Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_method SHELXL _publ_contact_author 'Daniel Miguel' _publ_contact_author_address ; Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_contact_author_phone +34-983-184096 _publ_contact_author_fax +34-983-423013 _publ_contact_author_email dmsj@qi.uva.es loop_ _publ_author_name _publ_author_address 'Daniel Miguel' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; 'Raul Garcia-Rodriguez' ; Departamento de Quimica Inorganica Facultad de Ciencias Universidad de Valladolid C/ Prado de la Magdalena s/n 47005 Valladolid SPAIN ; _publ_section_title ; Molybdenum carbonyl complexes with pyridylimino acidato ligands ; _publ_contact_author_name 'Daniel Miguel' #-------------------------- data section of block --------------------------- data_Compound_1_(rg36bm) _database_code_depnum_ccdc_archive 'CCDC 281340' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Mo N2 O6' _chemical_formula_weight 400.20 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' 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 7.311(5) _cell_length_b 16.795(10) _cell_length_c 12.823(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.026(10) _cell_angle_gamma 90.00 _cell_volume 1574.2(17) _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 DARK_RED _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.795011 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 7056 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 23.33 _reflns_number_total 2259 _reflns_number_gt 1752 _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^)+(0.0170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2259 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0522 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 0.43554(5) 0.693184(16) 0.69719(2) 0.03760(11) Uani 1 1 d . . . N1 N 0.3181(4) 0.61190(15) 0.57498(19) 0.0357(7) Uani 1 1 d . . . N2 N 0.4544(4) 0.56867(15) 0.75705(19) 0.0364(7) Uani 1 1 d . . . C1 C 0.6866(6) 0.69280(19) 0.6335(2) 0.0401(9) Uani 1 1 d . . . O1 O 0.8296(4) 0.69948(15) 0.6012(2) 0.0632(8) Uani 1 1 d . . . C2 C 0.3939(5) 0.7929(2) 0.6251(3) 0.0501(10) Uani 1 1 d . . . O2 O 0.3660(4) 0.85185(16) 0.5813(2) 0.0813(10) Uani 1 1 d . . . C3 C 0.5519(5) 0.7523(2) 0.8100(3) 0.0509(10) Uani 1 1 d . . . O3 O 0.6235(4) 0.78824(17) 0.8756(2) 0.0834(10) Uani 1 1 d . . . C4 C 0.1955(6) 0.7136(2) 0.7687(3) 0.0459(10) Uani 1 1 d . . . O4 O 0.0689(4) 0.73369(17) 0.8110(2) 0.0722(8) Uani 1 1 d . . . O5 O 0.8261(4) 0.57299(15) 0.81623(19) 0.0617(8) Uani 1 1 d . . . O6 O 0.7412(3) 0.58114(14) 0.98147(17) 0.0537(7) Uani 1 1 d . . . C11 C 0.2501(5) 0.6339(2) 0.4823(3) 0.0474(10) Uani 1 1 d . . . H11 H 0.2425 0.6879 0.4670 0.057 Uiso 1 1 calc R . . C12 C 0.1911(5) 0.5805(2) 0.4087(3) 0.0532(11) Uani 1 1 d . . . H12 H 0.1450 0.5985 0.3449 0.064 Uiso 1 1 calc R . . C13 C 0.1998(5) 0.5010(2) 0.4288(3) 0.0476(10) Uani 1 1 d . . . H13 H 0.1620 0.4639 0.3790 0.057 Uiso 1 1 calc R . . C14 C 0.2657(5) 0.4770(2) 0.5245(2) 0.0415(9) Uani 1 1 d . . . H14 H 0.2700 0.4232 0.5414 0.050 Uiso 1 1 calc R . . C15 C 0.3253(4) 0.53305(19) 0.5951(2) 0.0326(8) Uani 1 1 d . . . C16 C 0.3964(5) 0.51316(19) 0.6973(2) 0.0378(9) Uani 1 1 d . . . H16 H 0.3999 0.4604 0.7194 0.045 Uiso 1 1 calc R . . C17 C 0.5155(5) 0.5478(2) 0.8624(2) 0.0457(10) Uani 1 1 d . . . H17A H 0.4993 0.4911 0.8731 0.055 Uiso 1 1 calc R . . H17B H 0.4413 0.5757 0.9125 0.055 Uiso 1 1 calc R . . C18 C 0.7124(6) 0.56902(19) 0.8801(3) 0.0417(9) Uani 1 1 d . . . C19 C 0.9206(5) 0.6069(2) 1.0149(3) 0.0560(11) Uani 1 1 d . . . H19A H 0.9427 0.6612 0.9925 0.067 Uiso 1 1 calc R . . H19B H 1.0138 0.5728 0.9859 0.067 Uiso 1 1 calc R . . C20 C 0.9235(6) 0.6017(2) 1.1313(3) 0.0654(12) Uani 1 1 d . . . H20A H 0.8227 0.6314 1.1583 0.098 Uiso 1 1 calc R . . H20B H 1.0363 0.6234 1.1582 0.098 Uiso 1 1 calc R . . H20C H 0.9134 0.5470 1.1520 0.098 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 0.0496(2) 0.03106(17) 0.03198(17) -0.00097(15) -0.00245(13) -0.00344(16) N1 0.040(2) 0.0373(17) 0.0295(16) 0.0016(13) -0.0002(14) -0.0053(13) N2 0.043(2) 0.0349(17) 0.0306(16) 0.0027(13) -0.0040(14) -0.0056(14) C1 0.055(3) 0.0266(19) 0.038(2) -0.0029(16) -0.0066(19) -0.001(2) O1 0.058(2) 0.0656(19) 0.0663(18) -0.0075(14) 0.0097(15) -0.0066(16) C2 0.053(3) 0.040(3) 0.058(3) -0.0004(19) 0.008(2) -0.0019(19) O2 0.084(3) 0.051(2) 0.109(2) 0.0344(18) 0.0153(19) 0.0071(16) C3 0.054(3) 0.050(2) 0.048(2) -0.012(2) 0.003(2) -0.003(2) O3 0.087(3) 0.090(2) 0.073(2) -0.0427(17) -0.0129(17) -0.0132(18) C4 0.056(3) 0.040(2) 0.042(2) 0.0003(16) -0.007(2) -0.0085(19) O4 0.063(2) 0.079(2) 0.075(2) -0.0122(16) 0.0158(16) -0.0038(17) O5 0.060(2) 0.090(2) 0.0355(15) -0.0019(14) 0.0022(14) 0.0032(15) O6 0.0523(19) 0.0792(19) 0.0292(14) -0.0016(12) -0.0047(13) -0.0087(14) C11 0.060(3) 0.046(2) 0.037(2) 0.0070(17) -0.0066(19) -0.0029(19) C12 0.069(3) 0.060(3) 0.030(2) 0.000(2) -0.0114(19) -0.002(2) C13 0.053(3) 0.052(3) 0.038(2) -0.0138(18) -0.0041(19) -0.0033(19) C14 0.047(3) 0.038(2) 0.040(2) -0.0058(17) 0.0048(18) -0.0033(17) C15 0.032(2) 0.033(2) 0.0334(19) -0.0036(16) 0.0027(16) -0.0034(16) C16 0.048(3) 0.0288(19) 0.0370(19) 0.0068(16) 0.0029(18) -0.0035(16) C17 0.063(3) 0.045(2) 0.029(2) 0.0063(16) -0.0040(18) -0.0040(19) C18 0.054(3) 0.037(2) 0.034(2) 0.0057(17) -0.007(2) 0.0040(19) C19 0.051(3) 0.074(3) 0.044(2) 0.0012(19) -0.005(2) -0.008(2) C20 0.067(3) 0.085(3) 0.043(2) -0.001(2) -0.012(2) -0.009(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 1.934(4) . ? Mo1 C3 1.939(4) . ? Mo1 C1 2.022(4) . ? Mo1 C4 2.023(5) . ? Mo1 N2 2.231(3) . ? Mo1 N1 2.238(3) . ? N1 C11 1.333(4) . ? N1 C15 1.350(4) . ? N2 C16 1.275(4) . ? N2 C17 1.458(4) . ? C1 O1 1.137(4) . ? C2 O2 1.155(4) . ? C3 O3 1.154(4) . ? C4 O4 1.133(4) . ? O5 C18 1.179(4) . ? O6 C18 1.329(4) . ? O6 C19 1.439(4) . ? C11 C12 1.366(4) . ? C12 C13 1.362(4) . ? C13 C14 1.370(4) . ? C14 C15 1.371(4) . ? C15 C16 1.441(4) . ? C17 C18 1.496(5) . ? C19 C20 1.495(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Mo1 C3 88.67(16) . . ? C2 Mo1 C1 86.92(15) . . ? C3 Mo1 C1 85.05(15) . . ? C2 Mo1 C4 86.52(15) . . ? C3 Mo1 C4 87.01(15) . . ? C1 Mo1 C4 169.81(13) . . ? C2 Mo1 N2 169.79(13) . . ? C3 Mo1 N2 101.50(13) . . ? C1 Mo1 N2 94.87(12) . . ? C4 Mo1 N2 92.97(12) . . ? C2 Mo1 N1 97.96(14) . . ? C3 Mo1 N1 173.04(13) . . ? C1 Mo1 N1 93.14(12) . . ? C4 Mo1 N1 95.49(12) . . ? N2 Mo1 N1 71.93(10) . . ? C11 N1 C15 117.0(3) . . ? C11 N1 Mo1 126.0(2) . . ? C15 N1 Mo1 116.9(2) . . ? C16 N2 C17 118.3(3) . . ? C16 N2 Mo1 117.4(2) . . ? C17 N2 Mo1 124.1(2) . . ? O1 C1 Mo1 173.7(3) . . ? O2 C2 Mo1 178.7(4) . . ? O3 C3 Mo1 178.5(4) . . ? O4 C4 Mo1 172.0(3) . . ? C18 O6 C19 117.7(3) . . ? N1 C11 C12 122.8(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C14 118.2(3) . . ? C13 C14 C15 119.5(3) . . ? N1 C15 C14 122.4(3) . . ? N1 C15 C16 114.4(3) . . ? C14 C15 C16 123.1(3) . . ? N2 C16 C15 119.2(3) . . ? N2 C17 C18 111.2(3) . . ? O5 C18 O6 124.7(4) . . ? O5 C18 C17 126.6(3) . . ? O6 C18 C17 108.7(3) . . ? O6 C19 C20 106.0(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.415 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.059 #===END data_Compound_2a_(alacidcm) _database_code_depnum_ccdc_archive 'CCDC 281341' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H21 Mo N3 O6' _chemical_formula_weight 471.32 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' 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.094(3) _cell_length_b 10.836(3) _cell_length_c 12.111(4) _cell_angle_alpha 91.259(5) _cell_angle_beta 109.767(5) _cell_angle_gamma 109.143(4) _cell_volume 1049.