1.977(9) . ? Re1 O4 2.158(5) . ? Re1 N1 2.180(8) . ? Re1 P1 2.495(2) . ? P1 C31 1.812(8) . ? P1 C21 1.820(8) . ? P1 C41 1.839(8) . ? N1 C11 1.346(11) . ? N1 C15 1.365(11) . ? C1 O1 1.126(10) . ? C2 O2 1.171(11) . ? C3 O3 1.153(10) . ? O4 C16 1.257(11) . ? C11 C12 1.386(14) . ? C12 C13 1.334(14) . ? C13 C14 1.375(13) . ? C14 C15 1.374(13) . ? C15 C16 1.451(12) . ? C21 C26 1.377(12) . ? C21 C22 1.395(13) . ? C22 C23 1.368(14) . ? C23 C24 1.380(16) . ? C24 C25 1.363(18) . ? C25 C26 1.391(15) . ? C31 C32 1.387(12) . ? C31 C36 1.391(13) . ? C32 C33 1.399(13) . ? C33 C34 1.352(15) . ? C34 C35 1.376(17) . ? C35 C36 1.367(16) . ? C41 C46 1.358(12) . ? C41 C42 1.398(13) . ? C42 C43 1.396(14) . ? C43 C44 1.358(16) . ? C44 C45 1.371(16) . ? C45 C46 1.392(13) . ? S1 O13 1.425(8) . ? S1 O11 1.431(7) . ? S1 O12 1.433(8) . ? S1 C10 1.805(12) . ? C10 F1 1.302(13) . ? C10 F3 1.330(13) . ? C10 F2 1.350(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 90.0(4) . . ? C2 Re1 C1 87.6(4) . . ? C3 Re1 C1 88.6(3) . . ? C2 Re1 O4 98.2(3) . . ? C3 Re1 O4 171.2(3) . . ? C1 Re1 O4 94.6(3) . . ? C2 Re1 N1 172.3(3) . . ? C3 Re1 N1 97.7(3) . . ? C1 Re1 N1 91.8(3) . . ? O4 Re1 N1 74.1(2) . . ? C2 Re1 P1 88.6(3) . . ? C3 Re1 P1 93.2(2) . . ? C1 Re1 P1 175.7(3) . . ? O4 Re1 P1 84.15(15) . . ? N1 Re1 P1 91.83(18) . . ? C31 P1 C21 106.9(4) . . ? C31 P1 C41 105.6(4) . . ? C21 P1 C41 102.2(4) . . ? C31 P1 Re1 111.2(3) . . ? C21 P1 Re1 116.2(3) . . ? C41 P1 Re1 113.7(3) . . ? C11 N1 C15 116.0(8) . . ? C11 N1 Re1 128.6(6) . . ? C15 N1 Re1 115.4(5) . . ? O1 C1 Re1 174.5(8) . . ? O2 C2 Re1 177.3(8) . . ? O3 C3 Re1 177.7(8) . . ? C16 O4 Re1 117.8(5) . . ? N1 C11 C12 122.5(9) . . ? C13 C12 C11 120.2(8) . . ? C12 C13 C14 119.4(9) . . ? C13 C14 C15 118.8(9) . . ? N1 C15 C14 123.0(8) . . ? N1 C15 C16 114.0(8) . . ? C14 C15 C16 123.1(8) . . ? O4 C16 C15 118.7(7) . . ? C26 C21 C22 118.3(8) . . ? C26 C21 P1 124.0(7) . . ? C22 C21 P1 117.6(7) . . ? C23 C22 C21 121.2(9) . . ? C22 C23 C24 119.6(10) . . ? C25 C24 C23 120.2(10) . . ? C24 C25 C26 120.2(11) . . ? C21 C26 C25 120.4(10) . . ? C32 C31 C36 118.3(8) . . ? C32 C31 P1 119.6(6) . . ? C36 C31 P1 121.8(7) . . ? C31 C32 C33 120.1(9) . . ? C34 C33 C32 119.9(10) . . ? C33 C34 C35 120.8(10) . . ? C36 C35 C34 119.7(11) . . ? C35 C36 C31 121.2(10) . . ? C46 C41 C42 119.2(8) . . ? C46 C41 P1 122.6(7) . . ? C42 C41 P1 118.2(7) . . ? C43 C42 C41 119.6(10) . . ? C44 C43 C42 120.8(11) . . ? C43 C44 C45 119.3(9) . . ? C44 C45 C46 120.8(10) . . ? C41 C46 C45 120.4(10) . . ? O13 S1 O11 114.2(6) . . ? O13 S1 O12 115.1(5) . . ? O11 S1 O12 114.6(5) . . ? O13 S1 C10 104.2(5) . . ? O11 S1 C10 103.5(6) . . ? O12 S1 C10 103.1(5) . . ? F1 C10 F3 108.4(10) . . ? F1 C10 F2 106.8(9) . . ? F3 C10 F2 106.9(10) . . ? F1 C10 S1 113.4(9) . . ? F3 C10 S1 110.6(8) . . ? F2 C10 S1 110.4(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.425 _refine_diff_density_min -1.798 _refine_diff_density_rms 0.169 #===END data_Compound_4d_rg422vm _database_code_depnum_ccdc_archive 'CCDC 637229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H49 B F24 Mo N O4 P' _chemical_formula_weight 1513.78 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' 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 13.331(5) _cell_length_b 