Electronic Supplementary Information for Dalton Transactions This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Carlos Murillo' _publ_contact_author_address ; Texas A&M University Department of Chemistry Box 30012 College Station TX 77842-3012 UNITED STATES OF AMERICA ; _publ_contact_author_email MURILLO@TAMU.EDU _publ_section_title ; Increasing the solubility of strong reducing agents containing Mo24+ units and alkyl-substituted guanidinate ligands ; loop_ _publ_author_name 'Carlos Murillo' 'F. Albert Cotton' 'Xiaoping Wang.' 'Chad C. Wilkinson' data_1 _database_code_depnum_ccdc_archive 'CCDC 645811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H80 Mo2 N12' _chemical_formula_sum 'C44 H80 Mo2 N12' _chemical_formula_weight 969.08 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' 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 'I 2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 10.206(2) _cell_length_b 15.864(3) _cell_length_c 15.607(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.716(3) _cell_angle_gamma 90.00 _cell_volume 2432.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3340 _cell_measurement_theta_min 2.4375 _cell_measurement_theta_max 25.9565 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8865 _exptl_absorpt_correction_T_max 0.9556 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3618 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.08 _reflns_number_total 3618 _reflns_number_gt 3083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3618 _refine_ls_number_parameters 190 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.034 _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 -0.07592(3) 0.0000 0.03219(2) 0.02175(11) Uani 1 2 d S . . N1 N -0.0661(3) 0.0000 -0.1614(2) 0.0283(7) Uani 1 2 d S . . N2 N -0.2347(3) 0.0000 -0.0910(2) 0.0239(7) Uani 1 2 d S . . N3 N -0.2956(4) -0.0198(3) -0.2484(3) 0.0252(16) Uani 0.50 1 d P . . N4 N -0.0834(2) -0.13488(13) 0.03606(14) 0.0273(5) Uani 1 1 d . . . N5 N -0.0128(14) -0.2659(2) -0.0195(4) 0.0287(19) Uani 0.50 1 d PD . . C1 C -0.0211(4) 0.0000 -0.2428(3) 0.0382(10) Uani 1 2 d SD . . H1A H -0.0161 -0.0583 -0.2624 0.046 Uiso 0.50 1 calc PR . . H1B H 0.0706 0.0242 -0.2298 0.046 Uiso 0.50 1 calc PR . . C2 C -0.1192(5) 0.0518(3) -0.3206(3) 0.0287(12) Uani 0.50 1 d PD . . C3 C -0.2557(4) 0.0000 -0.3299(3) 0.0407(11) Uani 1 2 d SD . . H3A H -0.3304 0.0317 -0.3695 0.049 Uiso 0.50 1 calc PR . . H3B H -0.2476 -0.0533 -0.3598 0.049 Uiso 0.50 1 calc PR . . C5 C -0.4385(4) 0.0000 -0.2544(3) 0.0321(9) Uani 1 2 d S . . H4A H -0.4978 -0.0249 -0.3086 0.039 Uiso 0.50 1 calc PR . . H4B H -0.4519 0.0612 -0.2572 0.039 Uiso 0.50 1 calc PR . . C6 C -0.4752(5) -0.0356(3) -0.1722(4) 0.0301(13) Uani 0.50 1 d P . . C7 C -0.3772(4) 0.0000 -0.0936(3) 0.0357(10) Uani 1 2 d S . . H6A H -0.4040 0.0585 -0.0872 0.043 Uiso 0.50 1 calc PR . . H6B H -0.3868 -0.0309 -0.0413 0.043 Uiso 0.50 1 calc PR . . C4 C -0.1990(4) 0.0000 -0.1668(3) 0.0298(9) Uani 1 2 d S . . C8 C -0.1269(6) 0.1463(3) -0.3046(4) 0.0434(15) Uani 0.50 1 d P . . H8A H -0.0386 0.1716 -0.2993 0.065 Uiso 0.50 1 calc PR . . H8B H -0.1533 0.1557 -0.2502 0.065 Uiso 0.50 1 calc PR . . H8C H -0.1938 0.1716 -0.3543 0.065 Uiso 0.50 1 calc PR . . C9 C -0.0747(6) 0.0357(4) -0.4058(3) 0.0407(15) Uani 0.50 1 d P . . H9A H -0.0700 -0.0245 -0.4153 0.061 Uiso 0.50 1 calc PR . . H9B H 0.0142 0.0606 -0.3995 0.061 Uiso 0.50 1 calc PR . . H9C H -0.1401 0.0609 -0.4562 0.061 Uiso 0.50 1 calc PR . . C10 C -0.4599(6) -0.1300(3) -0.1632(4) 0.0432(15) Uani 0.50 1 d P . . H10A H -0.3667 -0.1455 -0.1595 0.065 Uiso 0.50 1 calc PR . . H10B H -0.5207 -0.1569 -0.2146 0.065 Uiso 0.50 1 calc PR . . H10C H -0.4826 -0.1482 -0.1096 0.065 Uiso 0.50 1 calc PR . . C11 C -0.6215(4) 0.0000 -0.1786(3) 0.0481(12) Uani 1 2 d S . . H11A H -0.6844 -0.0465 -0.1819 0.072 Uiso 0.50 1 calc PR . . H11B H -0.6516 0.0346 -0.2316 0.072 Uiso 0.50 1 calc PR . . H11C H -0.6188 0.0338 -0.1264 0.072 Uiso 0.50 1 calc PR . . C12 C 0.0000 -0.1787(2) 0.0000 0.0306(9) Uani 1 2 d S . . C13 C -0.1758(3) -0.17970(17) 0.07637(19) 0.0335(7) Uani 0.50 1 d PD A 1 H13A H -0.2583 -0.1459 0.0697 0.040 Uiso 0.50 1 calc PR A 1 H13B H -0.1325 -0.1864 0.1402 0.040 Uiso 0.50 1 calc PR A 1 C14 C -0.2169(5) -0.2694(3) 0.0338(4) 0.0306(9) Uani 0.50 1 d PD A 1 C15 C -0.092(2) -0.3184(8) 0.0348(11) 0.035(2) Uani 0.50 1 d PDU A 1 H15A H -0.1166 -0.3738 0.0074 0.043 Uiso 0.50 1 calc PR A 1 H15B H -0.0364 -0.3265 0.0961 0.043 Uiso 0.50 1 calc PR A 1 C16 C -0.2886(7) -0.3190(4) 0.0930(4) 0.0383(12) Uani 0.50 1 d P A 1 H16A H -0.3398 -0.2803 0.1196 0.057 Uiso 0.50 1 calc PR A 1 H16B H -0.2210 -0.3478 0.1395 0.057 Uiso 0.50 1 calc PR A 1 H16C H -0.3500 -0.3600 0.0570 0.057 Uiso 0.50 1 calc PR A 1 C17 C -0.3122(7) -0.2603(4) -0.0591(4) 0.0429(11) Uani 0.50 1 d P A 1 H17A H -0.2615 -0.2400 -0.0993 0.064 Uiso 0.50 1 calc PR A 1 H17B H -0.3837 -0.2205 -0.0578 0.064 Uiso 0.50 1 calc PR A 1 H17C H -0.3522 -0.3146 -0.0795 0.064 Uiso 0.50 1 calc PR A 1 C13' C -0.1758(3) -0.17970(17) 0.07637(19) 0.0335(7) Uani 0.50 1 d PD A 2 H13C H -0.2585 -0.1929 0.0292 0.040 Uiso 0.50 1 calc PR A 2 H13D H -0.2021 -0.1412 0.1179 0.040 Uiso 0.50 1 calc PR A 2 C14' C -0.1254(5) -0.2603(3) 0.1257(3) 0.0306(9) Uani 0.50 1 d PD A 2 C15' C -0.078(2) -0.3065(7) 0.0506(11) 0.035(2) Uani 0.50 1 d PD A 2 H15C H -0.1589 -0.3369 0.0157 0.043 Uiso 0.50 1 calc PR A 2 H15D H -0.0139 -0.3497 0.0810 0.043 Uiso 0.50 1 calc PR A 2 C16' C -0.2407(6) -0.3058(4) 0.1510(4) 0.0383(12) Uani 0.50 1 d P A 2 H16D H -0.2384 -0.3652 0.1368 0.057 Uiso 0.50 1 calc PR A 2 H16E H -0.3272 -0.2819 0.1179 0.057 Uiso 0.50 1 calc PR A 2 H16F H -0.2302 -0.2993 0.2143 0.057 Uiso 0.50 1 calc PR A 2 C17' C -0.0073(6) -0.2444(4) 0.2049(4) 0.0429(11) Uani 0.50 1 d P A 2 H17D H 0.0558 -0.2059 0.1887 0.064 Uiso 0.50 1 calc PR A 2 H17E H 0.0385 -0.2973 0.2251 0.064 Uiso 0.50 1 calc PR A 2 H17F H -0.0397 -0.2199 0.2523 0.064 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01958(16) 0.02465(19) 0.02070(19) 0.000 0.00488(13) 0.000 N1 0.0217(16) 0.0448(19) 0.0192(17) 0.000 0.0067(14) 0.000 N2 0.0207(15) 0.0295(17) 0.0211(17) 0.000 0.0051(14) 0.000 N3 0.0224(19) 0.029(5) 0.023(2) 0.0022(18) 0.0047(17) 0.0020(17) N4 0.0214(11) 0.0276(12) 0.0339(13) 0.0034(10) 0.0094(10) -0.0012(9) N5 0.035(5) 0.0234(19) 0.029(6) -0.001(2) 0.012(6) -0.003(2) C1 0.025(2) 0.064(3) 0.026(2) 0.000 0.0084(18) 0.000 C2 0.031(3) 0.031(3) 0.024(3) -0.004(2) 0.008(2) -0.001(2) C3 0.030(2) 0.074(3) 0.017(2) 0.000 0.0042(18) 0.000 C5 0.0216(19) 0.042(2) 0.030(2) 0.000 0.0017(17) 0.000 C6 0.024(3) 0.035(3) 0.031(3) 0.000(2) 0.007(2) -0.002(2) C7 0.025(2) 0.051(3) 0.032(2) 0.000 0.0081(19) 0.000 C4 0.025(2) 0.036(2) 0.025(2) 0.000 0.0021(17) 0.000 C8 0.050(4) 0.038(3) 0.040(4) 0.008(3) 0.007(3) 0.003(3) C9 0.044(3) 0.056(4) 0.024(3) 0.001(3) 0.012(3) -0.002(3) C10 0.039(3) 0.033(3) 0.053(4) 0.008(3) 0.005(3) -0.009(3) C11 0.022(2) 0.085(4) 0.034(3) 0.000 0.0027(19) 0.000 C12 0.0231(19) 0.024(2) 0.043(3) 0.000 0.0059(18) 0.000 C13 0.0298(15) 0.0366(17) 0.0358(17) 0.0035(13) 0.0117(14) -0.0033(12) C14 0.032(2) 0.029(2) 0.031(2) 0.0038(18) 0.0084(18) -0.0022(16) C15 0.028(3) 0.020(3) 0.055(5) -0.007(3) 0.006(4) -0.012(3) C16 0.041(3) 0.029(2) 0.049(4) 0.009(3) 0.018(3) -0.002(2) C17 0.047(3) 0.041(3) 0.036(3) 0.000(2) 0.003(2) -0.003(2) C13' 0.0298(15) 0.0366(17) 0.0358(17) 0.0035(13) 0.0117(14) -0.0033(12) C14' 0.032(2) 0.029(2) 0.031(2) 0.0038(18) 0.0084(18) -0.0022(16) C15' 0.028(3) 0.020(3) 0.055(5) -0.007(3) 0.006(4) -0.012(3) C16' 0.041(3) 0.029(2) 0.049(4) 0.009(3) 0.018(3) -0.002(2) C17' 0.047(3) 0.041(3) 0.036(3) 0.000(2) 0.003(2) -0.003(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 Mo1 2.0627(7) 5 ? Mo1 N1 2.141(3) 5 ? Mo1 N4 2.142(2) . ? Mo1 N2 2.153(3) . ? N1 C4 1.336(4) . ? N1 C1 1.462(4) . ? N2 C4 1.329(5) . ? N2 C7 1.444(4) . ? N3 C4 1.419(5) . ? N3 C5 1.469(5) . ? N3 C3 1.472(5) . ? N4 C12 1.336(3) . ? N4 C13 1.453(3) . ? N5 C12 1.414(5) . ? N5 C15 1.563(13) . ? N5 C15' 1.568(12) . ? C1 C2 1.579(5) . ? C2 C8 1.525(7) . ? C2 C9 1.538(7) . ? C2 C3 1.590(5) . ? C5 C6 1.538(6) . ? C6 C7 1.469(6) . ? C6 C10 1.508(7) . ? C6 C11 1.574(6) . ? C13 C14 1.578(5) . ? C14 C15 1.49(2) . ? C14 C17 1.518(8) . ? C14 C16 1.541(8) . ? C14' C17' 1.495(8) . ? C14' C16' 1.521(8) . ? C14' C15' 1.563(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 Mo1 Mo1 N1 93.02(8) 5 5 ? Mo1 Mo1 N4 92.93(5) 5 . ? N1 Mo1 N4 89.64(6) 5 . ? Mo1 Mo1 N4 92.93(5) 5 6 ? N1 Mo1 N4 89.64(6) 5 6 ? N4 Mo1 N4 174.13(10) . 6 ? Mo1 Mo1 N2 92.75(8) 5 . ? N1 Mo1 N2 174.23(10) 5 . ? N4 Mo1 N2 90.06(6) . . ? N4 Mo1 N2 90.06(6) 6 . ? C4 N1 C1 119.8(3) . 6 ? C4 N1 C1 119.8(3) . . ? C4 N1 Mo1 118.4(2) . 5 ? C1 N1 Mo1 121.8(2) 6 5 ? C1 N1 Mo1 121.8(2) . 5 ? C4 N2 C7 119.4(3) . . ? C4 N2 Mo1 118.3(2) . . ? C7 N2 Mo1 122.3(2) . . ? N3 N3 C4 77.18(17) 6 . ? N3 N3 C5 77.63(17) 6 6 ? C4 N3 C5 116.5(3) . 6 ? N3 N3 C5 77.63(17) 6 . ? C4 N3 C5 116.5(3) . . ? N3 N3 C3 77.65(17) 6 6 ? C4 N3 C3 116.1(3) . 6 ? C5 N3 C3 113.7(3) 6 6 ? C5 N3 C3 113.7(3) . 6 ? N3 N3 C3 77.65(17) 6 . ? C4 N3 C3 116.1(3) . . ? C5 N3 C3 113.7(3) 6 . ? C5 N3 C3 113.7(3) . . ? C12 N4 C13 119.3(2) . . ? C12 N4 Mo1 118.43(18) . . ? C13 N4 Mo1 122.23(16) . . ? N5 N5 C15' 103(3) 2 2 ? N5 N5 C12 77.9(2) 2 . ? C15' N5 C12 121.3(12) 2 . ? N5 N5 C15 92(2) 2 2 ? C12 N5 C15 125.2(12) . 2 ? N5 N5 C15 66(2) 2 . ? C15' N5 C15 117.3(4) 2 . ? C12 N5 C15 115.8(9) . . ? C15 N5 C15 107.7(11) 2 . ? N5 N5 C15' 56(2) 2 . ? C15' N5 C15' 122.0(10) 2 . ? C12 N5 C15' 106.5(7) . . ? C15 N5 C15' 111.1(8) 2 . ? N1 C1 C2 112.6(3) . . ? C8 C2 C9 110.1(4) . . ? C8 C2 C1 115.9(4) . 6 ? C9 C2 C1 107.7(4) . 6 ? C8 C2 C1 115.9(4) . . ? C9 C2 C1 107.7(4) . . ? C8 C2 C3 116.1(4) . 6 ? C9 C2 C3 107.0(4) . 6 ? C1 C2 C3 99.2(3) 6 6 ? C1 C2 C3 99.2(3) . 6 ? C8 C2 C3 116.1(4) . . ? C9 C2 C3 107.0(4) . . ? C1 C2 C3 99.2(3) 6 . ? C1 C2 C3 99.2(3) . . ? C8 C2 C2 169.4(3) . 6 ? C9 C2 C2 80.5(3) . 6 ? C1 C2 C2 58.64(19) 6 6 ? C1 C2 C2 58.64(19) . 6 ? C3 C2 C2 58.88(19) 6 6 ? C3 C2 C2 58.88(19) . 6 ? N3 C3 C2 118.2(3) . . ? N3 C5 C6 109.3(3) . . ? C6 C6 C7 67.4(2) 6 . ? C6 C6 C10 173.2(3) 6 . ? C7 C6 C10 105.9(4) . . ? C6 C6 C5 68.47(19) 6 6 ? C7 C6 C5 106.9(4) . 6 ? C10 C6 C5 113.5(4) . 6 ? C6 C6 C5 68.47(19) 6 . ? C7 C6 C5 106.9(4) . . ? C10 C6 C5 113.5(4) . . ? C6 C6 C11 68.98(18) 6 . ? C7 C6 C11 109.6(4) . . ? C10 C6 C11 115.8(4) . . ? C5 C6 C11 104.8(4) 6 . ? C5 C6 C11 104.8(4) . . ? N2 C7 C6 118.5(3) . . ? N2 C4 N1 117.5(3) . . ? N2 C4 N3 120.5(3) . . ? N1 C4 N3 120.3(3) . . ? N2 C4 N3 120.5(3) . 6 ? N1 C4 N3 120.3(3) . 6 ? N4 C12 N4 117.3(3) 2 . ? N4 C12 N5 116.8(6) 2 . ? N4 C12 N5 124.5(6) . . ? N4 C12 N5 124.5(6) 2 2 ? N4 C12 N5 116.8(6) . 2 ? N4 C13 C14 112.9(3) . . ? C15 C14 C17 112.6(8) . . ? C15 C14 C16 105.7(5) . . ? C17 C14 C16 109.6(5) . . ? C15 C14 C13 109.7(7) . . ? C17 C14 C13 110.2(4) . . ? C16 C14 C13 108.8(4) . . ? C14 C15 N5 106.5(11) . . ? C17' C14' C16' 111.9(5) . . ? C17' C14' C15' 110.9(10) . . ? C16' C14' C15' 112.8(6) . . ? C14' C15' N5 127.3(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.049 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.077 #===END of CIF for Compound 1 ======================== data_2 _database_code_depnum_ccdc_archive 'CCDC 645812' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H80 Mo2 N12, C32 H12 B F24' _chemical_formula_sum 'C76 H92 B F24 Mo2 N12' _chemical_formula_weight 1832.31 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 12.015(2) _cell_length_b 14.213(2) _cell_length_c 27.980(5) _cell_angle_alpha 88.823(3) _cell_angle_beta 88.470(3) _cell_angle_gamma 65.487(3) _cell_volume 4345.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7161 _cell_measurement_theta_min 2.1845 _cell_measurement_theta_max 27.493 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1874 _exptl_absorpt_coefficient_mu 0.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8506 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18888 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 22.50 _reflns_number_total 11130 _reflns_number_gt 9793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+55.5792P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11130 _refine_ls_number_parameters 1183 _refine_ls_number_restraints 505 _refine_ls_R_factor_all 0.1161 _refine_ls_R_factor_gt 0.1048 _refine_ls_wR_factor_ref 0.2378 _refine_ls_wR_factor_gt 0.2323 _refine_ls_goodness_of_fit_ref 1.311 _refine_ls_restrained_S_all 1.290 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 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 B1 B 0.9436(12) -0.0261(11) 0.2525(5) 0.040(3) Uani 1 1 d . . . Mo1 Mo 0.54133(8) 0.42235(6) 0.48996(3) 0.0241(3) Uani 1 1 d . . . Mo2 Mo 0.52664(9) 0.43316(8) 0.97951(3) 0.0376(3) Uani 1 1 d . . . N1 N 0.4882(7) 0.3721(6) 0.5543(3) 0.030(2) Uani 1 1 d . . . N2 N 0.3982(7) 0.5414(7) 0.5763(3) 0.030(2) Uani 1 1 d . . . N3 N 0.3772(7) 0.4153(7) 0.6283(3) 0.033(2) Uani 1 1 d . . . N4 N 0.3796(8) 0.4313(6) 0.4576(3) 0.032(2) Uani 1 1 d . . . N5 N 0.2907(7) 0.5987(6) 0.4799(3) 0.0247(19) Uani 1 1 d . . . N6 N 0.1744(8) 0.5298(7) 0.4383(4) 0.041(2) Uani 1 1 d . . . N7 N 0.4202(8) 0.5149(8) 0.9211(3) 0.040(2) Uani 1 1 d . . . N8 N 0.3646(8) 0.6620(7) 0.9655(3) 0.038(2) Uani 1 1 d . . . N9 N 0.2819(10) 0.6740(9) 0.8891(3) 0.053(3) Uani 1 1 d . . . N10 N 0.6832(8) 0.4494(8) 0.9511(3) 0.039(2) Uani 1 1 d . . . N11 N 0.6223(8) 0.5971(7) 0.9949(3) 0.037(2) Uani 1 1 d . . . N12 N 0.8046(9) 0.5430(9) 0.9478(3) 0.049(3) Uani 1 1 d . . . C1 C 0.5209(10) 0.2621(8) 0.5641(5) 0.042(3) Uani 1 1 d . . . H1A H 0.6016 0.2317 0.5787 0.051 Uiso 1 1 calc R . . H1B H 0.5270 0.2270 0.5337 0.051 Uiso 1 1 calc R . . C2 C 0.4292(10) 0.2423(8) 0.5971(5) 0.041(3) Uani 1 1 d . . . C3 C 0.4121(11) 0.3065(9) 0.6400(4) 0.043(3) Uani 1 1 d . . . H3A H 0.3487 0.3001 0.6609 0.052 Uiso 1 1 calc R . . H3B H 0.4885 0.2803 0.6578 0.052 Uiso 1 1 calc R . . C4 C 0.4239(8) 0.4407(8) 0.5872(4) 0.028(2) Uani 1 1 d . . . C5 C 0.3204(10) 0.4896(9) 0.6643(4) 0.042(3) Uani 1 1 d . . . H5A H 0.3836 0.4928 0.6848 0.050 Uiso 1 1 calc R . . H5B H 0.2673 0.4672 0.6842 0.050 Uiso 1 1 calc R . . C6 C 0.2443(10) 0.5976(8) 0.6443(4) 0.036(3) Uani 1 1 d . . . C7 C 0.3329(9) 0.6212(8) 0.6111(4) 0.035(3) Uani 1 1 d . . . H7A H 0.2867 0.6860 0.5938 0.042 Uiso 1 1 calc R . . H7B H 0.3929 0.6321 0.6306 0.042 Uiso 1 1 calc R . . C8 C 0.4793(13) 0.1272(10) 0.6121(6) 0.071(4) Uani 1 1 d . . . H8A H 0.5552 0.1084 0.6290 0.106 Uiso 1 1 calc R . . H8B H 0.4942 0.0849 0.5839 0.106 Uiso 1 1 calc R . . H8C H 0.4199 0.1161 0.6329 0.106 Uiso 1 1 calc