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.815529 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 6870 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 23.30 _reflns_number_total 5785 _reflns_number_gt 4516 _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^)+(0.0817P)^2^+0.8255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(7) _refine_ls_number_reflns 5785 _refine_ls_number_parameters 484 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.80382(7) 0.68585(6) 0.82007(6) 0.0543(4) Uani 1 1 d . . . N1 N 0.6148(17) 0.5040(15) 0.8268(13) 0.060(4) Uani 1 1 d . . . N2 N 0.6002(18) 0.7426(14) 0.8371(11) 0.051(4) Uani 1 1 d . . . C1 C 0.707(2) 0.6543(16) 0.6473(14) 0.053(4) Uani 1 1 d . . . O1 O 0.6444(19) 0.6294(16) 0.5465(15) 0.108(5) Uani 1 1 d . . . C2 C 0.965(3) 0.620(3) 0.794(2) 0.121(10) Uani 1 1 d . . . O2 O 1.060(2) 0.564(2) 0.7997(19) 0.143(7) Uani 1 1 d . . . C3 C 0.950(2) 0.8527(15) 0.8073(14) 0.055(5) Uani 1 1 d . . . O3 O 1.052(2) 0.9468(16) 0.7990(14) 0.113(5) Uani 1 1 d . . . C4 C 0.9373(13) 0.7204(14) 0.9908(15) 0.065(5) Uani 1 1 d . . . O4 O 1.0177(14) 0.7354(16) 1.0942(12) 0.096(4) Uani 1 1 d . . . C5 C 0.596(2) 0.8745(15) 0.8452(13) 0.057(5) Uani 1 1 d . . . H5 H 0.4939 0.8640 0.8614 0.068 Uiso 1 1 calc R . . O5 O 0.498(2) 0.8409(13) 0.6431(10) 0.109(6) Uani 1 1 d . . . C6 C 0.561(2) 0.9213(19) 0.7193(17) 0.060(5) Uani 1 1 d . . . O6 O 0.5822(17) 1.0439(12) 0.7263(10) 0.069(3) Uani 1 1 d . . . C7 C 0.7299(16) 0.9663(10) 0.9459(9) 0.079(3) Uani 1 1 d . . . H7A H 0.8354 0.9773 0.9389 0.118 Uiso 1 1 calc R . . H7B H 0.7275 0.9322 1.0180 0.118 Uiso 1 1 calc R . . H7C H 0.7155 1.0502 0.9471 0.118 Uiso 1 1 calc R . . C11 C 0.604(2) 0.3811(17) 0.8216(17) 0.062(5) Uani 1 1 d . . . H11 H 0.6979 0.3664 0.8197 0.074 Uiso 1 1 calc R . . C12 C 0.469(2) 0.2654(15) 0.8183(15) 0.071(5) Uani 1 1 d . . . H12 H 0.4722 0.1807 0.8132 0.085 Uiso 1 1 calc R . . C13 C 0.341(2) 0.2899(18) 0.8232(16) 0.070(5) Uani 1 1 d . . . H13 H 0.2492 0.2172 0.8208 0.084 Uiso 1 1 calc R . . C14 C 0.3252(18) 0.4079(12) 0.8313(13) 0.044(4) Uani 1 1 d . . . H14 H 0.2292 0.4187 0.8342 0.052 Uiso 1 1 calc R . . C15 C 0.4622(16) 0.5106(15) 0.8350(14) 0.044(4) Uani 1 1 d . . . C16 C 0.4749(19) 0.6392(16) 0.8455(13) 0.049(4) Uani 1 1 d . . . H16 H 0.3893 0.6573 0.8598 0.059 Uiso 1 1 calc R . . N31 N 0.6952(11) 0.1633(7) 0.5684(7) 0.090(4) Uani 1 1 d G . . H31A H 0.6583 0.1203 0.6221 0.108 Uiso 1 1 calc R . . H31B H 0.6084 0.1404 0.4986 0.108 Uiso 1 1 calc R . . C32 C 0.7511(12) 0.3101(8) 0.6068(7) 0.077(3) Uani 1 1 d G . . H32A H 0.6553 0.3335 0.6025 0.093 Uiso 1 1 calc R . . H32B H 0.8293 0.3337 0.6883 0.093 Uiso 1 1 calc R . . C33 C 0.8328(13) 0.3845(7) 0.5279(8) 0.109(5) Uani 1 1 d G . . H33A H 0.7486 0.3727 0.4497 0.130 Uiso 1 1 calc R . . H33B H 0.8800 0.4779 0.5592 0.130 Uiso 1 1 calc R . . C34 C 0.9675(11) 0.3415(12) 0.5167(9) 0.183(13) Uani 1 1 d G . . H34A H 0.9971 0.3795 0.4520 0.219 Uiso 1 1 calc R . . H34B H 1.0654 0.3785 0.5888 0.219 Uiso 1 1 calc R . . C35 C 0.9295(15) 0.1999(13) 0.4960(10) 0.237(18) Uani 1 1 d G . . H35A H 1.0339 0.1837 0.5223 0.285 Uiso 1 1 calc R . . H35B H 0.8753 0.1698 0.4112 0.285 Uiso 1 1 calc R . . C36 C 0.8215(16) 0.1198(9) 0.5555(9) 0.098(5) Uani 1 1 d G . . H36A H 0.7671 0.0309 0.5118 0.117 Uiso 1 1 calc R . . H36B H 0.8932 0.1144 0.6341 0.117 Uiso 1 1 calc R . . Mo51 Mo 0.19564(8) 0.31331(7) 0.17947(7) 0.0581(4) Uani 1 1 d . . . N51 N 0.3956(17) 0.5008(14) 0.1685(14) 0.053(4) Uani 1 1 d . . . N52 N 0.4017(15) 0.2566(12) 0.1520(10) 0.039(3) Uani 1 1 d . . . C51 C 0.058(3) 0.283(2) 0.000(2) 0.109(9) Uani 1 1 d . . . O51 O -0.040(3) 0.267(2) -0.0904(18) 0.170(10) Uani 1 1 d . . . C52 C 0.036(2) 0.3901(15) 0.1905(17) 0.065(5) Uani 1 1 d . . . O52 O -0.058(2) 0.428(2) 0.2155(19) 0.141(7) Uani 1 1 d . . . C53 C 0.044(2) 0.134(2) 0.1959(18) 0.094(8) Uani 1 1 d . . . O53 O -0.0259(17) 0.0339(12) 0.2079(12) 0.091(4) Uani 1 1 d . . . C54 C 0.3183(19) 0.3404(15) 0.374(2) 0.069(6) Uani 1 1 d . . . O54 O 0.3551(19) 0.3455(15) 0.4674(12) 0.083(4) Uani 1 1 d . . . C55 C 0.402(2) 0.1225(15) 0.1462(14) 0.057(5) Uani 1 1 d . . . H55 H 0.2847 0.0685 0.1008 0.069 Uiso 1 1 d R . . C56 C 0.436(2) 0.0795(17) 0.2626(13) 0.046(4) Uani 1 1 d . . . O55 O 0.4014(19) -0.0371(12) 0.2703(11) 0.082(4) Uani 1 1 d . . . O56 O 0.483(2) 0.1634(16) 0.3560(13) 0.120(6) Uani 1 1 d . . . C57 C 0.490(3) 0.0876(14) 0.0816(12) 0.126(7) Uani 1 1 d . . . H57A H 0.4662 0.1218 0.0076 0.189 Uiso 1 1 calc R . . H57B H 0.4546 -0.0068 0.0663 0.189 Uiso 1 1 calc R . . H57C H 0.6075 0.1243 0.1269 0.189 Uiso 1 1 calc R . . C61 C 0.382(3) 0.624(2) 0.172(2) 0.086(7) Uani 1 1 d . . . H61 H 0.2852 0.6336 0.1735 0.103 Uiso 1 1 calc R . . C62 C 0.508(3) 0.7263(18) 0.1730(19) 0.089(7) Uani 1 1 d . . . H62 H 0.4983 0.8088 0.1789 0.107 Uiso 1 1 calc R . . C63 C 0.659(2) 0.7212(14) 0.1657(15) 0.064(5) Uani 1 1 d . . . H63 H 0.7495 0.7946 0.1682 0.077 Uiso 1 1 calc R . . C64 C 0.652(2) 0.5921(18) 0.1545(15) 0.065(5) Uani 1 1 d . . . H64 H 0.7409 0.5765 0.1428 0.078 Uiso 1 1 calc R . . C65 C 0.5184(19) 0.4818(14) 0.1597(12) 0.042(4) Uani 1 1 d . . . C66 C 0.530(2) 0.3443(14) 0.1544(14) 0.047(4) Uani 1 1 d . . . H66 H 0.6239 0.3287 0.1533 0.057 Uiso 1 1 calc R . . N81 N 0.2824(10) 0.8847(8) 0.4462(8) 0.105(5) Uani 1 1 d G . . H81A H 0.3284 0.9116 0.3917 0.126 Uiso 1 1 d G . . H81B H 0.3597 0.8686 0.5076 0.126 Uiso 1 1 d G . . C82 C 0.2388(11) 0.9941(7) 0.4891(9) 0.078(3) Uani 1 1 d G . . H82A H 0.3408 1.0680 0.5323 0.094 Uiso 1 1 d G . . H82B H 0.1732 1.0241 0.4214 0.094 Uiso 1 1 d G . . C83 C 0.1427(11) 0.9503(10) 0.5673(8) 0.122(6) Uani 1 1 d G . . H83A H 0.2182 0.9434 0.6437 0.146 Uiso 1 1 d G . . H83B H 0.0981 1.0170 0.5800 0.146 Uiso 1 1 d G . . C84 C 0.0031(11) 0.8220(11) 0.5194(11) 0.29(3) Uani 1 1 d G . . H84A H -0.0842 0.8339 0.4524 0.352 Uiso 1 1 d G . . H84B H -0.0432 0.7939 0.5798 0.352 Uiso 1 1 d G . . C85 C 0.0529(15) 0.7162(8) 0.4805(11) 0.210(16) Uani 1 1 d G . . H85A H -0.0454 0.6375 0.4430 0.252 Uiso 1 1 d G . . H85B H 0.1279 0.6942 0.5489 0.252 Uiso 1 1 d G . . C86 C 0.1392(13) 0.7617(8) 0.3938(8) 0.136(7) Uani 1 1 d G . . H86A H 0.1769 0.6940 0.3723 0.164 Uiso 1 1 d G . . H86B H 0.0606 0.7754 0.3222 0.164 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 0.0360(8) 0.0485(8) 0.0798(10) 0.0292(7) 0.0213(7) 0.0156(6) N1 0.038(8) 0.063(9) 0.081(10) 0.030(8) 0.008(7) 0.032(7) N2 0.067(10) 0.044(8) 0.044(7) 0.009(6) 0.013(6) 0.029(7) C1 0.058(9) 0.047(8) 0.051(8) -0.005(6) 0.018(7) 0.018(6) O1 0.090(11) 0.092(9) 0.102(11) -0.010(8) 0.020(9) -0.002(7) C2 0.052(12) 0.120(16) 0.19(2) 0.107(15) 0.037(12) 0.027(12) O2 0.070(10) 0.140(14) 0.27(2) 0.059(14) 0.098(12) 0.058(10) C3 0.060(10) 0.042(8) 0.068(10) 0.040(7) 0.026(8) 0.019(8) O3 0.124(11) 0.090(10) 0.120(10) 0.031(8) 0.066(9) 0.008(9) C4 0.008(6) 0.057(8) 0.105(13) 0.029(8) -0.003(7) 0.002(5) O4 0.032(5) 0.135(11) 0.086(9) 0.048(7) -0.006(5) 0.014(6) C5 0.057(10) 0.052(10) 0.044(9) 0.012(7) 0.012(7) 0.004(8) O5 0.216(15) 0.069(8) 0.039(6) 0.001(6) 0.000(7) 0.093(9) C6 0.079(12) 0.061(11) 0.077(12) 0.038(9) 0.051(10) 0.047(10) O6 0.097(8) 0.062(8) 0.074(7) 0.045(6) 0.049(6) 0.041(7) C7 0.102(9) 0.053(6) 0.060(7) 0.007(5) 0.005(6) 0.028(6) C11 0.059(10) 0.056(11) 0.099(12) 0.043(9) 0.041(9) 0.042(9) C12 0.068(11) 0.032(8) 0.107(13) 0.003(8) 0.030(9) 0.014(7) C13 0.062(11) 0.067(12) 0.087(12) 0.023(9) 0.039(9) 0.015(9) C14 0.035(7) 0.027(7) 0.071(9) 0.027(6) 0.024(6) 0.008(5) C15 0.014(6) 0.048(9) 0.068(9) 0.026(7) 0.011(6) 0.015(6) C16 0.042(8) 0.076(11) 0.054(9) 0.031(7) 0.032(7) 0.033(8) N31 0.082(8) 0.104(9) 0.035(5) 0.028(5) 0.010(5) -0.019(7) C32 0.097(9) 0.061(7) 0.064(7) 0.001(5) 0.035(6) 0.011(6) C33 0.117(11) 0.105(10) 0.089(9) 0.033(8) 0.055(9) 0.001(9) C34 0.099(14) 0.28(3) 0.064(11) -0.024(14) 0.020(10) -0.051(17) C35 0.30(4) 0.29(4) 0.25(3) 0.21(3) 0.21(3) 0.13(3) C36 0.146(15) 0.077(10) 0.078(10) 0.026(8) 0.029(10) 0.061(11) Mo51 0.0347(8) 0.0497(8) 0.0889(11) 0.0311(8) 0.0194(7) 0.0156(6) N51 0.043(8) 0.039(7) 0.097(10) 0.033(7) 0.048(7) 0.014(6) N52 0.031(6) 0.038(7) 0.042(6) 0.025(5) 0.013(5) 0.006(5) C51 0.110(17) 0.136(19) 0.097(15) 0.095(15) 0.059(13) 0.037(14) O51 0.148(16) 0.21(2) 0.121(14) 0.096(14) 0.044(12) 0.020(14) C52 0.041(9) 0.049(7) 0.135(13) 0.040(8) 0.057(9) 0.028(7) O52 0.089(12) 0.133(14) 0.250(19) 0.109(14) 0.079(12) 0.078(11) C53 0.049(12) 0.108(18) 0.072(12) -0.007(11) 0.006(9) -0.021(11) O53 0.068(7) 0.045(6) 0.102(8) 0.030(6) 0.009(6) -0.029(6) C54 0.021(6) 0.035(8) 0.139(17) 0.024(9) 0.017(8) 0.005(5) O54 0.102(10) 0.095(9) 0.059(7) 0.016(6) 0.022(6) 0.052(8) C55 0.085(13) 0.039(9) 0.073(11) 0.022(8) 0.035(10) 0.045(9) C56 0.055(9) 0.056(9) 0.039(7) 0.012(7) 0.022(6) 0.029(7) O55 0.125(11) 0.046(7) 0.090(9) 0.033(6) 0.052(8) 0.035(7) O56 0.212(16) 0.143(14) 0.075(9) 0.053(9) 0.061(10) 0.141(13) C57 0.27(2) 0.087(9) 0.101(10) 0.057(8) 0.118(13) 0.115(13) C61 0.063(12) 0.061(12) 0.155(19) 0.041(12) 0.050(12) 0.038(10) C62 0.079(12) 0.065(11) 0.149(16) 0.079(11) 0.059(11) 0.037(10) C63 0.059(10) 0.021(7) 