13.619(6) _cell_length_c 19.907(8) _cell_angle_alpha 70.546(7) _cell_angle_beta 80.191(8) _cell_angle_gamma 89.759(8) _cell_volume 3353(2) _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 BLOCK _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.627283 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15038 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 23.28 _reflns_number_total 9527 _reflns_number_gt 7182 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0953P)^2^+6.8895P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9527 _refine_ls_number_parameters 876 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1871 _refine_ls_wR_factor_gt 0.1626 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.000 _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 0.20713(3) 0.03920(4) 0.85240(2) 0.04833(19) Uani 1 1 d . . . P1 P 0.14001(10) 0.22581(11) 0.82245(7) 0.0476(3) Uani 1 1 d . . . N1 N 0.0733(3) -0.0056(3) 0.8126(2) 0.0464(10) Uani 1 1 d . . . C1 C 0.3229(5) 0.1023(5) 0.8762(3) 0.0604(15) Uani 1 1 d . . . O1 O 0.3896(4) 0.1402(4) 0.8903(3) 0.0904(15) Uani 1 1 d . . . C2 C 0.1530(4) 0.0099(5) 0.9555(3) 0.0579(14) Uani 1 1 d . . . O2 O 0.1202(4) -0.0065(4) 1.0154(2) 0.0833(13) Uani 1 1 d . . . O3 O 0.2451(3) 0.0911(3) 0.73305(18) 0.0532(9) Uani 1 1 d . . . C3 C 0.3498(5) -0.0561(5) 0.8419(4) 0.0789(19) Uani 1 1 d . . . H3A H 0.3922 -0.0371 0.7943 0.095 Uiso 1 1 calc R . . H3B H 0.3886 -0.0715 0.8809 0.095 Uiso 1 1 calc R . . C4 C 0.2633(4) -0.1208(5) 0.8540(4) 0.0689(16) Uani 1 1 d . . . C5 C 0.2002(5) -0.1398(5) 0.9201(4) 0.0747(18) Uani 1 1 d . . . H5A H 0.2327 -0.1593 0.9623 0.090 Uiso 1 1 calc R . . H5B H 0.1360 -0.1786 0.9276 0.090 Uiso 1 1 calc R . . C6 C 0.2382(6) -0.1630(6) 0.7966(4) 0.087(2) Uani 1 1 d . . . H6A H 0.2774 -0.2224 0.7969 0.131 Uiso 1 1 calc R . . H6B H 0.2545 -0.1099 0.7498 0.131 Uiso 1 1 calc R . . H6C H 0.1668 -0.1834 0.8069 0.131 Uiso 1 1 calc R . . C11 C -0.0138(4) -0.0564(4) 0.8513(3) 0.0556(13) Uani 1 1 d . . . H11 H -0.0228 -0.0777 0.9015 0.067 Uiso 1 1 calc R . . C12 C -0.0919(5) -0.0791(5) 0.8198(4) 0.0696(17) Uani 1 1 d . . . H12 H -0.1512 -0.1159 0.8489 0.083 Uiso 1 1 calc R . . C13 C -0.0822(5) -0.0477(5) 0.7462(4) 0.0723(17) Uani 1 1 d . . . H13 H -0.1348 -0.0610 0.7246 0.087 Uiso 1 1 calc R . . C14 C 0.0070(5) 0.0041(5) 0.7050(3) 0.0641(15) Uani 1 1 d . . . H14 H 0.0169 0.0250 0.6548 0.077 Uiso 1 1 calc R . . C15 C 0.0820(4) 0.0246(4) 0.7390(3) 0.0507(13) Uani 1 1 d . . . C16 C 0.1790(4) 0.0787(4) 0.6999(3) 0.0562(14) Uani 1 1 d . . . H16 H 0.1912 0.1042 0.6496 0.067 Uiso 1 1 calc R . . C21 C 0.0819(4) 0.2677(4) 0.8973(3) 0.0551(14) Uani 1 1 d . . . C22 C -0.0073(5) 0.3207(5) 0.8972(3) 0.0667(16) Uani 1 1 d . . . H22 H -0.0446 0.3284 0.8606 0.080 Uiso 1 1 calc R . . C23 C -0.0415(6) 0.3625(5) 0.9517(4) 0.082(2) Uani 1 1 d . . . H23 H -0.1020 0.3965 0.9519 0.099 Uiso 1 1 calc R . . C24 C 0.0147(7) 0.3530(5) 1.0049(4) 0.081(2) Uani 1 1 d . . . H24 H -0.0073 0.3818 1.0408 0.097 Uiso 1 1 calc R . . C25 C 0.1027(7) 0.3016(5) 1.0055(3) 0.081(2) Uani 1 1 d . . . H25 H 0.1403 0.2958 1.0418 0.097 Uiso 1 1 calc R . . C26 C 0.1367(5) 0.2581(5) 0.9527(3) 0.0659(16) Uani 1 1 d . . . H26 H 0.1962 0.2222 0.9542 0.079 Uiso 1 1 calc R . . C31 C 0.2385(4) 0.3305(4) 