# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Comp1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H52 Cu2 Mo N16, 5(O)' _chemical_formula_sum 'C72 H52 Cu2 Mo N16 O5' _chemical_formula_weight 1444.31 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 2' _space_group_name_Hall 'C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.2194(18) _cell_length_b 11.4434(18) _cell_length_c 19.218(3) _cell_angle_alpha 90 _cell_angle_beta 90.342(4) _cell_angle_gamma 90 _cell_volume 3346.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.4625 _cell_measurement_theta_max 17.9785 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.433 _exptl_crystal_F_000 1472 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.260 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 0.878 _shelx_estimated_absorpt_T_min 0.804 _shelx_estimated_absorpt_T_max 0.991 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8038 _exptl_absorpt_correction_T_max 0.9913 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 10164 _diffrn_reflns_av_unetI/netI 0.1858 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.060 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.953 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.953 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.718 _diffrn_reflns_point_group_measured_fraction_full 0.771 _reflns_number_total 5528 _reflns_number_gt 3425 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.435 _reflns_Friedel_fraction_max 0.458 _reflns_Friedel_fraction_full 0.520 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 726 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.01(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 5528 _refine_ls_number_parameters 421 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.72738(8) 0.78116(11) 0.87992(7) 0.0250(4) Uani 1 1 d . . . . . Mo1 Mo 1.0000 1.00842(9) 1.0000 0.0163(3) Uani 1 2 d S T P . . N1 N 0.7886(6) 0.6488(8) 0.8340(5) 0.027(2) Uani 1 1 d . . . . . N2 N 0.7932(7) 0.8808(9) 0.7967(5) 0.038(3) Uani 1 1 d . . . . . H2 H 0.8333 0.9349 0.8227 0.045 Uiso 1 1 calc R U . . . N3 N 0.6038(6) 0.7505(8) 0.8034(4) 0.032(2) Uani 1 1 d . . . . . H3 H 0.5710 0.6823 0.8230 0.038 Uiso 1 1 calc R U . . . N4 N 0.6553(6) 0.9209(8) 0.9004(5) 0.031(2) Uani 1 1 d . . . . . N5 N 0.8451(6) 0.8331(8) 0.9406(5) 0.027(2) Uani 1 1 d . . . . . N6 N 1.1603(5) 1.1826(8) 0.9495(5) 0.023(2) Uani 1 1 d . . . . . N7 N 0.9222(6) 1.1416(10) 0.8587(5) 0.041(3) Uani 1 1 d . . . . . N8 N 1.0839(7) 0.8871(9) 0.8573(5) 0.039(3) Uani 1 1 d . . . . . C1 C 0.7758(7) 0.5343(11) 0.8510(6) 0.038(3) Uani 1 1 d . . . . . H5 H 0.7452 0.5165 0.8926 0.045 Uiso 1 1 calc R U . . . C2 C 0.8052(8) 0.4437(12) 0.8105(7) 0.043(3) Uani 1 1 d . . . . . H6 H 0.7959 0.3649 0.8241 0.052 Uiso 1 1 calc R U . . . C3 C 0.8486(9) 0.4698(13) 0.7498(8) 0.052(4) Uani 1 1 d . . . . . H7 H 0.8676 0.4091 0.7197 0.063 Uiso 1 1 calc R U . . . C4 C 0.8638(8) 0.5830(11) 0.7335(6) 0.035(3) Uani 1 1 d . . . . . H8 H 0.8951 0.6018 0.6924 0.041 Uiso 1 1 calc R U . . . C5 C 0.8344(7) 0.6714(11) 0.7762(6) 0.032(3) Uani 1 1 d . . . . . C6 C 0.8560(8) 0.7968(12) 0.7605(7) 0.041(3) Uani 1 1 d . . . . . H9 H 0.8527 0.8097 0.7096 0.050 Uiso 1 1 calc R U . . . H10 H 0.9169 0.8135 0.7759 0.050 Uiso 1 1 calc R U . . . C7 C 0.7413(8) 0.9568(11) 0.7554(6) 0.032(3) Uani 1 1 d . . . . . C8 C 0.7409(9) 1.0750(11) 0.7733(7) 0.048(4) Uani 1 1 d . . . . . H11 H 0.7788 1.1018 0.8093 0.058 Uiso 1 1 calc R U . . . C9 C 0.6877(8) 1.1521(12) 0.7405(7) 0.048(4) Uani 1 1 d . . . . . H12 H 0.6887 1.2321 0.7538 0.058 Uiso 1 1 calc R U . . . C10 C 0.6319(8) 1.1156(11) 0.6876(7) 0.040(3) Uani 1 1 d . . . . . C11 C 0.5762(8) 1.1941(12) 0.6524(7) 0.047(4) Uani 1 1 d . . . . . H13 H 0.5787 1.2751 0.6630 0.056 Uiso 1 1 calc R U . . . C12 C 0.5180(9) 1.1542(14) 0.6028(7) 0.049(4) Uani 1 1 d . . . . . H14 H 0.4823 1.2083 0.5780 0.059 Uiso 1 1 calc R U . . . C13 C 0.5110(8) 1.0393(13) 0.5889(6) 0.045(4) Uani 1 1 d . . . . . H15 H 0.4680 1.0132 0.5564 0.054 Uiso 1 1 calc R U . . . C14 C 0.5647(7) 0.9596(11) 0.6206(6) 0.032(3) Uani 1 1 d . . . . . H16 H 0.5597 0.8789 0.6096 0.038 Uiso 1 1 calc R U . . . C15 C 0.6276(7) 0.9978(12) 0.6696(5) 0.029(3) Uani 1 1 d . . . . . C16 C 0.6848(7) 0.9151(10) 0.7060(6) 0.029(3) Uani 1 1 d . . . . . C17 C 0.6737(6) 0.7877(10) 0.6906(5) 0.025(2) Uani 1 1 d . . . . . C18 C 0.7071(7) 0.7391(10) 0.6289(6) 0.028(3) Uani 1 1 d . . . . . C19 C 0.7557(7) 0.8096(11) 0.5809(6) 0.038(3) Uani 1 1 d . . . . . H17 H 0.7627 0.8911 0.5889 0.046 Uiso 1 1 calc R U . . . C20 C 0.7925(9) 0.7570(14) 0.5227(6) 0.050(4) Uani 1 1 d . . . . . H18 H 0.8231 0.8044 0.4902 0.060 Uiso 1 1 calc R U . . . C21 C 0.7861(9) 0.6379(14) 0.5102(7) 0.050(4) Uani 1 1 d . . . . . H19 H 0.8145 0.6035 0.4714 0.060 Uiso 1 1 calc R U . . . C22 C 0.7380(8) 0.5709(12) 0.5550(6) 0.045(4) Uani 1 1 d . . . . . H20 H 0.7307 0.4899 0.5456 0.054 Uiso 1 1 calc R U . . . C23 C 0.6992(8) 0.6189(10) 0.6144(6) 0.035(3) Uani 1 1 d . . . . . C24 C 0.6556(7) 0.5478(10) 0.6626(6) 0.036(3) Uani 1 1 d . . . . . H21 H 0.6481 0.4667 0.6537 0.043 Uiso 1 1 calc R U . . . C25 C 0.6252(8) 0.5943(10) 0.7204(6) 0.037(3) Uani 1 1 d . . . . . H22 H 0.5966 0.5445 0.7528 0.044 Uiso 1 1 calc R U . . . C26 C 0.6328(7) 0.7149(9) 0.7369(6) 0.028(3) Uani 1 1 d . . . . . C27 C 0.5464(7) 0.8523(9) 0.8128(6) 0.028(3) Uani 1 1 d . . . . . H23 H 0.4877 0.8244 0.8271 0.034 Uiso 1 1 calc R U . . . H24 H 0.5394 0.8920 0.7673 0.034 Uiso 1 1 calc R U . . . C28 C 0.5781(7) 0.9394(9) 0.8648(5) 0.024(3) Uani 1 1 d . . . . . C29 C 0.5306(8) 1.0382(10) 0.8771(6) 0.038(3) Uani 1 1 d . . . . . H25 H 0.4767 1.0503 0.8529 0.046 Uiso 1 1 calc R U . . . C30 C 0.5594(8) 1.1203(11) 0.9240(7) 0.047(4) Uani 1 1 d . . . . . H26 H 0.5264 1.1894 0.9318 0.056 Uiso 1 1 calc R U . . . C31 C 0.6370(9) 1.1010(12) 0.9594(8) 0.055(4) Uani 1 1 d . . . . . H27 H 0.6589 1.1564 0.9920 0.066 Uiso 1 1 calc R U . . . C32 C 0.6809(8) 1.0008(13) 0.9462(6) 0.047(3) Uani 1 1 d . . . . . H28 H 0.7337 0.9866 0.9715 0.056 Uiso 1 1 calc R U . . . C33 C 0.9009(7) 0.8916(9) 0.9636(5) 0.021(2) Uani 1 1 d . . . . . C34 C 1.1037(7) 1.1248(9) 0.9699(5) 0.020(2) Uani 1 1 d . . . . . C35 C 0.9498(6) 1.0970(9) 0.9091(6) 0.025(3) Uani 1 1 d . . . . . C36 C 1.0562(8) 0.9274(10) 0.9082(7) 0.028(3) Uani 1 1 d . . . . . O1 O 0.5000 0.474(3) 0.5000 0.241(14) Uiso 1 2 d S . P . . O3 O 0.587(2) 0.603(3) 0.3725(16) 0.352(17) Uiso 1 1 d . . . . . O2 O 0.452(2) 0.713(4) 0.5475(19) 0.43(2) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0239(8) 0.0255(9) 0.0254(8) -0.0007(6) -0.0032(6) 0.0027(6) Mo1 0.0127(7) 0.0152(7) 0.0209(8) 0.000 -0.0016(6) 0.000 N1 0.026(6) 0.033(6) 0.022(6) -0.004(4) -0.007(4) 0.003(5) N2 0.041(7) 0.036(7) 0.036(7) -0.011(5) -0.021(5) 0.000(5) N3 0.049(6) 0.022(6) 0.024(5) 0.003(4) 0.005(5) 0.001(5) N4 0.030(6) 0.027(6) 0.036(6) -0.001(5) -0.008(5) 0.007(5) N5 0.028(6) 0.023(5) 0.028(6) 0.000(4) -0.010(4) -0.007(4) N6 