0.090(11) 0.034(7) 0.012(8) 0.001(6) C64 0.042(8) 0.085(13) 0.063(9) 0.016(8) 0.011(7) 0.025(8) C65 0.051(9) 0.031(7) 0.039(7) 0.005(6) 0.018(6) 0.007(6) C66 0.043(9) 0.029(7) 0.064(9) 0.016(6) 0.003(6) 0.022(6) N81 0.096(11) 0.097(9) 0.052(7) 0.017(6) 0.012(7) -0.039(8) C82 0.074(7) 0.079(8) 0.096(9) 0.022(7) 0.038(7) 0.039(7) C83 0.067(8) 0.177(16) 0.094(10) 0.021(11) 0.041(8) -0.003(9) C84 0.141(18) 0.44(5) 0.109(15) -0.06(2) 0.086(14) -0.17(3) C85 0.16(2) 0.40(5) 0.20(3) 0.19(3) 0.17(2) 0.15(2) C86 0.137(14) 0.135(15) 0.066(9) -0.008(9) 0.031(9) -0.033(12) _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 C3 1.908(16) . ? Mo1 C2 1.93(3) . ? Mo1 C1 1.949(16) . ? Mo1 C4 1.964(15) . ? Mo1 N1 2.174(16) . ? Mo1 N2 2.202(14) . ? N1 C11 1.30(2) . ? N1 C15 1.45(2) . ? N2 C16 1.35(2) . ? N2 C5 1.45(2) . ? C1 O1 1.14(2) . ? C2 O2 1.19(3) . ? C3 O3 1.16(2) . ? C4 O4 1.19(2) . ? C5 C7 1.453(18) . ? C5 C6 1.58(2) . ? O5 C6 1.10(2) . ? C6 O6 1.276(19) . ? C11 C12 1.43(3) . ? C12 C13 1.29(2) . ? C13 C14 1.34(2) . ? C14 C15 1.36(2) . ? C15 C16 1.36(2) . ? N31 C36 1.4271 . ? N31 C32 1.5116 . ? C32 C33 1.4949 . ? C33 C34 1.4891 . ? C34 C35 1.4536 . ? C35 C36 1.4779 . ? Mo51 C52 1.934(13) . ? Mo51 C53 2.04(2) . ? Mo51 C51 2.06(2) . ? Mo51 C54 2.20(2) . ? Mo51 N52 2.273(13) . ? Mo51 N51 2.281(13) . ? N51 C65 1.237(19) . ? N51 C61 1.38(2) . ? N52 C66 1.23(2) . ? N52 C55 1.454(18) . ? C51 O51 1.12(3) . ? C52 O52 1.18(2) . ? C53 O53 1.11(3) . ? C54 O54 1.06(2) . ? C55 C57 1.41(2) . ? C55 C56 1.46(2) . ? C56 O55 1.211(18) . ? C56 O56 1.291(19) . ? C61 C62 1.30(3) . ? C62 C63 1.42(2) . ? C63 C64 1.38(2) . ? C64 C65 1.42(2) . ? C65 C66 1.53(2) . ? N81 C86 1.4630 . ? N81 C82 1.5011 . ? C82 C83 1.4805 . ? C83 C84 1.4804 . ? C84 C85 1.4840 . ? C85 C86 1.5116 . ? 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 Mo1 C2 84.0(8) . . ? C3 Mo1 C1 87.2(7) . . ? C2 Mo1 C1 82.8(9) . . ? C3 Mo1 C4 87.8(6) . . ? C2 Mo1 C4 88.4(9) . . ? C1 Mo1 C4 170.3(7) . . ? C3 Mo1 N1 173.7(6) . . ? C2 Mo1 N1 101.4(8) . . ? C1 Mo1 N1 90.3(6) . . ? C4 Mo1 N1 95.4(6) . . ? C3 Mo1 N2 100.4(6) . . ? C2 Mo1 N2 174.1(9) . . ? C1 Mo1 N2 93.4(6) . . ? C4 Mo1 N2 95.7(5) . . ? N1 Mo1 N2 74.0(5) . . ? C11 N1 C15 108.2(16) . . ? C11 N1 Mo1 133.4(13) . . ? C15 N1 Mo1 118.4(11) . . ? C16 N2 C5 120.5(15) . . ? C16 N2 Mo1 112.6(11) . . ? C5 N2 Mo1 126.9(12) . . ? O1 C1 Mo1 176.4(16) . . ? O2 C2 Mo1 165(2) . . ? O3 C3 Mo1 172.2(16) . . ? O4 C4 Mo1 177.0(14) . . ? N2 C5 C7 114.4(12) . . ? N2 C5 C6 109.9(13) . . ? C7 C5 C6 117.4(14) . . ? O5 C6 O6 131.5(18) . . ? O5 C6 C5 115.0(16) . . ? O6 C6 C5 111.6(16) . . ? N1 C11 C12 129.9(17) . . ? C13 C12 C11 113.3(16) . . ? C12 C13 C14 127.3(17) . . ? C13 C14 C15 114.0(15) . . ? C14 C15 C16 123.9(14) . . ? C14 C15 N1 127.3(15) . . ? C16 C15 N1 108.8(13) . . ? N2 C16 C15 125.9(14) . . ? C36 N31 C32 114.7 . . ? C33 C32 N31 109.8 . . ? C34 C33 C32 113.2 . . ? C35 C34 C33 116.6 . . ? C34 C35 C36 115.3 . . ? N31 C36 C35 117.8 . . ? C52 Mo51 C53 89.6(8) . . ? C52 Mo51 C51 83.2(9) . . ? C53 Mo51 C51 90.4(8) . . ? C52 Mo51 C54 92.2(7) . . ? C53 Mo51 C54 85.8(7) . . ? C51 Mo51 C54 174.1(8) . . ? C52 Mo51 N52 169.5(6) . . ? C53 Mo51 N52 100.3(7) . . ? C51 Mo51 N52 93.3(7) . . ? C54 Mo51 N52 91.9(5) . . ? C52 Mo51 N51 98.5(6) . . ? C53 Mo51 N51 171.5(8) . . ? C51 Mo51 N51 93.1(7) . . ? C54 Mo51 N51 91.2(6) . . ? N52 Mo51 N51 71.7(5) . . ? C65 N51 C61 122.9(15) . . ? C65 N51 Mo51 113.5(11) . . ? C61 N51 Mo51 123.6(13) . . ? C66 N52 C55 116.5(14) . . ? C66 N52 Mo51 119.1(11) . . ? C55 N52 Mo51 123.9(10) . . ? O51 C51 Mo51 167(2) . . ? O52 C52 Mo51 168.3(17) . . ? O53 C53 Mo51 174(2) . . ? O54 C54 Mo51 169.6(16) . . ? C57 C55 N52 118.4(14) . . ? C57 C55 C56 113.1(12) . . ? N52 C55 C56 111.6(13) . . ? O55 C56 O56 119.5(15) . . ? O55 C56 C55 120.0(15) . . ? O56 C56 C55 119.8(15) . . ? C62 C61 N51 119.0(19) . . ? C61 C62 C63 124.8(18) . . ? C64 C63 C62 110.6(16) . . ? C63 C64 C65 124.1(17) . . ? N51 C65 C64 118.4(14) . . ? N51 C65 C66 122.1(14) . . ? C64 C65 C66 119.5(15) . . ? N52 C66 C65 113.0(14) . . ? C86 N81 C82 113.8 . . ? C83 C82 N81 111.5 . . ? C84 C83 C82 113.7 . . ? C83 C84 C85 113.6 . . ? C84 C85 C86 110.1 . . ? N81 C86 C85 110.6 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.989 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.084 #===END data_Compound_3b_(rgacidm) _database_code_depnum_ccdc_archive 'CCDC 281342' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 Mo N2 O4' _chemical_formula_weight 370.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.6553(12) _cell_length_b 15.676(3) _cell_length_c 15.454(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.916(4) _cell_angle_gamma 90.00 _cell_volume 1588.2(5) _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 PLATE _exptl_crystal_colour RED _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 0.841 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.712642 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 6971 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2288 _reflns_number_gt 1871 _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^)+(0.0467P)^2^+0.7005P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2288 _refine_ls_number_parameters 192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0876 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.27615(5) 0.45971(2) 0.28133(2) 0.05226(17) Uani 1 1 d . . . C1 C 0.4757(7) 0.4348(3) 0.3919(3) 0.0603(11) Uani 1 1 d . . . O1 O 0.5842(5) 0.4098(2) 0.4518(2) 0.0890(10) Uani 1 1 d . . . C2 C 0.1369(8) 0.3561(3) 0.3107(3) 0.0731(13) Uani 1 1 d . . . O2 O 0.0537(7) 0.2971(2) 0.3291(3) 0.1148(14) Uani 1 1 d . . . C3 C 0.4579(8) 0.3921(3) 0.2215(3) 0.0785(14) Uani 1 1 d . . . O3 O 0.5669(7) 0.3549(2) 0.1856(3) 0.1261(17) Uani 1 1 d . . . C4 C 0.0838(8) 0.4549(3) 0.1643(3) 0.0709(12) Uani 1 1 d . . . O4 O -0.0167(7) 0.4395(3) 0.0996(3) 0.1216(15) Uani 1 1 d . . . N1 N 0.0999(5) 0.55601(19) 0.3457(2) 0.0495(8) Uani 1 1 d . . . N2 N 0.3981(5) 0.5879(2) 0.2569(2) 0.0527(8) Uani 1 1 d . . . C11 C -0.0512(7) 0.5407(3) 0.3890(3) 0.0658(11) Uani 1 1 d . . . H11 H -0.0959 0.4848 0.3924 0.079 Uiso 1 1 calc R . . C12 C -0.1456(8) 0.6040(4) 0.4292(3) 0.0835(15) Uani 1 1 d . . . H12 H -0.2496 0.5909 0.4602 0.100 Uiso 1 1 calc R . . C13 C -0.0832(8) 0.6866(4) 0.4227(3) 0.0862(15) Uani 1 1 d . . . H13 H -0.1450 0.7305 0.4490 0.103 Uiso 1 1 calc R . . C14 C 0.0698(8) 0.7039(3) 0.3775(3) 0.0747(13) Uani 1 1 d . . . H14 H 0.1127 0.7597 0.3716 0.090 Uiso 1 1 calc R . . C15 C 0.1600(6) 0.6377(2) 0.3407(3) 0.0566(10) Uani 1 1 d . . . C16 C 0.3236(6) 0.6497(3) 0.2906(3) 0.0626(11) Uani 1 1 d . . . H16 H 0.3732 0.7043 0.2836 0.075 Uiso 1 1 calc R . . C17 C 0.5553(7) 0.6056(3) 0.2024(3) 0.0740(13) Uani 1 1 d . . . H17A H 0.6142 0.6613 0.2179 0.089 Uiso 1 1 calc R . . H17B H 0.6634 0.5637 0.2157 0.089 Uiso 1 1 calc R . . C18 C 0.4754(7) 0.6037(3) 0.1076(3) 0.0735(13) Uani 1 1 d . . . H18 H 0.4181 0.5469 0.0928 0.088 Uiso 1 1 calc R . . C19 C 0.6515(10) 0.6177(4) 0.0564(4) 0.132(2) Uani 1 1 d . . . H19A H 0.7105 0.6729 0.0701 0.197 Uiso 1 1 calc R . . H19B H 0.6003 0.6142 -0.0055 0.197 Uiso 1 1 calc R . . H19C H 0.7535 0.5746 0.0726 0.197 Uiso 1 1 calc R . . C20 C 0.3131(10) 0.6681(4) 0.0773(4) 0.121(2) Uani 1 1 d . . . H20A H 0.1940 0.6550 0.1021 0.181 Uiso 1 1 calc R . . H20B H 0.2792 0.6667 0.0144 0.181 Uiso 1 1 calc R . . H20C H 0.3617 0.7239 0.0960 0.181 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 0.0685(3) 0.0401(2) 0.0495(2) 0.00443(15) 0.01416(17) 0.00177(17) C1 0.062(3) 0.062(3) 0.062(3) 0.012(2) 0.022(2) 0.008(2) O1 0.083(2) 0.103(3) 0.078(2) 0.026(2) 0.0070(19) 0.017(2) C2 0.093(3) 0.055(3) 0.070(3) 0.005(2) 0.008(3) -0.016(3) O2 0.151(4) 0.073(2) 0.119(3) 0.019(2) 0.021(3) -0.047(3) C3 0.114(4) 0.057(3) 0.071(3) 0.016(2) 0.033(3) 0.025(3) O3 0.189(4) 0.090(3) 0.119(3) 0.014(2) 0.081(3) 0.066(3) C4 0.096(3) 0.054(3) 0.059(3) -0.001(2) 0.001(3) -0.005(2) O4 0.147(4) 0.120(3) 0.082(3) -0.015(2) -0.024(3) -0.021(3) N1 0.0542(19) 0.0496(19) 0.0437(18) 0.0013(14) 0.0059(15) 0.0050(15) N2 0.060(2) 0.0488(19) 0.0490(19) 0.0058(15) 0.0103(16) -0.0048(16) C11 0.070(3) 0.072(3) 0.058(3) 0.004(2) 0.018(2) 0.001(2) C12 0.078(3) 0.112(4) 0.067(3) -0.003(3) 0.030(3) 0.012(3) C13 0.107(4) 0.083(4) 0.071(3) -0.018(3) 0.023(3) 0.030(3) C14 0.094(3) 0.062(3) 0.068(3) -0.012(2) 