0.7743(3) 0.0544(13) Uani 1 1 d . . . C32 C 0.2238(5) 0.4302(5) 0.7776(4) 0.0764(18) Uani 1 1 d . . . H32 H 0.1636 0.4436 0.8036 0.092 Uiso 1 1 calc R . . C33 C 0.2983(7) 0.5091(6) 0.7423(4) 0.094(2) Uani 1 1 d . . . H33 H 0.2880 0.5756 0.7446 0.113 Uiso 1 1 calc R . . C34 C 0.3866(7) 0.4903(6) 0.7044(4) 0.094(2) Uani 1 1 d . . . H34 H 0.4368 0.5437 0.6815 0.113 Uiso 1 1 calc R . . C35 C 0.4019(6) 0.3929(6) 0.6998(4) 0.089(2) Uani 1 1 d . . . H35 H 0.4617 0.3811 0.6726 0.107 Uiso 1 1 calc R . . C36 C 0.3290(5) 0.3125(5) 0.7354(3) 0.0701(17) Uani 1 1 d . . . H36 H 0.3406 0.2462 0.7333 0.084 Uiso 1 1 calc R . . C41 C 0.0465(4) 0.2448(4) 0.7638(3) 0.0527(13) Uani 1 1 d . . . C42 C -0.0514(4) 0.1977(5) 0.7915(3) 0.0609(15) Uani 1 1 d . . . H42 H -0.0703 0.1624 0.8409 0.073 Uiso 1 1 calc R . . C43 C -0.1199(5) 0.2031(5) 0.7465(4) 0.0793(19) Uani 1 1 d . . . H43 H -0.1851 0.1718 0.7657 0.095 Uiso 1 1 calc R . . C44 C -0.0932(7) 0.2541(6) 0.6738(5) 0.092(2) Uani 1 1 d . . . H44 H -0.1403 0.2576 0.6437 0.110 Uiso 1 1 calc R . . C45 C 0.0024(7) 0.3000(6) 0.6450(4) 0.086(2) Uani 1 1 d . . . H45 H 0.0203 0.3345 0.5954 0.103 Uiso 1 1 calc R . . C46 C 0.0733(5) 0.2952(5) 0.6901(3) 0.0671(16) Uani 1 1 d . . . H46 H 0.1386 0.3261 0.6704 0.081 Uiso 1 1 calc R . . B51 B 0.6186(5) 0.7534(5) 0.7222(3) 0.0486(14) Uani 1 1 d . . . C51 C 0.6123(4) 0.8508(4) 0.7538(3) 0.0459(12) Uani 1 1 d . . . C52 C 0.6129(4) 0.8388(4) 0.8264(3) 0.0490(12) Uani 1 1 d . . . H52 H 0.6115 0.7716 0.8593 0.059 Uiso 1 1 calc R . . C53 C 0.6153(4) 0.9214(5) 0.8516(3) 0.0512(13) Uani 1 1 d . . . C54 C 0.6149(4) 1.0224(5) 0.8048(3) 0.0550(14) Uani 1 1 d . . . H54 H 0.6144 1.0785 0.8217 0.066 Uiso 1 1 calc R . . C55 C 0.6153(4) 1.0383(4) 0.7325(3) 0.0534(13) Uani 1 1 d . . . C56 C 0.6153(4) 0.9533(4) 0.7084(3) 0.0503(13) Uani 1 1 d . . . H56 H 0.6175 0.9660 0.6593 0.060 Uiso 1 1 calc R . . C57 C 0.6142(5) 0.9020(5) 0.9289(3) 0.0643(16) Uani 1 1 d . . . C58 C 0.6091(6) 1.1436(5) 0.6809(4) 0.0759(18) Uani 1 1 d . . . C61 C 0.7419(4) 0.7542(4) 0.6915(3) 0.0491(12) Uani 1 1 d . . . C62 C 0.8114(4) 0.7102(4) 0.7366(3) 0.0540(13) Uani 1 1 d . . . H62 H 0.7873 0.6774 0.7858 0.065 Uiso 1 1 calc R . . C63 C 0.9159(5) 0.7136(5) 0.7105(3) 0.0630(15) Uani 1 1 d . . . C64 C 0.9546(5) 0.7619(5) 0.6387(4) 0.0688(16) Uani 1 1 d . . . H64 H 1.0242 0.7639 0.6213 0.083 Uiso 1 1 calc R . . C65 C 0.8882(5) 0.8078(5) 0.5925(3) 0.0625(15) Uani 1 1 d . . . C66 C 0.7845(4) 0.8046(4) 0.6191(3) 0.0542(13) Uani 1 1 d . . . H66 H 0.7416 0.8375 0.5871 0.065 Uiso 1 1 calc R . . C67 C 0.9825(6) 0.6598(8) 0.7619(5) 0.094(2) Uani 1 1 d . . . C68 C 0.9249(6) 0.8557(7) 0.5130(4) 0.089(2) Uani 1 1 d . . . C71 C 0.5748(4) 0.6428(4) 0.7847(3) 0.0520(13) Uani 1 1 d . . . C72 C 0.4850(4) 0.6356(5) 0.8339(3) 0.0586(14) Uani 1 1 d . . . H72 H 0.4508 0.6958 0.8319 0.070 Uiso 1 1 calc R . . C73 C 0.4448(5) 0.5421(6) 0.8856(3) 0.0709(17) Uani 1 1 d . . . C74 C 0.4922(6) 0.4506(5) 0.8896(4) 0.081(2) Uani 1 1 d . . . H74 H 0.4645 0.3874 0.9237 0.097 Uiso 1 1 calc R . . C75 C 0.5812(6) 0.4549(5) 0.8421(4) 0.0722(17) Uani 1 1 d . . . C76 C 0.6202(5) 0.5481(4) 0.7906(3) 0.0591(14) Uani 1 1 d . . . H76 H 0.6794 0.5482 0.7582 0.071 Uiso 1 1 calc R . . C77 C 0.3504(7) 0.5406(7) 0.9357(5) 0.097(2) Uani 1 1 