0.015(5) 0.023(5) 0.031(6) 0.004(4) -0.005(4) -0.003(4) N7 0.028(6) 0.056(8) 0.039(7) 0.018(6) -0.011(5) -0.008(5) N8 0.047(7) 0.033(6) 0.039(7) -0.006(5) 0.009(5) 0.005(5) C1 0.028(6) 0.046(10) 0.038(7) 0.002(6) -0.005(5) 0.009(6) C2 0.039(8) 0.037(8) 0.054(10) -0.011(7) -0.012(7) 0.001(6) C3 0.038(8) 0.061(11) 0.058(10) -0.032(8) -0.006(7) 0.022(7) C4 0.028(7) 0.047(9) 0.029(7) -0.015(6) 0.007(6) 0.004(6) C5 0.013(6) 0.050(8) 0.034(8) -0.004(6) -0.007(5) 0.000(6) C6 0.036(7) 0.044(9) 0.044(8) 0.012(7) -0.017(6) -0.003(7) C7 0.029(7) 0.035(7) 0.031(7) 0.003(6) -0.007(6) -0.005(6) C8 0.059(10) 0.030(8) 0.055(9) -0.010(7) -0.027(8) -0.017(7) C9 0.049(9) 0.028(8) 0.067(10) 0.007(7) -0.026(8) -0.009(7) C10 0.038(8) 0.029(8) 0.054(9) 0.010(6) 0.006(7) -0.011(6) C11 0.044(9) 0.033(8) 0.063(10) 0.026(7) 0.002(7) 0.001(7) C12 0.039(9) 0.061(11) 0.047(10) 0.031(8) 0.013(7) 0.020(8) C13 0.036(8) 0.072(12) 0.026(7) 0.009(7) -0.004(6) 0.003(7) C14 0.020(6) 0.041(8) 0.035(7) -0.001(6) -0.003(5) -0.002(5) C15 0.027(6) 0.028(7) 0.031(6) 0.015(6) 0.006(5) 0.000(6) C16 0.027(6) 0.032(7) 0.028(7) 0.013(5) -0.010(5) -0.002(6) C17 0.023(6) 0.029(6) 0.023(6) 0.004(5) -0.004(5) 0.002(5) C18 0.021(6) 0.038(7) 0.025(7) -0.002(5) -0.001(5) 0.005(5) C19 0.032(7) 0.047(9) 0.036(8) 0.009(6) 0.000(6) 0.008(6) C20 0.053(9) 0.072(12) 0.025(7) 0.010(7) 0.012(6) 0.008(8) C21 0.049(9) 0.061(11) 0.040(9) -0.023(7) 0.011(7) 0.015(8) C22 0.037(8) 0.061(10) 0.037(8) -0.017(7) -0.005(6) -0.002(7) C23 0.035(7) 0.036(8) 0.034(7) -0.002(6) -0.004(6) -0.007(6) C24 0.041(7) 0.033(7) 0.033(7) -0.017(5) -0.003(6) -0.010(6) C25 0.041(8) 0.027(7) 0.042(8) 0.007(6) -0.015(6) -0.008(6) C26 0.029(7) 0.020(6) 0.033(7) -0.005(5) -0.009(5) 0.005(5) C27 0.031(7) 0.024(6) 0.029(7) 0.002(5) -0.003(5) -0.002(5) C28 0.029(7) 0.019(6) 0.025(7) 0.003(5) -0.005(5) 0.003(5) C29 0.040(7) 0.034(8) 0.041(8) -0.001(6) -0.008(6) 0.003(6) C30 0.043(9) 0.032(8) 0.065(10) -0.018(7) -0.002(7) 0.012(7) C31 0.048(9) 0.038(9) 0.079(11) -0.032(8) -0.024(8) 0.004(7) C32 0.044(7) 0.053(9) 0.043(7) -0.019(8) -0.014(6) 0.017(8) C33 0.019(6) 0.022(6) 0.022(6) 0.001(5) 0.002(5) 0.004(5) C34 0.021(6) 0.017(6) 0.021(6) -0.008(5) -0.008(5) 0.008(5) C35 0.015(6) 0.027(7) 0.032(7) -0.001(5) -0.003(5) -0.005(5) C36 0.027(7) 0.021(7) 0.037(8) -0.001(6) 0.006(6) -0.006(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 Cu1 N4 1.980(9) . ? Cu1 N1 1.987(9) . ? Cu1 N6 2.029(9) 3_445 ? Cu1 N2 2.209(11) . ? Cu1 N5 2.213(9) . ? Cu1 N3 2.406(9) . ? Mo1 C33 2.131(11) . ? Mo1 C33 2.131(11) 2_757 ? Mo1 C34 2.147(12) 2_757 ? Mo1 C34 2.147(12) . ? Mo1 C35 2.155(11) . ? Mo1 C35 2.155(11) 2_757 ? Mo1 C36 2.173(13) . ? Mo1 C36 2.173(13) 2_757 ? N1 C5 1.340(14) . ? N1 C1 1.365(15) . ? N2 C7 1.416(14) . ? N2 C6 1.525(16) . ? N2 H2 1.0000 . ? N3 C26 1.414(14) . ? N3 C27 1.467(13) . ? N3 H3 1.0000 . ? N4 C32 1.326(14) . ? N4 C28 1.372(12) . ? N5 C33 1.166(11) . ? N6 C34 1.156(13) . ? N6 Cu1 2.029(9) 3 ? N7 C35 1.172(12) . ? N8 C36 1.163(14) . ? C1 C2 1.373(16) . ? C1 H5 0.9500 . ? C2 C3 1.378(18) . ? C2 H6 0.9500 . ? C3 C4 1.353(18) . ? C3 H7 0.9500 . ? C4 C5 1.378(15) . ? C4 H8 0.9500 . ? C5 C6 1.504(17) . ? C6 H9 0.9900 . ? C6 H10 0.9900 . ? C7 C16 1.364(14) . ? C7 C8 1.395(15) . ? C8 C9 1.351(16) . ? C8 H11 0.9500 . ? C9 C10 1.385(16) . ? C9 H12 0.9500 . ? C10 C15 1.393(17) . ? C10 C11 1.406(16) . ? C11 C12 1.376(18) . ? C11 H13 0.9500 . ? C12 C13 1.345(19) . ? C12 H14 0.9500 . ? C13 C14 1.365(16) . ? C13 H15 0.9500 . ? C14 C15 1.409(14) . ? C14 H16 0.9500 . ? C15 C16 1.462(14) . ? C16 C17 1.497(15) . ? C17 C26 1.371(15) . ? C17 C18 1.408(14) . ? C18 C23 1.408(15) . ? C18 C19 1.434(15) . ? C19 C20 1.392(17) . ? C19 H17 0.9500 . ? C20 C21 1.387(19) . ? C20 H18 0.9500 . ? C21 C22 1.368(18) . ? C21 H19 0.9500 . ? C22 C23 1.401(16) . ? C22 H20 0.9500 . ? C23 C24 1.403(16) . ? C24 C25 1.319(16) . ? C24 H21 0.9500 . ? C25 C26 1.421(14) . ? C25 H22 0.9500 . ? C27 C28 1.491(14) . ? C27 H23 0.9900 . ? C27 H24 0.9900 . ? C28 C29 1.364(14) . ? C29 C30 1.371(15) . ? C29 H25 0.9500 . ? C30 C31 1.377(16) . ? C30 H26 0.9500 . ? C31 C32 1.353(17) . ? C31 H27 0.9500 . ? C32 H28 0.9500 . ? 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 N4 Cu1 N1 164.9(4) . . ? N4 Cu1 N6 92.1(4) . 3_445 ? N1 Cu1 N6 96.2(4) . 3_445 ? N4 Cu1 N2 88.9(4) . . ? N1 Cu1 N2 81.7(4) . . ? N6 Cu1 N2 174.8(4) 3_445 . ? N4 Cu1 N5 97.2(4) . . ? N1 Cu1 N5 93.3(3) . . ? N6 Cu1 N5 102.2(3) 3_445 . ? N2 Cu1 N5 82.7(3) . . ? N4 Cu1 N3 78.9(3) . . ? N1 Cu1 N3 89.1(3) . . ? N6 Cu1 N3 85.8(3) 3_445 . ? N2 Cu1 N3 89.4(3) . . ? N5 Cu1 N3 171.3(3) . . ? C33 Mo1 C33 102.3(5) . 2_757 ? C33 Mo1 C34 87.6(4) . 2_757 ? C33 Mo1 C34 145.2(4) 2_757 2_757 ? C33 Mo1 C34 145.2(4) . . ? C33 Mo1 C34 87.6(4) 2_757 . ? C34 Mo1 C34 103.3(5) 2_757 . ? C33 Mo1 C35 77.4(4) . . ? C33 Mo1 C35 143.9(4) 2_757 . ? C34 Mo1 C35 70.7(4) 2_757 . ? C34 Mo1 C35 75.4(4) . . ? C33 Mo1 C35 143.9(4) . 2_757 ? C33 Mo1 C35 77.4(4) 2_757 2_757 ? C34 Mo1 C35 75.4(4) 2_757 2_757 ? C34 Mo1 C35 70.7(4) . 2_757 ? C35 Mo1 C35 123.9(6) . 2_757 ? C33 Mo1 C36 75.4(4) . . ? C33 Mo1 C36 73.6(4) 2_757 . ? C34 Mo1 C36 141.0(4) 2_757 . ? C34 Mo1 C36 75.7(4) . . ? C35 Mo1 C36 71.5(4) . . ? C35 Mo1 C36 136.0(4) 2_757 . ? C33 Mo1 C36 73.6(4) . 2_757 ? C33 Mo1 C36 75.4(4) 2_757 2_757 ? C34 Mo1 C36 75.7(4) 2_757 2_757 ? C34 Mo1 C36 141.0(4) . 2_757 ? C35 Mo1 C36 136.0(4) . 2_757 ? C35 Mo1 C36 71.5(4) 2_757 2_757 ? C36 Mo1 C36 129.5(6) . 2_757 ? C5 N1 C1 117.3(10) . . ? C5 N1 Cu1 117.9(8) . . ? C1 N1 Cu1 123.9(8) . . ? C7 N2 C6 118.7(10) . . ? C7 N2 Cu1 118.0(8) . . ? C6 N2 Cu1 107.0(7) . . ? C7 N2 H2 103.7 . . ? C6 N2 H2 103.7 . . ? Cu1 N2 H2 103.7 . . ? C26 N3 C27 121.9(8) . . ? C26 N3 Cu1 110.3(7) . . ? C27 N3 Cu1 105.8(6) . . ? C26 N3 H3 105.9 . . ? C27 N3 H3 105.9 . . ? Cu1 N3 H3 105.9 . . ? C32 N4 C28 118.1(10) . . ? C32 N4 Cu1 121.9(8) . . ? C28 N4 Cu1 120.0(7) . . ? C33 N5 Cu1 160.0(9) . . ? C34 N6 Cu1 156.9(9) . 