0.015(3) 0.010(3) C15 0.071(3) 0.045(2) 0.051(2) -0.0009(18) 0.003(2) 0.003(2) C16 0.073(3) 0.044(2) 0.071(3) 0.007(2) 0.013(2) -0.009(2) C17 0.080(3) 0.077(3) 0.067(3) 0.014(2) 0.020(3) -0.004(3) C18 0.097(3) 0.064(3) 0.064(3) 0.002(2) 0.026(3) -0.005(3) C19 0.163(6) 0.147(6) 0.105(5) 0.024(4) 0.080(5) 0.006(5) C20 0.132(5) 0.139(5) 0.083(4) 0.026(4) -0.005(4) 0.040(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 Mo1 C3 1.956(5) . ? Mo1 C2 1.962(5) . ? Mo1 C1 2.013(5) . ? Mo1 C4 2.029(5) . ? Mo1 N2 2.224(3) . ? Mo1 N1 2.247(3) . ? C1 O1 1.141(5) . ? C2 O2 1.138(5) . ? C3 O3 1.146(5) . ? C4 O4 1.130(6) . ? N1 C11 1.322(5) . ? N1 C15 1.348(5) . ? N2 C16 1.243(5) . ? N2 C17 1.478(5) . ? C11 C12 1.379(6) . ? C12 C13 1.369(7) . ? C13 C14 1.358(7) . ? C14 C15 1.370(6) . ? C15 C16 1.453(6) . ? C17 C18 1.471(6) . ? C18 C20 1.493(7) . ? C18 C19 1.538(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 90.9(2) . . ? C3 Mo1 C1 85.66(19) . . ? C2 Mo1 C1 84.96(18) . . ? C3 Mo1 C4 84.6(2) . . ? C2 Mo1 C4 85.67(19) . . ? C1 Mo1 C4 166.35(18) . . ? C3 Mo1 N2 97.79(16) . . ? C2 Mo1 N2 171.25(17) . . ? C1 Mo1 N2 96.46(15) . . ? C4 Mo1 N2 94.30(15) . . ? C3 Mo1 N1 170.38(16) . . ? C2 Mo1 N1 98.66(17) . . ? C1 Mo1 N1 94.19(14) . . ? C4 Mo1 N1 97.01(16) . . ? N2 Mo1 N1 72.65(11) . . ? O1 C1 Mo1 171.2(4) . . ? O2 C2 Mo1 178.3(5) . . ? O3 C3 Mo1 177.8(4) . . ? O4 C4 Mo1 169.6(4) . . ? C11 N1 C15 117.4(3) . . ? C11 N1 Mo1 127.1(3) . . ? C15 N1 Mo1 115.5(3) . . ? C16 N2 C17 117.7(4) . . ? C16 N2 Mo1 116.7(3) . . ? C17 N2 Mo1 125.5(3) . . ? N1 C11 C12 122.9(4) . . ? C13 C12 C11 118.7(4) . . ? C14 C13 C12 119.3(4) . . ? C13 C14 C15 119.0(5) . . ? N1 C15 C14 122.7(4) . . ? N1 C15 C16 114.2(3) . . ? C14 C15 C16 123.1(4) . . ? N2 C16 C15 120.8(4) . . ? C18 C17 N2 113.2(4) . . ? C17 C18 C20 114.6(4) . . ? C17 C18 C19 109.4(5) . . ? C20 C18 C19 108.5(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.657 _refine_diff_density_min -0.268 _refine_diff_density_rms 0.063 #===END data_Compound_3c_(rg58am) _database_code_depnum_ccdc_archive 'CCDC 281343' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H12 Mo N2 O4' _chemical_formula_weight 404.23 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4015(13) _cell_length_b 15.754(2) _cell_length_c 10.8180(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.019(2) _cell_angle_gamma 90.00 _cell_volume 1685.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PRISM _exptl_crystal_colour DARK_RED _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.800 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.841068 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 10821 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 23.28 _reflns_number_total 2418 _reflns_number_gt 1864 _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^)+(0.0252P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2418 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.90501(3) 0.841282(17) 0.75405(2) 0.04382(11) Uani 1 1 d . . . N1 N 0.9511(2) 0.85168(15) 0.5648(2) 0.0430(6) Uani 1 1 d . . . N2 N 0.7808(2) 0.94788(15) 0.6415(2) 0.0440(6) Uani 1 1 d . . . C1 C 0.7664(3) 0.7484(2) 0.6780(3) 0.0517(8) Uani 1 1 d . . . O1 O 0.6940(3) 0.69217(17) 0.6483(2) 0.0790(8) Uani 1 1 d . . . C2 C 0.8404(3) 0.8415(2) 0.9051(3) 0.0528(8) Uani 1 1 d . . . O2 O 0.8006(3) 0.84182(16) 0.9946(2) 0.0755(7) Uani 1 1 d . . . C3 C 1.0301(4) 0.7486(2) 0.8292(3) 0.0581(9) Uani 1 1 d . . . O3 O 1.1046(3) 0.69409(18) 0.8707(3) 0.0907(9) Uani 1 1 d . . . C4 C 1.0489(3) 0.9209(2) 0.8627(3) 0.0513(8) Uani 1 1 d . . . O4 O 1.1304(3) 0.96001(17) 0.9363(2) 0.0811(8) Uani 1 1 d . . . C11 C 1.0350(3) 0.8031(2) 0.5231(3) 0.0571(9) Uani 1 1 d . . . H11 H 1.0854 0.7620 0.5791 0.069 Uiso 1 1 calc R . . C12 C 1.0505(3) 0.8107(2) 0.4017(3) 0.0640(10) Uani 1 1 d . . . H12 H 1.1096 0.7752 0.3770 0.077 Uiso 1 1 calc R . . C13 C 0.9787(4) 0.8706(2) 0.3185(3) 0.0627(10) Uani 1 1 d . . . H13 H 0.9884 0.8770 0.2364 0.075 Uiso 1 1 calc R . . C14 C 0.8917(3) 0.9214(2) 0.3575(3) 0.0549(9) Uani 1 1 d . . . H14 H 0.8413 0.9627 0.3020 0.066 Uiso 1 1 calc R . . C15 C 0.8796(3) 0.91084(18) 0.4797(3) 0.0424(7) Uani 1 1 d . . . C16 C 0.7900(3) 0.96252(19) 0.5288(3) 0.0481(8) Uani 1 1 d . . . H16 H 0.7397 1.0060 0.4781 0.058 Uiso 1 1 calc R . . C17 C 0.6943(3) 1.00429(19) 0.6891(3) 0.0540(9) Uani 1 1 d . . . H17A H 0.6596 1.0488 0.6256 0.065 Uiso 1 1 calc R . . H17B H 0.7486 1.0309 0.7691 0.065 Uiso 1 1 calc R . . C21 C 0.5776(3) 0.9592(2) 0.7140(3) 0.0468(8) Uani 1 1 d . . . C22 C 0.5149(3) 0.8900(2) 0.6403(3) 0.0536(9) Uani 1 1 d . . . H22 H 0.5457 0.8702 0.5735 0.064 Uiso 1 1 calc R . . C23 C 0.4077(4) 0.8504(2) 0.6652(4) 0.0687(10) Uani 1 1 d . . . H23 H 0.3677 0.8035 0.6161 0.082 Uiso 1 1 calc R . . C24 C 0.3592(4) 0.8792(3) 0.7612(4) 0.0789(12) Uani 1 1 d . . . H24 H 0.2877 0.8517 0.7788 0.095 Uiso 1 1 calc R . . C25 C 0.4178(4) 0.9496(3) 0.8316(4) 0.0852(13) Uani 1 1 d . . . H25 H 0.3839 0.9707 0.8956 0.102 Uiso 1 1 calc R . . C26 C 0.5257(4) 0.9888(3) 0.8084(3) 0.0705(11) Uani 1 1 d . . . H26 H 0.5644 1.0361 0.8572 0.085 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 0.04672(18) 0.04368(18) 0.03776(17) 0.00456(14) 0.00823(12) 0.00165(15) N1 0.0391(14) 0.0440(16) 0.0428(15) 0.0002(13) 0.0082(12) 0.0000(13) N2 0.0431(15) 0.0409(15) 0.0452(16) 0.0023(12) 0.0096(12) 0.0019(12) C1 0.063(2) 0.046(2) 0.043(2) 0.0067(16) 0.0123(17) 0.0042(18) O1 0.094(2) 0.0569(17) 0.0786(19) -0.0027(14) 0.0161(15) -0.0232(15) C2 0.057(2) 0.047(2) 0.049(2) 0.0039(18) 0.0079(17) -0.0059(18) O2 0.0966(19) 0.0824(18) 0.0546(16) 0.0021(14) 0.0340(14) -0.0120(15) C3 0.068(2) 0.062(2) 0.043(2) 0.0061(18) 0.0142(18) 0.006(2) O3 0.099(2) 0.086(2) 0.081(2) 0.0247(16) 0.0183(16) 0.0449(18) C4 0.051(2) 0.057(2) 0.046(2) 0.0098(17) 0.0150(17) 0.0000(18) O4 0.0759(18) 0.088(2) 0.0709(18) -0.0112(15) 0.0102(15) -0.0267(16) C11 0.053(2) 0.061(2) 0.055(2) 0.0010(17) 0.0128(18) 0.0106(18) C12 0.060(2) 0.079(3) 0.056(2) -0.007(2) 0.0228(19) 0.010(2) C13 0.062(2) 0.083(3) 0.046(2) -0.0036(19) 0.0204(19) -0.003(2) C14 0.055(2) 0.062(2) 0.044(2) 0.0120(16) 0.0096(17) 0.0015(18) C15 0.0387(18) 0.0449(19) 0.0413(19) 0.0011(15) 0.0089(15) -0.0007(15) C16 0.050(2) 0.042(2) 0.048(2) 0.0116(16) 0.0090(16) 0.0042(16) C17 0.064(2) 0.044(2) 0.057(2) -0.0028(16) 0.0217(17) 0.0062(17) C21 0.0441(19) 0.052(2) 0.044(2) 0.0054(15) 0.0131(16) 0.0164(17) C22 0.047(2) 0.055(2) 0.056(2) -0.0063(18) 0.0137(17) 0.0099(18) C23 0.051(2) 0.056(2) 0.093(3) -0.005(2) 0.012(2) 0.006(2) C24 0.059(3) 0.096(3) 0.085(3) 0.017(3) 0.027(2) 0.008(2) C25 0.066(3) 0.133(4) 0.062(3) -0.009(3) 0.028(2) 0.004(3) C26 0.063(2) 0.089(3) 0.057(2) -0.017(2) 0.0160(19) -0.002(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 1.950(4) . ? Mo1 C3 1.957(4) . ? Mo1 C4 2.026(4) . ? Mo1 C1 2.041(4) . ? Mo1 N2 2.236(2) . ? Mo1 N1 2.249(2) . ? N1 C11 1.340(4) . ? N1 C15 1.359(3) . ? N2 C16 1.273(3) . ? N2 C17 1.467(3) . ? C1 O1 1.142(4) . ? C2 O2 1.164(4) . ? C3 O3 1.151(4) . ? C4 O4 1.146(4) . ? C11 C12 1.377(4) . ? C12 C13 1.357(5) . ? C13 C14 1.369(4) . ? C14 C15 1.376(4) . ? C15 C16 1.456(4) . ? C17 C21 1.501(4) . ? C21 C26 1.375(4) . ? C21 C22 1.390(4) . ? C22 C23 1.376(4) . ? C23 C24 1.364(5) . ? C24 C25 1.376(5) . ? C25 C26 1.370(5) . ? 