d . . . C78 C 0.6353(9) 0.3594(6) 0.8466(6) 0.104(3) Uani 1 1 d . . . C81 C 0.5537(4) 0.7708(4) 0.6566(3) 0.0468(12) Uani 1 1 d . . . C82 C 0.5766(4) 0.7146(4) 0.6085(3) 0.0523(13) Uani 1 1 d . . . H82 H 0.6285 0.6684 0.6151 0.063 Uiso 1 1 calc R . . C83 C 0.5252(5) 0.7253(4) 0.5522(3) 0.0571(14) Uani 1 1 d . . . C84 C 0.4489(5) 0.7938(5) 0.5400(3) 0.0625(15) Uani 1 1 d . . . H84 H 0.4157 0.8028 0.5011 0.075 Uiso 1 1 calc R . . C85 C 0.4227(4) 0.8490(5) 0.5867(3) 0.0592(14) Uani 1 1 d . . . C86 C 0.4744(4) 0.8360(4) 0.6440(3) 0.0546(13) Uani 1 1 d . . . H86 H 0.4544 0.8729 0.6753 0.066 Uiso 1 1 calc R . . C87 C 0.5578(7) 0.6663(6) 0.5015(4) 0.087(2) Uani 1 1 d . . . C88 C 0.3410(6) 0.9230(8) 0.5735(4) 0.093(2) Uani 1 1 d . . . F1 F 0.6673(6) 0.8289(6) 0.9581(3) 0.176(3) Uani 1 1 d . . . F2 F 0.5277(4) 0.8835(7) 0.9673(2) 0.187(4) Uani 1 1 d . . . F3 F 0.6501(7) 0.9790(6) 0.9425(3) 0.200(4) Uani 1 1 d . . . F4 F 0.6321(6) 1.2194(3) 0.7026(3) 0.142(2) Uani 1 1 d . . . F5 F 0.5192(5) 1.1583(4) 0.6613(4) 0.157(3) Uani 1 1 d . . . F6 F 0.6707(5) 1.1632(3) 0.6189(3) 0.138(2) Uani 1 1 d . . . F7 F 0.9644(6) 0.6705(9) 0.8225(4) 0.232(5) Uani 1 1 d . . . F8 F 0.9880(7) 0.5644(6) 0.7720(5) 0.218(4) Uani 1 1 d . . . F9 F 1.0789(5) 0.6892(8) 0.7387(4) 0.202(4) Uani 1 1 d . . . F10 F 1.0219(4) 0.8588(5) 0.4929(3) 0.155(3) Uani 1 1 d . . . F11 F 0.8840(6) 0.8068(6) 0.4763(3) 0.175(3) Uani 1 1 d . . . F12 F 0.8963(4) 0.9501(5) 0.4852(3) 0.138(2) Uani 1 1 d . . . F13 F 0.2691(5) 0.5479(9) 0.9108(4) 0.214(4) Uani 1 1 d . . . F14 F 0.3449(6) 0.6171(7) 0.9611(4) 0.204(4) Uani 1 1 d . . . F15 F 0.3329(6) 0.4623(6) 0.9942(4) 0.216(4) Uani 1 1 d . . . F16 F 0.5955(7) 0.2770(5) 0.8903(7) 0.295(7) Uani 1 1 d . . . F17 F 0.7230(7) 0.3605(6) 0.8596(7) 0.244(6) Uani 1 1 d . . . F18 F 0.6550(11) 0.3393(7) 0.7906(6) 0.266(7) Uani 1 1 d . . . F19 F 0.5765(5) 0.5685(4) 0.5367(3) 0.1295(19) Uani 1 1 d . . . F20 F 0.6378(6) 0.7059(6) 0.4553(4) 0.166(3) Uani 1 1 d . . . F21 F 0.4864(5) 0.6578(4) 0.4650(3) 0.133(2) Uani 1 1 d . . . F22 F 0.3300(5) 0.9623(6) 0.5072(3) 0.176(3) Uani 1 1 d . . . F23 F 0.2512(4) 0.8805(6) 0.6101(4) 0.168(3) Uani 1 1 d . . . F24 F 0.3496(5) 1.0015(5) 0.5973(4) 0.148(2) Uani 1 1 d . . . O90 O 0.8452(6) 0.4455(6) 0.5283(5) 0.182(4) Uani 1 1 d G . . C91 C 0.7889(8) 0.4399(9) 0.4740(6) 0.228(8) Uani 1 1 d G . . H91A H 0.7948 0.5083 0.4370 0.273 Uiso 1 1 d G . . H91B H 0.7175 0.4256 0.4964 0.273 Uiso 1 1 d G . . C92 C 0.8268(10) 0.5291(6) 0.5570(6) 0.235(9) Uani 1 1 d G . . H92A H 0.8755 0.5863 0.5279 0.282 Uiso 1 1 d G . . H92B H 0.7596 0.5527 0.5492 0.282 Uiso 1 1 d G . . C93 C 0.8165(10) 0.3645(10) 0.4382(6) 0.236(9) Uani 1 1 d G . . H93A H 0.8827 0.3844 0.4084 0.355 Uiso 1 1 d G . . H93B H 0.7673 0.3623 0.4087 0.355 Uiso 1 1 d G . . H93C H 0.8179 0.2969 0.4739 0.355 Uiso 1 1 d G . . C94 C 0.8312(13) 0.5121(10) 0.6315(7) 0.303(14) Uani 1 1 d G . . H94A H 0.7811 0.4582 0.6620 0.454 Uiso 1 1 d G . . H94B H 0.8177 0.5754 0.6417 0.454 Uiso 1 1 d G . . H94C H 0.8978 0.4912 0.6406 0.454 Uiso 1 1 d G . . 