3 ? N1 C1 C2 122.8(12) . . ? N1 C1 H5 118.6 . . ? C2 C1 H5 118.6 . . ? C3 C2 C1 118.5(13) . . ? C3 C2 H6 120.8 . . ? C1 C2 H6 120.8 . . ? C2 C3 C4 119.1(12) . . ? C2 C3 H7 120.4 . . ? C4 C3 H7 120.4 . . ? C3 C4 C5 120.6(12) . . ? C3 C4 H8 119.7 . . ? C5 C4 H8 119.7 . . ? N1 C5 C4 121.6(12) . . ? N1 C5 C6 117.7(11) . . ? C4 C5 C6 120.6(12) . . ? C5 C6 N2 111.8(11) . . ? C5 C6 H9 109.2 . . ? N2 C6 H9 109.2 . . ? C5 C6 H10 109.2 . . ? N2 C6 H10 109.2 . . ? H9 C6 H10 107.9 . . ? C16 C7 C8 120.5(11) . . ? C16 C7 N2 121.5(11) . . ? C8 C7 N2 117.4(11) . . ? C9 C8 C7 121.5(12) . . ? C9 C8 H11 119.3 . . ? C7 C8 H11 119.3 . . ? C8 C9 C10 120.5(13) . . ? C8 C9 H12 119.7 . . ? C10 C9 H12 119.7 . . ? C15 C10 C9 120.2(12) . . ? C15 C10 C11 118.1(11) . . ? C9 C10 C11 121.7(12) . . ? C12 C11 C10 120.4(13) . . ? C12 C11 H13 119.8 . . ? C10 C11 H13 119.8 . . ? C13 C12 C11 120.8(13) . . ? C13 C12 H14 119.6 . . ? C11 C12 H14 119.6 . . ? C12 C13 C14 121.2(12) . . ? C12 C13 H15 119.4 . . ? C14 C13 H15 119.4 . . ? C13 C14 C15 119.5(12) . . ? C13 C14 H16 120.2 . . ? C15 C14 H16 120.2 . . ? C10 C15 C14 119.9(11) . . ? C10 C15 C16 118.7(10) . . ? C14 C15 C16 121.3(11) . . ? C7 C16 C15 118.6(10) . . ? C7 C16 C17 123.3(10) . . ? C15 C16 C17 118.0(9) . . ? C26 C17 C18 118.3(11) . . ? C26 C17 C16 120.9(10) . . ? C18 C17 C16 120.7(10) . . ? C23 C18 C17 121.4(11) . . ? C23 C18 C19 117.8(11) . . ? C17 C18 C19 120.6(11) . . ? C20 C19 C18 119.0(12) . . ? C20 C19 H17 120.5 . . ? C18 C19 H17 120.5 . . ? C19 C20 C21 122.4(13) . . ? C19 C20 H18 118.8 . . ? C21 C20 H18 118.8 . . ? C22 C21 C20 118.7(13) . . ? C22 C21 H19 120.7 . . ? C20 C21 H19 120.7 . . ? C21 C22 C23 121.5(13) . . ? C21 C22 H20 119.3 . . ? C23 C22 H20 119.3 . . ? C22 C23 C18 120.6(12) . . ? C22 C23 C24 120.9(12) . . ? C18 C23 C24 118.5(11) . . ? C25 C24 C23 119.5(12) . . ? C25 C24 H21 120.3 . . ? C23 C24 H21 120.3 . . ? C24 C25 C26 123.5(12) . . ? C24 C25 H22 118.3 . . ? C26 C25 H22 118.3 . . ? C17 C26 C25 118.8(11) . . ? C17 C26 N3 123.9(10) . . ? C25 C26 N3 117.1(11) . . ? N3 C27 C28 115.0(8) . . ? N3 C27 H23 108.5 . . ? C28 C27 H23 108.5 . . ? N3 C27 H24 108.5 . . ? C28 C27 H24 108.5 . . ? H23 C27 H24 107.5 . . ? C29 C28 N4 119.7(10) . . ? C29 C28 C27 120.1(9) . . ? N4 C28 C27 120.3(9) . . ? C28 C29 C30 120.9(11) . . ? C28 C29 H25 119.6 . . ? C30 C29 H25 119.6 . . ? C31 C30 C29 119.1(12) . . ? C31 C30 H26 120.5 . . ? C29 C30 H26 120.5 . . ? C32 C31 C30 117.8(12) . . ? C32 C31 H27 121.1 . . ? C30 C31 H27 121.1 . . ? N4 C32 C31 124.4(11) . . ? N4 C32 H28 117.8 . . ? C31 C32 H28 117.8 . . ? N5 C33 Mo1 175.6(10) . . ? N6 C34 Mo1 175.1(9) . . ? N7 C35 Mo1 177.8(10) . . ? N8 C36 Mo1 177.0(11) . . ? _refine_diff_density_max 0.762 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.127 _shelxl_version_number 2013-4 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71073 15.2194 11.4434 19.2178 90.0000 90.3420 90.0000 ZERR 2.0 0.0018 0.0018 0.0027 0.0000 0.0040 0.0000 LATT -7 SYMM -X, +Y, -Z REM SPGR C2 monoclinic SFAC C H N O Cu Mo UNIT 144 104 32 10 4 2 SIZE 0.26 0.26 0.01 TEMP -173.0 L.S. 20 FMAP 2 PLAN -5 ACTA BOND $H MERG 2 OMIT -10.000000 55.000000 FREE H37B O7 FREE C37 O7 WGHT 0.048000 FVAR 0.16755 CU1 5 0.727380 0.781164 0.879920 11.00000 0.02388 0.02552 = 0.02542 -0.00071 -0.00324 0.00272 MO1 6 1.000000 1.008424 1.000000 10.50000 0.01265 0.01521 = 0.02089 0.00000 -0.00163 0.00000 N1 3 0.788634 0.648826 0.834043 11.00000 0.02593 0.03325 = 0.02178 -0.00444 -0.00745 0.00299 N2 3 0.793245 0.880802 0.796748 11.00000 0.04115 0.03594 = 0.03602 -0.01097 -0.02097 -0.00026 AFIX 13 H2 2 0.833295 0.934882 0.822720 11.00000 -1.20000 AFIX 0 N3 3 0.603770 0.750454 0.803434 11.00000 0.04945 0.02226 = 0.02383 0.00299 0.00467 0.00113 AFIX 13 H3 2 0.570978 0.682334 0.822974 11.00000 -1.20000 AFIX 0 N4 3 0.655329 0.920894 0.900390 11.00000 0.03039 0.02709 = 0.03625 -0.00114 -0.00838 0.00739 N5 3 0.845087 0.833140 0.940568 11.00000 0.02849 0.02331 = 0.02762 -0.00021 -0.01035 -0.00731 N6 3 1.160329 1.182573 0.949486 11.00000 0.01485 0.02259 = 0.03109 0.00416 -0.00508 -0.00257 N7 3 0.922158 1.141627 0.858658 11.00000 0.02765 0.05565 = 0.03928 0.01801 -0.01138 -0.00770 N8 3 1.083944 0.887113 0.857318 11.00000 0.04692 0.03279 = 0.03854 -0.00645 0.00931 0.00508 C1 1 0.775789 0.534296 0.851018 11.00000 0.02831 0.04612 = 0.03832 0.00161 -0.00486 0.00867 AFIX 43 H5 2 0.745173 0.516505 0.892629 11.00000 -1.20000 AFIX 0 C2 1 0.805216 0.443738 0.810538 11.00000 0.03881 0.03694 = 0.05448 -0.01147 -0.01247 0.00127 AFIX 43 H6 2 0.795886 0.364903 0.824113 11.00000 -1.20000 AFIX 0 C3 1 0.848591 0.469798 0.749771 11.00000 0.03830 0.06106 = 0.05801 -0.03179 -0.00573 0.02200 AFIX 43 H7 2 0.867555 0.409094 0.719669 11.00000 -1.20000 AFIX 0 C4 1 0.863817 0.583012 0.733542 11.00000 0.02767 0.04676 = 0.02937 -0.01534 0.00690 0.00421 AFIX 43 H8 2 0.895067 0.601768 0.692380 11.00000 -1.20000 AFIX 0 C5 1 0.834392 0.671370 0.776198 11.00000 0.01283 0.04983 = 0.03389 -0.00364 -0.00746 0.00038 C6 1 0.855974 0.796848 0.760544 11.00000 0.03594 0.04364 = 0.04433 0.01162 -0.01748 -0.00326 AFIX 23 H9 2 0.852736 0.809681 0.709649 11.00000 -1.20000 H10 2 0.916882 0.813537 0.775946 11.00000 -1.20000 AFIX 0 C7 1 0.741323 0.956840 0.755414 11.00000 0.02899 0.03507 = 0.03127 0.00318 -0.00722 -0.00544 C8 1 0.740889 1.074994 0.773292 11.00000 0.05944 0.02959 = 0.05467 -0.00961 -0.02712 -0.01656 AFIX 43 H11 2 0.778821 1.101807 0.809337 11.00000 -1.20000 AFIX 0 C9 1 0.687732 1.152129 0.740492 11.00000 0.04872 0.02841 = 0.06735 0.00716 -0.02585 -0.00911 AFIX 43 H12 2 0.688661 1.232081 0.753785 11.00000 -1.20000 AFIX 0 C10 1 0.631895 1.115610 0.687647 11.00000 0.03812 0.02857 = 0.05358 0.01016 0.00642 -0.01059 C11 1 0.576167 1.194098 0.652439 11.00000 0.04361 0.03344 = 0.06274 0.02591 0.00229 0.00096 AFIX 43 H13 2 0.578694 1.275138 0.662988 11.00000 -1.20000 AFIX 0 C12 1 0.518006 1.154164 0.602801 11.00000 0.03915 0.06134 = 0.04749 0.03148 0.01305 0.02025 AFIX 43 H14 2 0.482335 1.208350 0.578043 11.00000 -1.20000 AFIX 0 C13 1 0.511025 1.039310 0.588890 11.00000 0.03620 0.07153 = 0.02634 0.00944 -0.00400 0.00331 AFIX 43 H15 2 0.467969 1.013209 0.556445 11.00000 -1.20000 AFIX 0 C14 1 0.564705 0.959572 0.620559 11.00000 0.01967 0.04068 = 0.03495 -0.00064 -0.00257 -0.00206 AFIX 43 H16 2 0.559665 0.878880 0.609625 11.00000 -1.20000 AFIX 0 C15 1 0.627612 0.997835 0.669561 11.00000 0.02741 0.02769 = 0.03081 0.01458 0.00612 0.00034 C16 1 0.684778 0.915106 0.705992 11.00000 0.02719 0.03241 = 0.02822 0.01284 -0.01019 -0.00191 C17 1 0.673692 0.787698 0.690592 11.00000 0.02253 0.02865 = 0.02253 0.00437 -0.00440 0.00215 C18 1 0.707056 0.739073 0.628868 11.00000 0.02050 0.03831 = 0.02512 -0.00181 -0.00098 0.00539 C19 1 0.755703 0.809645 0.580946 11.00000 0.03244 0.04668 = 0.03622 0.00900 -0.00018 0.00766 AFIX 43 H17 2 0.762725 0.891069 0.588852 11.00000 -1.20000 AFIX 0 C20 1 0.792484 0.757008 0.522657 11.00000 0.05280 0.07220 = 0.02466 0.00985 0.01179 0.00813 AFIX 43 H18 2 0.823071 0.804376 0.490223 11.00000 -1.20000 AFIX 0 C21 1 0.786076 0.637866 0.510231 11.00000 0.04866 0.06128 = 0.03972 -0.02298 0.01100 0.01517 AFIX 43 H19 2 0.814513 0.603499 0.471408 11.00000 -1.20000 AFIX 0 C22 1 0.737966 0.570859 0.555027 11.00000 0.03673 0.06096 = 0.03698 -0.01675 -0.00508 -0.00210 AFIX 43 H20 2 0.730674 0.489928 0.545616 11.00000 -1.20000 AFIX 0 C23 1 0.699238 0.618923 0.614437 11.00000 0.03501 0.03576 = 0.03406 -0.00191 -0.00427 -0.00669 C24 1 0.655644 0.547766 0.662631 11.00000 0.04149 0.03273 = 0.03256 -0.01676 -0.00344 -0.00993 AFIX 43 H21 2 0.648130 0.466721 0.653689 11.00000 -1.20000 AFIX 0 C25 1 0.625187 0.594298 0.720438 11.00000 0.04123 0.02749 = 0.04158 0.00734 -0.01460 -0.00843 AFIX 43 H22 2 0.596627 0.544532 0.752768 11.00000 -1.20000 AFIX 0 C26 1 0.632813 0.714928 0.736945 11.00000 0.02873 0.02024 = 0.03348 -0.00501 -0.00850 0.00544 C27 1 0.546422 0.852269 0.812754 11.00000 0.03088 0.02423 = 0.02885 0.00208 -0.00336 -0.00197 AFIX 23 H23 2 0.487662 