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 C3 90.60(13) . . ? C2 Mo1 C4 84.07(13) . . ? C3 Mo1 C4 86.76(14) . . ? C2 Mo1 C1 87.45(13) . . ? C3 Mo1 C1 85.90(13) . . ? C4 Mo1 C1 168.72(12) . . ? C2 Mo1 N2 99.43(12) . . ? C3 Mo1 N2 169.87(12) . . ? C4 Mo1 N2 92.85(11) . . ? C1 Mo1 N2 95.87(11) . . ? C2 Mo1 N1 171.43(11) . . ? C3 Mo1 N1 97.54(11) . . ? C4 Mo1 N1 98.98(10) . . ? C1 Mo1 N1 90.47(10) . . ? N2 Mo1 N1 72.50(9) . . ? C11 N1 C15 116.2(3) . . ? C11 N1 Mo1 127.5(2) . . ? C15 N1 Mo1 116.17(19) . . ? C16 N2 C17 117.5(3) . . ? C16 N2 Mo1 117.1(2) . . ? C17 N2 Mo1 125.30(19) . . ? O1 C1 Mo1 172.6(3) . . ? O2 C2 Mo1 179.4(3) . . ? O3 C3 Mo1 178.3(3) . . ? O4 C4 Mo1 172.0(3) . . ? N1 C11 C12 123.5(3) . . ? C13 C12 C11 119.3(3) . . ? C12 C13 C14 118.9(3) . . ? C13 C14 C15 119.4(3) . . ? N1 C15 C14 122.7(3) . . ? N1 C15 C16 114.5(3) . . ? C14 C15 C16 122.8(3) . . ? N2 C16 C15 119.6(3) . . ? N2 C17 C21 113.2(2) . . ? C26 C21 C22 118.0(3) . . ? C26 C21 C17 119.9(3) . . ? C22 C21 C17 122.0(3) . . ? C23 C22 C21 120.6(3) . . ? C24 C23 C22 120.7(4) . . ? C23 C24 C25 119.0(4) . . ? C26 C25 C24 120.6(4) . . ? C25 C26 C21 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.439 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.050 #===END data_Compound_4_(rg60am) _database_code_depnum_ccdc_archive 'CCDC 281344' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H21 Mo N3 O6' _chemical_formula_weight 471.32 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.481(8) _cell_length_b 11.553(6) _cell_length_c 20.934(10) _cell_angle_alpha 90.00 _cell_angle_beta 98.40(2) _cell_angle_gamma 90.00 _cell_volume 4182(4) _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 RED _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.880337 _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 9331 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 23.71 _reflns_number_total 3065 _reflns_number_gt 2455 _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^)+(0.0612P)^2^+0.3612P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3065 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 0.695617(18) 0.52224(3) 0.210021(14) 0.04522(16) Uani 1 1 d . . . N1 N 0.72507(16) 0.5674(3) 0.31637(13) 0.0419(7) Uani 1 1 d . . . N2 N 0.81735(18) 0.4661(2) 0.24274(15) 0.0457(7) Uani 1 1 d . . . N3 N 0.98699(19) 0.7040(3) 0.00427(17) 0.0646(10) Uani 1 1 d . . . H3A H 0.9809 0.6403 0.0277 0.077 Uiso 1 1 calc R . . H3B H 1.0179 0.6854 -0.0250 0.077 Uiso 1 1 calc R . . C1 C 0.6489(3) 0.3648(4) 0.2288(2) 0.0679(13) Uani 1 1 d . . . O1 O 0.6169(2) 0.2792(4) 0.2322(2) 0.1108(15) Uani 1 1 d . . . C2 C 0.5888(3) 0.5821(4) 0.1917(2) 0.0652(12) Uani 1 1 d . . . O2 O 0.5281(2) 0.6177(4) 0.17945(19) 0.1067(13) Uani 1 1 d . . . C3 C 0.6877(2) 0.4708(4) 0.1203(2) 0.0583(11) Uani 1 1 d . . . O3 O 0.6832(2) 0.4414(3) 0.06687(15) 0.0899(11) Uani 1 1 d . . . C4 C 0.7268(2) 0.6781(4) 0.17633(19) 0.0526(10) Uani 1 1 d . . . O4 O 0.7385(2) 0.7618(3) 0.15055(15) 0.0769(9) Uani 1 1 d . . . C5 C 0.9387(2) 0.4507(4) 0.1050(2) 0.0505(10) Uani 1 1 d . . . O5 O 0.9862(2) 0.5104(3) 0.08362(18) 0.0808(10) Uani 1 1 d . . . O6 O 0.9208(2) 0.3510(3) 0.0845(2) 0.1047(13) Uani 1 1 d . . . C6 C 0.8953(3) 0.5013(3) 0.1566(2) 0.0599(11) Uani 1 1 d . . . H6A H 0.9292 0.5552 0.1827 0.072 Uiso 1 1 calc R . . H6B H 0.8513 0.5448 0.1355 0.072 Uiso 1 1 calc R . . C7 C 0.8670(2) 0.4121(3) 0.20059(18) 0.0539(10) Uani 1 1 d . . . H7A H 0.8382 0.3525 0.1748 0.065 Uiso 1 1 calc R . . H7B H 0.9109 0.3759 0.2267 0.065 Uiso 1 1 calc R . . C11 C 0.6787(2) 0.6170(3) 0.35407(18) 0.0472(9) Uani 1 1 d . . . H11 H 0.6286 0.6365 0.3359 0.057 Uiso 1 1 calc R . . C12 C 0.7020(3) 0.6404(3) 0.41884(19) 0.0575(11) Uani 1 1 d . . . H12 H 0.6680 0.6757 0.4431 0.069 Uiso 1 1 calc R . . C13 C 0.7745(3) 0.6120(3) 0.44700(19) 0.0574(11) Uani 1 1 d . . . H13 H 0.7908 0.6263 0.4906 0.069 Uiso 1 1 calc R . . C14 C 0.8229(2) 0.5618(3) 0.40924(18) 0.0509(10) Uani 1 1 d . . . H14 H 0.8731 0.5420 0.4270 0.061 Uiso 1 1 calc R . . C15 C 0.7969(2) 0.5402(3) 0.34426(17) 0.0439(9) Uani 1 1 d . . . C16 C 0.8452(2) 0.4855(3) 0.30167(19) 0.0470(9) Uani 1 1 d . . . H16 H 0.8959 0.4648 0.3173 0.056 Uiso 1 1 calc R . . C21 C 0.9114(3) 0.7411(4) -0.0294(2) 0.0795(14) Uani 1 1 d . . . H21A H 0.8877 0.6785 -0.0562 0.095 Uiso 1 1 calc R . . H21B H 0.9180 0.8065 -0.0572 0.095 Uiso 1 1 calc R . . C22 C 0.8601(3) 0.7749(5) 0.0189(3) 0.0898(17) Uani 1 1 d . . . H22A H 0.8485 0.7071 0.0431 0.108 Uiso 1 1 calc R . . H22B H 0.8117 0.8050 -0.0035 0.108 Uiso 1 1 calc R . . C23 C 0.8984(4) 0.8658(5) 0.0651(3) 0.0976(18) Uani 1 1 d . . . H23A H 0.9042 0.9370 0.0417 0.117 Uiso 1 1 calc R . . H23B H 0.8658 0.8819 0.0978 0.117 Uiso 1 1 calc R . . C24 C 0.9742(4) 0.8266(5) 0.0963(3) 0.0989(19) Uani 1 1 d . . . H24A H 0.9681 0.7600 0.1233 0.119 Uiso 1 1 calc R . . H24B H 0.9989 0.8877 0.1237 0.119 Uiso 1 1 calc R . . C25 C 1.0239(3) 0.7949(4) 0.0469(3) 0.0909(18) Uani 1 1 d . . . H25A H 1.0326 0.8627 0.0216 0.109 Uiso 1 1 calc R . . H25B H 1.0737 0.7678 0.0682 0.109 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 0.0415(2) 0.0596(3) 0.0343(2) -0.00017(14) 0.00475(14) -0.00205(15) N1 0.0377(17) 0.0513(17) 0.0378(16) 0.0011(13) 0.0096(14) -0.0041(14) N2 0.0422(18) 0.0509(19) 0.046(2) 0.0028(14) 0.0143(15) 0.0022(14) N3 0.070(3) 0.056(2) 0.076(3) -0.0064(17) 0.038(2) 0.0040(18) C1 0.064(3) 0.083(3) 0.051(3) 0.012(2) -0.008(2) -0.009(3) O1 0.108(3) 0.092(3) 0.121(3) 0.030(2) -0.022(2) -0.041(2) C2 0.056(3) 0.092(3) 0.047(2) 0.004(2) 0.009(2) -0.003(2) O2 0.051(2) 0.164(4) 0.104(3) 0.020(3) 0.0062(19) 0.036(2) C3 0.054(3) 0.070(3) 0.050(3) -0.001(2) 0.006(2) -0.008(2) O3 0.101(3) 0.127(3) 0.043(2) -0.0187(18) 0.0148(18) -0.021(2) C4 0.048(2) 0.065(3) 0.043(2) -0.0063(19) 0.0005(18) 0.001(2) O4 0.095(3) 0.0591(19) 0.074(2) 0.0112(16) 0.0044(18) -0.0092(17) C5 0.044(2) 0.052(3) 0.059(3) 0.0008(19) 0.0200(19) -0.0004(18) O5 0.082(2) 0.078(2) 0.094(3) 0.0025(17) 0.049(2) -0.0082(17) O6 0.119(3) 0.089(3) 0.126(3) -0.027(2) 0.083(3) -0.021(2) C6 0.061(3) 0.057(3) 0.069(3) -0.006(2) 0.034(2) -0.0049(19) C7 0.053(2) 0.060(3) 0.051(2) -0.0003(19) 0.0172(19) 0.0080(19) C11 0.044(2) 0.049(2) 0.051(2) 0.0020(17) 0.0149(18) -0.0047(17) C12 0.071(3) 0.058(3) 0.048(2) -0.0103(18) 0.026(2) -0.009(2) C13 0.069(3) 0.065(3) 0.037(2) -0.0076(18) 0.005(2) -0.014(2) C14 0.048(2) 0.061(2) 0.042(2) 0.0002(17) 0.0015(18) -0.0105(19) C15 0.043(2) 0.050(2) 0.039(2) 0.0030(16) 0.0066(17) -0.0084(17) C16 0.036(2) 0.061(2) 0.044(2) 0.0038(17) 0.0042(17) -0.0006(17) C21 0.093(4) 0.087(4) 0.056(3) -0.003(2) 0.003(3) -0.019(3) C22 0.041(3) 0.117(5) 0.111(4) 0.022(4) 0.009(3) 0.013(3) C23 0.110(5) 0.097(4) 0.093(4) -0.004(3) 0.039(4) 0.042(4) C24 0.126(5) 0.078(4) 0.086(4) -0.028(3) -0.007(4) 0.010(3) C25 0.054(3) 0.061(3) 0.152(6) -0.006(3) -0.005(3) -0.007(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 C3 1.955(5) . ? Mo1 C2 1.975(5) . ? Mo1 C4 2.037(5) . ? Mo1 C1 2.056(5) . ? Mo1 N2 2.235(3) . ? Mo1 N1 2.271(3) . ? N1 C11 1.340(5) . ? N1 C15 1.343(4) . ? N2 C16 1.278(5) . ? N2 C7 1.464(5) . ? N3 C25 1.466(6) . ? N3 C21 1.468(6) . ? C1 O1 1.143(5) . ? C2 O2 1.133(5) . ? C3 O3 1.161(5) . ? C4 O4 1.140(5) . ? C5 O5 1.215(5) . ? C5 O6 1.253(5) . ? C5 C6 1.524(6) . ? C6 C7 1.513(6) . ? C11 C12 1.384(5) . ? C12 C13 1.358(6) . ? C13 C14 1.368(6) . ? C14 C15 1.392(5) . ? C15 C16 1.459(5) . ? C21 C22 1.498(7) . ? C22 C23 1.517(7) . ? C23 C24 1.462(8) . ? C24 C25 1.489(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 89.30(18) . . ? C3 Mo1 C4 85.46(17) . . ? C2 Mo1 C4 85.21(18) . . ? C3 Mo1 C1 86.57(18) . . ? C2 Mo1 C1 87.48(19) . . ? C4 Mo1 C1 169.25(15) . . ? C3 Mo1 N2 97.85(15) . . ? C2 Mo1 N2 172.75(15) . . ? C4 Mo1 N2 94.11(13) . . ? C1 Mo1 N2 94.11(15) . . ? C3 Mo1 N1 170.16(15) . . ? C2 Mo1 N1 100.52(14) . . ? C4 Mo1 N1 95.89(13) . . ? C1 Mo1 N1 93.20(14) . . ? N2 Mo1 N1 72.35(11) . . ? C11 N1 C15 116.8(3) . . ? C11 N1 Mo1 127.3(2) . . ? C15 N1 Mo1 115.9(2) . . ? C16 N2 C7 118.7(3) . . ? C16 N2 Mo1 117.2(3) . . ? C7 N2 Mo1 124.1(2) . . ? C25 N3 C21 111.6(3) . . ? O1 C1 Mo1 171.6(4) . . ? O2 C2 Mo1 177.9(4) . . ? O3 C3 Mo1 179.3(4) . . ? O4 C4 Mo1 171.5(3) . . ? O5 C5 O6 123.1(4) . . ? O5 C5 C6 118.7(4) . . ? O6 C5 C6 118.1(4) . . ? C7 C6 C5 114.3(3) . . ? N2 C7 C6 110.7(3) . . ? N1 C11 C12 123.0(4) . . ? C13 C12 C11 120.0(4) . . ? C12 C13 C14 117.9(4) . . ? C13 C14 C15 120.0(4) . . ? N1 C15 C14 122.3(4) . . ? N1 C15 C16 115.1(3) . . ? C14 C15 C16 122.6(3) . . ? N2 C16 C15 119.5(3) . . ? N3 C21 C22 109.7(4) . . ? C21 C22 C23 111.1(4) . . ? C24 C23 C22 110.9(4) . . ? C23 C24 C25 110.5(5) . . ? N3 C25 C24 110.4(4) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 23.71 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.857 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.063 #===END data_Compound_5a_(rg55cm) _database_code_depnum_ccdc_archive 'CCDC 281345' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21 Mo N3 O6' _chemical_formula_weight 519.36 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' 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 6.6540(12) _cell_length_b 8.3742(15) _cell_length_c 21.538(4) _cell_angle_alpha 86.669(3) _cell_angle_beta 87.253(3) _cell_angle_gamma 69.782(4) _cell_volume 1123.8(4) _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 DARK_RED _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.755546 _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 4981 _diffrn_reflns_av_R_equivalents 0.0134 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 0.95 _diffrn_reflns_theta_max 23.27 _reflns_number_total 3207 _reflns_number_gt 3062 _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^)+(0.0524P)^2^+0.5313P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3207 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _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 0.68125(4) 0.12504(3) 0.154532(10) 0.03319(13) Uani 1 1 d . . . N1 N 0.4680(4) 0.3669(3) 0.10668(10) 0.0353(5) Uani 1 1 d . . . N2 N 0.6766(4) 0.3457(3) 0.21020(11) 0.0357(5) Uani 1 1 d . . . C1 C 0.4325(5) 0.0711(4) 0.20020(14) 0.0422(7) Uani 1 1 d . . . O1 O 0.3109(4) 0.0173(4) 0.22278(13) 0.0716(8) Uani 1 1 d . . . C2 C 0.6701(5) -0.0401(4) 0.09512(16) 0.0472(8) Uani 1 1 d . . . O2 O 0.6675(5) -0.1404(4) 0.06094(14) 0.0809(9) Uani 1 1 d . . . C3 C 0.8674(5) -0.0678(4) 0.20512(15) 0.0428(7) Uani 1 1 d . . . O3 O 0.9723(4) -0.1835(3) 0.23459(13) 0.0689(7) Uani 1 1 d . . . C4 C 0.9487(5) 0.1286(4) 0.10638(15) 0.0413(7) Uani 1 1 d . . . O4 O 1.1043(4) 0.1139(4) 0.07858(13) 0.0713(8) Uani 1 1 d . . . C5 C 1.2141(5) 0.2324(4) 0.42003(14) 0.0402(7) Uani 1 1 d . . . O5 O 1.1936(4) 0.1263(3) 0.46108(10) 0.0486(5) Uani 1 1 d . . . O6 O 1.3510(4) 0.3042(3) 0.41983(11) 0.0600(6) Uani 1 1 d . . . C11 C 0.3609(5) 0.3782(4) 0.05415(14) 0.0428(7) Uani 1 1 d . . . H11 H 0.3714 0.2784 0.0353 0.051 Uiso 1 1 calc R . . C12 C 0.2376(5) 0.5305(5) 0.02739(15) 0.0516(9) Uani 1 1 d . . . H12 H 0.1670 0.5326 -0.0091 0.062 Uiso 1 1 calc R . . C13 C 0.2177(5) 0.6799(5) 0.05413(16) 0.0548(9) Uani 1 1 d . . . H13 H 0.1341 0.7841 0.0363 0.066 Uiso 1 1 calc R . . C14 C 0.3246(5) 0.6717(4) 0.10800(15) 0.0496(8) Uani 1 1 d . . . H14 H 0.3134 0.7708 0.1275 0.060 Uiso 1 1 calc R . . C15 C 0.4485(4) 0.5149(4) 0.13275(13) 0.0384(7) Uani 1 1 d . . . C16 C 0.5708(5) 0.4961(4) 0.18867(13) 0.0413(7) Uani 1 1 d . . . H16 H 0.5723 0.5915 0.2084 0.050 Uiso 1 1 calc R . . C17 C 0.8054(5) 0.3274(3) 0.26390(13) 0.0360(7) Uani 1 1 d . . . C18 C 0.7747(5) 0.2287(4) 0.31454(13) 0.0389(7) Uani 1 1 d . . . H18 H 0.6700 0.1786 0.3143 0.047 Uiso 1 1 calc R . . C19 C 0.9021(5) 0.2054(4) 0.36573(14) 0.0395(7) Uani 1 1 d . . . H19 H 0.8784 0.1429 0.4007 0.047 Uiso 1 1 calc R . . C20 C 1.0646(5) 0.2742(3) 0.36559(13) 0.0365(7) Uani 1 1 d . . . C21 C 1.0909(5) 0.3741(4) 0.31441(14) 0.0450(7) Uani 1 1 d . . . H21 H 1.1973 0.4226 0.3141 0.054 Uiso 1 1 calc R . . C22 C 0.9611(5) 0.4025(4) 0.26378(14) 0.0438(7) Uani 1 1 d . . . H22 H 0.9781 0.4714 0.2300 0.053 Uiso 1 1 calc R . . N31 N 1.5501(4) 0.2100(3) 0.53243(11) 0.0422(6) Uani 1 1 d . . . H31A H 1.4960 0.2390 0.4942 0.051 Uiso 1 1 calc R . . H31B H 1.6230 0.0972 0.5340 0.051 Uiso 1 1 calc R . . C32 C 1.7006(6) 0.3026(5) 0.54247(15) 0.0488(8) Uani 1 1 d . . . H32A H 1.6267 0.4242 0.5364 0.059 Uiso 1 1 calc R . . H32B H 1.8191 0.2686 0.5123 0.059 Uiso 1 1 calc R . . C33 C 1.7857(5) 0.2634(4) 0.60761(15) 0.0479(8) Uani 1 1 d . . . H33A H 1.8737 0.1440 0.6119 0.057 Uiso 1 1 calc R . . H33B H 1.8753 0.3305 0.6143 0.057 Uiso 1 1 calc R . . C34 C 1.6070(6) 0.3020(5) 0.65621(15) 0.0559(9) Uani 1 1 d . . . H34A H 1.5284 0.4235 0.6553 0.067 Uiso 1 1 calc R . . H34B H 1.6665 0.2680 0.6971 0.067 Uiso 1 1 calc R . . C35 C 1.4561(6) 0.2073(6) 0.64420(16) 0.0641(10) Uani 1 1 d . . . H35A H 1.5313 0.0857 0.6495 0.077 Uiso 1 1 calc R . . H35B H 1.3371 0.2388 0.6742 0.077 Uiso 1 1 calc R . . C36 C 1.3716(6) 0.2484(5) 0.57927(16) 0.0600(9) Uani 1 1 d . . . H36A H 1.2817 0.1820 0.5720 0.072 Uiso 1 1 calc R . . H36B H 1.2845 0.3680 0.5752 0.072 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 0.03512(18) 0.03498(18) 0.03257(18) -0.00539(11) -0.00492(11) -0.01488(12) N1 0.0317(12) 0.0451(14) 0.0323(12) -0.0041(11) -0.0041(10) -0.0166(11) N2 0.0395(13) 0.0373(14) 0.0316(12) -0.0044(10) -0.0095(10) -0.0132(11) C1 0.0438(17) 0.0440(17) 0.0400(16) -0.0023(14) -0.0059(14) -0.0161(15) O1 0.0657(16) 0.091(2) 0.0724(18) 0.0069(15) 0.0052(14) -0.0475(16) C2 0.0438(18) 0.057(2) 0.0480(18) -0.0124(16) 0.0021(14) -0.0251(16) O2 0.087(2) 0.091(2) 0.0821(19) -0.0543(18) 0.0073(16) -0.0457(17) C3 0.0439(17) 0.0431(18) 0.0453(17) -0.0041(15) 0.0000(14) -0.0198(15) O3 0.0669(16) 0.0529(15) 0.0791(18) 0.0222(14) -0.0147(14) -0.0131(13) C4 0.0417(18) 0.0432(17) 0.0433(17) 0.0050(14) -0.0083(14) -0.0202(14) O4 0.0505(15) 0.088(2) 0.0752(18) 0.0089(15) 0.0109(14) -0.0271(14) C5 0.0432(17) 0.0384(16) 0.0379(16) -0.0100(14) -0.0081(13) -0.0106(14) O5 0.0583(14) 0.0450(12) 0.0434(12) 0.0051(10) -0.0166(10) -0.0181(11) O6 0.0674(15) 0.0739(16) 0.0522(14) 0.0116(12) -0.0276(12) -0.0403(14) C11 0.0387(16) 0.059(2) 0.0377(16) -0.0014(14) -0.0060(13) -0.0252(15) C12 0.0392(17) 0.077(3) 0.0413(17) 0.0080(17) -0.0139(14) -0.0243(17) C13 0.0433(18) 0.058(2) 0.053(2) 0.0088(17) -0.0112(16) -0.0055(16) C14 0.0465(18) 0.0430(18) 0.0519(19) -0.0029(15) -0.0073(15) -0.0049(15) C15 0.0356(15) 0.0415(17) 0.0363(15) -0.0029(13) -0.0027(12) -0.0104(13) C16 0.0496(17) 0.0355(17) 0.0379(16) -0.0083(13) -0.0076(14) -0.0116(14) C17 0.0396(16) 0.0317(15) 0.0355(15) -0.0089(12) -0.0078(12) -0.0087(12) C18 0.0409(16) 0.0431(17) 0.0373(16) -0.0042(13) -0.0061(13) -0.0193(13) C19 0.0464(17) 0.0379(16) 0.0341(15) -0.0025(12) -0.0038(13) -0.0138(14) C20 0.0428(16) 0.0303(15) 0.0359(15) -0.0089(12) -0.0095(12) -0.0098(12) C21 0.0552(19) 0.0421(17) 0.0460(18) -0.0025(14) -0.0154(15) -0.0256(15) C22 0.0573(19) 0.0417(17) 0.0391(16) 0.0028(13) -0.0119(14) -0.0248(15) N31 0.0468(14) 0.0459(14) 0.0340(13) -0.0008(11) -0.0118(11) -0.0149(12) C32 0.0554(19) 0.0524(19) 0.0436(18) -0.0021(15) -0.0055(15) -0.0244(16) C33 0.0463(18) 0.0473(18) 0.0495(19) -0.0093(15) -0.0136(15) -0.0127(15) C34 0.067(2) 0.058(2) 0.0390(18) -0.0099(16) -0.0112(16) -0.0148(18) C35 0.070(2) 0.085(3) 0.0406(19) -0.0097(18) 0.0108(17) -0.032(2) C36 0.0447(19) 0.081(3) 0.055(2) -0.0107(19) -0.0025(16) -0.0220(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 Mo1 C2 1.960(3) . ? Mo1 C3 1.968(3) . ? Mo1 C4 2.025(3) . ? Mo1 C1 2.054(3) . ? Mo1 N2 2.251(2) . ? Mo1 N1 2.256(2) . ? N1 C11 1.347(4) . ? N1 C15 1.353(4) . ? N2 C16 1.284(4) . ? N2 C17 1.442(3) . ? C1 O1 1.133(4) . ? C2 O2 1.153(4) . ? C3 O3 1.154(4) . ? C4 O4 1.143(4) . ? C5 O6 1.252(4) . ? C5 O5 1.253(4) . ? C5 C20 1.520(4) . ? C11 C12 1.367(5) . ? C12 C13 1.370(5) . ? C13 C14 1.376(5) . ? C14 C15 1.379(4) . ? C15 C16 1.456(4) . ? C17 C18 1.380(4) . ? C17 C22 1.385(4) . ? C18 C19 1.386(4) . ? C19 C20 1.390(4) . ? C20 C21 1.386(4) . ? C21 C22 1.382(4) . ? N31 C36 1.480(4) . ? N31 C32 1.492(4) . ? C32 C33 1.513(4) . ? C33 C34 1.506(5) . ? C34 C35 1.517(5) . ? C35 C36 1.508(5) . ? 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 C3 87.77(14) . . ? C2 Mo1 C4 85.97(13) . . ? C3 Mo1 C4 87.46(12) . . ? C2 Mo1 C1 85.10(13) . . ? C3 Mo1 C1 85.29(12) . . ? C4 Mo1 C1 168.70(12) . . ? C2 Mo1 N2 170.89(11) . . ? C3 Mo1 N2 100.85(11) . . ? C4 Mo1 N2 91.43(11) . . ? C1 Mo1 N2 98.43(11) . . ? C2 Mo1 N1 99.48(12) . . ? C3 Mo1 N1 172.70(10) . . ? C4 Mo1 N1 93.86(10) . . ? C1 Mo1 N1 94.43(10) . . ? N2 Mo1 N1 71.95(8) . . ? C11 N1 C15 116.9(3) . . ? C11 N1 Mo1 126.3(2) . . ? C15 N1 Mo1 116.82(18) . . ? C16 N2 C17 118.8(2) . . ? C16 N2 Mo1 117.38(18) . . ? C17 N2 Mo1 123.40(17) . . ? O1 C1 Mo1 169.7(3) . . ? O2 C2 Mo1 178.3(3) . . ? O3 C3 Mo1 177.9(3) . . ? O4 C4 Mo1 173.3(3) . . ? O6 C5 O5 125.0(3) . . ? O6 C5 C20 117.5(3) . . ? O5 C5 C20 117.5(3) . . ? N1 C11 C12 122.7(3) . . ? C11 C12 C13 120.1(3) . . ? C12 C13 C14 118.3(3) . . ? C13 C14 C15 119.2(3) . . ? N1 C15 C14 122.7(3) . . ? N1 C15 C16 114.8(2) . . ? C14 C15 C16 122.4(3) . . ? N2 C16 C15 118.9(3) . . ? C18 C17 C22 120.8(3) . . ? C18 C17 N2 118.4(3) . . ? C22 C17 N2 120.7(3) . . ? C17 C18 C19 119.1(3) . . ? C18 C19 C20 120.9(3) . . ? C21 C20 C19 118.8(3) . . ? C21 C20 C5 121.7(3) . . ? C19 C20 C5 119.4(3) . . ? C22 C21 C20 120.9(3) . . ? C21 C22 C17 119.4(3) . . ? C36 N31 C32 112.5(3) . . ? N31 C32 C33 110.4(3) . . ? C34 C33 C32 111.7(3) . . ? C33 C34 C35 110.3(3) . . ? C36 C35 C34 111.0(3) . . ? N31 C36 C35 110.7(3) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.375 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.065 #===END data_Compound_5b_(rg89am) _database_code_depnum_ccdc_archive 'CCDC 