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 0.0427(3) 0.0560(3) 0.0422(3) -0.0137(2) -0.00244(19) -0.0033(2) P1 0.0487(8) 0.0508(8) 0.0415(7) -0.0155(6) -0.0033(6) -0.0041(6) N1 0.046(2) 0.044(2) 0.046(2) -0.0163(19) 0.0019(19) -0.0016(19) C1 0.058(4) 0.069(4) 0.047(3) -0.012(3) -0.005(3) -0.010(3) O1 0.076(3) 0.116(4) 0.083(3) -0.032(3) -0.028(3) -0.025(3) C2 0.057(3) 0.068(4) 0.048(3) -0.020(3) -0.006(3) -0.002(3) O2 0.097(3) 0.099(3) 0.044(2) -0.018(2) -0.001(2) 0.004(3) O3 0.050(2) 0.061(2) 0.0457(19) -0.0185(17) 0.0019(17) -0.0056(17) C3 0.055(4) 0.083(5) 0.092(5) -0.022(4) -0.012(3) 0.019(3) C4 0.048(3) 0.065(4) 0.093(5) -0.033(4) 0.000(3) 0.007(3) C5 0.075(4) 0.058(4) 0.077(4) -0.007(3) -0.009(4) 0.008(3) C6 0.095(5) 0.072(4) 0.107(6) -0.041(4) -0.030(4) 0.025(4) C11 0.049(3) 0.055(3) 0.057(3) -0.015(3) 0.000(3) -0.002(3) C12 0.049(3) 0.066(4) 0.088(5) -0.019(3) -0.009(3) -0.007(3) C13 0.068(4) 0.068(4) 0.085(5) -0.024(4) -0.031(4) -0.007(3) C14 0.076(4) 0.063(4) 0.059(3) -0.024(3) -0.021(3) -0.002(3) C15 0.055(3) 0.051(3) 0.046(3) -0.019(2) -0.006(2) 0.005(3) C16 0.064(4) 0.060(3) 0.042(3) -0.017(3) -0.003(3) 0.000(3) C21 0.060(3) 0.054(3) 0.045(3) -0.013(3) 0.003(3) -0.009(3) C22 0.077(4) 0.061(4) 0.060(4) -0.022(3) -0.002(3) 0.004(3) C23 0.096(5) 0.066(4) 0.079(5) -0.031(4) 0.012(4) 0.004(4) C24 0.120(6) 0.063(4) 0.054(4) -0.023(3) 0.011(4) -0.012(4) C25 0.122(6) 0.070(4) 0.050(4) -0.020(3) -0.011(4) -0.016(4) C26 0.084(4) 0.060(4) 0.053(3) -0.021(3) -0.007(3) -0.007(3) C31 0.061(3) 0.052(3) 0.047(3) -0.014(2) -0.007(3) -0.011(3) C32 0.080(4) 0.063(4) 0.077(4) -0.021(3) 0.005(3) -0.006(3) C33 0.112(6) 0.062(4) 0.093(5) -0.018(4) 0.005(5) -0.026(4) C34 0.107(6) 0.076(5) 0.086(5) -0.017(4) 0.000(5) -0.044(5) C35 0.077(5) 0.086(5) 0.086(5) -0.018(4) 0.019(4) -0.023(4) C36 0.065(4) 0.068(4) 0.068(4) -0.021(3) 0.009(3) -0.011(3) C41 0.062(3) 0.050(3) 0.050(3) -0.019(3) -0.016(3) 0.009(3) C42 0.057(4) 0.058(3) 0.068(4) -0.021(3) -0.015(3) 0.010(3) C43 0.064(4) 0.075(4) 0.111(6) -0.039(4) -0.032(4) 0.009(3) C44 0.096(6) 0.085(5) 0.107(6) -0.031(5) -0.057(5) 0.021(5) C45 0.113(6) 0.086(5) 0.063(4) -0.021(4) -0.034(4) 0.019(5) C46 0.077(4) 0.063(4) 0.061(4) -0.016(3) -0.020(3) 0.004(3) B51 0.053(4) 0.051(3) 0.043(3) -0.018(3) -0.009(3) -0.003(3) C51 0.043(3) 0.052(3) 0.044(3) -0.018(2) -0.007(2) -0.002(2) C52 0.045(3) 0.059(3) 0.043(3) -0.017(2) -0.009(2) 0.004(2) C53 0.042(3) 0.070(4) 0.047(3) -0.027(3) -0.009(2) 0.001(3) C54 0.046(3) 0.068(4) 0.065(3) -0.040(3) -0.009(3) 0.002(3) C55 0.054(3) 0.054(3) 0.053(3) -0.018(3) -0.014(3) -0.004(3) C56 0.053(3) 0.058(3) 0.040(3) -0.020(3) -0.003(2) -0.006(3) C57 0.064(4) 0.089(5) 0.051(3) -0.034(3) -0.019(3) 0.009(3) C58 0.096(5) 0.060(4) 0.077(5) -0.025(4) -0.024(4) -0.002(4) C61 0.059(3) 0.045(3) 0.048(3) -0.022(2) -0.008(3) -0.003(2) C62 0.062(4) 0.055(3) 0.049(3) -0.022(3) -0.011(3) -0.002(3) C63 0.062(4) 0.064(4) 0.074(4) -0.033(3) -0.021(3) 0.008(3) C64 0.054(4) 0.078(4) 0.082(4) -0.039(4) -0.010(3) 0.005(3) C65 0.064(4) 0.059(4) 0.060(3) -0.022(3) 0.001(3) -0.004(3) C66 0.060(3) 0.049(3) 0.052(3) -0.017(3) -0.005(3) -0.002(3) C67 0.080(6) 0.110(7) 0.110(7) -0.049(5) -0.039(5) 0.039(5) C68 0.085(5) 0.088(6) 0.075(5) -0.018(4) 0.018(4) -0.015(4) C71 0.061(3) 0.053(3) 0.046(3) -0.020(2) -0.014(3) -0.006(3) C72 0.060(3) 0.059(3) 0.052(3) -0.014(3) -0.008(3) -0.008(3) C73 0.068(4) 0.079(5) 0.058(4) -0.017(3) -0.003(3) -0.015(4) C74 0.097(5) 0.063(4) 