0.824450 0.827104 11.00000 -1.20000 H24 2 0.539437 0.891987 0.767291 11.00000 -1.20000 AFIX 0 C28 1 0.578137 0.939424 0.864802 11.00000 0.02907 0.01855 = 0.02541 0.00343 -0.00532 0.00311 C29 1 0.530577 1.038202 0.877120 11.00000 0.03967 0.03370 = 0.04088 -0.00055 -0.00758 0.00261 AFIX 43 H25 2 0.476726 1.050321 0.852931 11.00000 -1.20000 AFIX 0 C30 1 0.559446 1.120270 0.923955 11.00000 0.04290 0.03232 = 0.06463 -0.01849 -0.00233 0.01221 AFIX 43 H26 2 0.526411 1.189404 0.931834 11.00000 -1.20000 AFIX 0 C31 1 0.636984 1.101047 0.959395 11.00000 0.04805 0.03823 = 0.07919 -0.03181 -0.02357 0.00386 AFIX 43 H27 2 0.658903 1.156359 0.992019 11.00000 -1.20000 AFIX 0 C32 1 0.680923 1.000777 0.946219 11.00000 0.04438 0.05272 = 0.04261 -0.01930 -0.01364 0.01670 AFIX 43 H28 2 0.733685 0.986623 0.971504 11.00000 -1.20000 AFIX 0 C33 1 0.900871 0.891599 0.963613 11.00000 0.01880 0.02172 = 0.02223 0.00103 0.00150 0.00450 C34 1 1.103705 1.124823 0.969898 11.00000 0.02083 0.01699 = 0.02111 -0.00820 -0.00799 0.00800 C35 1 0.949841 1.097000 0.909114 11.00000 0.01538 0.02723 = 0.03224 -0.00067 -0.00285 -0.00472 C36 1 1.056231 0.927356 0.908220 11.00000 0.02696 0.02085 = 0.03744 -0.00083 0.00568 -0.00567 O1 4 0.500000 0.473947 0.500000 10.50000 0.24092 O3 4 0.586543 0.602868 0.372516 11.00000 0.35191 O2 4 0.451787 0.712822 0.547543 11.00000 0.42810 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0564 for 3425 Fo > 4sig(Fo) and 0.0925 for all 5528 data REM 421 parameters refined using 1 restraints END WGHT 0.0503 0.0000 REM Highest difference peak 0.762, deepest hole -0.449, 1-sigma level 0.127 Q1 1 0.5432 0.5162 0.4341 11.00000 0.05 0.76 Q2 1 0.5000 0.5679 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15.45 -15 7 9 5.45 16.47 16 -6 10 77.44 27.94 16 -6 9 76.69 27.45 16 -6 8 23.02 18.82 16 -6 7 19.28 17.18 16 -6 6 8.14 15.13 16 -6 5 25.73 17.79 16 -6 4 10.24 15.94 16 -6 3 8.40 15.48 16 -6 2 42.28 20.73 16 -6 1 57.95 23.21 16 -6 0 16.20 15.45 16 -6 -1 8.93 15.13 16 -6 -2 32.13 19.71 16 -6 -3 20.88 17.88 16 -6 -4 9.72 16.10 16 -6 -5 17.82 16.63 16 -6 -6 36.22 21.91 16 -6 -7 63.03 26.75 -16 6 8 75.56 25.58 -16 6 8 46.36 23.03 -16 6 9 72.98 25.37 -16 6 9 51.90 25.35 17 -5 10 40.17 20.98 17 -5 9 31.12 18.72 17 -5 8 40.30 21.08 17 -5 7 18.05 18.36 17 -5 6 5.03 15.52 17 -5 5 22.80 17.17 17 -5 4 26.31 18.11 17 -5 3 18.53 16.58 17 -5 2 47.46 20.70 17 -5 1 10.14 14.70 17 -5 0 12.40 15.33 17 -5 -1 13.04 15.87 17 -5 -2 5.69 15.09 17 -5 -3 32.89 20.14 17 -5 -4 50.18 22.65 17 -5 -5 89.28 29.92 17 -5 -6 53.21 24.32 -17 5 7 36.05 22.31 -17 5 7 16.92 19.64 -17 5 8 4.15 18.16 -17 5 8 25.83 21.51 18 -4 2 32.21 17.52 18 -4 1 26.86 18.71 18 -4 0 29.19 19.43 18 -4 -1 15.70 17.24 18 -4 -2 13.76 15.97 18 -4 -3 8.68 15.09 18 -4 -4 13.43 18.15 -18 4 6 62.11 25.33 -18 4 6 70.32 27.86 -18 4 7 84.85 30.02 -18 4 7 82.53 29.98 -18 4 8 62.56 26.36 -18 4 8 38.49 25.28 17 -7 1 4.65 17.25 17 -7 0 17.36 17.86 18 -6 1 26.98 21.58 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 41627 _database_code_depnum_ccdc_archive 'CCDC 962107' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Comp2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H52 Co2 Mo N16, 5(O)' _chemical_formula_sum 'C72 H52 Co2 Mo N16 O5' _chemical_formula_weight 1435.09 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' Co Co 0.3494 0.9721 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 2' _space_group_name_Hall 'C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.943(7) _cell_length_b 11.568(7) _cell_length_c 19.366(10) _cell_angle_alpha 90 _cell_angle_beta 90.045(19) _cell_angle_gamma 90 _cell_volume 3348(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 299 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 20.887 _exptl_crystal_description plates _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_F_000 1464 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 0.738 _shelx_estimated_absorpt_T_min 0.930 _shelx_estimated_absorpt_T_max 0.993 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9300 _exptl_absorpt_correction_T_max 0.9927 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 9245 _diffrn_reflns_av_unetI/netI 0.6105 _diffrn_reflns_av_R_equivalents 0.2008 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.051 _diffrn_reflns_theta_max 25.498 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.902 _diffrn_reflns_point_group_measured_fraction_full 0.905 _reflns_number_total 5627 _reflns_number_gt 1318 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.715 _reflns_Friedel_fraction_max 0.794 _reflns_Friedel_fraction_full 0.800 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0654P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.00(10) _chemical_absolute_configuration rmad _refine_ls_number_reflns 5627 _refine_ls_number_parameters 423 _refine_ls_number_restraints 341 _refine_ls_R_factor_all 0.2450 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2482 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 0.691 _refine_ls_restrained_S_all 0.674 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2668(2) 0.2753(3) 0.38109(19) 0.0299(11) Uani 1 1 d . . . . . Mo1 Mo 0.0000 0.0506(2) 0.5000 0.0287(11) Uani 1 2 d S T P . . N1 N 0.2051(14) 0.415(2) 0.3334(13) 0.040(4) Uani 1 1 d . U . . . N2 N 0.3861(13) 0.3038(17) 0.3087(12) 0.035(5) Uani 1 1 d . U . . . H2 H 0.4192 0.3687 0.3313 0.041 Uiso 1 1 calc R U . . . N3 N 0.1912(15) 0.1868(19) 0.2914(13) 0.040(5) Uani 1 1 d . U . . . H3 H 0.1477 0.1326 0.3136 0.048 Uiso 1 1 calc R U . . . N4 N 0.3411(16) 0.1261(19) 0.3934(14) 0.050(5) Uani 1 1 d . U . . . N5 N 0.1584(14) 0.2249(17) 0.4403(12) 0.030(5) Uani 1 1 d . U . . . N6 N -0.1636(12) -0.1241(17) 0.4498(10) 0.022(4) Uani 1 1 d . U . . . N7 N 0.0722(15) -0.082(2) 0.3567(15) 0.061(7) Uani 1 1 d . U . . . N8 N -0.0849(16) 0.176(2) 0.3594(15) 0.054(7) Uani 1 1 d . U . . . O1 O 0.526(4) 0.607(4) 0.043(3) 0.30(3) Uiso 1 1 d . . . . . O2 O 0.536(4) 0.332(5) 0.034(4) 0.15(3) Uiso 0.5 1 d . . P . . O3 O 0.422(3) 0.457(4) -0.102(3) 0.28(3) Uiso 1 1 d . . . . . C1 C 0.2188(16) 0.527(2) 0.3476(16) 0.046(5) Uani 1 1 d . U . . . H1 H 0.2514 0.5445 0.3884 0.055 Uiso 1 1 calc R U . . . C2 C 0.1892(19) 0.621(3) 0.3072(18) 0.053(5) Uani 1 1 d . U . . . H2A H 0.1958 0.6987 0.3224 0.064 Uiso 1 1 calc R U . . . C3 C 0.1499(19) 0.595(3) 0.2441(18) 0.055(5) Uani 1 1 d . U . . . H3A H 0.1359 0.6551 0.2126 0.067 Uiso 1 1 calc R U . . . C4 C 0.131(2) 0.485(3) 0.2269(19) 0.054(5) Uani 1 1 d . U . . . H4 H 0.1003 0.4658 0.1856 0.065 Uiso 1 1 calc R U . . . C5 C 0.1603(18) 0.398(3) 0.2734(17) 0.046(4) Uani 1 1 d . U . . . C6 C 0.1376(17) 0.270(3) 0.2548(15) 0.045(5) Uani 1 1 d . U . . . H6 H 0.0737 0.2557 0.2652 0.054 Uiso 1 1 calc R U . . . H6A H 0.1463 0.2588 0.2046 0.054 Uiso 1 1 calc R U . . . C7 C 0.249(2) 0.116(3) 0.2499(16) 0.045(5) Uani 1 1 d . U . . . C8 C 0.243(2) -0.009(2) 0.2616(16) 0.048(5) Uani 1 1 d . U . . . H8 H 0.2003 -0.0403 0.2926 0.058 Uiso 1 1 calc R