281346' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H21.60 Mo N3 O6.30' _chemical_formula_weight 524.76 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.710(6) _cell_length_b 6.746(3) _cell_length_c 43.915(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.260(6) _cell_angle_gamma 90.00 _cell_volume 4654(3) _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 DARK_PURPLE _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 0.607 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.526901 _exptl_absorpt_correction_T_max 1.00000 _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 9975 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 0.93 _diffrn_reflns_theta_max 23.26 _reflns_number_total 3357 _reflns_number_gt 3081 _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^)+(0.0501P)^2^+50.3639P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3357 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.1896 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.430 _refine_ls_restrained_S_all 1.430 _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 0.19328(5) 0.07741(12) 0.924055(17) 0.0379(4) Uani 1 1 d . . . N1 N 0.0831(5) -0.0500(10) 0.94949(15) 0.0370(17) Uani 1 1 d . . . N2 N 0.0736(4) 0.1923(11) 0.90219(15) 0.0356(17) Uani 1 1 d . . . C1 C 0.2081(6) -0.1749(17) 0.8991(2) 0.051(3) Uani 1 1 d . . . O1 O 0.2297(6) -0.3142(14) 0.8869(2) 0.091(3) Uani 1 1 d . . . C2 C 0.2791(6) 0.2090(15) 0.8978(2) 0.046(2) Uani 1 1 d . . . O2 O 0.3284(5) 0.2814(15) 0.8831(2) 0.081(3) Uani 1 1 d . . . C3 C 0.2864(6) -0.0401(13) 0.9470(2) 0.044(2) Uani 1 1 d . . . O3 O 0.3409(5) -0.1193(12) 0.9604(2) 0.080(3) Uani 1 1 d . . . C4 C 0.2023(6) 0.3131(16) 0.9522(2) 0.043(2) Uani 1 1 d . . . O4 O 0.2165(6) 0.4401(14) 0.9684(2) 0.083(3) Uani 1 1 d . . . C5 C 0.1449(7) 0.409(3) 0.7979(2) 0.069(3) Uani 1 1 d . . . O5 O 0.1509(5) 0.5506(17) 0.77932(17) 0.087(3) Uani 1 1 d . . . O6 O 0.1696(8) 0.2444(18) 0.79289(18) 0.104(4) Uani 1 1 d . . . C11 C 0.0874(6) -0.1733(14) 0.9729(2) 0.047(2) Uani 1 1 d . . . H11 H 0.1411 -0.2114 0.9797 0.056 Uiso 1 1 calc R . . C12 C 0.0167(7) -0.2498(16) 0.9879(2) 0.057(3) Uani 1 1 d . . . H12 H 0.0231 -0.3308 1.0049 0.068 Uiso 1 1 calc R . . C13 C -0.0622(7) -0.2027(16) 0.9770(2) 0.058(3) Uani 1 1 d . . . H13 H -0.1106 -0.2544 0.9862 0.069 Uiso 1 1 calc R . . C14 C -0.0696(6) -0.0781(18) 0.9523(2) 0.054(3) Uani 1 1 d . . . H14 H -0.1228 -0.0427 0.9447 0.065 Uiso 1 1 calc R . . C15 C 0.0038(6) -0.0069(14) 0.93909(19) 0.038(2) Uani 1 1 d . . . C16 C 0.0026(6) 0.1330(15) 0.9138(2) 0.044(2) Uani 1 1 d . . . H16 H -0.0489 0.1791 0.9060 0.052 Uiso 1 1 calc R . . C17 C 0.0690(5) 0.3384(15) 0.87862(19) 0.039(2) Uani 1 1 d . . . C18 C 0.1095(5) 0.3088(16) 0.85120(19) 0.043(2) Uani 1 1 d . . . H18 H 0.1402 0.1930 0.8479 0.051 Uiso 1 1 calc R . . C19 C 0.1045(6) 0.4520(17) 0.8286(2) 0.048(2) Uani 1 1 d . . . C20 C 0.0632(7) 0.6250(18) 0.8342(2) 0.062(3) Uani 1 1 d . . . H20 H 0.0619 0.7230 0.8193 0.074 Uiso 1 1 calc R . . C21 C 0.0231(8) 0.6571(18) 0.8615(3) 0.067(3) Uani 1 1 d . . . H21 H -0.0055 0.7757 0.8650 0.080 Uiso 1 1 calc R . . C22 C 0.0254(6) 0.5148(15) 0.8836(2) 0.051(3) Uani 1 1 d . . . H22 H -0.0023 0.5358 0.9020 0.061 Uiso 1 1 calc R . . N31 N 0.1867(7) 0.2069(18) 0.7304(2) 0.079(3) Uani 1 1 d . . . H31A H 0.2385 0.1532 0.7277 0.094 Uiso 1 1 calc R . . H31B H 0.1832 0.2457 0.7500 0.094 Uiso 1 1 calc R . . C32 C 0.1233(11) 0.058(3) 0.7248(4) 0.120(6) Uani 1 1 d . . . H32A H 0.0675 0.1111 0.7296 0.144 Uiso 1 1 calc R . . H32B H 0.1336 -0.0546 0.7380 0.144 Uiso 1 1 calc R . . C33 C 0.1240(13) -0.010(4) 0.6922(5) 0.142(9) Uani 1 1 d . . . H33A H 0.1782 -0.0719 0.6878 0.170 Uiso 1 1 calc R . . H33B H 0.0794 -0.1068 0.6890 0.170 Uiso 1 1 calc R . . C34 C 0.1106(12) 0.161(4) 0.6715(4) 0.148(10) Uani 1 1 d . . . H34A H 0.0539 0.2150 0.6744 0.178 Uiso 1 1 calc R . . H34B H 0.1154 0.1183 0.6505 0.178 Uiso 1 1 calc R . . C35 C 0.1768(16) 0.321(3) 0.6782(4) 0.139(8) Uani 1 1 d . . . H35A H 0.2326 0.2723 0.6725 0.167 Uiso 1 1 calc R . . H35B H 0.1646 0.4368 0.6658 0.167 Uiso 1 1 calc R . . C36 C 0.1784(13) 0.380(2) 0.7109(3) 0.111(6) Uani 1 1 d . . . H36A H 0.2258 0.4693 0.7145 0.134 Uiso 1 1 calc R . . H36B H 0.1263 0.4502 0.7158 0.134 Uiso 1 1 calc R . . O90 O 0.0000 0.707(4) 0.7500 0.105(8) Uani 0.60 2 d SPG . . H90A H 0.0582 0.6300 0.7517 0.126 Uiso 0.60 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0334(5) 0.0397(5) 0.0408(5) 0.0018(4) 0.0048(3) 0.0051(4) N1 0.048(4) 0.024(4) 0.039(4) 0.000(3) 0.005(3) 0.004(3) N2 0.036(4) 0.040(4) 0.031(4) -0.001(3) 0.005(3) 0.007(3) C1 0.044(6) 0.056(7) 0.052(6) -0.020(5) 0.012(4) 0.004(5) O1 0.108(7) 0.065(6) 0.100(7) -0.035(5) 0.019(5) 0.011(6) C2 0.046(6) 0.043(6) 0.050(6) -0.006(5) 0.004(5) 0.010(5) O2 0.061(5) 0.091(7) 0.091(6) 0.015(5) 0.038(5) -0.003(5) C3 0.050(6) 0.025(5) 0.056(6) -0.004(4) -0.004(5) 0.004(4) O3 0.073(5) 0.057(5) 0.110(7) 0.004(5) -0.037(5) 0.015(5) C4 0.034(5) 0.044(6) 0.051(6) -0.005(5) 0.013(4) 0.005(4) O4 0.085(6) 0.065(6) 0.099(6) -0.037(5) 0.021(5) -0.006(5) C5 0.055(7) 0.102(11) 0.049(6) 0.011(8) 0.007(5) 0.002(8) O5 0.083(6) 0.134(9) 0.045(4) 0.034(5) 0.018(4) 0.014(6) O6 0.159(10) 0.110(9) 0.044(5) 0.004(5) 0.038(5) 0.036(8) C11 0.050(6) 0.037(5) 0.054(6) -0.001(5) 0.007(4) 0.001(5) C12 0.077(8) 0.040(6) 0.052(6) 0.008(5) 0.007(5) -0.012(6) C13 0.062(7) 0.049(7) 0.062(7) -0.004(5) 0.014(5) -0.024(6) C14 0.044(5) 0.066(7) 0.053(6) 0.001(6) 0.005(4) -0.013(6) C15 0.040(5) 0.041(5) 0.034(5) -0.002(4) 0.005(4) -0.005(4) C16 0.032(5) 0.057(7) 0.042(5) 0.003(4) 0.005(4) 0.004(4) C17 0.023(4) 0.055(6) 0.039(5) 0.007(4) 0.004(3) 0.005(4) C18 0.034(5) 0.055(6) 0.040(5) -0.002(5) 0.002(4) 0.008(5) C19 0.043(5) 0.061(7) 0.040(5) 0.011(5) 0.002(4) -0.002(5) C20 0.060(7) 0.069(8) 0.057(6) 0.032(6) 0.007(5) 0.007(6) C21 0.078(8) 0.057(7) 0.066(7) 0.012(6) 0.023(6) 0.031(6) C22 0.048(6) 0.053(7) 0.051(6) 0.004(5) 0.022(4) 0.012(5) N31 0.084(7) 0.098(9) 0.053(6) -0.013(6) 0.013(5) -0.009(7) C32 0.105(12) 0.147(17) 0.107(12) 0.002(12) 0.014(9) -0.043(13) C33 0.109(14) 0.18(2) 0.136(16) -0.062(16) -0.036(13) -0.035(14) C34 0.105(13) 0.23(3) 0.106(14) -0.060(17) -0.045(11) 0.073(17) C35 0.22(2) 0.124(16) 0.070(10) -0.001(11) 0.000(13) 0.024(18) C36 0.175(17) 0.077(11) 0.082(10) -0.008(9) 0.022(10) 0.002(11) O90 0.088(16) 0.103(19) 0.126(19) 0.000 -0.044(14) 0.000 _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 C3 1.943(10) . ? Mo1 C2 1.988(11) . ? Mo1 C4 2.017(11) . ? Mo1 C1 2.038(10) . ? Mo1 N1 2.236(7) . ? Mo1 N2 2.245(7) . ? N1 C11 1.323(12) . ? N1 C15 1.357(11) . ? N2 C16 1.292(11) . ? N2 C17 1.431(11) . ? C1 O1 1.135(12) . ? C2 O2 1.122(12) . ? C3 O3 1.167(11) . ? C4 O4 1.136(12) . ? C5 O6 1.195(17) . ? C5 O5 1.261(16) . ? C5 C19 1.521(15) . ? C11 C12 1.395(14) . ? C12 C13 1.363(15) . ? C13 C14 1.377(15) . ? C14 C15 1.379(13) . ? C15 C16 1.458(13) . ? C17 C18 1.379(12) . ? C17 C22 1.391(13) . ? C18 C19 1.387(14) . ? C19 C20 1.358(16) . ? C20 C21 1.377(15) . ? C21 C22 1.366(15) . ? N31 C32 1.435(19) . ? N31 C36 1.456(19) . ? C32 C33 1.50(2) . ? C33 C34 1.48(3) . ? C34 C35 1.53(3) . ? C35 C36 1.49(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Mo1 C2 88.4(4) . . ? C3 Mo1 C4 87.3(4) . . ? C2 Mo1 C4 87.5(4) . . ? C3 Mo1 C1 81.4(4) . . ? C2 Mo1 C1 89.0(4) . . ? C4 Mo1 C1 168.3(4) . . ? C3 Mo1 N1 99.6(3) . . ? C2 Mo1 N1 172.0(3) . . ? C4 Mo1 N1 92.9(3) . . ? C1 Mo1 N1 92.1(3) . . ? C3 Mo1 N2 172.0(3) . . ? C2 Mo1 N2 99.6(3) . . ? C4 Mo1 N2 92.6(3) . . ? C1 Mo1 N2 99.0(3) . . ? N1 Mo1 N2 72.4(3) . . ? C11 N1 C15 116.1(8) . . ? C11 N1 Mo1 126.3(6) . . ? C15 N1 Mo1 117.5(5) . . ? C16 N2 C17 117.2(7) . . ? C16 N2 Mo1 116.6(6) . . ? C17 N2 Mo1 125.9(5) . . ? O1 C1 Mo1 168.8(10) . . ? O2 C2 Mo1 179.0(10) . . ? O3 C3 Mo1 176.8(8) . . ? O4 C4 Mo1 172.4(9) . . ? O6 C5 O5 124.1(12) . . ? O6 C5 C19 118.5(12) . . ? O5 C5 C19 117.4(14) . . ? N1 C11 C12 124.2(10) . . ? C13 C12 C11 118.2(10) . . ? C12 C13 C14 119.5(9) . . ? C13 C14 C15 118.5(10) . . ? N1 C15 C14 123.4(9) . . ? N1 C15 C16 113.8(7) . . ? C14 C15 C16 122.6(9) . . ? N2 C16 C15 119.5(8) . . ? C18 C17 C22 119.4(9) . . ? C18 C17 N2 120.6(8) . . ? C22 C17 N2 119.9(8) . . ? C17 C18 C19 119.9(9) . . ? C20 C19 C18 119.7(9) . . ? C20 C19 C5 121.7(10) . . ? C18 C19 C5 118.6(11) . . ? C19 C20 C21 120.9(10) . . ? C22 C21 C20 119.9(10) . . ? C21 