R . . C9 C 0.3054(11) 0.2737(11) 0.5706(5) 0.059(4) Uani 1 1 d . . . H9A H 0.2472 0.2611 0.5914 0.088 Uiso 1 1 calc R . . H9B H 0.3194 0.2330 0.5419 0.088 Uiso 1 1 calc R . . H9C H 0.2731 0.3466 0.5620 0.088 Uiso 1 1 calc R . . C10 C 0.1370(11) 0.5979(10) 0.6161(5) 0.051(3) Uani 1 1 d . . . H10A H 0.0904 0.6667 0.6033 0.077 Uiso 1 1 calc R . . H10B H 0.0846 0.5781 0.6371 0.077 Uiso 1 1 calc R . . H10C H 0.1677 0.5492 0.5901 0.077 Uiso 1 1 calc R . . C11 C 0.1985(13) 0.6743(11) 0.6842(4) 0.059(4) Uani 1 1 d . . . H11A H 0.1506 0.7426 0.6710 0.088 Uiso 1 1 calc R . . H11B H 0.2675 0.6753 0.7011 0.088 Uiso 1 1 calc R . . H11C H 0.1478 0.6547 0.7061 0.088 Uiso 1 1 calc R . . C12 C 0.3755(10) 0.3376(8) 0.4381(4) 0.043(3) Uani 1 1 d . . . H12A H 0.3577 0.2983 0.4641 0.051 Uiso 1 1 calc R . . H12B H 0.4558 0.2939 0.4242 0.051 Uiso 1 1 calc R . . C13 C 0.2791(11) 0.3632(10) 0.4001(4) 0.046(3) Uani 1 1 d . . . C14 C 0.1637(11) 0.4370(10) 0.4201(6) 0.062(4) Uani 1 1 d . . . H14A H 0.1371 0.4038 0.4463 0.074 Uiso 1 1 calc R . . H14B H 0.1013 0.4579 0.3955 0.074 Uiso 1 1 calc R . . C15 C 0.2809(9) 0.5197(8) 0.4594(4) 0.029(2) Uani 1 1 d . . . C16 C 0.0633(10) 0.6230(10) 0.4435(5) 0.051(3) Uani 1 1 d . . . H16A H 0.0208 0.6192 0.4734 0.062 Uiso 1 1 calc R . . H16B H 0.0090 0.6289 0.4170 0.062 Uiso 1 1 calc R . . C17 C 0.0912(10) 0.7173(9) 0.4440(4) 0.043(3) Uani 1 1 d . . . C18 C 0.1817(9) 0.6976(8) 0.4841(4) 0.034(3) Uani 1 1 d . . . H18A H 0.2081 0.7542 0.4844 0.041 Uiso 1 1 calc R . . H18B H 0.1399 0.6982 0.5148 0.041 Uiso 1 1 calc R . . C19 C 0.2703(13) 0.2608(10) 0.3862(6) 0.079(5) Uani 1 1 d . . . H19A H 0.2105 0.2751 0.3614 0.118 Uiso 1 1 calc R . . H19B H 0.2454 0.2320 0.4141 0.118 Uiso 1 1 calc R . . H19C H 0.3495 0.2117 0.3746 0.118 Uiso 1 1 calc R . . C20 C 0.3197(15) 0.4045(12) 0.3560(5) 0.074(5) Uani 1 1 d . . . H20A H 0.3258 0.4685 0.3636 0.111 Uiso 1 1 calc R . . H20B H 0.2604 0.4175 0.3310 0.111 Uiso 1 1 calc R . . H20C H 0.3989 0.3541 0.3450 0.111 Uiso 1 1 calc R . . C21 C 0.1489(13) 0.7310(10) 0.3967(5) 0.064(4) Uani 1 1 d . . . H21A H 0.1656 0.7921 0.3981 0.097 Uiso 1 1 calc R . . H21B H 0.0931 0.7389 0.3710 0.097 Uiso 1 1 calc R . . H21C H 0.2248 0.6707 0.3910 0.097 Uiso 1 1 calc R . . C22 C -0.0256(11) 0.8108(10) 0.4547(5) 0.060(4) Uani 1 1 d . . . H22A H -0.0604 0.8005 0.4849 0.089 Uiso 1 1 calc R . . H22B H -0.0833 0.8205 0.4294 0.089 Uiso 1 1 calc R . . H22C H -0.0083 0.8714 0.4565 0.089 Uiso 1 1 calc R . . C23 C 0.4192(11) 0.4645(11) 0.8771(4) 0.050(3) Uani 1 1 d . . . H23A H 0.4365 0.3920 0.8840 0.060 Uiso 1 1 calc R . . H23B H 0.4849 0.4658 0.8559 0.060 Uiso 1 1 calc R . . C24 C 0.2976(11) 0.5146(11) 0.8509(4) 0.051(3) Uani 1 1 d . . . C25 C 0.2749(12) 0.6281(11) 0.8441(4) 0.055(4) Uani 1 1 d . . . H25A H 0.3359 0.6331 0.8215 0.066 Uiso 1 1 calc R . . H25B H 0.1938 0.6666 0.8306 0.066 Uiso 1 1 calc R . . C26 C 0.3557(9) 0.6193(8) 0.9245(4) 0.032(3) Uani 1 1 d . . . C27 C 0.2250(13) 0.7869(10) 0.8902(5) 0.058(4) Uani 1 1 d . . . H27A H 0.1523 0.8129 0.8702 0.070 Uiso 1 1 calc R . . H27B H 0.2825 0.8139 0.8771 0.070 Uiso 1 1 calc R . . C28 C 0.1883(12) 0.8250(10) 0.9414(5) 0.058(4) Uani 1 1 d . . . C29 C 0.3034(11) 0.7736(9) 0.9699(4) 0.050(3) Uani 1 1 d . . . H29A H 0.3608 0.8032 0.9597 0.060 Uiso 1 1 calc R . . H29B H 0.2828 0.7904 1.0037 0.060 Uiso 1 1 calc R . . C30 C 0.3076(13) 0.4658(13) 0.8025(5) 0.072(5) Uani 1 1 d . . . H30A H 0.2300 0.4987 0.7865 0.108 Uiso 1 1 calc R . . H30B H 0.3281 0.3926 0.8067 0.108 Uiso 1 1 calc R . . H30C H 0.3710 0.4748 0.7834 0.108 Uiso 1 1 calc R . . C31 C 0.1961(13) 0.5040(13) 0.8821(5) 0.070(4) Uani 1 1 d . . . H31A H 0.1904 0.5373 0.9125 0.105 Uiso 1 1 calc R . . H31B H 0.2153 0.4313 0.8875 0.105 Uiso 1 1 calc R . . H31C H 0.1187 0.5366 0.8660 0.105 Uiso 1 1 calc R . . C32 C 0.1448(16) 0.9409(12) 0.9415(6) 0.091(6) Uani 1 1 d . . . H32A H 0.2099 0.9590 0.9293 0.136 Uiso 1 1 calc R . . H32B H 0.1227 0.9661 0.9738 0.136 Uiso 1 1 calc R . . H32C H 0.0741 0.9723 0.9213 0.136 Uiso 1 1 calc R . . C33 C 0.0913(13) 0.7916(14) 0.9609(6) 0.082(5) Uani 1 1 d . . . H33A H 0.0687 0.8164 0.9933 0.122 Uiso 1 1 calc R . . H33B H 0.1234 0.7167 0.9609 0.122 Uiso 1 1 calc R . . H33C H 0.0199 0.8202 0.9409 0.122 Uiso 1 1 calc R . . C34 C 0.7677(11) 0.3727(10) 0.9202(4) 0.048(3) Uani 1 1 d . . . H34A H 0.7220 0.3469 0.8996 0.058 Uiso 1 1 calc R . . H34B H 0.8218 0.3145 0.9398 0.058 Uiso 1 1 calc R . . C35 C 0.8459(11) 0.4114(11) 0.8888(4) 0.053(4) Uani 1 1 d . . . C36 C 0.8988(11) 0.4639(11) 0.9206(5) 0.059(4) Uani 1 1 d . . . H36A H 0.9560 0.4129 0.9424 0.070 Uiso 1 1 calc R . . H36B H 0.9445 0.4947 0.9013 0.070 Uiso 1 1 calc R . . C37 C 0.7039(10) 0.5298(10) 0.9653(4) 0.040(3) Uani 1 1 d . . . C38 C 0.8307(12) 0.6314(12) 0.9625(5) 0.062(4) Uani 1 1 d . . . H38A H 0.8727 0.6509 0.9362 0.074 Uiso 1 1 calc R . . H38B H 0.8849 0.6108 0.9900 0.074 Uiso 1 1 calc R . . C39 C 0.7126(13) 0.7242(11) 0.9759(5) 0.057(4) Uani 1 1 d . . . C40 C 0.6427(12) 0.6863(10) 1.0113(4) 0.051(3) Uani 1 1 d . . . H40A H 0.6877 0.6673 1.0412 0.061 Uiso 1 1 calc R . . H40B H 0.5632 0.7432 1.0182 0.061 Uiso 1 1 calc R . . C41 C 0.9497(11) 0.3189(11) 0.8637(5) 0.058(4) Uani 1 1 d . . . H41A H 0.9987 0.3442 0.8436 0.087 Uiso 1 1 calc R . . H41B H 0.9143 0.2832 0.8442 0.087 Uiso 1 1 calc R . . H41C H 1.0010 0.2716 0.8877 0.087 Uiso 1 1 calc R . . C42 C 0.7677(13) 0.4874(12) 0.8516(5) 0.065(4) Uani 1 1 d . . . H42A H 0.7033 0.5454 0.8674 0.097 Uiso 1 1 calc R . . H42B H 0.7314 0.4532 0.8315 0.097 Uiso 1 1 calc R . . H42C H 0.8181 0.5121 0.8320 0.097 Uiso 1 1 calc R . . C43 C 0.7443(16) 0.8078(14) 0.9980(6) 0.085(5) Uani 1 1 d . . . H43A H 0.7928 0.7799 1.0262 0.127 Uiso 1 1 calc R . . H43B H 0.6694 0.8666 1.0068 0.127 Uiso 1 1 calc R . . H43C H 0.7906 0.8297 0.9748 0.127 Uiso 1 1 calc R . . C44 C 0.6375(14) 0.7669(13) 0.9308(5) 0.078(5) Uani 1 1 d . . . H44A H 0.6217 0.7126 0.9161 0.117 Uiso 1 1 calc R . . H44B H 0.6827 0.7915 0.9085 0.117 Uiso 1 1 calc R . . H44C H 0.5604 0.8236 0.9394 0.117 Uiso 1 1 calc R . . C45 C 1.0220(10) 0.0202(8) 0.2187(4) 0.043(3) Uani 1 1 d D . . C46 C 1.0852(10) -0.0317(9) 0.1776(4) 0.050(3) Uani 1 1 d D . . H46A H 1.0803 -0.0939 0.1699 0.060 Uiso 1 1 calc R . . C47 C 1.1553(10) 0.0030(8) 0.1473(4) 0.049(3) Uani 1 1 d D A . C48 C 1.1647(11) 0.0948(8) 0.1576(4) 0.050(3) Uani 1 1 d D . . H48A H 1.2127 0.1192 0.1383 0.060 Uiso 1 1 calc R . . C49 C 1.1013(11) 0.1479(8) 0.1968(4) 0.049(3) Uani 1 1 d D A . C50 C 1.0330(9) 0.1131(8) 0.2265(4) 0.043(3) Uani 1 1 d D . . H50A H 0.9922 0.1532 0.2531 0.051 Uiso 1 1 calc R . . C51 C 1.2238(9) -0.0638(8) 0.1070(4) 0.076(5) Uani 1 1 d D . . F1 F 1.3155(12) -0.1524(9) 0.1212(5) 0.073(4) Uani 0.600(4) 1 d PD A 1 F2 F 1.1523(12) -0.0948(13) 0.0810(6) 0.080(5) Uani 0.600(4) 1 d PD A 1 F3 F 1.2734(17) -0.0197(12) 0.0755(6) 0.118(8) Uani 0.600(4) 1 d PD A 1 F1A F 1.3427(13) -0.115(3) 0.1157(12) 0.073(4) Uani 0.263(7) 1 d PD A 2 F2A F 1.186(3) -0.133(2) 0.0915(17) 0.080(5) Uani 0.263(7) 1 d PD A 2 F3A F 1.215(4) 0.000(3) 0.0700(11) 0.118(8) Uani 0.263(7) 1 d PD A 2 F1B F 1.324(3) -0.047(5) 0.099(2) 0.073(4) Uani 0.137(7) 1 d PD A 3 F2B F 1.261(6) -0.1649(12) 0.1141(18) 0.080(5) Uani 0.137(7) 1 d PD A 3 F3B F 1.161(4) -0.039(4) 0.0667(10) 0.118(8) Uani 0.137(7) 1 d PD A 3 C52 C 1.1088(11) 0.2479(9) 0.2087(4) 0.066(4) Uani 1 1 d D . . F4 F 0.9962(14) 0.3301(13) 0.2111(7) 0.078(6) Uani 0.600(4) 1 d PD A 1 F5 F 1.151(2) 0.2475(14) 0.2551(6) 0.085(5) Uani 0.600(4) 1 d PD A 1 F6 F 1.181(2) 0.2769(16) 0.1808(8) 0.108(8) Uani 0.600(4) 1 d PD A 1 F4A F 1.021(4) 0.315(3) 0.2296(17) 0.078(6) Uani 0.263(7) 1 d PD A 2 F5A F 1.203(4) 0.238(3) 0.2292(18) 0.085(5) Uani 0.263(7) 1 d PD A 2 F6A F 1.102(5) 0.302(3) 0.1670(17) 0.108(8) Uani 0.263(7) 1 d PD A 2 F4B F 1.091(6) 0.269(4) 0.251(2) 0.078(6) Uani 0.137(7) 1 d PD A 3 F5B F 1.225(5) 0.231(5) 0.197(3) 0.085(5) Uani 0.137(7) 1 d PD A 3 F6B F 1.048(6) 0.314(4) 0.179(3) 0.108(8) Uani 0.137(7) 1 d PD A 3 C53 C 1.0142(8) -0.1521(8) 0.2574(4) 0.032(3) Uani 1 1 d D . . C54 C 0.9540(9) -0.2156(8) 0.2668(4) 0.037(3) Uani 1 1 d D . . H54A H 0.8682 -0.1849 0.2697 0.044 Uiso 1 1 calc R . . C55 C 1.0147(9) -0.3228(7) 0.2722(4) 0.037(3) Uani 1 1 d D A . C56 C 1.1411(9) -0.3688(8) 0.2702(4) 0.038(3) Uani 1 1 d D . . H56A H 1.1840 -0.4408 0.2733 0.046 Uiso 1 1 calc R . . C57 C 1.2025(8) -0.3068(7) 0.2634(4) 0.036(3) Uani 1 1 d D A . C58 C 1.1417(8) -0.2025(8) 0.2568(4) 0.037(3) Uani 1 1 d D . . H58A H 1.1874 -0.1631 0.2516 0.044 Uiso 1 1 calc R . . C59 C 0.9436(10) -0.3848(8) 0.2818(4) 0.053(3) Uani 1 1 d D . . F7 F 0.8382(14) -0.3527(14) 0.2584(6) 0.074(5) Uani 0.600(4) 1 d PD A 1 F8 F 0.9055(15) -0.3773(13) 0.3288(4) 0.061(4) Uani 0.600(4) 1 d PD A 1 F9 F 1.0039(17) -0.4866(10) 0.2741(9) 0.092(7) Uani 0.600(4) 1 d PD A 1 F7A F 0.825(2) -0.326(3) 0.2741(19) 0.074(5) Uani 0.263(7) 1 d PD A 2 F8A F 0.950(4) -0.424(3) 0.3251(9) 0.061(4) Uani 0.263(7) 1 d PD A 2 F9A F 0.975(5) -0.458(3) 0.2484(13) 0.092(7) Uani 0.263(7) 1 d PD A 2 F7B F 0.852(4) -0.336(4) 0.312(2) 0.074(5) Uani 0.137(7) 1 d PD A 3 F8B F 1.009(4) -0.478(3) 0.300(2) 0.061(4) Uani 0.137(7) 1 d PD A 3 F9B F 0.897(6) -0.397(5) 0.2409(12) 0.092(7) Uani 0.137(7) 1 d PD A 3 C60 C 1.3396(9) -0.3553(9) 0.2623(4) 0.062(4) Uani 1 1 d D . . F10 F 1.3794(13) -0.3569(19) 0.3083(6) 0.100(8) Uani 0.600(4) 1 d PD A 1 F11 F 1.3908(15) -0.4586(11) 0.2493(6) 0.067(5) Uani 0.600(4) 1 d PD A 1 F12 F 1.3910(16) -0.3077(14) 0.2349(10) 0.113(10) Uani 0.600(4) 1 d PD A 1 F10A F 1.397(3) -0.312(4) 0.2812(17) 0.100(8) Uani 0.263(7) 1 d PD A 2 F11A F 1.387(4) -0.449(3) 0.2705(16) 0.067(5) Uani 0.263(7) 1 d PD A 2 F12A F 1.377(4) -0.344(4) 0.2165(18) 0.113(10) Uani 0.263(7) 1 d PD A 2 F10B F 1.381(5) -0.288(4) 0.262(3) 0.100(8) Uani 0.137(7) 1 d PD A 3 F11B F 1.376(4) -0.409(4) 0.3033(19) 0.067(5) Uani 0.137(7) 1 d PD A 3 F12B F 1.380(4) -0.420(5) 0.230(2) 0.113(10) Uani 0.137(7) 1 d PD A 3 C61 C 0.9297(8) 0.0135(8) 0.3074(4) 0.035(3) Uani 1 1 d D . . C62 C 0.8249(9) 0.0346(8) 0.3360(3) 0.038(3) Uani 1 1 d D . . H62A H 0.7566 0.0313 0.3218 0.046 Uiso 1 1 calc R . . C63 C 0.8155(8) 0.0602(8) 0.3842(3) 0.036(3) Uani 1 1 d D A . C64 C 0.9140(8) 0.0683(9) 0.4058(4) 0.040(3) Uani 1 1 d D . . H64A H 0.9092 0.0874 0.4380 0.048 Uiso 1 1 calc R . . C65 C 1.0177(8) 0.0479(8) 0.3790(3) 0.039(3) Uani 1 1 d D A . C66 C 1.0258(9) 0.0213(8) 0.3315(4) 0.039(3) Uani 1 1 d D . . H66A H 1.0994 0.0078 0.3145 0.046 Uiso 1 1 calc R . . C67 C 0.7032(9) 0.0785(7) 0.4125(3) 0.046(3) Uani 1 1 d D . . F13 F 0.701(3) -0.0067(17) 0.4335(18) 0.092(5) Uani 0.600(4) 1 d PD A 1 F14 F 0.6028(16) 0.113(4) 0.3844(9) 0.075(5) Uani 0.600(4) 1 d PD A 1 F15 F 0.673(2) 0.149(3) 0.4470(12) 0.056(6) Uani 0.600(4) 1 d PD A 1 F13A F 0.710(7) -0.010(3) 0.433(4) 0.092(5) Uani 0.263(7) 1 d PD A 2 F14A F 0.598(3) 0.120(9) 0.390(2) 0.075(5) Uani 0.263(7) 1 d PD A 2 F15A F 0.699(6) 0.139(8) 0.449(3) 0.056(6) Uani 0.263(7) 1 d PD A 2 F13B F 0.685(6) -0.007(3) 0.412(2) 0.092(5) Uani 0.137(7) 1 d PD A 3 F14B F 0.606(3) 0.154(4) 0.3942(18) 0.075(5) Uani 0.137(7) 1 d PD A 3 F15B F 0.720(4) 0.096(4) 0.4573(9) 0.056(6) Uani 0.137(7) 1 d PD A 3 C68 C 1.1256(9) 0.0521(9) 0.4031(4) 0.057(4) Uani 1 1 d D . . F16 F 1.1777(18) -0.0284(12) 0.4344(7) 0.089(7) Uani 0.600(4) 1 d PD A 1 F17 F 1.2157(14) 0.0562(12) 0.3717(6) 0.061(5) Uani 0.600(4) 1 d PD A 1 F18 F 1.0947(19) 0.1388(15) 0.4290(6) 0.066(7) Uani 0.600(4) 1 d PD A 1 F16A F 1.149(4) 0.014(3) 0.4441(15) 0.089(7) Uani 0.263(7) 1 d PD A 2 F17A F 1.221(3) 0.013(3) 0.3785(16) 0.061(5) Uani 0.263(7) 1 d PD A 2 F18A F 1.105(5) 0.150(4) 0.4145(19) 0.066(7) Uani 0.263(7) 1 d PD A 2 F16B F 1.207(5) -0.037(4) 0.406(3) 0.089(7) Uani 0.137(7) 1 d PD A 3 F17B F 1.169(5) 0.105(4) 0.3729(19) 0.061(5) Uani 0.137(7) 1 d PD A 3 F18B F 1.094(6) 0.104(5) 0.440(2) 0.066(7) Uani 0.137(7) 1 d PD A 3 C69 C 0.8099(9) 0.0125(8) 0.2271(4) 0.045(3) Uani 1 1 d D . . C70 C 0.7820(10) -0.0468(9) 0.1941(4) 0.049(3) Uani 1 1 d D . . H70A H 0.8425 -0.1123 0.1860 0.059 Uiso 1 1 calc R . . C71 C 0.6683(10) -0.0129(9) 0.1728(5) 0.067(4) Uani 1 1 d D A . C72 C 0.5773(11) 0.0840(10) 0.1833(5) 0.076(5) Uani 1 1 d D . . H72A H 0.4995 0.1066 0.1698 0.091 Uiso 1 1 calc R . . C73 C 0.6035(9) 0.1463(8) 0.2139(4) 0.053(3) Uani 1 1 d D A . C74 C 0.7166(9) 0.1109(8) 0.2350(4) 0.044(3) Uani 1 1 d D . . H74A H 0.7316 0.1552 0.2558 0.053 Uiso 1 1 calc R . . C75 C 0.6428(13) -0.0822(11) 0.1406(5) 0.104(7) Uani 1 1 d D . . F19 F 0.599(4) -0.145(3) 0.1631(8) 0.169(12) Uani 0.600(4) 1 d PD A 1 F20 F 0.7440(17) -0.148(2) 0.1167(11) 0.142(13) Uani 0.600(4) 1 d PD A 1 F21 F 0.566(3) -0.0359(16) 0.1051(9) 0.144(10) Uani 0.600(4) 1 d PD A 1 F19A F 0.531(4) -0.076(6) 0.151(2) 0.169(12) Uani 0.263(7) 1 d PD A 2 F20A F 0.720(5) -0.180(2) 0.139(3) 0.142(13) Uani 0.263(7) 1 d PD A 2 F21A F 0.634(7) -0.042(5) 0.0965(10) 0.144(10) Uani 0.263(7) 1 d PD A 2 F19B F 0.525(3) -0.041(6) 0.131(4) 0.169(12) Uani 0.137(7) 1 d PD A 3 F20B F 0.671(11) -0.175(4) 0.160(3) 0.142(13) Uani 0.137(7) 1 d PD A 3 F21B F 0.706(8) -0.092(8) 0.0999(18) 0.144(10) Uani 0.137(7) 1 d PD A 3 C76 C 0.5058(10) 0.2507(9) 0.2255(4) 0.075(5) Uani 1 1 d D . . F22 F 0.5520(14) 0.3082(16) 0.2510(8) 0.063(5) Uani 0.600(4) 1 d PD A 1 F23 F 0.4133(16) 0.2457(18) 0.2546(7) 0.105(8) Uani 0.600(4) 1 d PD A 1 F24 F 0.4557(19) 0.3071(18) 0.1865(8) 0.115(9) Uani 0.600(4) 1 d PD A 1 F22A F 0.521(4) 0.306(4) 0.256(2) 0.063(5) Uani 0.263(7) 1 d PD A 2 F23A F 0.403(3) 0.251(4) 0.230(2) 0.105(8) Uani 0.263(7) 1 d PD A 2 F24A F 0.498(5) 0.316(4) 0.187(2) 0.115(9) Uani 0.263(7) 1 d PD A 2 F22B F 0.462(5) 0.248(4) 0.2659(19) 0.063(5) Uani 0.137(7) 1 d PD A 3 F23B F 0.414(4) 0.269(5) 0.195(2) 0.105(8) Uani 0.137(7) 1 d PD A 3 F24B F 0.540(5) 0.320(4) 0.217(3) 0.115(9) Uani 0.137(7) 1 d PD A 3 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 B1 0.036(8) 0.040(8) 0.044(8) 0.001(6) -0.005(6) -0.016(6) Mo1 0.0201(5) 0.0136(4) 0.0410(6) -0.0051(4) 0.0011(4) -0.0092(4) Mo2 0.0316(6) 0.0473(7) 0.0254(5) -0.0012(4) 0.0007(4) -0.0081(5) N1 0.026(5) 0.019(5) 0.049(6) -0.001(4) 0.003(4) -0.014(4) N2 0.023(5) 0.035(5) 0.036(5) -0.005(4) 0.000(4) -0.015(4) N3 0.022(5) 0.036(5) 0.042(5) 0.006(4) 0.008(4) -0.014(4) N4 0.028(5) 0.020(5) 0.044(5) -0.011(4) 0.005(4) -0.004(4) N5 0.017(4) 0.017(4) 0.039(5) -0.003(4) 0.002(4) -0.007(4) N6 0.018(5) 0.030(5) 0.076(7) -0.014(5) -0.011(5) -0.009(4) N7 0.025(5) 0.070(7) 0.020(5) -0.006(5) -0.001(4) -0.013(5) N8 0.027(5) 0.042(6) 0.035(5) -0.004(4) 0.005(4) -0.003(4) N9 0.053(7) 0.066(8) 0.035(6) 0.004(5) -0.007(5) -0.018(6) N10 0.036(5) 0.054(6) 