U . . . C9 C 0.3014(19) -0.082(3) 0.2272(15) 0.047(5) Uani 1 1 d . U . . . H9 H 0.3006 -0.1617 0.2376 0.057 Uiso 1 1 calc R U . . . C10 C 0.3618(19) -0.041(2) 0.1772(16) 0.044(4) Uani 1 1 d . U . . . C11 C 0.4158(18) -0.120(3) 0.1425(15) 0.045(5) Uani 1 1 d . U . . . H11 H 0.4095 -0.2008 0.1509 0.054 Uiso 1 1 calc R U . . . C12 C 0.4790(19) -0.080(3) 0.0953(16) 0.047(5) Uani 1 1 d . U . . . H12 H 0.5165 -0.1310 0.0700 0.057 Uiso 1 1 calc R U . . . C13 C 0.4837(17) 0.038(3) 0.0877(14) 0.048(5) Uani 1 1 d . U . . . H13 H 0.5292 0.0673 0.0584 0.058 Uiso 1 1 calc R U . . . C14 C 0.4295(18) 0.115(2) 0.1182(15) 0.043(5) Uani 1 1 d . U . . . H14 H 0.4337 0.1947 0.1073 0.052 Uiso 1 1 calc R U . . . C15 C 0.3650(17) 0.074(2) 0.1674(14) 0.040(4) Uani 1 1 d . U . . . C16 C 0.3081(19) 0.155(2) 0.1991(15) 0.040(5) Uani 1 1 d . U . . . C17 C 0.3208(16) 0.283(2) 0.1931(13) 0.033(4) Uani 1 1 d . U . . . C18 C 0.2908(18) 0.334(2) 0.1303(15) 0.037(4) Uani 1 1 d . U . . . C19 C 0.2438(17) 0.272(3) 0.0790(14) 0.044(4) Uani 1 1 d . U . . . H19 H 0.2351 0.1907 0.0834 0.052 Uiso 1 1 calc R U . . . C20 C 0.2104(19) 0.331(2) 0.0219(16) 0.048(5) Uani 1 1 d . U . . . H20 H 0.1755 0.2914 -0.0114 0.058 Uiso 1 1 calc R U . . . C21 C 0.228(2) 0.449(3) 0.0132(16) 0.051(5) Uani 1 1 d . U . . . H21 H 0.2074 0.4859 -0.0276 0.061 Uiso 1 1 calc R U . . . C22 C 0.2714(18) 0.510(2) 0.0593(15) 0.048(5) Uani 1 1 d . U . . . H22 H 0.2797 0.5907 0.0527 0.057 Uiso 1 1 calc R U . . . C23 C 0.3066(18) 0.454(2) 0.1200(15) 0.041(4) Uani 1 1 d . U . . . C24 C 0.3513(17) 0.518(2) 0.1695(14) 0.040(4) Uani 1 1 d . U . . . H24 H 0.3655 0.5964 0.1608 0.048 Uiso 1 1 calc R U . . . C25 C 0.3754(16) 0.469(2) 0.2306(14) 0.035(4) Uani 1 1 d . U . . . H25 H 0.4000 0.5155 0.2663 0.042 Uiso 1 1 calc R U . . . C26 C 0.3641(17) 0.351(2) 0.2407(15) 0.030(4) Uani 1 1 d . U . . . C27 C 0.4482(17) 0.210(2) 0.3129(16) 0.041(5) Uani 1 1 d . U . . . H27 H 0.5064 0.2398 0.3295 0.049 Uiso 1 1 calc R U . . . H27A H 0.4576 0.1781 0.2660 0.049 Uiso 1 1 calc R U . . . C28 C 0.4191(19) 0.115(2) 0.3588(18) 0.048(5) Uani 1 1 d . U . . . C29 C 0.4727(19) 0.017(2) 0.3728(16) 0.059(5) Uani 1 1 d . U . . . H29 H 0.5302 0.0114 0.3522 0.071 Uiso 1 1 calc R U . . . C30 C 0.444(2) -0.069(3) 0.4155(18) 0.064(6) Uani 1 1 d . U . . . H30 H 0.4795 -0.1348 0.4240 0.077 Uiso 1 1 calc R U . . . C31 C 0.360(2) -0.057(3) 0.4461(19) 0.066(6) Uani 1 1 d . U . . . H31 H 0.3350 -0.1188 0.4721 0.079 Uiso 1 1 calc R U . . . C32 C 0.3138(17) 0.050(3) 0.4373(16) 0.060(5) Uani 1 1 d . U . . . H32 H 0.2620 0.0653 0.4641 0.072 Uiso 1 1 calc R U . . . C33 C 0.1026(18) 0.164(2) 0.4640(16) 0.032(5) Uani 1 1 d . U . . . C34 C -0.1060(15) -0.063(2) 0.4702(13) 0.019(4) Uani 1 1 d . U . . . C35 C 0.0491(17) -0.034(3) 0.4069(18) 0.057(7) Uani 1 1 d . U . . . C36 C -0.053(2) 0.133(3) 0.410(2) 0.046(7) Uani 1 1 d . U . . . 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 Co1 0.024(2) 0.027(2) 0.039(3) 0.000(2) 0.001(2) 0.0005(18) Mo1 0.014(2) 0.032(3) 0.041(3) 0.000 -0.0019(19) 0.000 N1 0.019(9) 0.049(9) 0.052(11) 0.005(9) 0.006(8) -0.004(9) N2 0.023(10) 0.030(10) 0.051(13) -0.008(9) 0.002(10) 0.001(8) N3 0.034(12) 0.041(10) 0.045(13) -0.006(10) 0.000(10) -0.013(9) N4 0.042(10) 0.033(10) 0.076(13) -0.001(9) 0.004(9) 0.004(8) N5 0.030(12) 0.015(13) 0.046(15) 0.007(10) 0.002(10) 0.005(9) N6 0.013(10) 0.034(11) 0.019(11) -0.010(9) 0.005(8) -0.001(7) N7 0.017(12) 0.081(18) 0.09(2) -0.041(14) 0.002(12) -0.004(11) N8 0.044(15) 0.041(15) 0.08(2) 0.001(13) -0.009(13) -0.015(11) C1 0.027(10) 0.051(10) 0.059(12) 0.004(10) 0.007(9) 0.002(10) C2 0.035(11) 0.056(10) 0.069(13) 0.013(10) 0.008(10) 0.003(10) C3 0.036(11) 0.059(9) 0.071(13) 0.014(11) 0.003(10) 0.009(10) C4 0.035(11) 0.060(10) 0.067(12) 0.016(10) 0.000(9) 0.005(10) C5 0.025(9) 0.053(8) 0.058(11) 0.005(9) -0.001(8) 0.003(8) C6 0.025(10) 0.056(9) 0.055(12) 0.000(10) 0.001(9) -0.004(9) C7 0.050(11) 0.041(9) 0.043(11) -0.019(10) 0.002(8) -0.009(10) C8 0.055(11) 0.042(9) 0.047(12) -0.017(10) 0.006(8) -0.015(10) C9 0.056(11) 0.039(9) 0.046(12) -0.021(9) -0.001(8) -0.011(9) C10 0.048(10) 0.042(8) 0.041(10) -0.012(8) -0.005(7) 0.000(8) C11 0.046(11) 0.044(9) 0.044(12) -0.010(9) -0.009(8) 0.006(9) C12 0.044(11) 0.052(10) 0.046(12) -0.008(11) -0.006(8) 0.011(10) C13 0.044(11) 0.052(10) 0.048(12) -0.010(11) -0.003(8) 0.003(10) C14 0.042(11) 0.044(10) 0.045(12) -0.014(9) -0.005(8) -0.005(8) C15 0.041(10) 0.041(8) 0.038(10) -0.014(8) -0.008(7) -0.001(7) C16 0.043(11) 0.039(9) 0.039(11) -0.014(9) -0.005(8) -0.007(8) C17 0.033(10) 0.031(9) 0.036(9) 0.000(7) 0.005(8) 0.002(9) C18 0.040(9) 0.037(8) 0.035(9) 0.000(7) 0.003(7) 0.000(8) C19 0.048(11) 0.044(9) 0.038(10) 0.002(8) 0.000(8) -0.006(9) C20 0.054(11) 0.054(10) 0.037(10) 0.003(9) -0.002(9) -0.002(10) C21 0.057(12) 0.054(10) 0.041(11) 0.012(9) 0.000(9) 0.004(10) C22 0.053(11) 0.044(10) 0.046(10) 0.011(8) 0.004(9) 0.002(9) C23 0.044(9) 0.039(8) 0.040(9) 0.005(7) 0.005(7) -0.001(8) C24 0.044(10) 0.033(9) 0.043(10) 0.004(8) 0.010(8) -0.005(8) C25 0.033(10) 0.037(9) 0.035(9) -0.006(9) 0.015(8) -0.006(9) C26 0.022(10) 0.037(9) 0.030(10) 0.001(8) 0.010(8) 0.004(9) C27 0.025(10) 0.038(10) 0.059(12) -0.003(8) -0.008(9) 0.005(7) C28 0.034(9) 0.035(9) 0.075(12) 0.001(8) -0.002(8) 0.005(7) C29 0.041(10) 0.045(11) 0.091(14) 0.012(9) 0.003(10) 0.012(8) C30 0.047(11) 0.050(11) 0.096(15) 0.017(10) 0.014(11) 0.019(9) C31 0.051(11) 0.050(11) 0.096(15) 0.017(10) 0.016(10) 0.021(10) C32 0.050(11) 0.045(11) 0.085(14) 0.010(10) 0.013(9) 0.016(9) C33 0.030(12) 0.018(13) 0.048(15) 0.010(10) 0.001(11) 0.005(9) C34 0.009(10) 0.033(11) 0.017(12) -0.010(9) 0.005(8) 0.001(8) C35 0.010(13) 0.079(19) 0.08(2) -0.041(15) -0.005(13) -0.008(12) C36 0.031(15) 0.029(15) 0.08(2) 0.003(14) -0.002(14) -0.019(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 Co1 N6 2.05(2) 3 ? Co1 N4 2.07(2) . ? Co1 N5 2.07(2) . ? Co1 N1 2.08(2) . ? Co1 N2 2.29(2) . ? Co1 N3 2.31(2) . ? Mo1 C33 2.13(3) 2_556 ? Mo1 C33 2.13(3) . ? Mo1 C34 2.14(2) . ? Mo1 C34 2.14(2) 2_556 ? Mo1 C36 2.14(4) . ? Mo1 C36 2.14(4) 2_556 ? Mo1 C35 2.18(3) 2_556 ? Mo1 C35 2.18(3) . ? N1 C1 1.34(3) . ? N1 C5 1.35(4) . ? N2 C27 1.43(3) . ? N2 C26 1.46(3) . ? N2 H2 1.0000 . ? N3 C7 1.43(3) . ? N3 C6 1.44(3) . ? N3 H3 1.0000 . ? N4 C32 1.29(3) . ? N4 C28 1.35(3) . ? N5 C33 1.19(3) . ? N6 C34 1.18(3) . ? N6 Co1 2.051(19) 3_445 ? N7 C35 1.17(3) . ? N8 C36 1.20(4) . ? O2 O2 1.70(12) 2_655 ? C1 C2 1.41(4) . ? C1 H1 0.9500 . ? C2 C3 1.39(4) . ? C2 H2A 0.9500 . ? C3 C4 1.34(4) . ? C3 H3A 0.9500 . ? C4 C5 1.41(4) . ? C4 H4 0.9500 . ? C5 C6 1.56(4) . ? C6 H6 0.9900 . ? C6 H6A 0.9900 . ? C7 C16 1.40(4) . ? C7 C8 1.47(3) . ? C8 C9 1.38(4) . ? C8 H8 0.9500 . ? C9 C10 1.41(4) . ? C9 H9 0.9500 . ? C10 C15 1.35(4) . ? C10 C11 1.40(3) . ? C11 C12 1.40(4) . ? C11 H11 0.9500 . ? C12 C13 1.37(4) . ? C12 H12 0.9500 . ? C13 C14 1.34(3) . ? C13 H13 0.9500 . ? C14 C15 1.43(3) . ? C14 H14 0.9500 . ? C15 C16 1.40(3) . ? C16 C17 1.49(3) . ? C17 