0.070(4) -0.005(3) -0.015(4) -0.023(4) C75 0.091(5) 0.050(4) 0.075(4) -0.020(3) -0.015(4) -0.011(3) C76 0.066(4) 0.053(3) 0.059(3) -0.022(3) -0.008(3) -0.008(3) C77 0.087(6) 0.100(6) 0.090(6) -0.030(5) 0.020(5) -0.039(5) C78 0.130(8) 0.050(5) 0.129(7) -0.025(5) -0.024(6) 0.006(5) C81 0.049(3) 0.047(3) 0.042(3) -0.016(2) -0.004(2) -0.007(2) C82 0.058(3) 0.049(3) 0.053(3) -0.019(3) -0.014(3) 0.000(3) C83 0.073(4) 0.057(3) 0.050(3) -0.028(3) -0.015(3) 0.000(3) C84 0.068(4) 0.075(4) 0.056(3) -0.031(3) -0.024(3) 0.007(3) C85 0.052(3) 0.075(4) 0.054(3) -0.027(3) -0.010(3) 0.007(3) C86 0.051(3) 0.068(4) 0.051(3) -0.029(3) -0.007(3) 0.000(3) C87 0.128(7) 0.082(5) 0.078(5) -0.047(4) -0.046(5) 0.032(5) C88 0.075(5) 0.144(8) 0.080(5) -0.058(5) -0.029(4) 0.036(5) F1 0.254(7) 0.240(7) 0.079(3) -0.084(4) -0.091(4) 0.152(7) F2 0.096(4) 0.409(12) 0.055(3) -0.082(4) -0.007(3) 0.001(5) F3 0.359(11) 0.176(6) 0.078(3) -0.049(4) -0.059(5) -0.104(7) F4 0.267(7) 0.055(2) 0.122(4) -0.033(3) -0.076(4) 0.001(3) F5 0.129(4) 0.105(4) 0.205(6) 0.018(4) -0.084(4) 0.013(3) F6 0.228(7) 0.070(3) 0.083(3) 0.000(2) 0.010(4) -0.012(3) F7 0.228(8) 0.418(13) 0.123(5) -0.148(7) -0.122(5) 0.220(9) F8 0.258(10) 0.128(5) 0.305(11) -0.050(6) -0.202(9) 0.074(6) F9 0.091(4) 0.303(11) 0.184(7) -0.024(6) -0.070(4) 0.014(5) F10 0.094(4) 0.203(6) 0.107(4) 0.002(4) 0.036(3) 0.026(4) F11 0.244(8) 0.197(6) 0.068(3) -0.050(4) 0.026(4) -0.086(6) F12 0.142(5) 0.125(4) 0.092(3) 0.017(3) 0.019(3) 0.029(4) F13 0.076(4) 0.422(15) 0.157(6) -0.127(8) 0.006(4) -0.003(6) F14 0.179(7) 0.203(7) 0.210(7) -0.118(6) 0.114(6) -0.064(6) F15 0.192(7) 0.183(7) 0.148(6) 0.049(5) 0.093(5) 0.035(5) F16 0.232(9) 0.062(4) 0.432(16) 0.036(6) 0.124(10) 0.017(4) F17 0.188(8) 0.138(6) 0.470(18) -0.142(9) -0.149(10) 0.095(6) F18 0.470(18) 0.181(8) 0.237(10) -0.150(8) -0.145(11) 0.189(11) F19 0.203(6) 0.097(3) 0.130(4) -0.073(3) -0.068(4) 0.052(4) F20 0.183(6) 0.189(6) 0.142(5) -0.120(5) 0.061(5) -0.038(5) F21 0.179(5) 0.151(4) 0.137(4) -0.109(4) -0.088(4) 0.044(4) F22 0.207(6) 0.259(8) 0.095(4) -0.079(4) -0.078(4) 0.166(6) F23 0.070(3) 0.209(7) 0.212(7) -0.060(6) -0.014(4) 0.040(4) F24 0.159(5) 0.155(5) 0.191(6) -0.112(5) -0.088(5) 0.095(4) O90 0.240(10) 0.160(8) 0.186(8) -0.078(7) -0.106(8) 0.065(7) C91 0.212(18) 0.23(2) 0.220(19) -0.045(16) -0.062(15) 0.044(15) C92 0.240(19) 0.151(13) 0.32(3) -0.070(17) -0.090(18) 0.103(13) C93 0.235(18) 0.28(2) 0.27(2) -0.188(19) -0.039(15) 0.091(16) C94 0.53(4) 0.167(15) 0.23(2) -0.072(15) -0.09(2) 0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C2 1.961(6) . ? Mo1 C1 1.969(6) . ? Mo1 O3 2.208(4) . ? Mo1 N1 2.235(4) . ? Mo1 C4 2.293(6) . ? Mo1 C3 2.317(6) . ? Mo1 C5 2.353(6) . ? Mo1 P1 2.6018(18) . ? P1 C41 1.810(5) . ? P1 C21 1.820(6) . ? P1 C31 1.831(5) . ? N1 C11 1.329(7) . ? N1 C15 1.367(6) . ? C1 O1 1.149(7) . ? C2 O2 1.143(6) . ? O3 C16 1.231(6) . ? C3 C4 1.393(9) . ? C4 C5 1.380(9) . ? C4 C6 1.522(9) . ? C11 C12 1.388(8) . ? C12 C13 1.366(9) . ? C13 C14 1.368(9) . ? C14 C15 1.377(8) . ? C15 C16 1.450(8) . ? C21 C22 1.388(8) . ? C21 C26 1.395(8) . ? C22 C23 1.395(9) . ? C23 C24 1.371(10) . ? C24 C25 1.363(10) . ? C25 C26 1.383(9) . ? C31 C36 1.386(8) . ? C31 C32 1.392(9) . ? C32 C33 1.380(9) . ? C33 C34 1.357(11) . ? C34 C35 1.372(11) . ? C35 