0.024(5) -0.009(4) 0.005(4) -0.014(5) N11 0.039(6) 0.048(6) 0.029(5) 0.001(4) 0.003(4) -0.022(5) N12 0.033(6) 0.077(8) 0.045(6) -0.013(5) 0.012(5) -0.031(6) C1 0.024(6) 0.015(6) 0.090(9) 0.007(6) 0.005(6) -0.011(5) C2 0.031(6) 0.015(6) 0.077(9) 0.009(6) 0.006(6) -0.012(5) C3 0.041(7) 0.037(7) 0.054(8) 0.010(6) -0.004(6) -0.018(6) C4 0.009(5) 0.026(6) 0.049(7) 0.002(5) -0.005(5) -0.008(4) C5 0.030(6) 0.053(8) 0.044(7) 0.004(6) 0.006(5) -0.020(6) C6 0.029(6) 0.035(7) 0.043(7) -0.006(5) 0.008(5) -0.011(5) C7 0.023(6) 0.034(6) 0.049(7) -0.014(5) 0.005(5) -0.011(5) C8 0.065(10) 0.029(7) 0.118(13) 0.015(8) 0.008(9) -0.021(7) C9 0.045(8) 0.056(9) 0.094(11) -0.007(8) 0.007(7) -0.040(7) C10 0.031(7) 0.054(8) 0.064(9) 0.004(7) 0.002(6) -0.012(6) C11 0.058(9) 0.069(10) 0.049(8) -0.012(7) 0.018(7) -0.027(8) C12 0.039(7) 0.030(6) 0.064(8) -0.015(6) -0.004(6) -0.018(6) C13 0.041(7) 0.049(8) 0.059(8) -0.014(6) -0.012(6) -0.030(6) C14 0.038(8) 0.047(8) 0.108(12) -0.026(8) -0.012(7) -0.023(7) C15 0.027(6) 0.033(6) 0.036(6) -0.006(5) -0.001(5) -0.022(5) C16 0.026(6) 0.057(8) 0.072(9) -0.011(7) -0.005(6) -0.017(6) C17 0.030(6) 0.036(7) 0.057(8) -0.015(6) 0.000(6) -0.008(5) C18 0.033(6) 0.018(6) 0.045(7) -0.008(5) -0.001(5) -0.005(5) C19 0.055(9) 0.038(8) 0.146(15) -0.025(9) -0.033(9) -0.019(7) C20 0.094(12) 0.062(10) 0.059(9) -0.012(8) -0.006(8) -0.023(9) C21 0.075(10) 0.039(8) 0.058(9) 0.010(6) -0.014(8) -0.003(7) C22 0.034(7) 0.047(8) 0.081(10) -0.014(7) -0.018(7) 0.002(6) C23 0.038(7) 0.076(10) 0.034(7) -0.011(6) -0.003(5) -0.020(7) C24 0.040(7) 0.076(10) 0.040(7) 0.010(6) -0.011(6) -0.026(7) C25 0.041(7) 0.086(11) 0.038(7) 0.008(7) -0.004(6) -0.027(7) C26 0.011(5) 0.038(7) 0.039(7) 0.006(5) 0.005(5) -0.001(5) C27 0.066(9) 0.054(9) 0.052(8) 0.004(7) -0.006(7) -0.023(7) C28 0.050(8) 0.044(8) 0.052(8) 0.006(6) -0.005(6) 0.007(7) C29 0.038(7) 0.037(7) 0.050(8) -0.003(6) 0.003(6) 0.009(6) C30 0.052(9) 0.106(13) 0.049(8) -0.009(8) -0.019(7) -0.024(9) C31 0.058(9) 0.090(12) 0.076(10) 0.017(9) -0.004(8) -0.044(9) C32 0.090(13) 0.066(11) 0.077(11) 0.013(9) -0.008(9) 0.006(10) C33 0.048(9) 0.103(14) 0.071(10) -0.001(9) 0.007(8) -0.010(9) C34 0.034(7) 0.060(9) 0.047(7) -0.013(6) 0.011(6) -0.015(6) C35 0.029(7) 0.081(10) 0.043(7) -0.008(7) 0.013(6) -0.017(7) C36 0.029(7) 0.080(10) 0.063(9) -0.022(8) 0.012(6) -0.018(7) C37 0.030(6) 0.060(8) 0.023(6) 0.001(6) 0.001(5) -0.011(6) C38 0.039(8) 0.087(11) 0.067(9) -0.022(8) 0.010(7) -0.033(8) C39 0.072(10) 0.076(10) 0.045(8) -0.005(7) 0.007(7) -0.052(9) C40 0.052(8) 0.055(8) 0.045(7) -0.007(6) 0.005(6) -0.021(7) C41 0.034(7) 0.072(10) 0.065(9) -0.014(7) 0.020(6) -0.018(7) C42 0.064(9) 0.080(11) 0.045(8) -0.003(7) 0.007(7) -0.025(8) C43 0.097(13) 0.095(13) 0.088(12) -0.011(10) 0.006(10) -0.065(11) C44 0.073(11) 0.085(12) 0.067(10) 0.013(9) 0.012(8) -0.026(9) C45 0.035(7) 0.038(7) 0.051(7) -0.011(6) 0.002(6) -0.010(6) C46 0.039(7) 0.047(8) 0.055(8) -0.004(6) 0.002(6) -0.008(6) C47 0.052(8) 0.041(8) 0.052(8) 0.012(6) 0.007(6) -0.018(6) C48 0.046(8) 0.051(8) 0.055(8) 0.011(7) 0.000(6) -0.024(7) C49 0.052(8) 0.036(7) 0.066(9) 0.016(6) -0.009(7) -0.026(6) C50 0.027(6) 0.039(7) 0.050(7) -0.001(6) 0.000(5) -0.002(6) C51 0.053(10) 0.101(14) 0.061(10) -0.010(9) 0.027(8) -0.021(10) F1 0.059(8) 0.050(9) 0.108(10) -0.017(8) 0.031(7) -0.024(7) F2 0.066(10) 0.080(13) 0.072(11) -0.022(10) 0.006(7) -0.006(10) F3 0.18(2) 0.059(10) 0.105(10) -0.017(7) 0.104(13) -0.048(13) F1A 0.059(8) 0.050(9) 0.108(10) -0.017(8) 0.031(7) -0.024(7) F2A 0.066(10) 0.080(13) 0.072(11) -0.022(10) 0.006(7) -0.006(10) F3A 0.18(2) 0.059(10) 0.105(10) -0.017(7) 0.104(13) -0.048(13) F1B 0.059(8) 0.050(9) 0.108(10) -0.017(8) 0.031(7) -0.024(7) F2B 0.066(10) 0.080(13) 0.072(11) -0.022(10) 0.006(7) -0.006(10) F3B 0.18(2) 0.059(10) 0.105(10) -0.017(7) 0.104(13) -0.048(13) C52 0.068(11) 0.055(10) 0.081(11) 0.020(8) -0.008(9) -0.032(9) F4 0.054(10) 0.056(9) 0.115(18) 0.000(10) -0.026(9) -0.013(7) F5 0.104(15) 0.092(10) 0.085(14) -0.007(11) -0.017(11) -0.065(11) F6 0.129(19) 0.103(13) 0.148(17) -0.045(11) 0.084(17) -0.106(16) F4A 0.054(10) 0.056(9) 0.115(18) 0.000(10) -0.026(9) -0.013(7) F5A 0.104(15) 0.092(10) 0.085(14) -0.007(11) -0.017(11) -0.065(11) F6A 0.129(19) 0.103(13) 0.148(17) -0.045(11) 0.084(17) -0.106(16) F4B 0.054(10) 0.056(9) 0.115(18) 0.000(10) -0.026(9) -0.013(7) F5B 0.104(15) 0.092(10) 0.085(14) -0.007(11) -0.017(11) -0.065(11) F6B 0.129(19) 0.103(13) 0.148(17) -0.045(11) 0.084(17) -0.106(16) C53 0.019(6) 0.044(7) 0.032(6) -0.012(5) 0.008(4) -0.013(5) C54 0.022(6) 0.055(8) 0.040(6) -0.012(6) 0.006(5) -0.022(6) C55 0.043(7) 0.039(7) 0.035(6) 0.000(5) 0.002(5) -0.022(6) C56 0.045(7) 0.030(6) 0.036(6) 0.000(5) 0.005(5) -0.013(6) C57 0.028(6) 0.044(7) 0.038(6) -0.005(5) 0.000(5) -0.015(6) C58 0.026(6) 0.045(7) 0.042(7) 0.000(5) -0.006(5) -0.017(6) C59 0.052(8) 0.060(10) 0.059(9) 0.001(7) 0.004(7) -0.034(7) F7 0.083(8) 0.099(12) 0.079(14) 0.000(9) -0.025(8) -0.075(8) F8 0.063(12) 0.056(12) 0.067(7) 0.018(8) 0.002(7) -0.028(9) F9 0.108(14) 0.059(11) 0.127(17) -0.018(10) 0.040(14) -0.054(10) F7A 0.083(8) 0.099(12) 0.079(14) 0.000(9) -0.025(8) -0.075(8) F8A 0.063(12) 0.056(12) 0.067(7) 0.018(8) 0.002(7) -0.028(9) F9A 0.108(14) 0.059(11) 0.127(17) -0.018(10) 0.040(14) -0.054(10) F7B 0.083(8) 0.099(12) 0.079(14) 0.000(9) -0.025(8) -0.075(8) F8B 0.063(12) 0.056(12) 0.067(7) 0.018(8) 0.002(7) -0.028(9) F9B 0.108(14) 0.059(11) 0.127(17) -0.018(10) 0.040(14) -0.054(10) C60 0.028(7) 0.073(11) 0.082(11) -0.004(9) -0.003(7) -0.017(8) F10 0.021(6) 0.16(2) 0.111(16) -0.061(14) -0.011(9) -0.022(9) F11 0.046(6) 0.042(7) 0.088(15) -0.028(8) 0.000(10) 0.007(5) F12 0.023(7) 0.065(15) 0.24(3) 0.040(15) 0.043(12) -0.015(8) F10A 0.021(6) 0.16(2) 0.111(16) -0.061(14) -0.011(9) -0.022(9) F11A 0.046(6) 0.042(7) 0.088(15) -0.028(8) 0.000(10) 0.007(5) F12A 0.023(7) 0.065(15) 0.24(3) 0.040(15) 0.043(12) -0.015(8) F10B 0.021(6) 0.16(2) 0.111(16) -0.061(14) -0.011(9) -0.022(9) F11B 0.046(6) 0.042(7) 0.088(15) -0.028(8) 0.000(10) 0.007(5) F12B 0.023(7) 0.065(15) 0.24(3) 0.040(15) 0.043(12) -0.015(8) C61 0.022(6) 0.035(7) 0.049(7) -0.010(5) 0.003(5) -0.012(5) C62 0.035(7) 0.026(6) 0.055(8) -0.002(5) -0.006(6) -0.014(5) C63 0.035(7) 0.029(6) 0.042(7) -0.006(5) 0.002(5) -0.011(5) C64 0.030(7) 0.044(7) 0.043(7) -0.007(5) 0.001(5) -0.011(6) C65 0.030(6) 0.024(6) 0.055(8) -0.009(5) -0.009(6) -0.004(5) C66 0.030(6) 0.033(6) 0.049(7) -0.006(5) -0.002(5) -0.008(5) C67 0.038(7) 0.033(7) 0.056(8) -0.008(6) 0.007(6) -0.006(6) F13 0.060(8) 0.064(6) 0.142(12) 0.019(7) 0.042(8) -0.019(5) F14 0.028(4) 0.117(12) 0.063(8) -0.039(9) 0.006(5) -0.013(6) F15 0.029(14) 0.064(12) 0.063(6) -0.023(8) 0.015(9) -0.007(13) F13A 0.060(8) 0.064(6) 0.142(12) 0.019(7) 0.042(8) -0.019(5) F14A 0.028(4) 0.117(12) 0.063(8) -0.039(9) 0.006(5) -0.013(6) F15A 0.029(14) 0.064(12) 0.063(6) -0.023(8) 0.015(9) -0.007(13) F13B 0.060(8) 0.064(6) 0.142(12) 0.019(7) 0.042(8) -0.019(5) F14B 0.028(4) 0.117(12) 0.063(8) -0.039(9) 0.006(5) -0.013(6) F15B 0.029(14) 0.064(12) 0.063(6) -0.023(8) 0.015(9) -0.007(13) C68 0.041(8) 0.063(10) 0.069(9) -0.008(8) -0.012(7) -0.022(7) F16 0.096(13) 0.048(11) 0.132(15) 0.029(12) -0.080(12) -0.035(11) F17 0.028(6) 0.059(16) 0.101(9) -0.030(11) 0.012(6) -0.022(9) F18 0.064(7) 0.084(11) 0.070(16) -0.026(11) 0.010(9) -0.050(7) F16A 0.096(13) 0.048(11) 0.132(15) 0.029(12) -0.080(12) -0.035(11) F17A 0.028(6) 0.059(16) 0.101(9) -0.030(11) 0.012(6) -0.022(9) F18A 0.064(7) 0.084(11) 0.070(16) -0.026(11) 0.010(9) -0.050(7) F16B 0.096(13) 0.048(11) 0.132(15) 0.029(12) -0.080(12) -0.035(11) F17B 0.028(6) 0.059(16) 0.101(9) -0.030(11) 0.012(6) -0.022(9) F18B 0.064(7) 0.084(11) 0.070(16) -0.026(11) 0.010(9) -0.050(7) C69 0.036(7) 0.053(8) 0.039(7) -0.009(6) 0.004(5) -0.011(6) C70 0.037(7) 0.057(8) 0.049(7) -0.014(6) -0.007(6) -0.013(6) C71 0.043(8) 0.085(11) 0.065(9) -0.020(8) -0.021(7) -0.017(8) C72 0.030(8) 0.102(13) 0.087(11) -0.016(10) -0.017(7) -0.019(8) C73 0.028(7) 0.056(8) 0.064(9) -0.009(7) 0.001(6) -0.005(6) C74 0.030(7) 0.052(8) 0.048(7) -0.008(6) -0.001(5) -0.014(6) C75 0.087(14) 0.103(16) 0.126(18) -0.039(14) -0.038(13) -0.039(13) F19 0.21(3) 0.16(3) 0.20(3) -0.03(2) -0.04(2) -0.13(3) F20 0.101(14) 0.131(16) 0.14(2) -0.085(17) -0.065(14) 0.009(13) F21 0.098(18) 0.136(14) 0.150(15) -0.041(12) -0.114(15) 0.007(16) F19A 0.21(3) 0.16(3) 0.20(3) -0.03(2) -0.04(2) -0.13(3) F20A 0.101(14) 0.131(16) 0.14(2) -0.085(17) -0.065(14) 0.009(13) F21A 0.098(18) 0.136(14) 0.150(15) -0.041(12) -0.114(15) 0.007(16) F19B 0.21(3) 0.16(3) 0.20(3) -0.03(2) -0.04(2) -0.13(3) F20B 0.101(14) 0.131(16) 0.14(2) -0.085(17) -0.065(14) 0.009(13) F21B 0.098(18) 0.136(14) 0.150(15) -0.041(12) -0.114(15) 0.007(16) C76 0.038(9) 0.083(12) 0.083(12) -0.005(10) -0.003(8) -0.005(8) F22 0.013(10) 0.058(6) 0.108(10) -0.017(6) 0.003(8) -0.004(7) F23 0.030(7) 0.138(12) 0.15(2) -0.056(16) 0.029(12) -0.033(7) F24 0.085(18) 0.091(10) 0.116(11) 0.005(8) -0.071(12) 0.019(11) F22A 0.013(10) 0.058(6) 0.108(10) -0.017(6) 0.003(8) -0.004(7) F23A 0.030(7) 0.138(12) 0.15(2) -0.056(16) 0.029(12) -0.033(7) F24A 0.085(18) 0.091(10) 0.116(11) 0.005(8) -0.071(12) 0.019(11) F22B 0.013(10) 0.058(6) 0.108(10) -0.017(6) 0.003(8) -0.004(7) F23B 0.030(7) 0.138(12) 0.15(2) -0.056(16) 0.029(12) -0.033(7) F24B 0.085(18) 0.091(10) 0.116(11) 0.005(8) -0.071(12) 0.019(11) _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 B1 C45 1.629(17) . ? B1 C61 1.629(16) . ? B1 C53 1.637(16) . ? B1 C69 1.643(16) . ? Mo1 Mo1 2.0920(17) 2_666 ? Mo1 N1 2.103(8) . ? Mo1 N2 2.105(8) 2_666 ? Mo1 N5 2.110(8) 2_666 ? Mo1 N4 2.120(9) . ? Mo2 Mo2 2.092(2) 2_667 ? Mo2 N8 2.111(9) 2_667 ? Mo2 N11 2.111(9) 2_667 ? Mo2 N7 2.111(9) . ? Mo2 N10 2.121(9) . ? N1 C4 1.330(13) . ? N1 C1 1.467(12) . ? N2 C4 1.363(13) . ? N2 C7 1.454(13) . ? N2 Mo1 2.105(8) 2_666 ? N3 C4 1.371(13) . ? N3 C5 1.416(14) . ? N3 C3 1.458(14) . ? N4 C15 1.324(13) . ? N4 C12 1.470(13) . ? N5 C15 1.320(12) . ? N5 C18 1.475(12) . ? N5 Mo1 2.110(8) 2_666 ? N6 C15 1.375(13) . ? N6 C16 1.446(14) . ? N6 C14 1.479(14) . ? N7 C26 1.363(14) . ? N7 C23 1.440(14) . ? N8 C26 1.336(14) . ? N8 C29 1.452(14) . ? N8 Mo2 2.111(9) 2_667 ? N9 C26 1.347(14) . ? N9 C25 1.451(16) . ? N9 C27 1.461(16) . ? N10 C37 1.337(15) . ? N10 C34 1.427(14) . ? N11 C37 1.332(14) . ? N11 C40 1.471(15) . ? N11 Mo2 2.111(9) 2_667 ? N12 C37 1.374(15) . ? N12 C36 1.435(15) . ? N12 C38 1.485(17) . ? C1 C2 1.530(15) . ? C2 C3 1.481(16) . ? C2 C8 1.543(15) . ? C2 C9 1.568(17) . ? C5 C6 1.527(16) . ? C6 C11 1.501(16) . ? C6 C10 1.528(16) . ? C6 C7 1.530(15) . ? C12 C13 1.518(16) . ? C13 C14 1.453(17) . ? C13 C20 1.511(19) . ? C13 C19 1.559(16) . ? C16 C17 1.511(17) . ? C17 C22 1.507(16) . ? C17 C18 1.523(15) . ? C17 C21 1.524(18) . ? C23 C24 1.534(16) . ? C24 C30 1.513(18) . ? C24 C25 1.529(19) . ? C24 C31 1.536(18) . ? C27 C28 1.529(18) . ? C28 C32 1.51(2) . ? C28 C29 1.509(17) . ? C28 C33 1.51(2) . ? C34 C35 1.525(17) . ? C35 C36 1.483(18) . ? C35 C42 1.516(18) . ? C35 C41 1.551(17) . ? C38 C39 1.526(19) . ? C39 C40 1.512(17) . ? C39 C44 1.53(2) . ? C39 C43 1.534(19) . ? C45 C46 1.402(12) . ? C45 C50 1.404(12) . ? C46 C47 1.401(12) . ? C47 C48 1.391(12) . ? C47 C51 1.482(12) . ? C48 C49 1.367(12) . ? C49 C50 1.375(12) . ? C49 C52 1.505(12) . ? C51 F3B 1.329(9) . ? C51 F2B 1.329(9) . ? C51 F1B 1.332(9) . ? C51 F1A 1.333(9) . ? C51 F2A 1.333(9) . ? C51 F3 1.336(8) . ? C51 F3A 1.336(9) . ? C51 F1 1.345(8) . ? C51 F2 1.350(8) . ? C52 F4B 1.22(5) . ? C52 F5A 1.23(3) . ? C52 F4A 1.24(4) . ? C52 F6B 1.25(6) . ? C52 F6 1.334(16) . ? C52 F5B 1.35(5) . ? C52 F6A 1.37(4) . ? C52 F4 1.373(17) . ? C52 F5 1.405(16) . ? C53 C54 1.389(11) . ? C53 C58 1.395(11) . ? C54 C55 1.397(12) . ? C55 C56 1.382(12) . ? C55 C59 1.476(12) . ? C56 C57 1.372(12) . ? C57 C58 1.365(11) . ? C57 C60 1.499(12) . ? C59 F7B 1.31(2) . ? C59 F8A 1.318(18) . ? C59 F8B 1.33(2) . ? C59 F9B 1.33(2) . ? C59 F9A 1.334(19) . ? C59 F7 1.338(14) . ? C59 F9 1.342(13) . ? C59 F7A 1.342(19) . ? C59 F8 1.372(13) . ? C60 F11A 1.24(3) . ? C60 F10A 1.24(4) . ? C60 F10B 1.24(5) . ? C60 F12B 1.24(6) . ? C60 F12 1.313(17) . ? C60 F11B 1.34(5) . ? C60 F12A 1.37(4) . ? C60 F10 1.383(17) . ? C60 F11 1.388(16) . ? C61 C66 1.396(11) . ? C61 C62 1.398(12) . ? C62 C63 1.396(11) . ? C63 C64 1.389(12) . ? C63 C67 1.474(12) . ? C64 C65 1.363(12) . ? C65 C66 1.380(11) . ? C65 C68 1.500(12) . ? C67 F14B 1.32(2) . ? C67 F15B 1.32(2) . ? C67 F14A 1.324(19) . ? C67 F13B 1.32(2) . ? C67 F15A 1.34(2) . ? C67 F13A 1.34(2) . ? C67 F15 1.342(14) . ? C67 F13 1.347(15) . ? C67 F14 1.362(14) . ? C68 F16B 1.24(5) . ? C68 F18B 1.24(6) . ? C68 F17A 1.24(3) . ? C68 F16A 1.25(4) . ? C68 F17B 1.35(5) . ? C68 F18 1.350(18) . ? C68 F18A 1.36(4) . ? C68 F16 1.364(17) . ? C68 F17 1.395(16) . ? C69 C74 1.399(12) . ? C69 C70 1.401(12) . ? C70 C71 1.393(12) . ? C71 C72 1.389(13) . ? C71 C75 1.474(13) . ? C72 C73 1.376(13) . ? C73 C74 1.383(12) . ? C73 C76 1.497(12) . ? C75 F20A 1.316(19) . ? C75 F19B 1.32(2) . ? C75 F21B 1.33(2) . ? C75 F20B 1.33(2) . ? C75 F21 1.338(14) . ? C75 F19A 1.339(19) . ? C75 F21A 1.340(19) . ? C75 F19 1.348(16) . ? C75 F20 1.359(15) . ? C76 F22A 1.24(4) . ? C76 F24B 1.24(6) . ? C76 F23A 1.24(3) . ? C76 F22B 1.24(5) . ? C76 F24 1.338(18) . ? C76 F23B 1.35(5) . ? C76 F24A 1.38(4) . ? C76 F22 1.380(18) . ? C76 F23 1.385(17) . ? 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 C45 B1 C61 112.4(10) . . ? C45 B1 C53 111.0(9) . . ? C61 B1 C53 103.9(9) . . ? C45 B1 C69 105.2(10) . . ? C61 B1 C69 111.5(9) . . ? C53 B1 C69 113.0(10) . . ? Mo1 Mo1 N1 92.7(2) 2_666 . ? Mo1 Mo1 N2 92.5(2) 2_666 2_666 ? N1 Mo1 N2 174.9(3) . 2_666 ? Mo1 Mo1 N5 92.3(2) 2_666 2_666 ? N1 Mo1 N5 90.2(3) . 2_666 ? N2 Mo1 N5 89.6(3) 2_666 2_666 ? Mo1 Mo1 N4 92.3(2) 2_666 . ? N1 Mo1 N4 90.0(3) . . ? N2 Mo1 N4 89.8(3) 2_666 . ? N5 Mo1 N4 175.4(3) 2_666 . ? Mo2 Mo2 N8 92.7(3) 2_667 2_667 ? Mo2 Mo2 N11 92.6(3) 2_667 2_667 ? N8 Mo2 N11 89.6(4) 2_667 2_667 ? Mo2 Mo2 N7 92.8(3) 2_667 . ? N8 Mo2 N7 174.4(4) 2_667 . ? N11 Mo2 N7 89.1(3) 2_667 . ? Mo2 Mo2 N10 92.7(3) 2_667 . ? N8 Mo2 N10 89.1(4) 2_667 . ? N11 Mo2 N10 174.6(4) 2_667 . ? N7 Mo2 N10 91.7(3) . . ? C4 N1 C1 118.6(9) . . ? C4 N1 Mo1 120.0(7) . . ? C1 N1 Mo1 121.4(7) . . ? C4 N2 C7 119.6(9) . . ? C4 N2 Mo1 119.1(7) . 2_666 ? C7 N2 Mo1 121.3(7) . 2_666 ? C4 N3 C5 121.0(9) . . ? C4 N3 C3 118.9(9) . . ? C5 N3 C3 118.5(9) . . ? C15 N4 C12 121.3(9) . . ? C15 N4 Mo1 118.7(6) . . ? C12 N4 Mo1 119.7(7) . . ? C15 N5 C18 119.2(8) . . ? C15 N5 Mo1 119.2(7) . 2_666 ? C18 N5 Mo1 121.4(6) . 