C26 1.38(3) . ? C17 C18 1.43(4) . ? C18 C19 1.41(4) . ? C18 C23 1.43(3) . ? C19 C20 1.39(4) . ? C19 H19 0.9500 . ? C20 C21 1.39(4) . ? C20 H20 0.9500 . ? C21 C22 1.31(4) . ? C21 H21 0.9500 . ? C22 C23 1.44(4) . ? C22 H22 0.9500 . ? C23 C24 1.38(3) . ? C24 C25 1.36(3) . ? C24 H24 0.9500 . ? C25 C26 1.39(3) . ? C25 H25 0.9500 . ? C27 C28 1.47(4) . ? C27 H27 0.9900 . ? C27 H27A 0.9900 . ? C28 C29 1.41(3) . ? C29 C30 1.37(4) . ? C29 H29 0.9500 . ? C30 C31 1.38(4) . ? C30 H30 0.9500 . ? C31 C32 1.43(4) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 N6 Co1 N4 97.3(9) 3 . ? N6 Co1 N5 101.3(8) 3 . ? N4 Co1 N5 97.0(9) . . ? N6 Co1 N1 94.1(9) 3 . ? N4 Co1 N1 160.0(10) . . ? N5 Co1 N1 96.8(8) . . ? N6 Co1 N2 85.5(8) 3 . ? N4 Co1 N2 76.8(9) . . ? N5 Co1 N2 171.5(8) . . ? N1 Co1 N2 87.8(8) . . ? N6 Co1 N3 170.7(9) 3 . ? N4 Co1 N3 88.8(9) . . ? N5 Co1 N3 84.8(9) . . ? N1 Co1 N3 78.1(9) . . ? N2 Co1 N3 89.1(8) . . ? C33 Mo1 C33 104.4(14) 2_556 . ? C33 Mo1 C34 86.1(9) 2_556 . ? C33 Mo1 C34 145.2(10) . . ? C33 Mo1 C34 145.2(10) 2_556 2_556 ? C33 Mo1 C34 86.1(9) . 2_556 ? C34 Mo1 C34 104.2(13) . 2_556 ? C33 Mo1 C36 74.3(12) 2_556 . ? C33 Mo1 C36 74.2(11) . . ? C34 Mo1 C36 77.1(10) . . ? C34 Mo1 C36 140.2(11) 2_556 . ? C33 Mo1 C36 74.2(11) 2_556 2_556 ? C33 Mo1 C36 74.3(12) . 2_556 ? C34 Mo1 C36 140.2(11) . 2_556 ? C34 Mo1 C36 77.1(10) 2_556 2_556 ? C36 Mo1 C36 127.4(17) . 2_556 ? C33 Mo1 C35 76.3(11) 2_556 2_556 ? C33 Mo1 C35 142.1(11) . 2_556 ? C34 Mo1 C35 72.3(11) . 2_556 ? C34 Mo1 C35 75.5(9) 2_556 2_556 ? C36 Mo1 C35 138.5(10) . 2_556 ? C36 Mo1 C35 69.5(13) 2_556 2_556 ? C33 Mo1 C35 142.1(11) 2_556 . ? C33 Mo1 C35 76.3(11) . . ? C34 Mo1 C35 75.5(9) . . ? C34 Mo1 C35 72.3(11) 2_556 . ? C36 Mo1 C35 69.5(13) . . ? C36 Mo1 C35 138.5(10) 2_556 . ? C35 Mo1 C35 126.4(18) 2_556 . ? C1 N1 C5 113(3) . . ? C1 N1 Co1 126(2) . . ? C5 N1 Co1 119(2) . . ? C27 N2 C26 119(2) . . ? C27 N2 Co1 111.1(16) . . ? C26 N2 Co1 115.5(15) . . ? C27 N2 H2 103.0 . . ? C26 N2 H2 103.0 . . ? Co1 N2 H2 103.0 . . ? C7 N3 C6 116(3) . . ? C7 N3 Co1 112.5(18) . . ? C6 N3 Co1 110.2(17) . . ? C7 N3 H3 105.7 . . ? C6 N3 H3 105.7 . . ? Co1 N3 H3 105.7 . . ? C32 N4 C28 123(3) . . ? C32 N4 Co1 118(2) . . ? C28 N4 Co1 119(2) . . ? C33 N5 Co1 159(2) . . ? C34 N6 Co1 158(2) . 3_445 ? N1 C1 C2 126(3) . . ? N1 C1 H1 117.2 . . ? C2 C1 H1 117.2 . . ? C3 C2 C1 117(3) . . ? C3 C2 H2A 121.6 . . ? C1 C2 H2A 121.6 . . ? C4 C3 C2 121(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 117(3) . . ? C3 C4 H4 121.7 . . ? C5 C4 H4 121.7 . . ? N1 C5 C4 127(3) . . ? N1 C5 C6 116(3) . . ? C4 C5 C6 117(3) . . ? N3 C6 C5 114(2) . . ? N3 C6 H6 108.8 . . ? C5 C6 H6 108.8 . . ? N3 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? H6 C6 H6A 107.7 . . ? C16 C7 N3 126(3) . . ? C16 C7 C8 117(3) . . ? N3 C7 C8 116(3) . . ? C9 C8 C7 119(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 122(3) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C15 C10 C11 124(3) . . ? C15 C10 C9 117(3) . . ? C11 C10 C9 119(3) . . ? C12 C11 C10 119(3) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C13 C12 C11 116(3) . . ? C13 C12 H12 122.1 . . ? C11 C12 H12 122.1 . . ? C14 C13 C12 126(3) . . ? C14 C13 H13 117.2 . . ? C12 C13 H13 117.2 . . ? C13 C14 C15 119(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C10 C15 C16 125(3) . . ? C10 C15 C14 116(3) . . ? C16 C15 C14 119(3) . . ? C15 C16 C7 119(3) . . ? C15 C16 C17 123(3) . . ? C7 C16 C17 117(2) . . ? C26 C17 C18 118(3) . . ? C26 C17 C16 125(3) . . ? C18 C17 C16 116(2) . . ? C19 C18 C23 119(3) . . ? C19 C18 C17 123(3) . . ? C23 C18 C17 118(3) . . ? C20 C19 C18 119(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C21 C20 C19 121(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 122(3) . . ? C22 C21 H21 118.8 . . ? C20 C21 H21 118.8 . . ? C21 C22 C23 120(3) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C18 120(3) . . ? C24 C23 C22 120(3) . . ? C18 C23 C22 119(3) . . ? C25 C24 C23 121(3) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120(3) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C17 C26 C25 122(3) . . ? C17 C26 N2 119(2) . . ? C25 C26 N2 118(3) . . ? N2 C27 C28 114(2) . . ? N2 C27 H27 108.8 . . ? C28 C27 H27 108.8 . . ? N2 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? H27 C27 H27A 107.7 . . ? N4 C28 C29 118(3) . . ? N4 C28 C27 119(3) . . ? C29 C28 C27 123(3) . . ? C30 C29 C28 121(3) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 119(3) . . ? C29 C30 H30 120.7 . . ? C31 C30 H30 120.7 . . ? C30 C31 C32 118(3) . . ? C30 C31 H31 121.1 . . ? C32 C31 H31 121.1 . . ? N4 C32 C31 121(3) . . ? N4 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? N5 C33 Mo1 176(3) . . ? N6 C34 Mo1 176(2) . . ? N7 C35 Mo1 177(2) . . ? N8 C36 Mo1 178(3) . . ? _refine_diff_density_max 0.517 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.122 _shelxl_version_number 2013-4 _shelx_res_file ; TITL REM Yadorkari-X generated CELL 0.71073 14.9434 11.5678 19.3664 90.0000 90.0450 90.0000 ZERR 2.0 0.0069 0.0069 0.0104 0.0000 0.0190 0.0000 LATT -7 SYMM -X, +Y, -Z REM SPGR C2 monoclinic SFAC C H N Co Mo O UNIT 144 104 32 4 2 10 SIZE 0.10 0.10 0.01 TEMP -173.0 L.S. 20 FMAP 2 PLAN -5 ACTA BOND $H MERG 2 OMIT -10.000000 51.000000 DELU 0.005 0.005 C7 > C16 SIMU 0.01 0.02 1.7 C7 > C16 DELU 0.005 0.005 C17 > C26 SIMU 0.01 0.02 1.7 C17 > C26 DELU 0.003 0.003 N5 > N8 C33 > C36 SIMU 0.005 0.01 1.7 N5 > N8 C33 > C36 DELU 0.005 0.005 N1 N3 C1 > C6 SIMU 0.01 0.02 1.7 N1 N3 C1 > C6 DELU 0.005 0.005 N2 N4 C27 > C32 SIMU 0.01 0.02 1.7 N2 N4 C27 > C32 WGHT 0.065400 FVAR 0.13376 CO1 4 0.266751 0.275265 0.381094 11.00000 0.02391 0.02696 = 0.03881 -0.00047 0.00056 0.00049 MO1 5 0.000000 0.050625 0.500000 10.50000 0.01364 0.03171 = 0.04065 0.00000 -0.00193 0.00000 N1 3 0.205067 0.415171 0.333366 11.00000 0.01940 0.04927 = 0.05249 0.00535 0.00615 -0.00378 N2 3 0.386091 0.303813 0.308687 11.00000 0.02305 0.02971 = 0.05089 -0.00759 0.00164 0.00120 AFIX 13 H2 2 0.419205 0.368673 0.331345 11.00000 -1.20000 AFIX 0 N3 3 0.191150 0.186820 0.291411 11.00000 0.03412 0.04115 = 0.04454 -0.00563 -0.00015 -0.01324 AFIX 13 H3 2 0.147721 0.132616 0.313633 11.00000 -1.20000 AFIX 0 N4 3 0.341146 0.126069 0.393396 11.00000 0.04160 0.03294 = 0.07555 -0.00097 0.00390 0.00449 N5 3 0.158394 0.224883 0.440349 11.00000 0.02976 0.01540 = 0.04558 0.00720 0.00153 0.00503 N6 3 -0.163614 -0.124114 0.449829 11.00000 0.01347 0.03359 = 0.01897 -0.01031 0.00492 -0.00110 N7 3 0.072169 -0.081683 0.356664 11.00000 0.01747 0.08085 = 0.08581 -0.04089 0.00234 -0.00442 N8 3 -0.084859 0.175958 0.359350 11.00000 0.04370 0.04146 = 0.07758 0.00052 -0.00948 -0.01473 O1 6 0.526194 0.607461 0.043341 11.00000 0.30363 O2 6 0.536115 0.332143 0.033994 10.50000 0.15187 O3 6 0.421973 0.456989 -0.102372 11.00000 0.28296 C1 1 0.218831 0.526942 0.347584 11.00000 0.02681 0.05106 = 0.05927 0.00391 0.00740 0.00163 AFIX 43 H1 2 0.251367 0.544497 0.388421 11.00000 -1.20000 AFIX 0 C2 1 0.189206 0.621107 