C36 1.380(9) . ? C41 C46 1.380(8) . ? C41 C42 1.394(8) . ? C42 C43 1.369(9) . ? C43 C44 1.365(11) . ? C44 C45 1.364(11) . ? C45 C46 1.398(9) . ? B51 C71 1.634(8) . ? B51 C81 1.641(7) . ? B51 C51 1.644(8) . ? B51 C61 1.651(8) . ? C51 C56 1.384(7) . ? C51 C52 1.400(7) . ? C52 C53 1.377(7) . ? C53 C54 1.381(8) . ? C53 C57 1.470(8) . ? C54 C55 1.383(7) . ? C55 C56 1.392(7) . ? C55 C58 1.472(9) . ? C57 F2 1.245(7) . ? C57 F1 1.256(8) . ? C57 F3 1.280(8) . ? C58 F4 1.302(7) . ? C58 F6 1.306(8) . ? C58 F5 1.316(8) . ? C61 C66 1.391(7) . ? C61 C62 1.395(7) . ? C62 C63 1.397(8) . ? C63 C64 1.366(9) . ? C63 C67 1.475(10) . ? C64 C65 1.382(9) . ? C65 C66 1.389(8) . ? C65 C68 1.491(9) . ? C67 F7 1.248(9) . ? C67 F8 1.250(10) . ? C67 F9 1.305(10) . ? C68 F10 1.284(9) . ? C68 F12 1.303(9) . ? C68 F11 1.317(9) . ? C71 C72 1.392(8) . ? C71 C76 1.400(8) . ? C72 C73 1.383(8) . ? C73 C74 1.379(10) . ? C73 C77 1.462(10) . ? C74 C75 1.374(10) . ? C75 C76 1.375(8) . ? C75 C78 1.467(11) . ? C77 F13 1.256(10) . ? C77 F15 1.277(10) . ? C77 F14 1.298(10) . ? C78 F18 1.221(11) . ? C78 F16 1.222(10) . ? C78 F17 1.241(11) . ? C81 C86 1.379(8) . ? C81 C82 1.407(7) . ? C82 C83 1.379(7) . ? C83 C84 1.375(8) . ? C83 C87 1.497(9) . ? C84 C85 1.380(8) . ? C85 C86 1.392(7) . ? C85 C88 1.477(10) . ? C87 F20 1.271(10) . ? C87 F21 1.318(8) . ? C87 F19 1.328(8) . ? C88 F22 1.283(8) . ? C88 F23 1.314(10) . ? C88 F24 1.318(9) . ? O90 C92 1.4375 . ? O90 C91 1.4387 . ? C91 C93 1.4457 . ? C92 C94 1.4340 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C1 82.3(2) . . ? C2 Mo1 O3 169.6(2) . . ? C1 Mo1 O3 101.73(18) . . ? C2 Mo1 N1 102.22(19) . . ? C1 Mo1 N1 170.4(2) . . ? O3 Mo1 N1 72.44(14) . . ? C2 Mo1 C4 100.7(2) . . ? C1 Mo1 C4 102.6(2) . . ? O3 Mo1 C4 87.8(2) . . ? N1 Mo1 C4 85.06(19) . . ? C2 Mo1 C3 108.6(3) . . ? C1 Mo1 C3 70.1(3) . . ? O3 Mo1 C3 81.7(2) . . ? N1 Mo1 C3 115.7(2) . . ? C4 Mo1 C3 35.2(2) . . ? C2 Mo1 C5 67.5(2) . . ? C1 Mo1 C5 105.9(2) . . ? O3 Mo1 C5 119.7(2) . . ? N1 Mo1 C5 83.7(2) . . ? C4 Mo1 C5 34.5(2) . . ? C3 Mo1 C5 60.2(2) . . ? C2 Mo1 P1 90.25(18) . . ? C1 Mo1 P1 83.99(19) . . ? O3 Mo1 P1 80.76(10) . . ? N1 Mo1 P1 87.49(11) . . ? C4 Mo1 P1 167.82(18) . . ? C3 Mo1 P1 144.86(18) . . ? C5 Mo1 P1 153.50(17) . . ? C41 P1 C21 105.6(3) . . ? C41 P1 C31 104.9(3) . . ? C21 P1 C31 101.2(2) . . ? C41 P1 Mo1 111.40(18) . . ? C21 P1 Mo1 118.28(19) . . ? C31 P1 Mo1 114.1(2) . . ? C11 N1 C15 116.2(4) . . ? C11 N1 Mo1 128.3(4) . . ? C15 N1 Mo1 115.5(3) . . ? O1 C1 Mo1 179.1(6) . . ? O2 C2 Mo1 179.0(6) . . ? C16 O3 Mo1 118.0(3) . . ? C4 C3 Mo1 71.5(3) . . ? C5 C4 C3 115.2(7) . . ? C5 C4 C6 122.7(6) . . ? C3 C4 C6 122.0(6) . . ? C5 C4 Mo1 75.1(4) . . ? C3 C4 Mo1 73.4(4) . . ? C6 C4 Mo1 118.1(4) . . ? C4 C5 Mo1 70.3(4) . . ? N1 C11 C12 122.7(5) . . ? C13 C12 C11 120.3(6) . . ? C12 C13 C14 118.2(6) . . ? C13 C14 C15 119.1(6) . . ? N1 C15 C14 123.5(5) . . ? N1 C15 C16 113.6(5) . . ? C14 C15 C16 122.9(5) . . ? O3 C16 C15 120.3(5) . . ? C22 C21 C26 118.3(5) . . ? C22 C21 P1 123.2(4) . . ? C26 C21 P1 118.0(5) . . ? C21 C22 C23 120.7(6) . . ? C24 C23 C22 119.6(7) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 120.7(7) . . ? C25 C26 C21 120.2(7) . . ? C36 C31 C32 118.8(5) . . ? C36 C31 P1 121.4(4) . . ? C32 C31 P1 119.8(5) . . ? C33 C32 