2_666 ? C15 N6 C16 121.2(9) . . ? C15 N6 C14 119.6(9) . . ? C16 N6 C14 117.6(9) . . ? C26 N7 C23 119.4(9) . . ? C26 N7 Mo2 118.6(7) . . ? C23 N7 Mo2 121.9(8) . . ? C26 N8 C29 118.5(9) . . ? C26 N8 Mo2 119.4(7) . 2_667 ? C29 N8 Mo2 122.1(7) . 2_667 ? C26 N9 C25 122.7(11) . . ? C26 N9 C27 120.5(10) . . ? C25 N9 C27 115.6(10) . . ? C37 N10 C34 121.3(10) . . ? C37 N10 Mo2 118.0(7) . . ? C34 N10 Mo2 120.6(8) . . ? C37 N11 C40 119.2(10) . . ? C37 N11 Mo2 118.7(8) . 2_667 ? C40 N11 Mo2 122.0(7) . 2_667 ? C37 N12 C36 121.3(11) . . ? C37 N12 C38 121.5(10) . . ? C36 N12 C38 116.5(10) . . ? N1 C1 C2 113.6(9) . . ? C3 C2 C1 106.8(9) . . ? C3 C2 C8 109.4(11) . . ? C1 C2 C8 110.6(9) . . ? C3 C2 C9 110.9(10) . . ? C1 C2 C9 109.3(10) . . ? C8 C2 C9 109.7(10) . . ? N3 C3 C2 112.7(9) . . ? N1 C4 N2 115.7(9) . . ? N1 C4 N3 123.6(9) . . ? N2 C4 N3 120.5(9) . . ? N3 C5 C6 113.1(9) . . ? C11 C6 C5 110.2(10) . . ? C11 C6 C10 110.2(10) . . ? C5 C6 C10 110.5(10) . . ? C11 C6 C7 110.9(10) . . ? C5 C6 C7 104.6(9) . . ? C10 C6 C7 110.3(9) . . ? N2 C7 C6 114.9(9) . . ? N4 C12 C13 111.8(9) . . ? C14 C13 C20 112.6(12) . . ? C14 C13 C12 108.0(10) . . ? C20 C13 C12 109.2(11) . . ? C14 C13 C19 111.2(10) . . ? C20 C13 C19 107.7(12) . . ? C12 C13 C19 108.0(10) . . ? C13 C14 N6 111.7(10) . . ? N5 C15 N4 117.5(9) . . ? N5 C15 N6 121.6(9) . . ? N4 C15 N6 120.8(9) . . ? N6 C16 C17 110.8(9) . . ? C22 C17 C16 108.7(10) . . ? C22 C17 C18 110.5(9) . . ? C16 C17 C18 105.4(10) . . ? C22 C17 C21 110.9(11) . . ? C16 C17 C21 111.4(10) . . ? C18 C17 C21 109.7(10) . . ? N5 C18 C17 113.7(8) . . ? N7 C23 C24 113.5(10) . . ? C30 C24 C25 109.4(11) . . ? C30 C24 C23 110.7(11) . . ? C25 C24 C23 105.2(11) . . ? C30 C24 C31 111.2(12) . . ? C25 C24 C31 111.1(12) . . ? C23 C24 C31 109.1(10) . . ? N9 C25 C24 111.1(10) . . ? N8 C26 N9 122.7(10) . . ? N8 C26 N7 116.5(9) . . ? N9 C26 N7 120.7(10) . . ? N9 C27 C28 110.6(10) . . ? C32 C28 C29 110.6(13) . . ? C32 C28 C33 112.0(13) . . ? C29 C28 C33 109.7(12) . . ? C32 C28 C27 108.6(12) . . ? C29 C28 C27 105.3(10) . . ? C33 C28 C27 110.3(13) . . ? N8 C29 C28 115.2(11) . . ? N10 C34 C35 114.0(11) . . ? C36 C35 C42 109.8(13) . . ? C36 C35 C34 107.1(10) . . ? C42 C35 C34 110.2(10) . . ? C36 C35 C41 110.1(10) . . ? C42 C35 C41 109.7(10) . . ? C34 C35 C41 109.9(11) . . ? N12 C36 C35 110.9(10) . . ? N11 C37 N10 118.0(10) . . ? N11 C37 N12 122.2(11) . . ? N10 C37 N12 119.8(10) . . ? N12 C38 C39 110.8(10) . . ? C40 C39 C38 107.3(12) . . ? C40 C39 C44 110.1(11) . . ? C38 C39 C44 109.2(11) . . ? C40 C39 C43 111.1(11) . . ? C38 C39 C43 109.3(12) . . ? C44 C39 C43 109.9(13) . . ? N11 C40 C39 114.3(10) . . ? C46 C45 C50 113.5(10) . . ? C46 C45 B1 121.3(10) . . ? C50 C45 B1 125.2(9) . . ? C47 C46 C45 124.3(10) . . ? C48 C47 C46 119.4(9) . . ? C48 C47 C51 122.3(9) . . ? C46 C47 C51 118.1(9) . . ? C49 C48 C47 117.2(9) . . ? C48 C49 C50 123.0(9) . . ? C48 C49 C52 118.5(9) . . ? C50 C49 C52 118.4(9) . . ? C49 C50 C45 122.5(10) . . ? F3B C51 F2B 107.5(10) . . ? F3B C51 F1B 107.0(10) . . ? F2B C51 F1B 107.0(10) . . ? F3B C51 F1A 133(3) . . ? F2B C51 F1A 65(2) . . ? F3B C51 F2A 64(2) . . ? F2B C51 F2A 46(2) . . ? F1B C51 F2A 134(3) . . ? F1A C51 F2A 106.6(9) . . ? F3B C51 F3 69(3) . . ? F2B C51 F3 126(2) . . ? F1A C51 F3 78.3(16) . . ? F2A C51 F3 119(3) . . ? F3B C51 F3A 45(2) . . ? F2B C51 F3A 137(3) . . ? F1B C51 F3A 66(2) . . ? F1A C51 F3A 106.6(9) . . ? F2A C51 F3A 106.4(9) . . ? F3B C51 F1 131(2) . . ? F1B C51 F1 76(3) . . ? F2A C51 F1 79.0(15) . . ? F3 C51 F1 106.2(8) . . ? F3A C51 F1 131.7(18) . . ? F2B C51 F2 72(3) . . ? F1B C51 F2 137(2) . . ? F1A C51 F2 128.2(17) . . ? F3 C51 F2 105.2(8) . . ? F3A C51 F2 85(2) . . ? F1 C51 F2 104.3(8) . . ? F3B C51 C47 112(2) . . ? F2B C51 C47 116(2) . . ? F1B C51 C47 107(2) . . ? F1A C51 C47 112.4(16) . . ? F2A C51 C47 118.0(19) . . ? F3 C51 C47 114.9(11) . . ? F3A C51 C47 106.1(18) . . ? F1 C51 C47 113.3(10) . . ? F2 C51 C47 112.1(11) . . ? F4B C52 F5A 67(3) . . ? F4B C52 F4A 49(3) . . ? F5A C52 F4A 108(3) . . ? F4B C52 F6B 119(3) . . ? F5A C52 F6B 129(3) . . ? F4A C52 F6B 72(3) . . ? F4B C52 F6 123(3) . . ? F5A C52 F6 68(2) . . ? F4A C52 F6 119(3) . . ? F6B C52 F6 69(3) . . ? F4B C52 F5B 109(3) . . ? F4A C52 F5B 137(3) . . ? F6B C52 F5B 103(3) . . ? F4B C52 F6A 136(3) . . ? F5A C52 F6A 108(2) . . ? F4A C52 F6A 97(2) . . ? F5B C52 F6A 74(3) . . ? F4B C52 F4 75(3) . . ? F5A C52 F4 127(2) . . ? F6B C52 F4 47(3) . . ? F6 C52 F4 107.2(14) . . ? F5B C52 F4 138(3) . . ? F6A C52 F4 75(2) . . ? F4A C52 F5 76(2) . . ? F6B C52 F5 137(3) . . ? F6 C52 F5 104.3(13) . . ? F5B C52 F5 82(3) . . ? F6A C52 F5 136.8(19) . . ? F4 C52 F5 101.1(13) . . ? F4B C52 C49 113(3) . . ? F5A C52 C49 114.9(19) . . ? F4A C52 C49 118(2) . . ? F6B C52 C49 108(2) . . ? F6 C52 C49 117.1(12) . . ? F5B C52 C49 104(2) . . ? F6A C52 C49 108.0(18) . . ? F4 C52 C49 112.9(12) . . ? F5 C52 C49 112.6(11) . . ? C54 C53 C58 114.9(9) . . ? C54 C53 B1 123.3(9) . . ? C58 C53 B1 121.5(9) . . ? C53 C54 C55 123.2(9) . . ? C56 C55 C54 119.1(8) . . ? C56 C55 C59 121.0(9) . . ? C54 C55 C59 119.8(8) . . ? C57 C56 C55 118.5(9) . . ? C58 C57 C56 121.5(8) . . ? C58 C57 C60 119.4(8) . . ? C56 C57 C60 119.1(9) . . ? C57 C58 C53 122.5(9) . . ? F7B C59 F8A 63(3) . . ? F7B C59 F8B 108(3) . . ? F8A C59 F8B 48(3) . . ? F7B C59 F9B 108(3) . . ? F8A C59 F9B 134(3) . . ? F8B C59 F9B 108(2) . . ? F7B C59 F9A 139(3) . . ? F8A C59 F9A 112(2) . . ? F8B C59 F9A 68(3) . . ? F7B C59 F7 71(3) . . ? F8A C59 F7 119(2) . . ? F8B C59 F7 128(3) . . ? F9A C59 F7 80(2) . . ? F7B C59 F9 129(3) . . ? F8A C59 F9 77.5(17) . . ? F9B C59 F9 77(3) . . ? F7 C59 F9 107.1(13) . . ? F7B C59 F7A 49(3) . . ? F8A C59 F7A 106(2) . . ? F8B C59 F7A 137(3) . . ? F9B C59 F7A 62(3) . . ? F9A C59 F7A 104(2) . . ? F9 C59 F7A 127(2) . . ? F8B C59 F8 76(3) . . ? F9B C59 F8 134(3) . . ? F9A C59 F8 135.4(19) . . ? F7 C59 F8 102.6(12) . . ? F9 C59 F8 104.9(11) . . ? F7A C59 F8 83(2) . . ? F7B C59 C55 110(2) . . ? F8A C59 C55 116.9(19) . . ? F8B C59 C55 114(2) . . ? F9B C59 C55 109(2) . . ? F9A C59 C55 107.8(18) . . ? F7 C59 C55 114.7(12) . . ? F9 C59 C55 115.5(11) . . ? F7A C59 C55 109(2) . . ? F8 C59 C55 110.9(10) . . ? F11A C60 F10A 111(3) . . ? F11A C60 F10B 133(3) . . ? F11A C60 F12B 57(3) . . ? F10A C60 F12B 126(3) . . ? F10B C60 F12B 115(3) . . ? F11A C60 F12 124(2) . . ? F10A C60 F12 61(2) . . ? F12B C60 F12 82(3) . . ? F11A C60 F11B 49(2) . . ? F10A C60 F11B 77(3) . . ? F10B C60 F11B 107(3) . . ? F12B C60 F11B 105(3) . . ? F12 C60 F11B 131(3) . . ? F11A C60 F12A 105(2) . . ? F10A C60 F12A 95(2) . . ? F10B C60 F12A 71(3) . . ? F12B C60 F12A 51(3) . . ? F11B C60 F12A 143(3) . . ? F11A C60 F10 79(2) . . ? F10A C60 F10 47(2) . . ? F10B C60 F10 76(3) . . ? F12B C60 F10 131(3) . . ? F12 C60 F10 107.7(14) . . ? F12A C60 F10 138(2) . . ? F10A C60 F11 124(2) . . ? F10B C60 F11 132(3) . . ? F12 C60 F11 107.2(13) . . ? F11B C60 F11 75(2) . . ? F12A C60 F11 81(2) . . ? F10 C60 F11 103.8(12) . . ? F11A C60 C57 115(2) . . ? F10A C60 C57 120.4(19) . . ? F10B C60 C57 111(3) . . ? F12B C60 C57 111(3) . . ? F12 C60 C57 115.2(12) . . ? F11B C60 C57 107(2) . . ? F12A C60 C57 107(2) . . ? F10 C60 C57 108.2(10) . . ? F11 C60 C57 114.0(11) . . ? C66 C61 C62 113.9(9) . . ? C66 C61 B1 122.5(9) . . ? C62 C61 B1 123.4(9) . . ? C63 C62 C61 124.0(9) . . ? C64 C63 C62 119.2(8) . . ? C64 C63 C67 119.9(8) . . ? C62 C63 C67 121.0(8) . . ? C65 C64 C63 118.3(9) . . ? C64 C65 C66 121.7(8) . . ? C64 C65 C68 117.9(8) . . ? C66 C65 C68 120.3(8) . . ? C65 C66 C61 122.9(9) . . ? F14B C67 F15B 112(2) . . ? F15B C67 F14A 125(4) . . ? F14B C67 F13B 108(3) . . ? F15B C67 F13B 107(3) . . ? F14A C67 F13B 85(6) . . ? F14B C67 F15A 90(5) . . ? F14A C67 F15A 109(3) . . ? F13B C67 F15A 129(5) . . ? F14B C67 F13A 127(5) . . ? F15B C67 F13A 81(6) . . ? F14A C67 F13A 107(3) . . ? F15A C67 F13A 105(3) . . ? F14B C67 F15 79(3) . . ? F14A C67 F15 96(6) . . ? F13B C67 F15 128(3) . . ? F13A C67 F15 108(7) . . ? F14B C67 F13 123(4) . . ? F15B C67 F13 80(4) . . ? F14A C67 F13 103(7) . . ? F15A C67 F13 104(7) . . ? F15 C67 F13 105.8(15) . . ? F15B C67 F14 133(2) . . ? F13B C67 F14 82(4) . . ? F15A C67 F14 116(6) . . ? F13A C67 F14 106(7) . . ? F15 C67 F14 103.8(14) . . ? F13 C67 F14 102.9(15) . . ? F14B C67 C63 112(3) . . ? F15B C67 C63 109(2) . . ? F14A C67 C63 118(3) . . ? F13B C67 C63 108(3) . . ? F15A C67 C63 108(2) . . ? F13A C67 C63 110(3) . . ? F15 C67 C63 116.7(14) . . ? F13 C67 C63 114.7(15) . . ? F14 C67 C63 111.6(14) . . ? F16B C68 F18B 118(4) . . ? F16B C68 F17A 52(3) . . ? F18B C68 F17A 136(3) . . ? F16B C68 F16A 64(4) . . ? F18B C68 F16A 57(4) . . ? F17A C68 F16A 107(3) . . ? F16B C68 F17B 106(3) . . ? F18B C68 F17B 106(3) . . ? F17A C68 F17B 55(3) . . ? F16A C68 F17B 136(3) . . ? F16B C68 F18 134(3) . . ? F17A C68 F18 124(2) . . ? F16A C68 F18 80(2) . . ? F17B C68 F18 81(2) . . ? F16B C68 F18A 140(3) . . ? F18B C68 F18A 45(4) . . ? F17A C68 F18A 110(3) . . ? F16A C68 F18A 97(3) . . ? F17B C68 F18A 62(3) . . ? F18B C68 F16 84(3) . . ? F17A C68 F16 87(2) . . ? F17B C68 F16 135(3) . . ? F18 C68 F16 105.8(13) . . ? F18A C68 F16 122(3) . . ? F16B C68 F17 78(3) . . ? F18B C68 F17 122(3) . . ? F16A C68 F17 122(3) . . ? F18 C68 F17 102.7(11) . . ? F18A C68 F17 86(2) . . ? F16 C68 F17 109.2(13) . . ? F16B C68 C65 109(3) . . ? F18B C68 C65 111(3) . . ? F17A C68 C65 112(2) . . ? F16A C68 C65 118(2) . . ? F17B C68 C65 106(2) . . ? F18 C68 C65 112.4(12) . . ? F18A C68 C65 111(2) . . ? F16 C68 C65 111.8(11) . . ? F17 C68 C65 114.3(11) . . ? C74 C69 C70 114.5(9) . . ? C74 C69 B1 122.0(9) . . ? C70 C69 B1 123.3(9) . . ? C71 C70 C69 122.7(10) . . ? C72 C71 C70 120.2(9) . . ? C72 C71 C75 120.0(9) . . ? C70 C71 C75 119.7(10) . . ? C73 C72 C71 118.6(10) . . ? C72 C73 C74 120.3(9) . . ? C72 C73 C76 118.8(9) . . ? C74 C73 C76 120.9(9) . . ? C73 C74 C69 123.6(10) . . ? F20A C75 F19B 129(4) . . ? F20A C75 F21B 75(4) . . ? F19B C75 F21B 109(3) . . ? F19B C75 F20B 108(3) . . ? F21B C75 F20B 109(3) . . ? F20A C75 F21 123(3) . . ? F21B C75 F21 70(4) . . ? F20B C75 F21 128(3) . . ? F20A C75 F19A 109(3) . . ? F21B C75 F19A 133(3) . . ? F20B C75 F19A 80(4) . . ? F21 C75 F19A 69(3) . . ? F20A C75 F21A 109(2) . . ? F19B C75 F21A 75(4) . . ? F20B C75 F21A 137(3) . . ? F19A C75 F21A 105(2) . . ? F20A C75 F19 67(3) . . ? F19B C75 F19 76(4) . . ? F21B C75 F19 132(3) . . ? F21 C75 F19 106.3(16) . . ? F19A C75 F19 45(3) . . ? F21A C75 F19 135(2) . . ? F19B C75 F20 134(3) . . ? F20B C75 F20 73(4) . . ? F21 C75 F20 102.3(15) . . ? F19A C75 F20 136(3) . . ? F21A C75 F20 75(3) . . ? F19 C75 F20 103.7(17) . . ? F20A C75 C71 118(2) . . ? F19B C75 C71 108(3) . . ? F21B C75 C71 110(2) . . ? F20B C75 C71 113(3) . . ? F21 C75 C71 115.8(14) . . ? F19A C75 C71 109(2) . . ? F21A C75 C71 107(2) . . ? F19 C75 C71 114.2(15) . . ? F20 C75 C71 113.2(14) . . ? F22A C76 F24B 55(4) . . ? F22A C76 F23A 110(3) . . ? F24B C76 F23A 132(3) . . ? F22A C76 F22B 64(3) . . ? F24B C76 F22B 118(3) . . ? F23A C76 F22B 59(3) . . ? F22A C76 F24 110(4) . . ? F24B C76 F24 67(3) . . ? F23A C76 F24 82(3) . . ? F22B C76 F24 131(3) . . ? F22A C76 F23B 132(3) . . ? F24B C76 F23B 105(3) . . ? F23A C76 F23B 47(3) . . ? F22B C76 F23B 106(3) . . ? F22A C76 F24A 96(3) . . ? F24B C76 F24A 45(3) . . ? F23A C76 F24A 106(3) . . ? F22B C76 F24A 143(3) . . ? F23B C76 F24A 63(3) . . ? F23A C76 F22 127(3) . . ? F22B C76 F22 79(3) . . ? F24 C76 F22 106.0(15) . . ? F23B C76 F22 138(3) . . ? F24A C76 F22 87(3) . . ? F22A C76 F23 88(3) . . ? F24B C76 F23 133(3) . . ? F24 C76 F23 108.7(14) . . ? F23B C76 F23 77(3) . . ? F24A C76 F23 129(3) . . ? F22 C76 F23 104.7(14) . . ? F22A C76 C73 121(2) . . ? F24B C76 C73 112(3) . . ? F23A C76 C73 113(2) . . ? F22B C76 C73 109(2) . . ? F24 C76 C73 113.0(14) . . ? F23B C76 C73 107(2) . . ? F24A C76 C73 108(2) . . ? F22 C76 C73 111.2(11) . . ? F23 C76 C73 112.8(13) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.018 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.116 #===END of CIF for compound 2 =========================== data_2CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 645813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H80 Mo2 N12, C32 H12 B F24, C H2 Cl2' _chemical_formula_sum 'C77 H94 B Cl2 F24 Mo2 N12' _chemical_formula_weight 1917.23 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.020(4) _cell_length_b 14.276(5) _cell_length_c 28.222(10) _cell_angle_alpha 90.799(7) _cell_angle_beta 90.432(6) _cell_angle_gamma 114.659(6) _cell_volume 4400(3) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7071 _cell_measurement_theta_min 2.156 _cell_measurement_theta_max 25.074 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1958 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8564 _exptl_absorpt_correction_T_max 0.9738 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24824 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 23.00 _reflns_number_total 12127 _reflns_number_gt 9862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+54.5878P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12127 _refine_ls_number_parameters 1184 _refine_ls_number_restraints 279 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.1050 _refine_ls_wR_factor_ref 0.2790 _refine_ls_wR_factor_gt 0.2660 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.015 _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 B1 B 0.4446(12) 0.5078(10) 0.7516(4) 0.039(3) Uani 1 1 d . . . Mo1 Mo 0.04053(7) 0.07586(6) 0.51341(3) 0.0286(3) Uani 1 1 d . . . Mo2 Mo 0.02789(8) 0.06912(7) 0.01996(3) 0.0381(3) Uani 1 1 d . . . N1 N 0.2100(8) 0.1062(6) 0.4800(3) 0.036(2) Uani 1 1 d . . . N2 N 0.1225(8) -0.0574(7) 0.4512(3) 0.040(2) Uani 1 1 d . . . N3 N 0.3233(8) 0.0433(7) 0.4311(4) 0.051(3) Uani 1 1 d . . . N4 N 0.1031(8) 0.0300(6) 0.5753(3) 0.036(2) Uani 1 1 d . . . N5 N 0.0166(7) -0.1346(6) 0.5457(3) 0.034(2) Uani 1 1 d . . . N6 N 0.1188(9) -0.1023(7) 0.6205(3) 0.044(2) Uani 1 1 d . . . N7 N -0.1208(9) 0.0995(7) -0.0059(3) 0.044(2) Uani 1 1 d . . . N8 N -0.1824(8) -0.0560(8) -0.0487(3) 0.043(2) Uani 1 1 d . . . N9 N -0.3019(9) 0.0399(9) -0.0522(3) 0.056(3) Uani 1 1 d . . . N10 N -0.0787(8) -0.0049(8) 0.0784(3) 0.044(2) Uani 1 1 d . . . N11 N -0.1396(8) -0.1561(8) 0.0351(3) 0.048(2) Uani 1 1 d . . . N12 N -0.2214(10) -0.1620(9) 0.1106(3) 0.060(3) Uani 1 1 d . . . C1 C 0.3173(10) 0.2058(8) 0.4850(4) 0.045(3) Uani 1 1 d . . . H1A H 0.3641 0.2045 0.5133 0.054 Uiso 1 1 calc R . . H1B H 0.2888 0.2603 0.4898 0.054 Uiso 1 1 calc R . . C2 C 0.4008(11) 0.2322(8) 0.4431(4) 0.047(3) Uani 1 1 d . . . C3 C 0.4333(11) 0.1416(10) 0.4363(6) 0.071(4) Uani 1 1 d . . . H3A H 0.4834 0.1520 0.4080 0.086 Uiso 1 1 calc R . . H3B H 0.4822 0.1379 0.4636 0.086 Uiso 1 1 calc