0.307174 11.00000 0.03541 0.05575 = 0.06880 0.01327 0.00845 0.00344 AFIX 43 H2A 2 0.195847 0.698715 0.322382 11.00000 -1.20000 AFIX 0 C3 1 0.149853 0.594681 0.244053 11.00000 0.03602 0.05916 = 0.07125 0.01401 0.00329 0.00938 AFIX 43 H3A 2 0.135883 0.655128 0.212637 11.00000 -1.20000 AFIX 0 C4 1 0.131318 0.484589 0.226922 11.00000 0.03507 0.05969 = 0.06744 0.01560 0.00002 0.00473 AFIX 43 H4 2 0.100251 0.465767 0.185609 11.00000 -1.20000 AFIX 0 C5 1 0.160326 0.398492 0.273380 11.00000 0.02484 0.05336 = 0.05830 0.00524 -0.00083 0.00288 C6 1 0.137624 0.270129 0.254807 11.00000 0.02468 0.05578 = 0.05474 0.00024 0.00132 -0.00395 AFIX 23 H6 2 0.073737 0.255664 0.265180 11.00000 -1.20000 H6A 2 0.146280 0.258829 0.204582 11.00000 -1.20000 AFIX 0 C7 1 0.248523 0.115903 0.249854 11.00000 0.04967 0.04136 = 0.04275 -0.01856 0.00242 -0.00854 C8 1 0.243289 -0.009355 0.261595 11.00000 0.05476 0.04245 = 0.04709 -0.01745 0.00609 -0.01511 AFIX 43 H8 2 0.200256 -0.040253 0.292603 11.00000 -1.20000 AFIX 0 C9 1 0.301378 -0.081505 0.227207 11.00000 0.05586 0.03928 = 0.04615 -0.02053 -0.00061 -0.01099 AFIX 43 H9 2 0.300638 -0.161747 0.237633 11.00000 -1.20000 AFIX 0 C10 1 0.361820 -0.040650 0.177159 11.00000 0.04821 0.04170 = 0.04075 -0.01233 -0.00476 -0.00046 C11 1 0.415758 -0.120340 0.142489 11.00000 0.04610 0.04428 = 0.04398 -0.00969 -0.00913 0.00594 AFIX 43 H11 2 0.409485 -0.200834 0.150921 11.00000 -1.20000 AFIX 0 C12 1 0.478970 -0.080034 0.095304 11.00000 0.04369 0.05207 = 0.04562 -0.00849 -0.00629 0.01139 AFIX 43 H12 2 0.516455 -0.130998 0.069969 11.00000 -1.20000 AFIX 0 C13 1 0.483677 0.037798 0.087732 11.00000 0.04412 0.05205 = 0.04782 -0.00979 -0.00280 0.00335 AFIX 43 H13 2 0.529218 0.067304 0.058419 11.00000 -1.20000 AFIX 0 C14 1 0.429484 0.114787 0.118177 11.00000 0.04153 0.04381 = 0.04459 -0.01450 -0.00535 -0.00479 AFIX 43 H14 2 0.433725 0.194685 0.107319 11.00000 -1.20000 AFIX 0 C15 1 0.364992 0.074469 0.167421 11.00000 0.04065 0.04086 = 0.03759 -0.01357 -0.00842 -0.00141 C16 1 0.308127 0.154889 0.199075 11.00000 0.04302 0.03907 = 0.03855 -0.01422 -0.00540 -0.00664 C17 1 0.320774 0.282567 0.193113 11.00000 0.03271 0.03105 = 0.03639 0.00006 0.00533 0.00218 C18 1 0.290750 0.334051 0.130307 11.00000 0.03990 0.03720 = 0.03495 0.00023 0.00306 0.00041 C19 1 0.243761 0.271687 0.079009 11.00000 0.04803 0.04432 = 0.03826 0.00226 -0.00040 -0.00551 AFIX 43 H19 2 0.235057 0.190663 0.083354 11.00000 -1.20000 AFIX 0 C20 1 0.210432 0.331270 0.021931 11.00000 0.05405 0.05363 = 0.03748 0.00273 -0.00205 -0.00171 AFIX 43 H20 2 0.175454 0.291357 -0.011400 11.00000 -1.20000 AFIX 0 C21 1 0.227865 0.448758 0.013227 11.00000 0.05740 0.05403 = 0.04142 0.01165 -0.00033 0.00391 AFIX 43 H21 2 0.207444 0.485858 -0.027613 11.00000 -1.20000 AFIX 0 C22 1 0.271403 0.510014 0.059305 11.00000 0.05294 0.04376 = 0.04583 0.01057 0.00419 0.00218 AFIX 43 H22 2 0.279664 0.590678 0.052661 11.00000 -1.20000 AFIX 0 C23 1 0.306595 0.454296 0.120003 11.00000 0.04383 0.03857 = 0.03964 0.00537 0.00517 -0.00095 C24 1 0.351342 0.517634 0.169538 11.00000 0.04439 0.03348 = 0.04307 0.00357 0.01022 -0.00538 AFIX 43 H24 2 0.365480 0.596360 0.160830 11.00000 -1.20000 AFIX 0 C25 1 0.375438 0.468935 0.230567 11.00000 0.03281 0.03725 = 0.03477 -0.00553 0.01542 -0.00595 AFIX 43 H25 2 0.400028 0.515458 0.266277 11.00000 -1.20000 AFIX 0 C26 1 0.364099 0.351204 0.240687 11.00000 0.02228 0.03659 = 0.03037 0.00072 0.00987 0.00390 C27 1 0.448178 0.209820 0.312884 11.00000 0.02503 0.03792 = 0.05920 -0.00328 -0.00809 0.00492 AFIX 23 H27 2 0.506376 0.239780 0.329543 11.00000 -1.20000 H27A 2 0.457593 0.178124 0.265965 11.00000 -1.20000 AFIX 0 C28 1 0.419124 0.115422 0.358823 11.00000 0.03385 0.03524 = 0.07462 0.00084 -0.00201 0.00488 C29 1 0.472740 0.017489 0.372826 11.00000 0.04057 0.04494 = 0.09093 0.01187 0.00339 0.01187 AFIX 43 H29 2 0.530188 0.011446 0.352165 11.00000 -1.20000 AFIX 0 C30 1 0.443524 -0.068653 0.415508 11.00000 0.04687 0.05008 = 0.09625 0.01668 0.01371 0.01856 AFIX 43 H30 2 0.479536 -0.134832 0.423989 11.00000 -1.20000 AFIX 0 C31 1 0.360422 -0.057377 0.446069 11.00000 0.05121 0.05041 = 0.09583 0.01666 0.01639 0.02069 AFIX 43 H31 2 0.335014 -0.118770 0.472077 11.00000 -1.20000 AFIX 0 C32 1 0.313792 0.049969 0.437257 11.00000 0.04960 0.04469 = 0.08520 0.01034 0.01308 0.01622 AFIX 43 H32 2 0.261968 0.065272 0.464128 11.00000 -1.20000 AFIX 0 C33 1 0.102627 0.163607 0.464012 11.00000 0.02982 0.01762 = 0.04800 0.01026 0.00143 0.00503 C34 1 -0.106004 -0.062843 0.470154 11.00000 0.00856 0.03262 = 0.01695 -0.00978 0.00533 0.00132 C35 1 0.049127 -0.034341 0.406946 11.00000 0.01038 0.07943 = 0.08066 -0.04135 -0.00539 -0.00769 C36 1 -0.053122 0.132608 0.409832 11.00000 0.03097 0.02900 = 0.07709 0.00310 -0.00167 -0.01870 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM REM R1 = 0.0782 for 1318 Fo > 4sig(Fo) and 0.2450 for all 5627 data REM 423 parameters refined using 341 restraints END WGHT 0.0655 0.0000 REM Highest difference peak 0.517, deepest hole -0.558, 1-sigma level 0.122 Q1 1 0.5000 0.2717 0.0000 10.50000 0.05 0.52 Q2 1 0.5689 0.2745 0.1162 11.00000 0.05 0.48 Q3 1 0.5479 0.5447 0.0840 11.00000 0.05 0.47 Q4 1 0.5000 0.6294 0.0000 10.50000 0.05 0.43 Q5 1 0.3310 0.6344 0.0476 11.00000 0.05 0.38 ; _shelx_res_checksum 74734 _shelx_hkl_file ; 0 0 1 -1.11 2.59 0 0 2 23.02 8.98 0 0 3 -1.04 9.97 0 0 4 63.75 20.08 0 0 5 -4.80 15.49 0 0 6 42.65 23.27 0 0 7 99.21 29.99 0 0 8 254.74 37.64 0 0 9 47.36 28.38 0 0 10 13.18 22.01 0 0 11 11.23 24.12 0 0 12 10.76 22.83 0 0 13 14.74 26.02 0 0 14 -2.92 22.63 0 0 14 -16.18 14.87 0 0 15 19.53 26.83 0 0 15 40.16 27.74 0 0 16 96.33 41.83 0 0 16 93.90 40.89 0 0 17 49.57 33.25 0 0 17 55.38 37.98 0 0 18 3.99 32.03 0 0 18 5.80 23.36 0 0 19 13.79 30.06 0 0 19 1.22 24.85 0 0 20 20.00 36.56 0 0 20 -12.96 23.92 0 0 21 20.44 42.46 0 0 21 11.16 32.14 0 0 22 10.43 31.30 0 0 23 10.30 29.02 0 0 24 12.94 32.54 1 -1 24 24.88 36.51 1 -1 23 25.24 34.58 1 -1 22 20.43 38.02 1 -1 21 16.39 43.59 1 -1 21 7.07 25.69 1 -1 20 43.19 42.09 1 -1 20 40.01 36.28 1 -1 19 22.96 30.76 1 -1 18 32.75 32.93 1 -1 17 25.57 31.27 1 -1 16 98.96 44.69 1 -1 15 20.69 27.98 1 -1 14 21.69 27.33 1 -1 13 3.29 20.07 1 -1 12 20.77 26.35 1 -1 11 104.51 38.45 1 -1 10 114.65 38.85 1 -1 9 44.23 28.69 1 -1 8 -1.63 20.64 1 -1 7 65.53 28.01 1 -1 6 218.19 32.67 1 -1 5 139.75 27.11 1 -1 4 820.63 47.47 -1 1 -3 399.44 28.92 1 -1 3 474.26 33.48 -1 1 -2 869.39 32.73 -1 1 -2 709.49 33.07 1 -1 2 810.39 36.18 -1 1 -1 1407.16 33.28 -1 1 -1 1262.45 39.78 1 -1 1 1316.82 38.61 1 -1 1 1366.72 39.19 -1 1 0 19.03 9.07 -1 1 0 35.74 9.15 -1 1 1 883.87 27.49 -1 1 2 309.91 23.88 -1 1 2 252.00 18.52 -1 1 3 58.20 17.26 -1 1 3 69.05 17.01 -1 1 4 24.87 17.85 -1 1 4 27.66 17.48 -1 1 5 35.68 18.64 -1 1 5 31.53 19.26 -1 1 6 14.81 17.69 -1 1 6 37.01 20.15 -1 1 7 126.80 27.14 -1 1 7 107.70 29.98 -1 1 8 132.06 29.77 -1 1 8 105.53 31.95 -1 1 9 126.17 30.78 -1 1 9 144.52 33.58 -1 1 10 80.79 31.93 -1 1 10 55.82 28.65 -1 1 11 184.96 