C22 C17 120.1(9) . . ? C32 N31 C36 113.6(13) . . ? N31 C32 C33 111.6(14) . . ? C34 C33 C32 110.2(19) . . ? C33 C34 C35 109.7(14) . . ? C36 C35 C34 112.4(17) . . ? N31 C36 C35 110.7(14) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.661 _refine_diff_density_min -1.316 _refine_diff_density_rms 0.116 #===END data_Compound_6a_(rg99ct) _database_code_depnum_ccdc_archive 'CCDC 281347' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17.10 H10.20 Cl0.20 Mo N2 O6' _chemical_formula_weight 442.70 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 24.17(3) _cell_length_b 10.648(11) _cell_length_c 16.561(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.79(2) _cell_angle_gamma 90.00 _cell_volume 4156(8) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description NEEDDLE _exptl_crystal_colour BLACK _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1762 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.329254 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _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 9235 _diffrn_reflns_av_R_equivalents 0.0902 _diffrn_reflns_av_sigmaI/netI 0.1072 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.40 _reflns_number_total 3007 _reflns_number_gt 985 _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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00233(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3007 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2523 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.2065 _refine_ls_wR_factor_gt 0.1765 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 0.30955(8) 0.15874(17) 0.23339(9) 0.0644(8) Uani 1 1 d . . . N1 N 0.3141(6) 0.0070(15) 0.1467(7) 0.056(4) Uani 1 1 d . . . N2 N 0.3642(6) 0.0040(15) 0.3011(7) 0.057(4) Uani 1 1 d . . . C1 C 0.3704(10) 0.246(3) 0.2192(14) 0.093(8) Uani 1 1 d . . . O1 O 0.4061(8) 0.3133(16) 0.2028(13) 0.138(7) Uani 1 1 d . . . C2 C 0.2659(12) 0.2764(18) 0.1612(13) 0.110(9) Uani 1 1 d . . . O2 O 0.2396(7) 0.3429(18) 0.1116(9) 0.138(6) Uani 1 1 d . . . C3 C 0.3071(7) 0.263(2) 0.3126(9) 0.060(6) Uani 1 1 d . . . O3 O 0.3051(5) 0.3387(14) 0.3675(7) 0.088(4) Uani 1 1 d . . . C4 C 0.2383(8) 0.0944(17) 0.2552(11) 0.057(6) Uani 1 1 d . . . O4 O 0.1944(7) 0.0710(14) 0.2702(12) 0.128(6) Uani 1 1 d . . . C5 C 0.4680(8) 0.015(2) 0.6373(9) 0.064(6) Uani 1 1 d . . . O5 O 0.4846(6) 0.1181(12) 0.6701(7) 0.076(4) Uani 1 1 d . . . H5 H 0.5000 0.1257 0.7500 0.5(4) Uiso 1 2 d SR . . O6 O 0.4739(6) -0.0832(13) 0.6769(7) 0.083(4) Uani 1 1 d . . . H6 H 0.5000 -0.0614 0.7500 0.100 Uiso 1 2 d SR . . C11 C 0.2910(7) 0.004(2) 0.0641(10) 0.065(6) Uani 1 1 d . . . H11 H 0.2719 0.0738 0.0387 0.077 Uiso 1 1 calc R . . C12 C 0.2951(9) -0.097(2) 0.0189(11) 0.073(7) Uani 1 1 d . . . H12 H 0.2777 -0.0970 -0.0372 0.088 Uiso 1 1 calc R . . C13 C 0.3240(11) -0.200(2) 0.0522(16) 0.091(9) Uani 1 1 d . . . H13 H 0.3283 -0.2690 0.0202 0.109 Uiso 1 1 calc R . . C14 C 0.3464(8) -0.197(2) 0.1348(12) 0.079(8) Uani 1 1 d . . . H14 H 0.3637 -0.2679 0.1614 0.095 Uiso 1 1 calc R . . C15 C 0.3440(9) -0.097(2) 0.1762(10) 0.060(6) Uani 1 1 d . . . C16 C 0.3688(7) -0.0940(19) 0.2589(10) 0.058(5) Uani 1 1 d . . . H16 H 0.3889 -0.1633 0.2842 0.069 Uiso 1 1 calc R . . C17 C 0.3912(7) 0.010(2) 0.3882(9) 0.049(5) Uani 1 1 d . . . C18 C 0.3906(7) -0.0951(18) 0.4331(10) 0.062(6) Uani 1 1 d . . . H18 H 0.3751 -0.1699 0.4093 0.075 Uiso 1 1 calc R . . C19 C 0.4148(8) -0.085(2) 0.5180(10) 0.071(6) Uani 1 1 d . . . H19 H 0.4121 -0.1518 0.5530 0.085 Uiso 1 1 calc R . . C20 C 0.4425(8) 0.022(2) 0.5499(11) 0.059(6) Uani 1 1 d . . . C21 C 0.4414(7) 0.1203(19) 0.5019(10) 0.058(6) Uani 1 1 d . . . H21 H 0.4580 0.1946 0.5250 0.070 Uiso 1 1 calc R . . C22 C 0.4169(8) 0.1179(18) 0.4200(10) 0.062(6) Uani 1 1 d . . . H22 H 0.4177 0.1879 0.3867 0.075 Uiso 1 1 calc R . . Cl91 Cl 0.585(2) 0.463(9) 0.515(5) 0.18(2) Uiso 0.10 1 d PG . . C90 C 0.526(4) 0.50(2) 0.436(5) 0.18(2) Uiso 0.10 1 d PG . . H90A H 0.5185 0.4378 0.3942 0.217 Uiso 0.10 1 d PG . . H90B H 0.5324 0.5814 0.4103 0.217 Uiso 0.10 1 d PG . . Cl92 Cl 0.468(2) 0.517(9) 0.484(5) 0.18(2) Uiso 0.10 1 d PG . . 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 0.0699(14) 0.0679(12) 0.0465(10) 0.0035(12) -0.0062(7) 0.0080(15) N1 0.037(10) 0.088(13) 0.042(9) 0.028(9) 0.007(7) 0.009(10) N2 0.062(11) 0.065(11) 0.033(9) -0.006(8) -0.010(7) 0.010(10) C1 0.050(17) 0.12(2) 0.104(18) 0.020(17) 0.017(14) 0.013(16) O1 0.109(16) 0.099(16) 0.209(19) -0.003(13) 0.043(14) -0.001(12) C2 0.18(3) 0.030(13) 0.087(17) -0.007(12) -0.033(17) 0.008(17) O2 0.142(15) 0.137(16) 0.104(12) 0.016(12) -0.040(10) 0.032(15) C3 0.063(14) 0.107(17) 0.015(9) 0.002(10) 0.015(9) 0.022(13) O3 0.091(10) 0.104(11) 0.062(8) 0.011(9) 0.004(7) 0.032(11) C4 0.031(14) 0.067(13) 0.072(12) -0.013(10) 0.007(10) 0.033(11) O4 0.041(10) 0.152(14) 0.196(15) -0.028(14) 0.034(10) -0.012(12) C5 0.064(14) 0.11(2) 0.010(11) -0.010(12) -0.006(9) -0.024(16) O5 0.091(10) 0.085(12) 0.038(7) -0.009(7) -0.018(6) -0.004(9) O6 0.097(11) 0.107(11) 0.031(7) 0.014(7) -0.014(7) -0.019(10) C11 0.059(14) 0.096(17) 0.032(11) 0.011(12) -0.004(10) -0.025(13) C12 0.105(19) 0.079(17) 0.038(12) -0.038(14) 0.019(12) -0.040(16) C13 0.13(3) 0.034(15) 0.12(2) -0.027(14) 0.06(2) -0.026(16) C14 0.082(16) 0.10(2) 0.043(13) -0.023(13) -0.011(12) 0.000(14) C15 0.082(16) 0.061(14) 0.031(12) -0.018(11) -0.002(11) 0.016(13) C16 0.054(13) 0.066(14) 0.049(12) -0.012(11) 0.002(10) 0.015(11) C17 0.045(13) 0.069(15) 0.031(11) 0.006(11) 0.004(9) 0.020(12) C18 0.060(14) 0.081(15) 0.037(11) 0.018(10) -0.008(9) -0.013(12) C19 0.074(16) 0.087(17) 0.045(12) 0.023(12) 0.002(11) 0.017(14) C20 0.065(15) 0.045(14) 0.057(14) 0.002(12) -0.002(11) 0.005(12) C21 0.046(12) 0.077(18) 0.044(11) -0.013(12) -0.005(9) -0.009(12) C22 0.067(14) 0.073(16) 0.040(11) -0.007(10) -0.005(9) 0.002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C3 1.729(19) . ? Mo1 C1 1.80(3) . ? Mo1 C2 1.89(2) . ? Mo1 C4 1.96(2) . ? Mo1 N1 2.180(15) . ? Mo1 N2 2.250(14) . ? N1 C15 1.35(2) . ? N1 C11 1.358(17) . ? N2 C16 1.274(18) . ? N2 C17 1.448(18) . ? C1 O1 1.20(2) . ? C2 O2 1.16(2) . ? C3 O3 1.224(18) . ? C4 O4 1.168(19) . ? C5 O6 1.22(2) . ? C5 O5 1.25(2) . ? C5 C20 1.44(2) . ? C11 C12 1.32(2) . ? C12 C13 1.35(2) . ? C13 C14 1.36(3) . ? C14 C15 1.27(2) . ? C15 C16 1.37(2) . ? C17 C18 1.35(2) . ? C17 C22 1.35(2) . ? C18 C19 1.40(2) . ? C19 C20 1.36(2) . ? C20 C21 1.31(2) . ? C21 C22 1.35(2) . ? Cl91 Cl92 1.30(10) 5_666 ? Cl91 C90 1.7612 . ? C90 Cl92 1.32(12) 5_666 ? C90 Cl92 1.7689 . ? Cl92 Cl91 1.30(10) 5_666 ? Cl92 C90 1.32(16) 5_666 ? Cl92 Cl92 1.58(10) 5_666 ? 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 Mo1 C1 86.2(10) . . ? C3 Mo1 C2 87.0(8) . . ? C1 Mo1 C2 86.1(11) . . ? C3 Mo1 C4 84.6(8) . . ? C1 Mo1 C4 169.0(9) . . ? C2 Mo1 C4 87.6(10) . . ? C3 Mo1 N1 172.0(7) . . ? C1 Mo1 N1 97.9(9) . . ? C2 Mo1 N1 100.2(7) . . ? C4 Mo1 N1 92.1(6) . . ? C3 Mo1 N2 101.9(6) . . ? C1 Mo1 N2 92.2(8) . . ? C2 Mo1 N2 170.8(8) . . ? C4 Mo1 N2 95.5(6) . . ? N1 Mo1 N2 71.1(5) . . ? C15 N1 C11 114.2(16) . . ? C15 N1 Mo1 117.9(11) . . ? C11 N1 Mo1 127.9(15) . . ? C16 N2 C17 120.6(16) . . ? C16 N2 Mo1 116.1(11) . . ? C17 N2 Mo1 123.3(12) . . ? O1 C1 Mo1 172(2) . . ? O2 C2 Mo1 175(2) . . ? O3 C3 Mo1 178.6(16) . . ? O4 C4 Mo1 171.8(17) . . ? O6 C5 O5 121.9(15) . . ? O6 C5 C20 124(2) . . ? O5 C5 C20 114(2) . . ? C12 C11 N1 121.7(19) . . ? C11 C12 C13 121.4(19) . . ? C12 C13 C14 116.8(19) . . ? C15 C14 C13 120(2) . . ? C14 C15 N1 125.0(16) . . ? C14 C15 C16 120(2) . . ? N1 C15 C16 115.2(18) . . ? N2 C16 C15 119.6(19) . . ? C18 C17 C22 123.4(15) . . ? C18 C17 N2 117.0(18) . . ? C22 C17 N2 119.6(17) . . ? C17 C18 C19 115.8(18) . . ? C20 C19 C18 120.9(18) . . ? C21 C20 C19 119.2(17) . . ? C21 C20 C5 126(2) . . ? C19 C20 C5 114(2) . . ? C20 C21 C22 122.5(18) . . ? C17 C22 C21 117.8(18) . . ? Cl92 Cl91 C90 48(6) 5_666 . ? Cl92 C90 Cl91 47(4) 5_666 . ? Cl92 C90 Cl92 60(4) 5_666 . ? Cl91 C90 Cl92 106.8 . . ? Cl91 Cl92 C90 85(6) 5_666 5_666 ? Cl91 Cl92 Cl92 159(10) 5_666 5_666 ? C90 Cl92 Cl92 75(6) 5_666 5_666 ? Cl91 Cl92 C90 155(6) 5_666 . ? C90 Cl92 C90 120(5) 5_666 . ? Cl92 Cl92 C90 46(4) 5_666 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 23.40 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.784 _refine_diff_density_min -0.693 _refine_diff_density_rms 0.153 #===END