R . . C4 C 0.2179(9) 0.0273(8) 0.4546(4) 0.038(3) Uani 1 1 d . . . C5 C 0.3402(10) -0.0422(10) 0.4081(6) 0.072(4) Uani 1 1 d D . . H5A H 0.3768 -0.0728 0.4309 0.086 Uiso 1 1 calc R . . H5B H 0.3967 -0.0160 0.3817 0.086 Uiso 1 1 calc R . . C6 C 0.2195(11) -0.1244(9) 0.3897(5) 0.061(4) Uani 1 1 d D . . C7 C 0.1276(11) -0.1507(9) 0.4273(5) 0.052(3) Uani 1 1 d . . . H7A H 0.1464 -0.1913 0.4513 0.063 Uiso 1 1 calc R . . H7B H 0.0468 -0.1938 0.4136 0.063 Uiso 1 1 calc R . . C8 C 0.5181(12) 0.3291(10) 0.4541(5) 0.071(4) Uani 1 1 d . . . H8A H 0.5587 0.3178 0.4818 0.106 Uiso 1 1 calc R . . H8B H 0.4975 0.3870 0.4602 0.106 Uiso 1 1 calc R . . H8C H 0.5724 0.3439 0.4272 0.106 Uiso 1 1 calc R . . C9 C 0.3369(14) 0.2485(12) 0.3996(5) 0.074(4) Uani 1 1 d . . . H9A H 0.2633 0.1866 0.3927 0.112 Uiso 1 1 calc R . . H9B H 0.3912 0.2634 0.3728 0.112 Uiso 1 1 calc R . . H9C H 0.3152 0.3059 0.4054 0.112 Uiso 1 1 calc R . . C10 C 0.2348(15) -0.2166(11) 0.3700(6) 0.084(5) Uani 1 1 d . . . H10A H 0.2656 -0.2464 0.3947 0.126 Uiso 1 1 calc R . . H10B H 0.2923 -0.1954 0.3441 0.126 Uiso 1 1 calc R . . H10C H 0.1563 -0.2673 0.3584 0.126 Uiso 1 1 calc R . . C11 C 0.1738(16) -0.0767(12) 0.3489(5) 0.083(5) Uani 1 1 d . . . H11A H 0.1658 -0.0156 0.3607 0.125 Uiso 1 1 calc R . . H11B H 0.0948 -0.1266 0.3373 0.125 Uiso 1 1 calc R . . H11C H 0.2321 -0.0580 0.3234 0.125 Uiso 1 1 calc R . . C12 C 0.1680(11) 0.1071(9) 0.6134(4) 0.046(3) Uani 1 1 d . . . H12A H 0.1074 0.1157 0.6339 0.055 Uiso 1 1 calc R . . H12B H 0.2163 0.1737 0.5990 0.055 Uiso 1 1 calc R . . C13 C 0.2525(10) 0.0758(9) 0.6434(4) 0.045(3) Uani 1 1 d . . . C14 C 0.1773(12) -0.0310(9) 0.6597(4) 0.051(3) Uani 1 1 d . . . H14A H 0.2298 -0.0556 0.6775 0.061 Uiso 1 1 calc R . . H14B H 0.1142 -0.0296 0.6811 0.061 Uiso 1 1 calc R . . C15 C 0.0771(9) -0.0691(9) 0.5812(4) 0.039(3) Uani 1 1 d . . . C16 C 0.0820(12) -0.2117(9) 0.6269(4) 0.050(3) Uani 1 1 d . . . H16A H 0.0019 -0.2411 0.6421 0.060 Uiso 1 1 calc R . . H16B H 0.1411 -0.2217 0.6481 0.060 Uiso 1 1 calc R . . C17 C 0.0743(10) -0.2679(8) 0.5810(4) 0.044(3) Uani 1 1 d . . . C18 C -0.0164(11) -0.2451(9) 0.5490(5) 0.052(3) Uani 1 1 d . . . H18A H -0.0176 -0.2738 0.5172 0.062 Uiso 1 1 calc R . . H18B H -0.0990 -0.2791 0.5618 0.062 Uiso 1 1 calc R . . C19 C 0.3598(11) 0.0785(12) 0.6144(5) 0.067(4) Uani 1 1 d . . . H19A H 0.3295 0.0308 0.5877 0.101 Uiso 1 1 calc R . . H19B H 0.4127 0.0588 0.6341 0.101 Uiso 1 1 calc R . . H19C H 0.4056 0.1477 0.6030 0.101 Uiso 1 1 calc R . . C20 C 0.3020(13) 0.1514(10) 0.6864(5) 0.066(4) Uani 1 1 d . . . H20A H 0.2339 0.1504 0.7050 0.099 Uiso 1 1 calc R . . H20B H 0.3490 0.2206 0.6752 0.099 Uiso 1 1 calc R . . H20C H 0.3541 0.1306 0.7060 0.099 Uiso 1 1 calc R . . C21 C 0.0185(15) -0.3861(10) 0.5881(6) 0.078(4) Uani 1 1 d . . . H21A H 0.0731 -0.4036 0.6079 0.116 Uiso 1 1 calc R . . H21B H 0.0078 -0.4210 0.5575 0.116 Uiso 1 1 calc R . . H21C H -0.0602 -0.4076 0.6032 0.116 Uiso 1 1 calc R . . C22 C 0.1974(12) -0.2328(11) 0.5578(5) 0.060(3) Uani 1 1 d . . . H22A H 0.2315 -0.1588 0.5537 0.090 Uiso 1 1 calc R . . H22B H 0.1877 -0.2670 0.5271 0.090 Uiso 1 1 calc R . . H22C H 0.2521 -0.2501 0.5776 0.090 Uiso 1 1 calc R . . C23 C -0.1400(12) 0.1886(10) 0.0097(4) 0.058(3) Uani 1 1 d . . . H23A H -0.0601 0.2456 0.0163 0.070 Uiso 1 1 calc R . . H23B H -0.1851 0.1722 0.0394 0.070 Uiso 1 1 calc R . . C24 C -0.2077(13) 0.2233(11) -0.0248(4) 0.059(3) Uani 1 1 d . . . C25 C -0.3270(12) 0.1289(12) -0.0378(5) 0.067(4) Uani 1 1 d . . . H25A H -0.3814 0.1105 -0.0105 0.081 Uiso 1 1 calc R . . H25B H -0.3689 0.1463 -0.0639 0.081 Uiso 1 1 calc R . . C26 C -0.2032(10) 0.0282(10) -0.0353(4) 0.043(3) Uani 1 1 d . . . C27 C -0.3968(12) -0.0425(12) -0.0796(5) 0.066(4) Uani 1 1 d . . . H27A H -0.4407 -0.0130 -0.0996 0.079 Uiso 1 1 calc R . . H27B H -0.4559 -0.0906 -0.0580 0.079 Uiso 1 1 calc R . . C28 C -0.3441(11) -0.0998(10) -0.1103(4) 0.051(3) Uani 1 1 d . . . C29 C -0.2679(11) -0.1339(9) -0.0788(4) 0.050(3) Uani 1 1 d . . . H29A H -0.3228 -0.1895 -0.0589 0.060 Uiso 1 1 calc R . . H29B H -0.2229 -0.1627 -0.0987 0.060 Uiso 1 1 calc R . . C30 C -0.2388(16) 0.3094(13) -0.0045(6) 0.090(5) Uani 1 1 d . . . H30A H -0.2874 0.2856 0.0237 0.135 Uiso 1 1 calc R . . H30B H -0.2851 0.3281 -0.0280 0.135 Uiso 1 1 calc R . . H30C H -0.1638 0.3691 0.0035 0.135 Uiso 1 1 calc R . . C31 C -0.1333(13) 0.2593(12) -0.0699(5) 0.075(4) Uani 1 1 d . . . H31A H -0.1179 0.2031 -0.0835 0.112 Uiso 1 1 calc R . . H31B H -0.0560 0.3169 -0.0623 0.112 Uiso 1 1 calc R . . H31C H -0.1789 0.2807 -0.0925 0.112 Uiso 1 1 calc R . . C32 C -0.4485(12) -0.1911(11) -0.1349(5) 0.067(4) Uani 1 1 d . . . H32A H -0.4993 -0.2377 -0.1113 0.100 Uiso 1 1 calc R . . H32B H -0.4144 -0.2275 -0.1553 0.100 Uiso 1 1 calc R . . H32C H -0.4977 -0.1659 -0.1538 0.100 Uiso 1 1 calc R . . C33 C -0.2617(17) -0.0230(13) -0.1478(5) 0.086(5) Uani 1 1 d . . . H33A H -0.1963 0.0344 -0.1318 0.129 Uiso 1 1 calc R . . H33B H -0.3109 0.0026 -0.1665 0.129 Uiso 1 1 calc R . . H33C H -0.2269 -0.0583 -0.1685 0.129 Uiso 1 1 calc R . . C34 C -0.0777(11) 0.0477(11) 0.1231(4) 0.055(3) Uani 1 1 d . . . H34A H -0.0586 0.1201 0.1168 0.066 Uiso 1 1 calc R . . H34B H -0.0126 0.0458 0.1436 0.066 Uiso 1 1 calc R . . C35 C -0.1993(12) 0.0003(11) 0.1493(4) 0.059(4) Uani 1 1 d . . . C36 C -0.2272(13) -0.1128(12) 0.1553(4) 0.066(4) Uani 1 1 d . . . H36A H -0.1681 -0.1188 0.1778 0.079 Uiso 1 1 calc R . . H36B H -0.3091 -0.1484 0.1685 0.079 Uiso 1 1 calc R . . C37 C -0.1453(10) -0.1106(9) 0.0759(4) 0.045(3) Uani 1 1 d . . . C38 C -0.2826(14) -0.2754(11) 0.1094(5) 0.071(4) Uani 1 1 d . . . H38A H -0.3562 -0.2984 0.1288 0.085 Uiso 1 1 calc R . . H38B H -0.2276 -0.3033 0.1229 0.085 Uiso 1 1 calc R . . C39 C -0.3182(12) -0.3168(11) 0.0589(4) 0.065(4) Uani 1 1 d . . . C40 C -0.2017(11) -0.2722(10) 0.0301(5) 0.060(4) Uani 1 1 d . . . H40A H -0.1454 -0.3014 0.0409 0.072 Uiso 1 1 calc R . . H40B H -0.2218 -0.2916 -0.0033 0.072 Uiso 1 1 calc R . . C41 C -0.1870(14) 0.0551(14) 0.1971(5) 0.079(5) Uani 1 1 d . . . H41A H -0.1244 0.0466 0.2161 0.119 Uiso 1 1 calc R . . H41B H -0.2646 0.0255 0.2133 0.119 Uiso 1 1 calc R . . H41C H -0.1642 0.1279 0.1922 0.119 Uiso 1 1 calc R . . C42 C -0.3007(13) 0.0139(13) 0.1193(6) 0.079(4) Uani 1 1 d . . . H42A H -0.3093 -0.0208 0.0888 0.118 Uiso 1 1 calc R . . H42B H -0.2781 0.0867 0.1146 0.118 Uiso 1 1 calc R . . H42C H -0.3777 -0.0158 0.1359 0.118 Uiso 1 1 calc R . . C43 C -0.4132(13) -0.2820(14) 0.0392(5) 0.090(6) Uani 1 1 d . . . H43A H -0.3805 -0.2074 0.0407 0.135 Uiso 1 1 calc R . . H43B H -0.4869 -0.3110 0.0578 0.135 Uiso 1 1 calc R . . H43C H -0.4325 -0.3055 0.0065 0.135 Uiso 1 1 calc R . . C44 C -0.3623(17) -0.4340(12) 0.0579(6) 0.096(6) Uani 1 1 d . . . H44A H -0.2982 -0.4517 0.0703 0.144 Uiso 1 1 calc R . . H44B H -0.3820 -0.4597 0.0255 0.144 Uiso 1 1 calc R . . H44C H -0.4347 -0.4650 0.0772 0.144 Uiso 1 1 calc R . . C45 C 0.4319(10) 0.4668(8) 0.6966(4) 0.038(2) Uani 1 1 d . . . C46 C 0.3276(10) 0.4488(8) 0.6681(4) 0.040(3) Uani 1 1 d . . . H46A H 0.2602 0.4542 0.6825 0.048 Uiso 1 1 calc R . . C47 C 0.3187(9) 0.4237(8) 0.6200(4) 0.034(2) Uani 1 1 d . A . C48 C 0.4168(11) 0.4167(8) 0.5973(4) 0.045(3) Uani 1 1 d . . . H48A H 0.4121 0.3999 0.5648 0.054 Uiso 1 1 calc R . . C49 C 0.5234(10) 0.4352(8) 0.6238(4) 0.041(3) Uani 1 1 d . . . C50 C 0.5293(10) 0.4600(8) 0.6715(4) 0.044(3) Uani 1 1 d . . . H50A H 0.6025 0.4731 0.6882 0.053 Uiso 1 1 calc R . . C51 C 0.2065(9) 0.4079(5) 0.5923(3) 0.046(3) Uani 1 1 d D . . C52 C 0.6259(10) 0.4290(9) 0.5984(4) 0.055(3) Uani 1 1 d D . . C53 C 0.5158(10) 0.6341(8) 0.7458(3) 0.039(3) Uani 1 1 d . . . C54 C 0.6434(10) 0.6875(9) 0.7450(4) 0.043(3) Uani 1 1 d . . . H54A H 0.6918 0.6508 0.7496 0.052 Uiso 1 1 calc R . . C55 C 0.6987(10) 0.7891(9) 0.7377(4) 0.041(3) Uani 1 1 d . A . C56 C 0.6345(11) 0.8479(9) 0.7305(4) 0.045(3) Uani 1 1 d . . . H56A H 0.6751 0.9195 0.7265 0.054 Uiso 1 1 calc R . . C57 C 0.5054(11) 0.7970(9) 0.7293(4) 0.042(3) Uani 1 1 d . A . C58 C 0.4507(9) 0.6964(8) 0.7367(4) 0.038(3) Uani 1 1 d . . . H58A H 0.3646 0.6643 0.7361 0.045 Uiso 1 1 calc R . . C59 C 0.8396(12) 0.8418(7) 0.7381(3) 0.064(4) Uani 1 1 d D . . C60 C 0.4343(10) 0.8584(8) 0.7197(3) 0.061(4) Uani 1 1 d D . . C61 C 0.5306(10) 0.4665(8) 0.7838(4) 0.043(3) Uani 1 1 d . . . C62 C 0.5319(10) 0.3709(9) 0.7765(4) 0.046(3) Uani 1 1 d . . . H62A H 0.4843 0.3279 0.7517 0.055 Uiso 1 1 calc R . . C63 C 0.6020(11) 0.3367(11) 0.8051(5) 0.055(3) Uani 1 1 d . A . C64 C 0.6667(12) 0.3957(11) 0.8439(4) 0.059(3) Uani 1 1 d . . . H64A H 0.7124 0.3726 0.8639 0.071 Uiso 1 1 calc R . . C65 C 0.6619(12) 0.4910(10) 0.8522(5) 0.058(3) Uani 1 1 d . A . C66 C 0.5930(11) 0.5219(10) 0.8239(4) 0.051(3) Uani 1 1 d . . . H66A H 0.5870 0.5839 0.8316 0.061 Uiso 1 1 calc R . . C67 C 0.6052(9) 0.2353(11) 0.7938(4) 0.069(4) Uani 1 1 d D . . C68 C 0.7327(11) 0.5583(10) 0.8927(4) 0.081(5) Uani 1 1 d D . . C69 C 0.3154(10) 0.4683(9) 0.7764(4) 0.045(3) Uani 1 1 d . . . C70 C 0.2209(11) 0.3733(10) 0.7684(4) 0.049(3) Uani 1 1 d . . . H70A H 0.2331 0.3286 0.7465 0.058 Uiso 1 1 calc R . . C71 C 0.1075(11) 0.3386(10) 0.7907(4) 0.057(3) Uani 1 1 d . A . C72 C 0.0841(13) 0.4027(12) 0.8225(5) 0.068(4) Uani 1 1 d . . . H72A H 0.0068 0.3814 0.8365 0.082 Uiso 1 1 calc R . . C73 C 0.1761(14) 0.4983(12) 0.8335(5) 0.072(4) Uani 1 1 d . A . C74 C 0.2861(12) 0.5310(10) 0.8115(4) 0.050(3) Uani 1 1 d . . . H74A H 0.3463 0.5972 0.8192 0.061 Uiso 1 1 calc R . . C75 C 0.0114(11) 0.2342(12) 0.7790(4) 0.079(5) Uani 1 1 d D . . C76 C 0.1526(11) 0.5675(12) 0.8674(5) 0.088(5) Uani 1 1 d D . . F4 F 0.5972(8) 0.3378(7) 0.5762(3) 0.095(3) Uani 1 1 d D . . F5 F 0.6722(9) 0.4975(7) 0.5663(3) 0.113(4) Uani 1 1 d D . . F6 F 0.7182(7) 0.4369(7) 0.6273(3) 0.088(3) Uani 1 1 d D . . F1 F 0.197(6) 0.499(2) 0.5940(15) 0.077(5) Uani 0.206(4) 1 d PD A 1 F2 F 0.118(3) 0.3360(18) 0.6173(13) 0.054(3) Uani 0.206(4) 1 d PD A 1 F3 F 0.208(5) 0.376(2) 0.5472(6) 0.048(3) Uani 0.206(4) 1 d PD A 1 F7 F 0.889(7) 0.927(2) 0.7612(19) 0.104(5) Uani 0.206(4) 1 d PD A 1 F8 F 0.865(6) 0.864(5) 0.6946(8) 0.143(8) Uani 0.206(4) 1 d PD A 1 F9 F 0.900(5) 0.790(4) 0.750(2) 0.105(5) Uani 0.206(4) 1 d PD A 1 F10 F 0.446(5) 0.902(3) 0.7616(8) 0.152(8) Uani 0.206(4) 1 d PD A 1 F11 F 0.489(4) 0.928(3) 0.6879(14) 0.123(6) Uani 0.206(4) 1 d PD A 1 F12 F 0.3190(16) 0.806(4) 0.7086(17) 0.115(6) Uani 0.206(4) 1 d PD A 1 F13 F 0.788(5) 0.656(2) 0.879(3) 0.094(6) Uani 0.206(4) 1 d PD A 1 F14 F 0.818(5) 0.526(5) 0.904(2) 0.154(11) Uani 0.206(4) 1 d PD A 1 F15 F 0.665(4) 0.553(5) 0.9306(13) 0.087(5) Uani 0.206(4) 1 d PD A 1 F16 F 0.714(3) 0.245(4) 0.811(2) 0.134(9) Uani 0.206(4) 1 d PD A 1 F17 F 0.521(3) 0.151(2) 0.8135(18) 0.066(4) Uani 0.206(4) 1 d PD A 1 F18 F 0.605(6) 0.213(5) 0.7476(7) 0.099(6) Uani 0.206(4) 1 d PD A 1 F19 F 0.028(6) 0.193(5) 0.7383(9) 0.073(4) Uani 0.206(4) 1 d PD A 1 F20 F 0.016(5) 0.178(5) 0.8161(15) 0.105(6) Uani 0.206(4) 1 d PD A 1 F21 F -0.094(4) 0.245(7) 0.7780(17) 0.115(7) Uani 0.206(4) 1 d PD A 1 F22 F 0.044(4) 0.533(7) 0.887(3) 0.157(12) Uani 0.206(4) 1 d PD A 1 F23 F 0.236(5) 0.596(7) 0.901(2) 0.146(10) Uani 0.206(4) 1 d PD A 1 F24 F 0.167(8) 0.650(5) 0.843(3) 0.179(13) Uani 0.206(4) 1 d PD A 1 F1A F 0.2140(16) 0.4941(9) 0.5712(5) 0.077(5) Uani 0.617(10) 1 d PD A 2 F2A F 0.1040(9) 0.3765(9) 0.6185(4) 0.054(3) Uani 0.617(10) 1 d PD A 2 F3A F 0.1814(13) 0.3360(7) 0.5576(3) 0.048(3) Uani 0.617(10) 1 d PD A 2 F7A F 0.8818(16) 0.9405(8) 0.7385(5) 0.104(5) Uani 0.794(4) 1 d PD A 2 F8A F 0.8885(12) 0.8167(12) 0.7030(5) 0.143(8) Uani 0.794(4) 1 d PD A 2 F9A F 0.8842(11) 0.8191(10) 0.7756(4) 0.105(5) Uani 0.794(4) 1 d PD A 2 F10A F 0.4895(12) 0.9573(8) 0.7287(6) 0.152(8) Uani 0.794(4) 1 d PD A 2 F11A F 0.4002(14) 0.8513(13) 0.6749(4) 0.123(6) Uani 0.794(4) 1 d PD A 2 F12A F 0.3316(11) 0.8263(10) 0.7427(5) 0.115(6) Uani 0.794(4) 1 d PD A 2 F13A F 0.8316(13) 0.6391(12) 0.8780(7) 0.094(6) Uani 0.617(10) 1 d PD A 2 F14A F 0.776(2) 0.5156(16) 0.9255(6) 0.154(11) Uani 0.617(10) 1 d PD A 2 F15A F 0.6701(15) 0.6013(14) 0.9169(5) 0.087(5) Uani 0.617(10) 1 d PD A 2 F16A F 0.6539(19) 0.1956(13) 0.8261(6) 0.134(9) Uani 0.617(10) 1 d PD A 2 F17A F 0.4946(10) 0.1593(9) 0.7835(6) 0.066(4) Uani 0.617(10) 1 d PD A 2 F18A F 0.6693(15) 0.2402(15) 0.7544(5) 0.099(6) Uani 0.617(10) 1 d PD A 2 F19A F 0.0485(17) 0.1744(13) 0.7523(4) 0.073(4) Uani 0.617(10) 1 d PD A 2 F20A F -0.0343(14) 0.1783(14) 0.8175(5) 0.105(6) Uani 0.617(10) 1 d PD A 2 F21A F -0.0869(14) 0.2319(19) 0.7555(6) 0.115(7) Uani 0.617(10) 1 d PD A 2 F22A F 0.092(3) 0.524(2) 0.9055(6) 0.157(12) Uani 0.617(10) 1 d PD A 2 F23A F 0.2510(18) 0.6453(17) 0.8847(9) 0.146(10) Uani 0.617(10) 1 d PD A 2 F24A F 0.088(3) 0.613(3) 0.8488(9) 0.179(13) Uani 0.617(10) 1 d PD A 2 F1B F 0.115(4) 0.423(3) 0.6134(19) 0.077(5) Uani 0.177(9) 1 d PD A 3 F2B F 0.154(4) 0.3124(16) 0.5728(14) 0.054(3) Uani 0.177(9) 1 d PD A 3 F3B F 0.239(4) 0.472(2) 0.5552(9) 0.048(3) Uani 0.177(9) 1 d PD A 3 F13B F 0.722(5) 0.645(3) 0.904(2) 0.094(6) Uani 0.177(9) 1 d PD A 3 F14B F 0.851(2) 0.582(5) 0.8858(18) 0.154(11) Uani 0.177(9) 1 d PD A 3 F15B F 0.698(5) 0.497(4) 0.9302(13) 0.087(5) Uani 0.177(9) 1 d PD A 3 F16B F 0.718(2) 0.245(4) 0.784(2) 0.134(9) Uani 0.177(9) 1 d PD A 3 F17B F 0.574(5) 0.188(3) 0.8355(10) 0.066(4) Uani 0.177(9) 1 d PD A 3 F18B F 0.529(4) 0.173(4) 0.7609(16) 0.099(6) Uani 0.177(9) 1 d PD A 3 F19B F -0.040(4) 0.252(4) 0.7399(11) 0.073(4) Uani 0.177(9) 1 d PD A 3 F20B F 0.046(7) 0.159(4) 0.767(2) 0.105(6) Uani 0.177(9) 1 d PD A 3 F21B F -0.080(4) 0.192(5) 0.8094(18) 0.115(7) Uani 0.177(9) 1 d PD A 3 F22B F 0.0336(18) 0.541(6) 0.864(3) 0.157(12) Uani 0.177(9) 1 d PD A 3 F23B F 0.176(8) 0.541(5) 0.9097(11) 0.146(10) Uani 0.177(9) 1 d PD A 3 F24B F 0.208(6) 0.6685(16) 0.865(4) 0.179(13) Uani 0.177(9) 1 d PD A 3 Cl2S Cl 0.0900(8) 0.5576(11) 0.7141(3) 0.176(5) Uani 0.839(9) 1 d PD B 1 Cl1S Cl -0.1392(9) 0.5420(12) 0.7427(5) 0.234(6) Uani 0.839(9) 1 d PD B 1 C1S C -0.0630(17) 0.474(2) 0.7182(11) 0.31(4) Uani 0.839(9) 1 d PD B 1 H1SA H -0.0971 0.4469 0.6867 0.375 Uiso 0.839(9) 1 calc PR B 1 H1SB H -0.0720 0.4159 0.7383 0.375 Uiso 0.839(9) 1 calc PR B 1 Cl2A Cl 0.095(4) 0.637(6) 0.7406(16) 0.176(5) Uani 0.161(9) 1 d PD B 2 Cl1A Cl -0.038(5) 0.570(6) 0.738(3) 0.234(6) Uani 0.161(9) 1 d PD B 2 C1SA C 0.026(9) 0.591(11) 0.794(2) 0.31(4) Uani 0.161(9) 1 d PD B 2 H1SC H 0.0101 0.6377 0.8158 0.375 Uiso 0.161(9) 1 calc PR B 2 H1SD H 0.0405 0.5349 0.8090 0.375 Uiso 0.161(9) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.039(7) 0.036(7) 0.042(7) 0.002(5) -0.008(6) 0.014(6) Mo1 0.0245(5) 0.0226(5) 0.0403(5) -0.0020(4) -0.0043(4) 