38.62 -1 1 11 144.88 35.62 -1 1 12 57.18 30.08 -1 1 12 22.77 25.45 -1 1 13 102.48 37.63 -1 1 13 63.16 34.54 -1 1 14 132.64 44.19 -1 1 14 72.05 32.99 -1 1 15 72.27 36.22 -1 1 15 41.72 26.93 -1 1 16 31.11 29.33 -1 1 16 18.70 22.84 -1 1 17 3.49 26.26 -1 1 17 -4.80 20.03 -1 1 18 2.00 29.44 -1 1 18 -8.13 16.58 -1 1 19 16.81 32.56 -1 1 19 0.66 20.00 -1 1 20 22.88 39.43 -1 1 20 18.08 24.12 -1 1 21 3.93 37.05 -1 1 21 21.97 28.39 -1 1 22 4.52 27.91 -1 1 23 9.77 28.59 -1 1 24 2.72 32.73 -1 1 25 4.26 32.44 2 -2 24 11.57 33.10 2 -2 23 -5.36 27.10 2 -2 22 7.66 35.94 2 -2 21 22.58 39.13 2 -2 20 -10.81 25.58 2 -2 19 -23.96 24.15 2 -2 18 35.42 34.15 2 -2 17 118.05 51.94 2 -2 16 28.21 30.69 2 -2 15 35.83 31.69 2 -2 14 21.26 25.80 2 -2 13 21.59 26.40 2 -2 12 22.51 25.11 2 -2 11 17.68 24.82 2 -2 10 104.68 39.02 2 -2 9 135.37 33.84 2 -2 8 431.94 50.51 2 -2 7 153.05 33.39 2 -2 6 580.48 51.31 -2 2 -5 362.99 38.51 2 -2 5 396.37 41.29 -2 2 -4 639.41 41.54 -2 2 -4 554.51 42.77 2 -2 4 625.44 46.40 -2 2 -3 50.41 17.96 -2 2 -3 35.95 18.91 2 -2 3 29.90 19.94 -2 2 -2 528.81 30.66 -2 2 -2 422.09 35.04 2 -2 2 540.68 37.75 2 -2 2 512.05 37.37 -2 2 -1 259.19 21.04 -2 2 -1 207.36 26.38 2 -2 1 223.04 24.35 2 -2 1 248.17 25.07 -2 2 0 579.89 38.90 -2 2 0 627.29 34.15 -2 2 1 178.48 25.47 -2 2 1 220.48 22.60 -2 2 2 194.17 27.23 -2 2 2 206.14 22.09 -2 2 3 133.46 25.94 -2 2 3 83.72 19.68 -2 2 4 39.44 20.10 -2 2 4 13.86 15.33 -2 2 5 236.98 34.08 -2 2 5 161.31 25.25 -2 2 6 89.90 29.39 -2 2 6 74.30 25.45 -2 2 7 366.51 42.00 -2 2 7 276.09 36.10 -2 2 8 177.37 33.20 -2 2 8 118.50 27.47 -2 2 9 235.72 39.01 -2 2 9 215.39 37.24 -2 2 10 230.55 39.47 -2 2 10 252.38 39.95 -2 2 11 12.09 21.67 -2 2 11 14.54 23.21 -2 2 12 80.78 34.23 -2 2 12 46.89 29.15 -2 2 13 14.27 24.69 -2 2 13 -1.56 19.70 -2 2 14 36.57 29.10 -2 2 14 9.61 20.54 -2 2 15 49.71 33.92 -2 2 15 28.46 24.18 -2 2 16 36.27 32.83 -2 2 16 29.85 24.56 -2 2 17 50.19 35.17 -2 2 17 14.33 22.82 -2 2 18 46.94 36.86 -2 2 18 9.07 20.09 -2 2 19 93.73 48.42 -2 2 19 35.96 29.97 -2 2 20 -7.23 33.34 -2 2 20 14.84 26.06 -2 2 21 29.11 42.23 -2 2 21 -10.91 20.04 -2 2 22 18.03 27.85 -2 2 23 1.88 27.51 -2 2 24 -8.80 31.59 3 -3 23 8.70 36.75 3 -3 22 11.35 29.35 3 -3 21 34.70 33.53 3 -3 20 43.19 38.11 3 -3 19 44.68 41.14 3 -3 18 12.78 34.47 3 -3 17 -3.70 26.79 3 -3 16 69.18 42.17 3 -3 15 54.59 35.89 3 -3 14 22.45 29.56 3 -3 13 -3.94 22.48 3 -3 12 82.15 38.15 3 -3 11 107.58 40.99 3 -3 10 163.49 40.13 3 -3 9 45.03 31.14 3 -3 8 40.76 28.84 -3 3 -7 39.17 25.03 3 -3 7 95.74 34.59 -3 3 -6 117.34 32.79 3 -3 6 144.90 31.75 -3 3 -5 103.37 25.69 -3 3 -5 94.33 30.33 3 -3 5 94.01 31.24 -3 3 -4 90.84 22.57 -3 3 -4 90.15 28.65 3 -3 4 79.47 29.21 -3 3 -3 312.86 29.82 -3 3 -3 283.87 36.30 3 -3 3 335.27 37.06 -3 3 -2 277.68 27.31 -3 3 -2 189.12 30.37 3 -3 2 266.94 32.01 3 -3 2 239.78 31.05 -3 3 -1 316.79 27.43 -3 3 -1 205.80 31.05 3 -3 1 285.37 32.41 3 -3 1 337.72 34.44 -3 3 0 159.45 28.91 -3 3 0 203.41 27.47 -3 3 1 258.59 34.70 -3 3 1 235.78 28.13 -3 3 2 66.43 24.81 -3 3 2 64.98 21.63 -3 3 3 97.67 28.47 -3 3 3 115.49 25.21 -3 3 4 164.93 31.03 -3 3 4 139.59 25.13 -3 3 5 189.48 33.44 -3 3 5 204.17 29.50 -3 3 6 116.88 33.03 -3 3 6 147.50 27.56 -3 3 7 52.76 27.52 -3 3 7 33.29 21.74 -3 3 8 3.02 18.91 -3 3 8 4.55 18.51 -3 3 9 57.49 30.20 -3 3 9 54.38 27.27 -3 3 10 70.37 31.60 -3 3 10 86.01 33.12 -3 3 11 64.52 34.73 -3 3 11 45.29 27.56 -3 3 12 10.97 24.55 -3 3 12 -0.18 20.77 -3 3 13 26.01 24.89 -3 3 13 24.84 27.67 -3 3 14 73.82 35.78 -3 3 14 31.82 24.70 -3 3 15 78.39 39.62 -3 3 15 19.91 21.64 -3 3 16 15.95 31.42 -3 3 16 22.31 22.13 -3 3 17 -0.27 30.14 -3 3 17 9.40 19.39 -3 3 18 2.98 31.94 -3 3 18 6.72 20.73 -3 3 19 57.38 43.66 -3 3 19 -7.41 21.52 -3 3 20 23.51 39.04 -3 3 20 9.40 23.69 -3 3 21 -0.68 27.11 4 -4 22 41.73 39.24 4 -4 21 -2.50 29.78 4 -4 20 5.07 27.74 4 -4 19 46.01 50.18 4 -4 18 17.30 42.68 4 -4 17 46.77 44.93 4 -4 16 27.63 36.53 4 -4 15 6.87 32.76 4 -4 14 -10.21 27.90 4 -4 13 18.41 31.21 4 -4 12 23.20 28.76 4 -4 11 -3.41 21.36 4 -4 10 36.02 29.97 -4 4 -9 88.13 36.36 4 -4 9 139.86 45.29 -4 4 -8 53.11 31.29 4 -4 8 101.88 39.00 -4 4 -7 154.00 35.63 4 -4 7 167.77 37.59 -4 4 -6 50.43 26.36 -4 4 -6 15.25 20.09 4 -4 6 45.55 28.96 -4 4 -5 88.67 28.50 -4 4 -5 65.28 29.55 4 -4 5 103.46 35.86 -4 4 -4 191.17 29.70 -4 4 -4 109.62 33.48 4 -4 4 150.08 32.06 -4 4 -3 101.14 23.16 -4 4 -3 87.51 31.11 4 -4 3 110.76 31.93 4 -4 3 111.68 33.30 -4 4 -2 582.13 39.75 -4 4 -2 422.08 48.26 4 -4 2 510.27 46.14 4 -4 2 557.36 48.11 -4 4 -1 756.58 43.32 -4 4 -1 574.39 54.31 4 -4 1 668.55 50.84 4 -4 1 691.73 51.51 -4 4 0 521.61 36.78 -4 4 0 434.94 48.12 -4 4 0 510.74 44.17 -4 4 1 132.52 36.15 -4 4 1 116.60 29.52 -4 4 2 100.59 31.56 -4 4 2 136.74 26.78 -4 4 3 115.45 34.06 -4 4 3 115.07 29.49 -4 4 4 58.03 26.77 -4 4 4 77.35 27.52 -4 4 5 28.80 24.10 -4 4 5 32.92 20.84 -4 4 6 -3.00 19.09 -4 4 6 6.35 17.29 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140.37 28.16 -5 5 -4 95.96 35.72 5 -5 4 100.77 38.04 -5 5 -3 383.35 38.44 -5 5 -3 255.92 43.60 5 -5 3 350.96 44.87 5 -5 3 360.20 45.46 -5 5 -2 252.25 32.03 -5 5 -2 164.21 37.38 5 -5 2 196.37 36.15 5 -5 2 221.61 37.91 -5 5 -1 83.99 25.25 -5 5 -1 36.46 25.85 5 -5 1 108.27 32.87 5 -5 1 97.66 33.38 -5 5 0 65.76 24.11 -5 5 0 24.60 24.09 -5 5 0 64.24 28.35 -5 5 1 37.26 26.58 -5 5 1 56.82 26.32 -5 5 2 4.95 19.35 -5 5 2 10.61 19.29 -5 5 3 56.34 29.45 -5 5 3 77.91 28.44 -5 5 4 74.68 32.41 -5 5 4 66.31 27.79 -5 5 5 92.50 36.51 -5 5 5 132.77 32.67 -5 5 6 218.22 42.98 -5 5 6 200.02 37.50 -5 5 7 86.64 36.26 -5 5 7 41.96 26.20 -5 5 8 -1.93 19.99 -5 5 8 16.21 22.03 -5 5 9 41.66 30.03 -5 5 9 41.21 27.97 -5 5 10 28.93 28.70 -5 5 10 19.85 24.25 -5 5 11 8.67 24.45 -5 5 11 14.20 23.80 -5 5 12 15.32 29.00 -5 5 12 22.10 27.23 -5 5 13 21.10 28.56 -5 5 13 11.71 24.73 -5 5 14 94.37 45.10 -5 5 15 54.32 36.28 -5 5 16 -3.82 29.14 -5 5 17 1.09 31.43 -5 5 18 1.80 31.47 -5 5 19 20.06 45.19 -5 5 20 -24.00 38.06 6 -6 20 17.36 59.59 6 -6 19 -0.57 58.59 6 -6 18 14.46 53.58 6 -6 17 60.80 57.43 6 -6 16 -11.61 34.05 6 -6 15 24.80 40.11 6 -6 14 28.83 41.77 6 -6 13 34.58 39.15 6 -6 12 20.45 35.54 -6 6 -11 -12.77 24.40 6 -6 11 1.52 30.42 -6 6 -10 59.66 34.93 6 -6 10 68.12 44.83 -6 6 -9 85.43 39.29 6 -6 9 60.80 38.95 -6 6 -8 35.00 29.81 6 -6 8 28.18 31.03 -6 6 -7 46.44 30.45 -6 6 -7 6.30 20.45 6 -6 7 -0.06 21.44 -6 6 -6 17.54 24.80 -6 6 -6 26.51 24.55 6 -6 6 27.94 28.99 -6 6 -5 22.88 24.52 -6 6 -5 -8.96 18.21 6 -6 5 8.56 26.89 -6 6 -4 110.32 31.42 -6 6 -4 56.73 29.70 6 -6 4 69.61 35.12 -6 6 -3 48.87 24.81 -6 6 -3 21.89 24.41 6 -6 3 50.70 31.01 -6 6 -2 112.72 31.15 -6 6 -2 47.37 28.56 6 -6 2 77.32 32.07 6 -6 2 113.51 38.90 -6 6 -1 226.44 34.00 -6 6 -1 158.26 45.16 6 -6 1 232.56 40.26 6 -6 1 192.87 38.73 -6 6 0 260.20 35.61 -6 6 0 154.18 37.74 6 -6 0 272.37 42.10 6 -6 0 229.45 42.29 -6 6 1 110.12 26.85 -6 6 1 98.10 37.48 -6 6 1 110.46 36.68 -6 6 2 53.70 30.76 -6 6 2 56.13 29.29 -6 6 3 9.36 21.32 -6 6 3 11.60 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