C31 120.1(7) . . ? C34 C33 C32 120.5(7) . . ? C33 C34 C35 120.3(7) . . ? C34 C35 C36 120.2(7) . . ? C35 C36 C31 120.1(6) . . ? C46 C41 C42 118.6(5) . . ? C46 C41 P1 121.0(5) . . ? C42 C41 P1 119.9(4) . . ? C43 C42 C41 120.6(6) . . ? C44 C43 C42 120.5(7) . . ? C45 C44 C43 120.3(7) . . ? C44 C45 C46 120.0(7) . . ? C41 C46 C45 120.0(6) . . ? C71 B51 C81 106.8(4) . . ? C71 B51 C51 112.2(4) . . ? C81 B51 C51 112.7(4) . . ? C71 B51 C61 112.4(5) . . ? C81 B51 C61 110.5(4) . . ? C51 B51 C61 102.4(4) . . ? C56 C51 C52 114.5(5) . . ? C56 C51 B51 121.5(4) . . ? C52 C51 B51 123.7(5) . . ? C53 C52 C51 123.5(5) . . ? C52 C53 C54 120.1(5) . . ? C52 C53 C57 120.1(5) . . ? C54 C53 C57 119.7(5) . . ? C53 C54 C55 118.5(5) . . ? C54 C55 C56 119.9(5) . . ? C54 C55 C58 121.0(5) . . ? C56 C55 C58 119.0(5) . . ? C51 C56 C55 123.4(5) . . ? F2 C57 F1 106.4(7) . . ? F2 C57 F3 103.1(7) . . ? F1 C57 F3 102.7(7) . . ? F2 C57 C53 114.5(5) . . ? F1 C57 C53 114.5(6) . . ? F3 C57 C53 114.2(6) . . ? F4 C58 F6 103.3(6) . . ? F4 C58 F5 108.6(7) . . ? F6 C58 F5 102.5(6) . . ? F4 C58 C55 114.9(6) . . ? F6 C58 C55 113.9(6) . . ? F5 C58 C55 112.5(6) . . ? C66 C61 C62 115.2(5) . . ? C66 C61 B51 122.1(5) . . ? C62 C61 B51 122.6(5) . . ? C61 C62 C63 122.3(5) . . ? C64 C63 C62 120.8(6) . . ? C64 C63 C67 121.0(6) . . ? C62 C63 C67 118.2(6) . . ? C63 C64 C65 118.6(6) . . ? C64 C65 C66 120.2(6) . . ? C64 C65 C68 121.0(6) . . ? C66 C65 C68 118.6(6) . . ? C65 C66 C61 122.9(5) . . ? F7 C67 F8 107.5(10) . . ? F7 C67 F9 103.7(8) . . ? F8 C67 F9 99.2(8) . . ? F7 C67 C63 116.2(7) . . ? F8 C67 C63 114.7(7) . . ? F9 C67 C63 113.8(8) . . ? F10 C68 F12 106.8(7) . . ? F10 C68 F11 106.9(8) . . ? F12 C68 F11 101.3(8) . . ? F10 C68 C65 114.9(7) . . ? F12 C68 C65 113.9(7) . . ? F11 C68 C65 111.9(6) . . ? C72 C71 C76 115.0(5) . . ? C72 C71 B51 121.5(5) . . ? C76 C71 B51 123.4(5) . . ? C73 C72 C71 122.4(6) . . ? C74 C73 C72 120.6(6) . . ? C74 C73 C77 120.0(7) . . ? C72 C73 C77 119.4(7) . . ? C75 C74 C73 118.5(6) . . ? C74 C75 C76 120.4(6) . . ? C74 C75 C78 119.8(7) . . ? C76 C75 C78 119.8(7) . . ? C75 C76 C71 123.0(6) . . ? F13 C77 F15 104.7(8) . . ? F13 C77 F14 101.1(10) . . ? F15 C77 F14 100.9(9) . . ? F13 C77 C73 116.8(8) . . ? F15 C77 C73 116.4(9) . . ? F14 C77 C73 114.6(7) . . ? F18 C78 F16 102.5(10) . . ? F18 C78 F17 98.6(11) . . ? F16 C78 F17 103.8(11) . . ? F18 C78 C75 116.0(9) . . ? F16 C78 C75 118.0(10) . . ? F17 C78 C75 115.3(8) . . ? C86 C81 C82 115.0(5) . . ? C86 C81 B51 125.5(5) . . ? C82 C81 B51 119.5(5) . . ? C83 C82 C81 122.7(5) . . ? C84 C83 C82 120.5(5) . . ? C84 C83 C87 120.1(5) . . ? C82 C83 C87 119.2(6) . . ? C83 C84 C85 118.6(5) . . ? C84 C85 C86 120.0(5) . . ? C84 C85 C88 118.7(5) . . ? C86 C85 C88 121.3(6) . . ? C81 C86 C85 123.1(5) . . ? F20 C87 F21 107.1(7) . . ? F20 C87 F19 106.5(8) . . ? F21 C87 F19 104.4(7) . . ? F20 C87 C83 113.8(7) . . ? F21 C87 C83 112.6(7) . . ? F19 C87 C83 111.7(6) . . ? F22 C88 F23 105.9(7) . . ? F22 C88 F24 106.9(8) . . ? F23 C88 F24 101.1(7) . . ? F22 C88 C85 115.2(6) . . ? F23 C88 C85 112.5(8) . . ? F24 C88 C85 114.1(6) . . ? C92 O90 C91 118.1 . . ? O90 C91 C93 118.3 . . ? C94 C92 O90 120.0 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.790 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.074 #===END