0.0114(4) Mo2 0.0338(6) 0.0407(6) 0.0305(5) -0.0023(4) -0.0053(4) 0.0066(4) N1 0.030(5) 0.031(5) 0.048(5) -0.003(4) 0.000(4) 0.013(4) N2 0.028(5) 0.037(5) 0.057(6) -0.008(4) 0.001(4) 0.015(4) N3 0.030(5) 0.030(5) 0.089(7) -0.011(5) 0.008(5) 0.008(4) N4 0.041(5) 0.019(4) 0.053(5) 0.001(4) -0.012(4) 0.017(4) N5 0.033(5) 0.017(4) 0.059(5) -0.003(4) -0.018(4) 0.018(4) N6 0.045(6) 0.030(5) 0.060(6) 0.003(4) -0.013(5) 0.018(4) N7 0.053(6) 0.041(6) 0.038(5) -0.004(4) -0.014(4) 0.020(5) N8 0.036(5) 0.061(7) 0.027(4) -0.006(4) -0.008(4) 0.017(5) N9 0.047(6) 0.069(7) 0.053(6) -0.013(5) -0.016(5) 0.028(6) N10 0.032(5) 0.069(7) 0.028(5) -0.010(4) -0.003(4) 0.019(5) N11 0.034(5) 0.057(6) 0.040(5) -0.001(5) -0.004(4) 0.005(5) N12 0.053(6) 0.077(8) 0.039(6) 0.003(5) -0.002(5) 0.015(6) C1 0.032(6) 0.034(6) 0.060(7) -0.013(5) -0.006(5) 0.006(5) C2 0.047(7) 0.028(6) 0.053(7) -0.012(5) -0.001(6) 0.003(5) C3 0.031(7) 0.054(9) 0.113(12) -0.015(8) 0.018(7) 0.002(6) C4 0.024(6) 0.039(7) 0.054(7) -0.002(5) 0.001(5) 0.016(5) C5 0.034(7) 0.065(9) 0.122(12) -0.030(9) 0.004(7) 0.026(7) C6 0.076(9) 0.040(7) 0.071(9) -0.008(6) 0.022(7) 0.027(7) C7 0.039(7) 0.044(7) 0.076(8) -0.016(6) 0.003(6) 0.019(6) C8 0.050(8) 0.051(8) 0.089(10) -0.005(7) 0.023(7) -0.002(7) C9 0.064(9) 0.070(10) 0.073(9) 0.010(8) -0.001(7) 0.012(8) C10 0.078(11) 0.057(9) 0.124(13) -0.026(9) 0.022(10) 0.036(8) C11 0.089(12) 0.065(10) 0.078(10) -0.003(8) -0.002(9) 0.014(9) C12 0.046(7) 0.048(7) 0.048(6) -0.011(5) -0.020(5) 0.024(6) C13 0.036(6) 0.052(7) 0.047(6) 0.001(5) -0.014(5) 0.017(6) C14 0.056(8) 0.047(7) 0.046(7) -0.006(5) -0.013(6) 0.019(6) C15 0.027(6) 0.052(7) 0.047(6) 0.008(5) -0.001(5) 0.025(5) C16 0.052(7) 0.037(7) 0.060(7) 0.014(6) -0.006(6) 0.017(6) C17 0.033(6) 0.028(6) 0.074(8) 0.007(5) -0.010(5) 0.016(5) C18 0.048(7) 0.053(8) 0.066(8) 0.012(6) 0.003(6) 0.031(6) C19 0.029(7) 0.095(11) 0.075(9) 0.017(8) -0.005(6) 0.023(7) C20 0.071(9) 0.048(8) 0.070(9) -0.009(7) -0.024(7) 0.017(7) C21 0.098(12) 0.039(8) 0.101(11) 0.013(7) -0.008(9) 0.035(8) C22 0.056(8) 0.064(9) 0.073(9) 0.001(7) 0.002(7) 0.038(7) C23 0.059(8) 0.065(9) 0.049(7) -0.007(6) -0.014(6) 0.024(7) C24 0.070(9) 0.065(9) 0.054(7) -0.004(6) -0.019(7) 0.039(8) C25 0.047(8) 0.080(10) 0.074(9) -0.009(8) -0.008(7) 0.026(8) C26 0.036(6) 0.061(8) 0.036(6) -0.001(5) -0.004(5) 0.023(6) C27 0.039(7) 0.085(10) 0.073(9) -0.022(8) -0.021(6) 0.026(7) C28 0.037(7) 0.059(8) 0.054(7) -0.006(6) -0.021(5) 0.018(6) C29 0.048(7) 0.050(7) 0.046(7) -0.008(6) -0.018(6) 0.015(6) C30 0.090(12) 0.079(12) 0.113(13) -0.012(10) -0.026(10) 0.049(10) C31 0.061(9) 0.081(11) 0.079(10) 0.005(8) -0.018(8) 0.026(8) C32 0.045(8) 0.075(10) 0.074(9) -0.026(7) -0.033(7) 0.021(7) C33 0.122(14) 0.099(13) 0.039(7) 0.012(8) -0.005(8) 0.049(11) C34 0.039(7) 0.071(9) 0.047(7) -0.013(6) -0.002(5) 0.017(6) C35 0.049(8) 0.081(10) 0.038(6) 0.002(6) 0.006(5) 0.017(7) C36 0.054(8) 0.099(12) 0.044(7) 0.016(7) 0.006(6) 0.030(8) C37 0.031(6) 0.050(7) 0.041(6) 0.013(5) -0.011(5) 0.004(5) C38 0.063(9) 0.068(10) 0.062(8) 0.023(7) -0.007(7) 0.008(8) C39 0.051(8) 0.069(10) 0.048(7) 0.008(6) -0.003(6) -0.001(7) C40 0.040(7) 0.045(8) 0.066(8) 0.007(6) -0.010(6) -0.010(6) C41 0.068(10) 0.107(13) 0.057(8) -0.019(8) 0.005(7) 0.033(9) C42 0.049(9) 0.103(13) 0.093(11) 0.005(9) -0.002(8) 0.041(9) C43 0.048(9) 0.106(13) 0.071(10) -0.002(9) -0.016(7) -0.012(9) C44 0.093(13) 0.068(11) 0.085(11) 0.008(9) -0.003(9) -0.009(9) C45 0.038(6) 0.026(6) 0.048(6) 0.005(5) -0.005(5) 0.012(5) C46 0.036(6) 0.033(6) 0.057(7) 0.005(5) -0.007(5) 0.020(5) C47 0.036(6) 0.028(6) 0.040(6) -0.005(4) -0.012(5) 0.015(5) C48 0.053(7) 0.034(6) 0.046(6) -0.002(5) -0.008(6) 0.017(6) C49 0.044(7) 0.029(6) 0.046(6) -0.006(5) 0.001(5) 0.012(5) C50 0.029(6) 0.037(6) 0.061(7) 0.002(5) -0.004(5) 0.008(5) C51 0.037(7) 0.041(7) 0.059(7) -0.004(6) -0.010(6) 0.015(6) C52 0.046(7) 0.054(8) 0.056(7) 0.004(6) 0.004(6) 0.012(6) C53 0.037(6) 0.039(6) 0.034(6) -0.007(5) -0.011(5) 0.011(5) C54 0.040(7) 0.047(7) 0.044(6) -0.007(5) -0.011(5) 0.020(6) C55 0.031(6) 0.040(7) 0.044(6) -0.002(5) -0.001(5) 0.007(5) C56 0.049(7) 0.030(6) 0.048(7) -0.002(5) -0.002(5) 0.011(6) C57 0.047(7) 0.043(7) 0.042(6) 0.013(5) 0.003(5) 0.025(6) C58 0.027(6) 0.045(7) 0.040(6) 0.001(5) -0.012(4) 0.013(5) C59 0.049(8) 0.047(9) 0.075(9) -0.006(7) -0.013(7) -0.001(7) C60 0.067(9) 0.066(10) 0.066(9) 0.016(7) 0.003(7) 0.044(8) C61 0.042(7) 0.032(6) 0.048(7) -0.001(5) 0.002(5) 0.007(5) C62 0.039(7) 0.053(8) 0.048(7) 0.005(6) -0.003(5) 0.022(6) C63 0.045(7) 0.065(9) 0.063(8) 0.011(7) 0.006(6) 0.030(7) C64 0.060(8) 0.071(10) 0.049(7) 0.015(7) -0.003(6) 0.031(7) C65 0.054(8) 0.053(8) 0.059(8) 0.009(6) -0.008(6) 0.015(7) C66 0.046(7) 0.058(8) 0.048(7) 0.009(6) -0.004(6) 0.021(6) C67 0.065(10) 0.083(11) 0.079(10) 0.017(8) -0.003(8) 0.051(9) C68 0.068(11) 0.121(15) 0.067(10) -0.016(10) -0.034(8) 0.053(11) C69 0.043(7) 0.047(7) 0.045(6) 0.000(5) -0.010(5) 0.020(6) C70 0.052(8) 0.051(8) 0.042(6) -0.001(5) -0.003(6) 0.022(6) C71 0.044(7) 0.060(8) 0.055(7) 0.008(6) -0.001(6) 0.011(6) C72 0.052(8) 0.084(11) 0.063(8) 0.004(8) 0.017(7) 0.022(8) C73 0.074(10) 0.075(10) 0.047(7) -0.002(7) 0.018(7) 0.010(8) C74 0.061(8) 0.048(7) 0.040(6) -0.010(5) 0.000(6) 0.021(6) C75 0.046(9) 0.078(11) 0.091(11) 0.007(9) 0.013(8) 0.005(8) C76 0.086(12) 0.100(14) 0.078(11) -0.022(10) 0.009(10) 0.039(11) F4 0.079(6) 0.102(7) 0.114(7) -0.043(6) 0.000(5) 0.048(6) F5 0.108(8) 0.119(9) 0.139(9) 0.056(7) 0.070(7) 0.072(7) F6 0.055(5) 0.135(8) 0.088(6) -0.031(5) -0.018(4) 0.055(5) F1 0.071(10) 0.063(7) 0.110(15) 0.004(9) -0.021(11) 0.043(6) F2 0.030(5) 0.054(9) 0.075(6) -0.022(8) -0.009(5) 0.016(6) F3 0.048(10) 0.042(8) 0.044(6) -0.006(5) -0.012(5) 0.010(8) F7 0.048(6) 0.067(7) 0.165(16) 0.007(8) 0.003(11) -0.006(5) F8 0.040(8) 0.189(19) 0.173(13) -0.089(12) 0.026(7) 0.021(8) F9 0.044(6) 0.109(11) 0.140(13) 0.023(10) -0.025(9) 0.009(6) F10 0.134(12) 0.041(7) 0.30(2) -0.023(10) -0.092(14) 0.058(8) F11 0.139(13) 0.184(17) 0.094(9) 0.000(9) -0.037(9) 0.115(13) F12 0.105(9) 0.111(10) 0.172(15) 0.052(11) 0.059(10) 0.087(9) F13 0.066(11) 0.081(9) 0.111(10) -0.019(9) -0.031(10) 0.009(8) F14 0.27(3) 0.100(12) 0.101(17) -0.029(12) -0.142(17) 0.089(17) F15 0.091(10) 0.074(13) 0.070(10) -0.012(8) -0.014(8) 0.008(10) F16 0.22(2) 0.083(15) 0.147(17) -0.025(11) -0.102(17) 0.118(16) F17 0.073(9) 0.042(6) 0.089(11) 0.003(7) -0.005(7) 0.030(6) F18 0.113(17) 0.097(14) 0.110(10) 0.007(9) 0.040(11) 0.066(15) F19 0.074(10) 0.047(9) 0.083(10) 0.004(8) -0.018(10) 0.011(7) F20 0.060(15) 0.090(9) 0.111(10) 0.025(8) 0.029(11) -0.024(12) F21 0.032(6) 0.130(15) 0.18(2) -0.062(16) -0.040(11) 0.030(8) F22 0.144(18) 0.138(14) 0.105(16) -0.057(16) 0.088(15) -0.024(16) F23 0.119(14) 0.076(16) 0.18(2) -0.067(13) 0.087(12) -0.024(11) F24 0.23(3) 0.27(3) 0.15(2) -0.064(19) -0.02(2) 0.22(3) F1A 0.071(10) 0.063(7) 0.110(15) 0.004(9) -0.021(11) 0.043(6) F2A 0.030(5) 0.054(9) 0.075(6) -0.022(8) -0.009(5) 0.016(6) F3A 0.048(10) 0.042(8) 0.044(6) -0.006(5) -0.012(5) 0.010(8) F7A 0.048(6) 0.067(7) 0.165(16) 0.007(8) 0.003(11) -0.006(5) F8A 0.040(8) 0.189(19) 0.173(13) -0.089(12) 0.026(7) 0.021(8) F9A 0.044(6) 0.109(11) 0.140(13) 0.023(10) -0.025(9) 0.009(6) F10A 0.134(12) 0.041(7) 0.30(2) -0.023(10) -0.092(14) 0.058(8) F11A 0.139(13) 0.184(17) 0.094(9) 0.000(9) -0.037(9) 0.115(13) F12A 0.105(9) 0.111(10) 0.172(15) 0.052(11) 0.059(10) 0.087(9) F13A 0.066(11) 0.081(9) 0.111(10) -0.019(9) -0.031(10) 0.009(8) F14A 0.27(3) 0.100(12) 0.101(17) -0.029(12) -0.142(17) 0.089(17) F15A 0.091(10) 0.074(13) 0.070(10) -0.012(8) -0.014(8) 0.008(10) F16A 0.22(2) 0.083(15) 0.147(17) -0.025(11) -0.102(17) 0.118(16) F17A 0.073(9) 0.042(6) 0.089(11) 0.003(7) -0.005(7) 0.030(6) F18A 0.113(17) 0.097(14) 0.110(10) 0.007(9) 0.040(11) 0.066(15) F19A 0.074(10) 0.047(9) 0.083(10) 0.004(8) -0.018(10) 0.011(7) F20A 0.060(15) 0.090(9) 0.111(10) 0.025(8) 0.029(11) -0.024(12) F21A 0.032(6) 0.130(15) 0.18(2) -0.062(16) -0.040(11) 0.030(8) F22A 0.144(18) 0.138(14) 0.105(16) -0.057(16) 0.088(15) -0.024(16) F23A 0.119(14) 0.076(16) 0.18(2) -0.067(13) 0.087(12) -0.024(11) F24A 0.23(3) 0.27(3) 0.15(2) -0.064(19) -0.02(2) 0.22(3) F1B 0.071(10) 0.063(7) 0.110(15) 0.004(9) -0.021(11) 0.043(6) F2B 0.030(5) 0.054(9) 0.075(6) -0.022(8) -0.009(5) 0.016(6) F3B 0.048(10) 0.042(8) 0.044(6) -0.006(5) -0.012(5) 0.010(8) F13B 0.066(11) 0.081(9) 0.111(10) -0.019(9) -0.031(10) 0.009(8) F14B 0.27(3) 0.100(12) 0.101(17) -0.029(12) -0.142(17) 0.089(17) F15B 0.091(10) 0.074(13) 0.070(10) -0.012(8) -0.014(8) 0.008(10) F16B 0.22(2) 0.083(15) 0.147(17) -0.025(11) -0.102(17) 0.118(16) F17B 0.073(9) 0.042(6) 0.089(11) 0.003(7) -0.005(7) 0.030(6) F18B 0.113(17) 0.097(14) 0.110(10) 0.007(9) 0.040(11) 0.066(15) F19B 0.074(10) 0.047(9) 0.083(10) 0.004(8) -0.018(10) 0.011(7) F20B 0.060(15) 0.090(9) 0.111(10) 0.025(8) 0.029(11) -0.024(12) F21B 0.032(6) 0.130(15) 0.18(2) -0.062(16) -0.040(11) 0.030(8) F22B 0.144(18) 0.138(14) 0.105(16) -0.057(16) 0.088(15) -0.024(16) F23B 0.119(14) 0.076(16) 0.18(2) -0.067(13) 0.087(12) -0.024(11) F24B 0.23(3) 0.27(3) 0.15(2) -0.064(19) -0.02(2) 0.22(3) Cl2S 0.115(5) 0.354(16) 0.112(6) 0.064(8) 0.028(5) 0.147(8) Cl1S 0.089(6) 0.310(16) 0.308(14) -0.023(12) 0.033(7) 0.091(8) C1S 0.48(9) 0.07(2) 0.28(5) 0.03(3) -0.28(6) 0.02(3) Cl2A 0.115(5) 0.354(16) 0.112(6) 0.064(8) 0.028(5) 0.147(8) Cl1A 0.089(6) 0.310(16) 0.308(14) -0.023(12) 0.033(7) 0.091(8) C1SA 0.48(9) 0.07(2) 0.28(5) 0.03(3) -0.28(6) 0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 C69 1.587(17) . ? B1 C45 1.634(16) . ? B1 C53 1.652(17) . ? B1 C61 1.658(17) . ? Mo1 Mo1 2.0966(18) 2_556 ? Mo1 N5 2.112(8) 2_556 ? Mo1 N4 2.114(8) . ? Mo1 N2 2.124(8) 2_556 ? Mo1 N1 2.129(8) . ? Mo2 N8 2.102(9) 2 ? Mo2 N10 2.105(9) . ? Mo2 Mo2 2.106(2) 2 ? Mo2 N11 2.110(9) 2 ? Mo2 N7 2.134(9) . ? N1 C4 1.363(13) . ? N1 C1 1.472(13) . ? N2 C4 1.275(13) . ? N2 C7 1.508(14) . ? N2 Mo1 2.124(8) 2_556 ? N3 C4 1.368(13) . ? N3 C5 1.463(15) . ? N3 C3 1.477(15) . ? N4 C15 1.328(13) . ? N4 C12 1.488(13) . ? N5 C15 1.341(14) . ? N5 C18 1.462(14) . ? N5 Mo1 2.112(8) 2_556 ? N6 C15 1.384(13) . ? N6 C16 1.450(14) . ? N6 C14 1.453(14) . ? N7 C26 1.352(14) . ? N7 C23 1.446(15) . ? N8 C26 1.375(15) . ? N8 C29 1.421(14) . ? N8 Mo2 2.102(9) 2 ? N9 C26 1.350(14) . ? N9 C27 1.458(16) . ? N9 C25 1.475(17) . ? N10 C37 1.383(15) . ? N10 C34 1.455(14) . ? N11 C37 1.331(15) . ? N11 C40 1.512(15) . ? N11 Mo2 2.110(9) 2 ? N12 C37 1.345(15) . ? N12 C36 1.450(17) . ? N12 C38 1.473(18) . ? C1 C2 1.504(16) . ? C2 C3 1.509(18) . ? C2 C9 1.516(18) . ? C2 C8 1.534(16) . ? C5 C6 1.517(19) . ? C6 C7 1.473(17) . ? C6 C10 1.503(17) . ? C6 C11 1.55(2) . ? C12 C13 1.526(15) . ? C13 C14 1.492(17) . ? C13 C19 1.519(17) . ? C13 C20 1.552(17) . ? C16 C17 1.497(17) . ? C17 C22 1.508(17) . ? C17 C18 1.550(15) . ? C17 C21 1.550(16) . ? C23 C24 1.480(17) . ? C24 C31 1.53(2) . ? C24 C30 1.532(19) . ? C24 C25 1.541(19) . ? C27 C28 1.497(18) . ? C28 C29 1.496(16) . ? C28 C32 1.534(16) . ? C28 C33 1.565(19) . ? C34 C35 1.532(17) . ? C35 C36 1.52(2) . ? C35 C41 1.525(18) . ? C35 C42 1.556(19) . ? C38 C39 1.523(18) . ? C39 C40 1.520(18) . ? C39 C43 1.53(2) . ? C39 C44 1.53(2) . ? C45 C50 1.410(15) . ? C45 C46 1.412(15) . ? C46 C47 1.392(15) . ? C47 C48 1.385(16) . ? C47 C51 1.485(15) . ? C48 C49 1.404(16) . ? C49 C50 1.379(15) . ? C49 C52 1.464(17) . ? C51 F1B 1.342(10) . ? C51 F1A 1.343(9) . ? C51 F2 1.344(10) . ? C51 F3A 1.346(8) . ? C51 F3 1.347(10) . ? C51 F1 1.347(10) . ? C51 F2B 1.347(10) . ? C51 F3B 1.348(10) . ? C51 F2A 1.351(8) . ? C52 F5 1.291(14) . ? C52 F6 1.337(11) . ? C52 F4 1.344(11) . ? C53 C54 1.399(16) . ? C53 C58 1.434(15) . ? C54 C55 1.339(16) . ? C55 C56 1.372(16) . ? C55 C59 1.540(17) . ? C56 C57 1.412(16) . ? C57 C58 1.328(15) . ? C57 C60 1.484(16) . ? C59 F8A 1.278(9) . ? C59 F7 1.278(11) . ? C59 F9 1.279(11) . ? C59 F8 1.282(11) . ? C59 F7A 1.282(9) . ? C59 F9A 1.287(9) . ? C60 F12 1.303(11) . ? C60 F10A 1.305(9) . ? C60 F12A 1.306(9) . ? C60 F11 1.306(11) . ? C60 F10 1.309(11) . ? C60 F11A 1.314(9) . ? C61 C62 1.385(16) . ? C61 C66 1.391(16) . ? C62 C63 1.393(16) . ? C63 C64 1.387(18) . ? C63 C67 1.495(19) . ? C64 C65 1.402(19) . ? C65 C66 1.350(17) . ? C65 C68 1.49(2) . ? C67 F16A 1.333(10) . ? C67 F17 1.335(11) . ? C67 F16B 1.336(11) . ? C67 F18B 1.337(11) . ? C67 F18 1.337(11) . ? C67 F16 1.339(11) . ? C67 F17B 1.341(11) . ? C67 F18A 1.342(10) . ? C67 F17A 1.345(10) . ? C68 F14A 1.329(10) . ? C68 F13B 1.331(11) . ? C68 F15 1.333(11) . ? C68 F13 1.334(11) . ? C68 F14B 1.335(11) . ? C68 F14 1.336(11) . ? C68 F15B 1.336(11) . ? C68 F15A 1.337(10) . ? C68 F13A 1.339(10) . ? C69 C70 1.372(17) . ? C69 C74 1.467(16) . ? C70 C71 1.398(17) . ? C71 C72 1.386(19) . ? C71 C75 1.49(2) . ? C72 C73 1.38(2) . ? C73 C74 1.363(18) . ? C73 C76 1.48(2) . ? C75 F20B 1.338(11) . ? C75 F20A 1.338(10) . ? C75 F21A 1.338(10) . ? C75 F19 1.338(11) . ? C75 F21 1.339(11) . ? C75 F21B 1.340(11) . ? C75 F19B 1.340(11) . ? C75 F20 1.340(11) . ? C75 F19A 1.342(10) . ? C76 F22A 1.314(12) . ? C76 F24A 1.316(11) . ? C76 F24B 1.316(13) . ? C76 F22 1.317(13) . ? C76 F24 1.318(13) . ? C76 F23B 1.318(13) . ? C76 F23 1.319(13) . ? C76 F22B 1.319(13) . ? C76 F23A 1.324(12) . ? Cl2S C1S 1.73(2) . ? Cl1S C1S 1.73(2) . ? Cl2A Cl1A 1.48(8) . ? Cl2A C1SA 1.73(2) . ? Cl1A C1SA 1.73(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 C69 B1 C45 111.7(9) . . ? C69 B1 C53 115.2(10) . . ? C45 B1 C53 102.0(8) . . ? C69 B1 C61 106.6(9) . . ? C45 B1 C61 111.7(9) . . ? C53 B1 C61 109.6(9) . . ? Mo1 Mo1 N5 92.9(2) 2_556 2_556 ? Mo1 Mo1 N4 92.1(2) 2_556 . ? N5 Mo1 N4 175.0(3) 2_556 . ? Mo1 Mo1 N2 91.7(2) 2_556 2_556 ? N5 Mo1 N2 89.6(3) 2_556 2_556 ? N4 Mo1 N2 89.7(3) . 2_556 ? Mo1 Mo1 N1 92.7(2) 2_556 . ? N5 Mo1 N1 90.1(3) 2_556 . ? N4 Mo1 N1 90.3(3) . . ? N2 Mo1 N1 175.6(3) 2_556 . ? N8 Mo2 N10 91.6(3) 2 . ? N8 Mo2 Mo2 93.5(3) 2 2 ? N10 Mo2 Mo2 93.1(3) . 2 ? N8 Mo2 N11 88.2(4) 2 2 ? N10 Mo2 N11 174.8(4) . 2 ? Mo2 Mo2 N11 92.1(3) 2 2 ? N8 Mo2 N7 173.6(4) 2 . ? N10 Mo2 N7 89.2(4) . . ? Mo2 Mo2 N7 92.8(2) 2 . ? N11 Mo2 N7 90.5(4) 2 . ? C4 N1 C1 120.2(9) . . ? C4 N1 Mo1 117.1(7) . . ? C1 N1 Mo1 122.7(6) . . ? C4 N2 C7 120.6(9) . . ? C4 N2 Mo1 120.6(7) . 2_556 ? C7 N2 Mo1 118.3(7) . 2_556 ? C4 N3 C5 121.1(9) . . ? C4 N3 C3 121.3(10) . . ? C5 N3 C3 116.4(9) . . ? C15 N4 C12 120.4(9) . . ? C15 N4 Mo1 119.4(7) . . ? C12 N4 Mo1 120.1(6) . . ? C15 N5 C18 121.2(9) . . ? C15 N5 Mo1 118.4(6) . 2_556 ? C18 N5 Mo1 120.3(7) . 2_556 ? C15 N6 C16 119.5(9) . . ? C15 N6 C14 120.0(9) . . ? C16 N6 C14 119.3(9) . . ? C26 N7 C23 120.1(10) . . ? C26 N7 Mo2 117.5(7) . . ? C23 N7 Mo2 122.3(7) . . ? C26 N8 C29 120.2(9) . . ? C26 N8 Mo2 117.8(7) . 2 ? C29 N8 Mo2 121.9(8) . 2 ? C26 N9 C27 120.8(11) . . ? C26 N9 C25 121.3(10) . . ? C27 N9 C25 117.2(10) . . ? C37 N10 C34 117.8(10) . . ? C37 N10 Mo2 118.5(7) . . ? C34 N10 Mo2 123.5(8) . . ? C37 N11 C40 119.7(10) . . ? C37 N11 Mo2 120.4(8) . 2 ? C40 N11 Mo2 119.5(7) . 2 ? C37 N12 C36 122.3(12) . . ? C37 N12 C38 120.7(11) . . ? C36 N12 C38 115.7(11) . . ? N1 C1 C2 113.9(9) . . ? C1 C2 C3 105.3(10) . . ? C1 C2 C9 110.6(11) . . ? C3 C2 C9 111.4(11) . . ? C1 C2 C8 110.3(9) . . ? C3 C2 C8 109.0(11) . . ? C9 C2 C8 110.1(11) . . ? N3 C3 C2 112.0(10) . . ? N2 C4 N1 117.9(9) . . ? N2 C4 N3 122.3(10) . . ? N1 C4 N3 119.6(9) . . ? N3 C5 C6 111.4(9) . . ? C7 C6 C10 113.1(11) . . ? C7 C6 C5 109.5(11) . . ? C10 C6 C5 111.5(11) . . ? C7 C6 C11 106.8(11) . . ? C10 C6 C11 108.1(12) . . ? C5 C6 C11 107.5(12) . . ? C6 C7 N2 113.3(10) . . ? N4 C12 C13 112.6(9) . . ? C14 C13 C19 110.5(11) . . ? C14 C13 C12 106.7(10) . . ? C19 C13 C12 110.6(10) . . ? C14 C13 C20 110.6(10) . . ? C19 C13 C20 109.1(10) . . ? C12 C13 C20 109.4(10) . . ? N6 C14 C13 112.4(10) . . ? N4 C15 N5 117.2(9) . . ? N4 C15 N6 121.4(10) . . ? N5 C15 N6 121.2(10) . . ? N6 C16 C17 112.2(9) . . ? C16 C17 C22 111.9(10) . . ? C16 C17 C18 106.1(9) . . ? C22 C17 C18 110.5(10) . . ? C16 C17 C21 111.0(11) . . ? C22 C17 C21 110.2(11) . . ? C18 C17 C21 107.0(10) . . ? N5 C18 C17 112.0(10) . . ? N7 C23 C24 114.4(10) . . ? C23 C24 C31 109.9(12) . . ? C23 C24 C30 112.5(11) . . ? C31 C24 C30 109.9(13) . . ? C23 C24 C25 107.0(12) . . ? C31 C24 C25 108.0(11) . . ? C30 C24 C25 109.4(12) . . ? N9 C25 C24 111.1(11) . . ? N9 C26 N7 121.4(11) . . ? N9 C26 N8 120.3(10) . . ? N7 C26 N8 118.3(9) . . ? N9 C27 C28 111.6(10) . . ? C29 C28 C27 107.1(10) . . ? C29 C28 C32 112.2(11) . . ? C27 C28 C32 109.4(10) . . ? C29 C28 C33 110.2(11) . . ? C27 C28 C33 107.6(12) . . ? C32 C28 C33 110.3(11) . . ? N8 C29 C28 115.5(10) . . ? N10 C34 C35 113.4(10) . . ? C36 C35 C41 111.3(11) . . ? C36 C35 C34 106.2(11) . . ? C41 C35 C34 109.8(11) . . ? C36 C35 C42 111.4(12) . . ? C41 C35 C42 108.8(12) . . ? C34 C35 C42 109.3(11) . . ? N12 C36 C35 111.8(10) . . ? N11 C37 N12 122.2(11) . . ? N11 C37 N10 115.8(9) . . ? N12 C37 N10 121.6(11) . . ? N12 C38 C39 111.2(10) . . ? C40 C39 C38 106.6(11) . . ? C40 C39 C43 110.3(11) . . ? C38 C39 C43 109.7(13) . . ? C40 C39 C44 107.2(13) . . ? C38 C39 C44 109.8(12) . . ? C43 C39 C44 113.0(12) . . ? N11 C40 C39 111.5(11) . . ? C50 C45 C46 113.7(10) . . ? C50 C45 B1 123.2(10) . . ? C46 C45 B1 122.5(10) . . ? C47 C46 C45 124.0(10) . . ? C48 C47 C46 119.8(10) . . ? C48 C47 C51 119.6(9) . . ? C46 C47 C51 120.6(9) . . ? C47 C48 C49 118.6(10) . . ? C50 C49 C48 120.2(10) . . ? C50 C49 C52 122.8(10) . . ? C48 C49 C52 117.0(9) . . ? C49 C50 C45 123.7(10) . . ? F1B C51 F1A 78.7(17) . . ? F1B C51 F2 56(2) . . ? F1A C51 F2 132.5(19) . . ? F1B C51 F3A 120(3) . . ? F1A C51 F3A 106.3(8) . . ? F2 C51 F3A 87.2(15) . . ? F1B C51 F3 127(4) . . ? F1A C51 F3 82.7(16) . . ? F2 C51 F3 111.7(16) . . ? F1B C51 F1 56(2) . . ? F2 C51 F1 111.5(16) . . ? F3A C51 F1 132(2) . . ? F3 C51 F1 111.3(16) . . ? F1B C51 F2B 105.7(18) . . ? F1A C51 F2B 125(2) . . ? F2 C51 F2B 63(2) . . ? F3 C51 F2B 50(2) . . ? F1 C51 F2B 142(4) . . ? F1B C51 F3B 105.7(17) . . ? F2 C51 F3B 149(3) . . ? F3A C51 F3B 82.2(16) . . ? F3 C51 F3B 56.4(19) . . ? F1 C51 F3B 59(2) . . ? F2B C51 F3B 105.1(17) . . ? F1A C51 F2A 105.2(8) . . ? F3A C51 F2A 105.3(8) . . ? F3 C51 F2A 123(2) . . ? F1 C51 F2A 83(2) . . ? F2B C51 F2A 84.6(17) . . ? F3B C51 F2A 129(2) . . ? F1B C51 C47 120(3) . . ? F1A C51 C47 112.8(11) . . ? F2 C51 C47 102(2) . . ? F3A C51 C47 112.6(10) . . ? F3 C51 C47 114(2) . . ? F1 C51 C47 106(3) . . ? F2B C51 C47 111(2) . . ? F3B C51 C47 108(2) . . ? F2A C51 C47 113.9(9) . . ? F5 C52 F6 106.7(9) . . ? F5 C52 F4 105.5(8) . . ? F6 C52 F4 102.8(10) . . ? F5 C52 C49 114.6(11) . . ? F6 C52 C49 112.6(9) . . ? F4 C52 C49 113.6(9) . . ? C54 C53 C58 114.5(10) . . ? C54 C53 B1 123.3(10) . . ? C58 C53 B1 122.0(9) . . ? C55 C54 C53 122.1(11) . . ? C54 C55 C56 122.5(11) . . ? C54 C55 C59 118.5(10) . . ? C56 C55 C59 118.9(10) . . ? C55 C56 C57 117.7(10) . . ? C58 C57 C56 119.8(10) . . ? C58 C57 C60 121.7(10) . . ? C56 C57 C60 118.6(10) . . ? C57 C58 C53 123.4(10) . . ? F8A C59 F7 125(4) . . ? F8A C59 F9 67(2) . . ? F7 C59 F9 106(2) . . ? F7 C59 F8 106(2) . . ? F9 C59 F8 106(2) . . ? F8A C59 F7A 106.4(10) . . ? F9 C59 F7A 125(3) . . ? F8 C59 F7A 77(3) . . ? F8A C59 F9A 106.1(10) . . ? F7 C59 F9A 76(2) . . ? F8 C59 F9A 141(3) . . ? F7A C59 F9A 105.7(9) . . ? F8A C59 C55 114.2(11) . . ? F7 C59 C55 116(4) . . ? F9 C59 C55 119(3) . . ? F8 C59 C55 103(3) . . ? F7A C59 C55 112.8(13) . . ? F9A C59 C55 111.1(10) . . ? F12 C60 F10A 127(3) . . ? F10A C60 F12A 105.6(9) . . ? F12 C60 F11 111.0(15) . . ? F10A C60 F11 56(2) . . ? F12A C60 F11 137(3) . . ? F12 C60 F10 110.7(15) . . ? F10A C60 F10 54.7(18) . . ? F12A C60 F10 67(2) . . ? F11 C60 F10 110.4(15) . . ? F12 C60 F11A 61.3(18) . . ? F10A C60 F11A 104.7(8) . . ? F12A C60 F11A 104.0(9) . . ? F11 C60 F11A 55.3(18) . . ? F10 C60 F11A 150(2) . . ? F12 C60 C57 116(3) . . ? F10A C60 C57 116.6(10) . . ? F12A C60 C57 113.0(10) . . ? F11 C60 C57 110(3) . . ? F10 C60 C57 98(2) . . ? F11A C60 C57 111.8(10) . . ? C62 C61 C66 116.2(11) . . ? C62 C61 B1 122.9(10) . . ? C66 C61 B1 120.4(10) . . ? C61 C62 C63 121.7(12) . . ? C64 C63 C62 120.3(12) . . ? C64 C63 C67 120.6(11) . . ? C62 C63 C67 119.1(11) . . ? C63 C64 C65 118.0(12) . . ? C66 C65 C64 120.3(12) . . ? C66 C65 C68 119.9(12) . . ? C64 C65 C68 119.8(11) . . ? C65 C66 C61 123.2(13) . . ? F16A C67 F17 67.9(19) . . ? F16A C67 F16B 65.6(19) . . ? F17 C67 F16B 123(3) . . ? F16A C67 F18B 119(3) . . ? F17 C67 F18B 69(2) . . ? F16B C67 F18B 107.9(17) . . ? F16A C67 F18 121(3) . . ? F17 C67 F18 106.5(19) . . ? F16B C67 F18 73(3) . . ? F17 C67 F16 106.2(18) . . ? F18B C67 F16 133(4) . . ? F18 C67 F16 106.0(18) . . ? F16B C67 F17B 107.5(17) . . ? F18B C67 F17B 107.4(17) . . ? F18 C67 F17B 140(3) . . ? F16 C67 F17B 78(2) . . ? F16A C67 F18A 104.4(10) . . ? F17 C67 F18A 128(2) . . ? F18B C67 F18A 72(2) . . ? F16 C67 F18A 77(3) . . ? F17B C67 F18A 143(2) . . ? F16A C67 F17A 104.7(10) . . ? F16B C67 F17A 131(3) . . ? F18 C67 F17A 74(2) . . ? F16 C67 F17A 138(2) . . ? F17B C67 F17A 78(2) . . ? F18A C67 F17A 103.4(10) . . ? F16A C67 C63 117.8(13) . . ? F17 C67 C63 118(2) . . ? F16B C67 C63 112(3) . . ? F18B C67 C63 120(3) . . ? F18 C67 C63 116(3) . . ? F16 C67 C63 104(3) . . ? F17B C67 C63 101(2) . . ? F18A C67 C63 111.3(13) . . ? F17A C67 C63 113.8(10) . . ? F14A C68 F13B 118(3) . . ? F14A C68 F15 76(2) . . ? F13B C68 F15 65(3) . . ? F14A C68 F13 125(3) . . ? F13B C68 F13 45(3) . . ? F15 C68 F13 109(2) . . ? F14A C68 F14B 69(2) . . ? F13B C68 F14B 108.0(18) . . ? F15 C68 F14B 135(3) . . ? F13 C68 F14B 71(2) . . ? F13B C68 F14 131(4) . . ? F15 C68 F14 109(2) . . ? F13 C68 F14 109(2) . . ? F13B C68 F15B 107.7(18) . . ? F15 C68 F15B 46(2) . . ? F13 C68 F15B 144(4) . . ? F14B C68 F15B 107.3(17) . . ? F14 C68 F15B 69(2) . . ? F14A C68 F15A 104.8(11) . . ? F13 C68 F15A 79(3) . . ? F14B C68 F15A 135(3) . . ? F14 C68 F15A 134(3) . . ? F15B C68 F15A 79(3) . . ? F14A C68 F13A 104.5(11) . . ? F13B C68 F13A 71(3) . . ? F15 C68 F13A 128(3) . . ? F14 C68 F13A 81(3) . . ? F15B C68 F13A 139(3) . . ? F15A C68 F13A 103.8(11) . . ? F14A C68 C65 117.3(15) . . ? F13B C68 C65 121(3) . . ? F15 C68 C65 114(3) . . ? F13 C68 C65 110(3) . . ? F14B C68 C65 108(3) . . ? F14 C68 C65 106(3) . . ? F15B C68 C65 104(3) . . ? F15A C68 C65 113.5(12) . . ? F13A C68 C65 111.7(13) . . ? C70 C69 C74 112.9(11) . . ? C70 C69 B1 124.8(11) . . ? C74 C69 B1 122.4(11) . . ? C69 C70 C71 124.5(12) . . ? C72 C71 C70 119.9(12) . . ? C72 C71 C75 120.3(11) . . ? C70 C71 C75 119.8(11) . . ? C73 C72 C71 119.0(13) . . ? C74 C73 C72 120.3(13) . . ? C74 C73 C76 120.0(13) . . ? C72 C73 C76 119.6(13) . . ? C73 C74 C69 123.3(12) . . ? F20B C75 F20A 85(2) . . ? F20B C75 F21A 115(4) . . ? F20A C75 F21A 104.4(12) . . ? F20A C75 F19 122(3) . . ? F21A C75 F19 82(2) . . ? F20B C75 F21 135(5) . . ? F20A C75 F21 85(3) . . ? F19 C75 F21 111(2) . . ? F20B C75 F21B 106(2) . . ? F21A C75 F21B 76(2) . . ? F19 C75 F21B 127(5) . . ? F21 C75 F21B 55(3) . . ? F20B C75 F19B 106(2) . . ? F20A C75 F19B 133(2) . . ? F19 C75 F19B 63(3) . . ? F21 C75 F19B 55(3) . . ? F21B C75 F19B 105(2) . . ? F20B C75 F20 68(4) . . ? F21A C75 F20 129(3) . . ? F19 C75 F20 111(2) . . ? F21 C75 F20 111(2) . . ? F21B C75 F20 56(3) . . ? F19B C75 F20 154(4) . . ? F20A C75 F19A 103.8(12) . . ? F21A C75 F19A 103.8(11) . . ? F21 C75 F19A 130(3) . . ? F21B C75 F19A 120(3) . . ? F19B C75 F19A 88(2) . . ? F20 C75 F19A 87(3) . . ? F20B C75 C71 119(4) . . ? F20A C75 C71 112.6(13) . . ? F21A C75 C71 115.7(15) . . ? F19 C75 C71 115(3) . . ? F21 C75 C71 105(4) . . ? F21B C75 C71 118(3) . . ? F19B C75 C71 102(2) . . ? F20 C75 C71 103(3) . . ? F19A C75 C71 115.1(13) . . ? F22A C76 F24A 104.1(13) . . ? F22A C76 F24B 121(5) . . ? F24A C76 F24B 64(3) . . ? F24A C76 F22 71(3) . . ? F24B C76 F22 115(7) . . ? F22A C76 F24 134(4) . . ? F22 C76 F24 108(3) . . ? F24A C76 F23B 138(3) . . ? F24B C76 F23B 108(2) . . ? F22 C76 F23B 78(3) . . ? F24 C76 F23B 140(4) . . ? F22A C76 F23 76(3) . . ? F24A C76 F23 132(4) . . ? F24B C76 F23 75(3) . . ? F22 C76 F23 108(3) . . ? F24 C76 F23 108(3) . . ? F22A C76 F22B 66(3) . . ? F24A C76 F22B 48(3) . . ? F24B C76 F22B 108(2) . . ? F24 C76 F22B 87(4) . . ? F23B C76 F22B 107(2) . . ? F23 C76 F22B 136(3) . . ? F22A C76 F23A 103.4(12) . . ? F24A C76 F23A 103.2(13) . . ? F22 C76 F23A 124(4) . . ? F24 C76 F23A 72(4) . . ? F23B C76 F23A 72(3) . . ? F22B C76 F23A 138(3) . . ? F22A C76 C73 115.8(17) . . ? F24A C76 C73 113.1(15) . . ? F24B C76 C73 122(5) . . ? F22 C76 C73 118(5) . . ? F24 C76 C73 106(4) . . ? F23B C76 C73 106(3) . . ? F23 C76 C73 109(3) . . ? F22B C76 C73 105(3) . . ? F23A C76 C73 115.6(15) . . ? Cl1S C1S Cl2S 107.8(18) . . ? Cl1A Cl2A C1SA 64.8(14) . . ? Cl2A Cl1A C1SA 64.7(14) . . ? Cl2A C1SA Cl1A 51(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.964 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.138 #===END of CIF for Compound 2.CH2Cl2 ============== data_3 _database_code_depnum_ccdc_archive 'CCDC 645814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H80 Mo2 N12, 2(C32 H12B F24)' _chemical_formula_sum 'C108 H104 B2 F48 Mo2 N12' _chemical_formula_weight 2695.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' B B 0.0013 0.0007 '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 14.506(2) _cell_length_b 14.554(3) _cell_length_c 15.193(3) _cell_angle_alpha 86.936(3) _cell_angle_beta 87.882(3) _cell_angle_gamma 62.453(3) _cell_volume 2839.5(8) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 9716 _cell_measurement_theta_min 2.6855 _cell_measurement_theta_max 25.0665 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1362 _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8601 _exptl_absorpt_correction_T_max 0.9359 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16861 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.10 _reflns_number_total 9930 _reflns_number_gt 8509 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+6.4342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9930 _refine_ls_number_parameters 836 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.06572(2) 0.99842(3) 0.03165(2) 0.02710(12) Uani 1 1 d . . . B1 B 0.6729(3) 0.6622(3) 0.3468(3) 0.0279(9) Uani 1 1 d . . . N1 N -0.0043(3) 0.8398(3) 0.0177(2) 0.0314(7) Uani 1 1 d . . . N2 N 0.1373(3) 0.8421(3) -0.0536(2) 0.0331(7) Uani 1 1 d . . . N3 N 0.1282(3) 0.6852(3) -0.0363(3) 0.0430(9) Uani 1 1 d . . . N4 N 0.0003(3) 0.9724(3) 0.1559(2) 0.0314(7) Uani 1 1 d . . . N5 N 0.1448(2) 0.9692(3) 0.0855(2) 0.0302(7) Uani 1 1 d . . . N6 N 0.1433(3) 0.9480(3) 0.2405(2) 0.0376(8) Uani 1 1 d . . . C39 C 0.6215(3) 0.5827(3) 0.3472(2) 0.0300(8) Uani 1 1 d . . . C31 C 0.8002(3) 0.6023(3) 0.3553(2) 0.0280(8) Uani 1 1 d . . . C23 C 0.6137(3) 0.7355(3) 0.4308(2) 0.0278(8) Uani 1 1 d . . . C1 C 0.0878(3) 0.7875(3) -0.0252(3) 0.0331(9) Uani 1 1 d . . . C2 C -0.0610(4) 0.7833(3) 0.0498(3) 0.0441(11) Uani 1 1 d . . . H2A H -0.1073 0.7857 0.0033 0.053 Uiso 1 1 calc R . . H2B H -0.1046 0.8186 0.1004 0.053 Uiso 1 1 calc R . . C3 C 0.0081(4) 0.6719(4) 0.0768(3) 0.0450(11) Uani 1 1 d . . . C4 C 0.0771(5) 0.6241(4) -0.0022(4) 0.0564(13) Uani 1 1 d . . . H4A H 0.1301 0.5539 0.0144 0.068 Uiso 1 1 calc R . . H4B H 0.0351 0.6187 -0.0488 0.068 Uiso 1 1 calc R . . C5 C 0.2231(4) 0.6316(4) -0.0898(4) 0.0558(13) Uani 1 1 d . . . H5A H 0.2046 0.6378 -0.1520 0.067 Uiso 1 1 calc R . . H5B H 0.2576 0.5577 -0.0721 0.067 Uiso 1 1 calc R . . C6 C 0.2970(4) 0.6761(4) -0.0793(3) 0.0464(11) Uani 1 1 d . . . C7 C 0.2377(4) 0.7905(4) -0.1000(3) 0.0475(11) Uani 1 1 d . . . H7A H 0.2806 0.8231 -0.0847 0.057 Uiso 1 1 calc R . . H7B H 0.2257 0.8018 -0.1636 0.057 Uiso 1 1 calc R . . C8 C -0.0583(5) 0.6163(4) 0.0980(4) 0.0657(16) Uani 1 1 d . . . H8A H -0.0989 0.6217 0.0468 0.099 Uiso 1 1 calc R . . H8B H -0.1047 0.6484 0.1472 0.099 Uiso 1 1 calc R . . H8C H -0.0134 0.5438 0.1132 0.099 Uiso 1 1 calc R . . C9 C 0.0725(5) 0.6648(5) 0.1561(4) 0.0712(17) Uani 1 1 d . . . H9A H 0.1142 0.7000 0.1416 0.107 Uiso 1 1 calc R . . H9B H 0.1179 0.5925 0.1718 0.107 Uiso 1 1 calc R . . H9C H 0.0266 0.6974 0.2055 0.107 Uiso 1 1 calc R . . C10 C 0.3349(4) 0.6566(5) 0.0155(4) 0.0662(15) Uani 1 1 d . . . H10A H 0.2759 0.6889 0.0554 0.099 Uiso 1 1 calc R . . H10B H 0.3821 0.6860 0.0223 0.099 Uiso 1 1 calc R . . H10C H 0.3710 0.5825 0.0291 0.099 Uiso 1 1 calc R . . C11 C 0.3898(5) 0.6246(4) -0.1417(4) 0.0691(17) Uani 1 1 d . . . H11A H 0.3659 0.6367 -0.2020 0.104 Uiso 1 1 calc R . . H11B H 0.4254 0.5505 -0.1278 0.104 Uiso 1 1 calc R . . H11C H 0.4373 0.6536 -0.1349 0.104 Uiso 1 1 calc R . . C12 C 0.0971(3) 0.9617(3) 0.1624(3) 0.0311(8) Uani 1 1 d . . . C13 C -0.0567(4) 0.9682(4) 0.2368(3) 0.0399(10) Uani 1 1 d . . . H13A H -0.0459 0.8970 0.2478 0.048 Uiso 1 1 calc R . . H13B H -0.1312 1.0126 0.2276 0.048 Uiso 1 1 calc R . . C14 C -0.0245(3) 1.0024(4) 0.3174(3) 0.0423(10) Uani 1 1 d . . . C15 C 0.0921(4) 0.9370(5) 0.3228(3) 0.0529(13) Uani 1 1 d . . . H15A H 0.1182 0.9585 0.3721 0.063 Uiso 1 1 calc R . . H15B H 0.1087 0.8640 0.3337 0.063 Uiso 1 1 calc R . . C16 C 0.2450(3) 0.9437(4) 0.2489(3) 0.0466(11) Uani 1 1 d . . . H16A H 0.2976 0.8710 0.2564 0.056 Uiso 1 1 calc R . . H16B H 0.2449 0.9794 0.3018 0.056 Uiso 1 1 calc R . . C17 C 0.2744(3) 0.9926(3) 0.1700(3) 0.0332(9) Uani 1 1 d . . . C18 C 0.2531(3) 0.9493(4) 0.0897(3) 0.0403(10) Uani 1 1 d . . . H18A H 0.2701 0.9803 0.0367 0.048 Uiso 1 1 calc R . . H18B H 0.2986 0.8743 0.0901 0.048 Uiso 1 1 calc R . . C19 C -0.0785(4) 0.9829(6) 0.3991(3) 0.0646(16) Uani 1 1 d . . . H19A H -0.0598 0.9097 0.4052 0.097 Uiso 1 1 calc R . . H19B H -0.1532 1.0231 0.3930 0.097 Uiso 1 1 calc R . . H19C H -0.0567 1.0035 0.4509 0.097 Uiso 1 1 calc R . . C20 C -0.0532(5) 1.1179(5) 0.3073(4) 0.0629(15) Uani 1 1 d . . . H20A H -0.0185 1.1297 0.2554 0.094 Uiso 1 1 calc R . . H20B H -0.0313 1.1386 0.3590 0.094 Uiso 1 1 calc R . . H20C H -0.1279 1.1584 0.3010 0.094 Uiso 1 1 calc R . . C21 C 0.3887(3) 0.9652(4) 0.1736(3) 0.0497(12) Uani 1 1 d . . . H21A H 0.4304 0.8904 0.1741 0.075 Uiso 1 1 calc R . . H21B H 0.4014 0.9915 0.2267 0.075 Uiso 1 1 calc R . . H21C H 0.4073 0.9960 0.1223 0.075 Uiso 1 1 calc R . . C22 C 0.20968(17) 1.10921(18) 0.16930(16) 0.0539(13) Uani 1 1 d . . . H22A H 0.1366 1.1270 0.1672 0.081 Uiso 1 1 calc R . . H22B H 0.2282 1.1400 0.1180 0.081 Uiso 1 1 calc R . . H22C H 0.2227 1.1354 0.2223 0.081 Uiso 1 1 calc R . . C47 C 0.65573(17) 0.73175(18) 0.25241(16) 0.0284(8) Uani 1 1 d R . . C48 C 0.66042(17) 0.82494(18) 0.25365(16) 0.0309(8) Uani 1 1 d R . . H23A H 0.6668 0.8504 0.3075 0.037 Uiso 1 1 calc R . . C49 C 0.6555(3) 0.8811(3) 0.1742(3) 0.0346(9) Uani 1 1 d . B . C50 C 0.6457(3) 0.8450(3) 0.0940(3) 0.0393(10) Uani 1 1 d . . . H25A H 0.6418 0.8830 0.0411 0.047 Uiso 1 1 calc R . . C51 C 0.6418(3) 0.7520(4) 0.0941(3) 0.0378(10) Uani 1 1 d . A . C52 C 0.6468(3) 0.6961(3) 0.1726(3) 0.0317(8) Uani 1 1 d . . . H27A H 0.6441 0.6329 0.1711 0.038 Uiso 1 1 calc R . . C54 C 0.6304(4) 0.7120(4) 0.0089(3) 0.0557(13) Uani 1 1 d D . . C53 C 0.6564(3) 0.9820(4) 0.1733(3) 0.0484(12) Uani 1 1 d D . . C44 C 0.6662(3) 0.4856(3) 0.3908(3) 0.0330(9) Uani 1 1 d . . . H30A H 0.7327 0.4604 0.4149 0.040 Uiso 1 1 calc R . . C43 C 0.6149(3) 0.4248(3) 0.3998(3) 0.0382(10) Uani 1 1 d . . . C42 C 0.5171(4) 0.4596(4) 0.3669(3) 0.0447(11) Uani 1 1 d . . . H32A H 0.4823 0.4189 0.3737 0.054 Uiso 1 1 calc R . . C41 C 0.4707(3) 0.5556(4) 0.3237(3) 0.0421(10) Uani 1 1 d . C . C40 C 0.5225(3) 0.6152(3) 0.3137(3) 0.0352(9) Uani 1 1 d . . . H34A H 0.4897 0.6800 0.2832 0.042 Uiso 1 1 calc R . . C45 C 0.3653(4) 0.5923(4) 0.2874(3) 0.0612(15) Uani 1 1 d D . . C46 C 0.6671(4) 0.3177(4) 0.4431(3) 0.0519(12) Uani 1 1 d . . . C32 C 0.8604(3) 0.5104(3) 0.3126(3) 0.0314(8) Uani 1 1 d . . . H37A H 0.8268 0.4797 0.2828 0.038 Uiso 1 1 calc R . . C33 C 0.9679(3) 0.4629(3) 0.3124(3) 0.0366(9) Uani 1 1 d . D . C34 C 1.0206(3) 0.5068(4) 0.3538(3) 0.0400(10) Uani 1 1 d . . . H39A H 1.0937 0.4745 0.3539 0.048 Uiso 1 1 calc R . . C35 C 0.9635(3) 0.5984(3) 0.3948(3) 0.0361(9) Uani 1 1 d . . . C36 C 0.8548(3) 0.6455(3) 0.3962(3) 0.0320(8) Uani 1 1 d . . . H41A H 0.8176 0.7079 0.4253 0.038 Uiso 1 1 calc R . . C38 C 1.0194(4) 0.6494(4) 0.4359(3) 0.0462(11) Uani 1 1 d . . . C37 C 1.0303(4) 0.3620(4) 0.2681(4) 0.0511(12) Uani 1 1 d . . . C28 C 0.5208(3) 0.8264(3) 0.4211(3) 0.0291(8) Uani 1 1 d . . . H44A H 0.4954 0.8509 0.3641 0.035 Uiso 1 1 calc R . . C27 C 0.4638(3) 0.8825(3) 0.4931(3) 0.0296(8) Uani 1 1 d . . . C26 C 0.4993(3) 0.8494(3) 0.5773(3) 0.0335(9) Uani 1 1 d . . . H46A H 0.4617 0.8873 0.6259 0.040 Uiso 1 1 calc R . . C25 C 0.5918(3) 0.7588(3) 0.5891(3) 0.0319(8) Uani 1 1 d . . . C24 C 0.6475(3) 0.7031(3) 0.5173(3) 0.0304(8) Uani 1 1 d . . . H48A H 0.7097 0.6419 0.5271 0.036 Uiso 1 1 calc R . . C29 C 0.6291(4) 0.7241(4) 0.6812(3) 0.0410(10) Uani 1 1 d . . . C30 C 0.3621(3) 0.9760(3) 0.4784(3) 0.0372(9) Uani 1 1 d . . . F1 F 0.6012(9) 0.6355(7) 0.0186(6) 0.061(3) Uani 0.38 1 d PD A 1 F2 F 0.7222(7) 0.6658(11) -0.0362(7) 0.082(4) Uani 0.38 1 d PD A 1 F3 F 0.5637(9) 0.7810(6) -0.0465(7) 0.068(2) Uiso 0.38 1 d PD A 1 F1B F 0.6575(12) 0.6124(5) 0.0067(8) 0.061(3) Uani 0.33 1 d PD A 2 F2B F 0.6747(12) 0.7384(12) -0.0596(7) 0.082(4) Uani 0.33 1 d PD A 2 F3B F 0.5261(6) 0.7603(9) -0.0116(8) 0.068(2) Uiso 0.33 1 d PD A 2 F1C F 0.7186(13) 0.6228(10) -0.0088(10) 0.059(4) Uani 0.29 1 d P A 3 F2C F 0.6218(10) 0.7783(9) -0.0591(6) 0.041(3) Uani 0.29 1 d P A 3 F3C F 0.5538(12) 0.6932(15) 0.0101(9) 0.069(3) Uiso 0.29 1 d P A 3 F4 F 0.7357(6) 0.9843(7) 0.1227(6) 0.0345(15) Uiso 0.410(9) 1 d PD B 1 F5 F 0.6763(11) 1.0047(12) 0.2551(5) 0.049(2) Uiso 0.410(9) 1 d PD B 1 F6 F 0.5698(4) 1.0655(5) 0.1483(8) 0.0447(18) Uiso 0.410(9) 1 d PD B 1 F4B F 0.7498(5) 0.9736(8) 0.1470(6) 0.0345(15) Uiso 0.282(6) 1 d PD B 2 F5B F 0.6234(9) 1.0330(8) 0.2437(5) 0.049(2) Uiso 0.282(6) 1 d PD B 2 F6B F 0.5920(6) 1.0455(7) 0.1048(6) 0.0447(18) Uiso 0.282(6) 1 d PD B 2 F4C F 0.7044(13) 1.0071(12) 0.1165(9) 0.064(4) Uiso 0.308(12) 1 d P B 3 F5C F 0.7062(13) 0.9912(15) 0.2595(8) 0.058(5) Uani 0.308(12) 1 d P B 3 F6C F 0.5673(7) 1.0578(7) 0.1985(9) 0.051(3) Uiso 0.308(12) 1 d P B 3 F7 F 0.3335(8) 0.6807(7) 0.2324(8) 0.0530(17) Uiso 0.310(7) 1 d PD C 1 F8 F 0.3678(15) 0.5199(8) 0.2333(8) 0.054(2) Uani 0.310(7) 1 d PD C 1 F9 F 0.2868(7) 0.6119(11) 0.3440(6) 0.0593(18) Uiso 0.310(7) 1 d PD C 1 F7B F 0.3106(6) 0.6934(4) 0.2764(8) 0.0530(17) Uiso 0.473(9) 1 d PD C 2 F8B F 0.3613(9) 0.5477(6) 0.2134(4) 0.054(2) Uani 0.473(9) 1 d PD C 2 F9B F 0.3082(6) 0.5612(7) 0.3484(5) 0.0593(18) Uiso 0.473(9) 1 d PD C 2 F7C F 0.3609(18) 0.606(2) 0.2029(15) 0.098(8) Uiso 0.218(11) 1 d P C 3 F8C F 0.3098(16) 0.5514(17) 0.3025(18) 0.091(7) Uiso 0.218(11) 1 d P C 3 F9C F 0.2994(10) 0.6880(11) 0.3210(11) 0.055(5) Uani 0.218(11) 1 d P C 3 F10 F 0.6822(3) 0.2452(2) 0.3855(2) 0.0729(9) Uani 1 1 d . . . F11 F 0.7598(3) 0.2919(3) 0.4742(3) 0.0886(12) Uani 1 1 d . . . F12 F 0.6094(3) 0.3043(3) 0.5072(2) 0.0834(12) Uani 1 1 d . . . F13 F 1.1070(3) 0.5814(3) 0.4735(3) 0.0914(13) Uani 1 1 d . . . F14 F 1.0468(3) 0.7030(3) 0.3772(2) 0.0763(10) Uani 1 1 d . . . F15 F 0.9645(3) 0.7143(3) 0.4970(2) 0.0850(12) Uani 1 1 d . . . F16 F 0.9716(4) 0.3360(5) 0.2161(6) 0.061(2) Uiso 0.649(19) 1 d P D 1 F17 F 1.0831(10) 0.2830(5) 0.3204(5) 0.073(3) Uani 0.649(19) 1 d P D 1 F18 F 1.1022(7) 0.3698(6) 0.2092(6) 0.0580(19) Uani 0.649(19) 1 d P D 1 F16B F 1.0749(13) 0.3679(13) 0.1971(11) 0.057(4) Uiso 0.351(19) 1 d P D 2 F17B F 0.9779(7) 0.3122(8) 0.2573(10) 0.057(4) Uiso 0.351(19) 1 d P D 2 F18B F 1.1105(13) 0.3007(15) 0.3242(12) 0.067(5) Uiso 0.351(19) 1 d P D 2 F19 F 0.3329(2) 1.0410(2) 0.5445(2) 0.0641(9) Uani 1 1 d . . . F20 F 0.28452(19) 0.9511(2) 0.46927(19) 0.0511(7) Uani 1 1 d . . . F21 F 0.3603(2) 1.0312(2) 0.40506(18) 0.0499(7) Uani 1 1 d . . . F22 F 0.7125(3) 0.6323(3) 0.6869(2) 0.0739(10) Uani 1 1 d . . . F23 F 0.6491(4) 0.7905(3) 0.7208(2) 0.0854(12) Uani 1 1 d . . . F24 F 0.5584(3) 0.7122(3) 0.73295(19) 0.0731(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02552(19) 0.0322(2) 0.02707(19) -0.00546(13) 0.00367(13) -0.01619(15) B1 0.025(2) 0.030(2) 0.028(2) -0.0039(17) 0.0032(17) -0.0130(18) N1 0.0305(17) 0.0320(18) 0.0343(17) -0.0030(14) 0.0023(14) -0.0168(15) N2 0.0318(18) 0.0303(18) 0.0371(18) -0.0069(14) 0.0079(14) -0.0141(15) N3 0.044(2) 0.034(2) 0.053(2) -0.0116(17) 0.0131(18) -0.0194(17) N4 0.0296(17) 0.0402(19) 0.0290(17) -0.0052(14) 0.0026(13) -0.0198(15) N5 0.0252(16) 0.0388(18) 0.0289(16) -0.0066(14) 0.0019(13) -0.0162(15) N6 0.0318(18) 0.054(2) 0.0294(17) 0.0005(16) -0.0004(14) -0.0220(17) C39 0.032(2) 0.035(2) 0.0274(19) -0.0098(16) 0.0081(16) -0.0184(18) C31 0.0266(19) 0.031(2) 0.0265(18) 0.0016(15) 0.0021(15) -0.0133(16) C23 0.0276(19) 0.031(2) 0.0300(19) -0.0048(16) 0.0026(15) -0.0179(17) C1 0.036(2) 0.032(2) 0.032(2) -0.0066(16) 0.0001(17) -0.0154(18) C2 0.039(2) 0.041(2) 0.059(3) 0.004(2) 0.003(2) -0.025(2) C3 0.046(3) 0.039(2) 0.053(3) 0.003(2) 0.004(2) -0.023(2) C4 0.069(3) 0.039(3) 0.070(3) -0.009(2) 0.014(3) -0.033(3) C5 0.053(3) 0.040(3) 0.071(3) -0.022(2) 0.016(3) -0.018(2) C6 0.037(2) 0.041(3) 0.054(3) -0.010(2) 0.010(2) -0.012(2) C7 0.043(3) 0.042(3) 0.053(3) -0.010(2) 0.018(2) -0.016(2) C8 0.063(4) 0.046(3) 0.093(4) 0.008(3) 0.013(3) -0.032(3) C9 0.082(4) 0.084(4) 0.053(3) 0.022(3) -0.015(3) -0.044(4) C10 0.046(3) 0.073(4) 0.066(4) 0.000(3) -0.004(3) -0.016(3) C11 0.057(3) 0.049(3) 0.087(4) -0.024(3) 0.033(3) -0.014(3) C12 0.033(2) 0.033(2) 0.029(2) -0.0022(16) -0.0018(16) -0.0166(18) C13 0.043(2) 0.056(3) 0.031(2) -0.0024(19) 0.0047(18) -0.032(2) C14 0.038(2) 0.064(3) 0.032(2) -0.007(2) 0.0068(18) -0.029(2) C15 0.046(3) 0.085(4) 0.031(2) 0.005(2) -0.001(2) -0.033(3) C16 0.034(2) 0.067(3) 0.040(2) 0.004(2) -0.0100(19) -0.024(2) C17 0.0241(19) 0.041(2) 0.035(2) -0.0059(17) 0.0016(16) -0.0148(18) C18 0.027(2) 0.057(3) 0.037(2) -0.013(2) 0.0045(17) -0.018(2) C19 0.059(3) 0.114(5) 0.035(3) -0.005(3) 0.009(2) -0.053(4) C20 0.064(3) 0.071(4) 0.062(3) -0.029(3) 0.020(3) -0.037(3) C21 0.029(2) 0.073(3) 0.046(3) -0.007(2) -0.0006(19) -0.023(2) C22 0.042(3) 0.044(3) 0.078(4) -0.008(2) -0.005(2) -0.020(2) C47 0.0192(18) 0.032(2) 0.031(2) -0.0031(16) 0.0035(15) -0.0099(16) C48 0.0221(19) 0.035(2) 0.035(2) -0.0039(17) 0.0050(15) -0.0121(17) C49 0.0220(19) 0.033(2) 0.045(2) -0.0015(18) 0.0113(17) -0.0105(17) C50 0.029(2) 0.044(2) 0.036(2) 0.0056(19) 0.0071(17) -0.0114(19) C51 0.027(2) 0.047(3) 0.035(2) -0.0046(19) 0.0012(17) -0.0132(19) C52 0.027(2) 0.034(2) 0.034(2) -0.0024(16) 0.0028(16) -0.0132(17) C54 0.058(3) 0.074(4) 0.038(3) 0.002(2) -0.006(2) -0.033(3) C53 0.048(3) 0.041(3) 0.056(3) 0.000(2) 0.018(2) -0.021(2) C44 0.034(2) 0.039(2) 0.032(2) -0.0060(17) 0.0066(16) -0.0219(19) C43 0.043(2) 0.039(2) 0.037(2) -0.0079(18) 0.0126(19) -0.023(2) C42 0.043(3) 0.046(3) 0.058(3) -0.020(2) 0.020(2) -0.031(2) C41 0.032(2) 0.049(3) 0.051(3) -0.021(2) 0.0111(19) -0.023(2) C40 0.030(2) 0.036(2) 0.041(2) -0.0096(18) 0.0068(17) -0.0160(18) C45 0.038(3) 0.068(4) 0.088(4) -0.012(3) 0.006(3) -0.033(3) C46 0.062(3) 0.046(3) 0.056(3) 0.000(2) 0.014(3) -0.033(3) C32 0.030(2) 0.030(2) 0.034(2) 0.0001(16) 0.0010(16) -0.0139(17) C33 0.032(2) 0.033(2) 0.040(2) 0.0021(18) 0.0061(18) -0.0116(18) C34 0.024(2) 0.047(3) 0.044(2) 0.006(2) -0.0002(18) -0.0131(19) C35 0.034(2) 0.044(2) 0.034(2) 0.0062(18) -0.0029(17) -0.021(2) C36 0.032(2) 0.033(2) 0.032(2) 0.0018(16) 0.0009(16) -0.0158(18) C38 0.043(3) 0.064(3) 0.042(2) 0.005(2) -0.005(2) -0.034(2) C37 0.038(3) 0.042(3) 0.061(3) -0.006(2) 0.009(2) -0.009(2) C28 0.0267(19) 0.035(2) 0.0290(19) -0.0034(16) 0.0025(15) -0.0174(17) C27 0.0258(19) 0.032(2) 0.035(2) -0.0058(16) 0.0032(16) -0.0164(17) C26 0.033(2) 0.042(2) 0.030(2) -0.0120(17) 0.0092(16) -0.0212(19) C25 0.032(2) 0.038(2) 0.032(2) -0.0023(17) 0.0007(16) -0.0217(18) C24 0.0258(19) 0.033(2) 0.035(2) -0.0043(16) 0.0028(16) -0.0159(17) C29 0.042(2) 0.046(3) 0.037(2) -0.0042(19) -0.0007(19) -0.021(2) C30 0.031(2) 0.041(2) 0.038(2) -0.0091(19) 0.0040(17) -0.0151(19) F1 0.079(8) 0.039(4) 0.043(4) -0.016(3) -0.009(6) -0.005(6) F2 0.092(10) 0.110(13) 0.043(6) -0.019(7) 0.021(6) -0.046(9) F1B 0.079(8) 0.039(4) 0.043(4) -0.016(3) -0.009(6) -0.005(6) F2B 0.092(10) 0.110(13) 0.043(6) -0.019(7) 0.021(6) -0.046(9) F1C 0.072(10) 0.041(7) 0.046(8) -0.016(6) -0.010(7) -0.010(6) F2C 0.044(6) 0.054(6) 0.014(4) 0.007(4) -0.005(4) -0.013(5) F5C 0.091(11) 0.082(11) 0.045(6) 0.000(5) -0.008(6) -0.076(11) F8 0.060(3) 0.041(5) 0.058(4) 0.018(4) -0.037(4) -0.020(4) F8B 0.060(3) 0.041(5) 0.058(4) 0.018(4) -0.037(4) -0.020(4) F9C 0.028(7) 0.073(10) 0.028(8) 0.006(6) -0.013(5) 0.008(6) F10 0.092(3) 0.0425(17) 0.077(2) -0.0146(15) 0.0170(19) -0.0248(17) F11 0.089(3) 0.067(2) 0.123(3) 0.044(2) -0.042(2) -0.049(2) F12 0.114(3) 0.061(2) 0.078(2) -0.0007(17) 0.048(2) -0.046(2) F13 0.070(2) 0.093(3) 0.123(3) 0.022(2) -0.057(2) -0.046(2) F14 0.113(3) 0.108(3) 0.0544(18) 0.0087(18) -0.0072(18) -0.091(3) F15 0.083(2) 0.139(3) 0.072(2) -0.051(2) 0.0205(19) -0.081(3) F17 0.094(7) 0.027(3) 0.063(4) 0.002(2) 0.015(4) 0.001(3) F18 0.038(4) 0.062(4) 0.068(4) -0.024(3) 0.023(3) -0.018(3) F19 0.0537(17) 0.0554(18) 0.0555(17) -0.0294(14) -0.0044(14) 0.0013(14) F20 0.0304(13) 0.0594(17) 0.0639(17) 0.0004(14) -0.0003(12) -0.0212(13) F21 0.0437(15) 0.0407(14) 0.0557(16) 0.0079(12) 0.0026(12) -0.0125(12) F22 0.067(2) 0.076(2) 0.0434(17) 0.0069(15) -0.0072(15) -0.0034(18) F23 0.146(4) 0.091(3) 0.0526(18) 0.0112(17) -0.042(2) -0.083(3) F24 0.071(2) 0.115(3) 0.0400(16) 0.0135(17) 0.0030(15) -0.051(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 N5 2.066(3) 2_575 ? Mo1 N1 2.075(3) . ? Mo1 N4 2.085(3) . ? Mo1 N2 2.099(3) 2_575 ? Mo1 Mo1 2.1222(7) 2_575 ? B1 C39 1.641(6) . ? B1 C31 1.645(6) . ? B1 C23 1.650(5) . ? N1 C1 1.355(5) . ? N1 C2 1.464(5) . ? N2 C1 1.341(5) . ? N2 C7 1.467(5) . ? N2 Mo1 2.099(3) 2_575 ? N3 C1 1.342(5) . ? N3 C4 1.464(6) . ? N3 C5 1.469(6) . ? N4 C12 1.345(5) . ? N4 C13 1.470(5) . ? N5 C12 1.362(5) . ? N5 C18 1.463(5) . ? N5 Mo1 2.066(3) 2_575 ? N6 C12 1.344(5) . ? N6 C16 1.457(5) . ? N6 C15 1.469(5) . ? C39 C44 1.392(6) . ? C39 C40 1.395(6) . ? C31 C32 1.394(5) . ? C31 C36 1.395(6) . ? C23 C28 1.390(6) . ? C23 C24 1.399(5) . ? C2 C3 1.503(6) . ? C3 C4 1.511(7) . ? C3 C9 1.521(7) . ? C3 C8 1.536(6) . ? C5 C6 1.503(7) . ? C6 C7 1.500(7) . ? C6 C11 1.524(6) . ? C6 C10 1.526(7) . ? C13 C14 1.512(6) . ? C14 C15 1.512(7) . ? C14 C19 1.525(6) . ? C14 C20 1.534(7) . ? C16 C17 1.509(6) . ? C17 C18 1.507(6) . ? C17 C22 1.512(5) . ? C17 C21 1.517(6) . ? C47 C48 1.3902 . ? C49 C50 1.390(6) . ? C49 C53 1.475(6) . ? C50 C51 1.380(6) . ? C51 C52 1.392(6) . ? C51 C54 1.492(6) . ? C54 F3C 1.262(14) . ? C54 F3 1.313(7) . ? C54 F1B 1.317(7) . ? C54 F2B 1.334(7) . ? C54 F2C 1.343(11) . ? C54 F2 1.360(7) . ? C54 F1 1.362(7) . ? C54 F1C 1.368(15) . ? C54 F3B 1.381(7) . ? C53 F4C 1.232(14) . ? C53 F5B 1.282(7) . ? C53 F6C 1.314(10) . ? C53 F6 1.332(6) . ? C53 F4B 1.349(6) . ? C53 F4 1.371(6) . ? C53 F5 1.377(7) . ? C53 F6B 1.407(7) . ? C53 F5C 1.559(13) . ? C44 C43 1.395(6) . ? C43 C42 1.371(7) . ? C43 C46 1.507(7) . ? C42 C41 1.378(7) . ? C41 C40 1.386(6) . ? C41 C45 1.484(7) . ? C45 F8C 1.21(2) . ? C45 F7C 1.29(2) . ? C45 F7B 1.314(6) . ? C45 F9 1.331(7) . ? C45 F8B 1.346(7) . ? C45 F8 1.358(8) . ? C45 F9C 1.387(15) . ? C45 F7 1.391(7) . ? C45 F9B 1.413(6) . ? C46 F11 1.316(6) . ? C46 F12 1.325(6) . ? C46 F10 1.341(6) . ? C32 C33 1.383(6) . ? C33 C34 1.384(6) . ? C33 C37 1.503(6) . ? C34 C35 1.372(6) . ? C35 C36 1.398(6) . ? C35 C38 1.497(6) . ? C38 F15 1.316(6) . ? C38 F13 1.323(6) . ? C38 F14 1.323(5) . ? C37 F16B 1.257(17) . ? C37 F17B 1.290(10) . ? C37 F17 1.293(8) . ? C37 F16 1.369(8) . ? C37 F18B 1.381(18) . ? C37 F18 1.390(9) . ? C28 C27 1.396(5) . ? C27 C26 1.373(6) . ? C27 C30 1.489(6) . ? C26 C25 1.389(6) . ? C25 C24 1.386(6) . ? C25 C29 1.494(6) . ? C29 F23 1.310(5) . ? C29 F22 1.326(5) . ? C29 F24 1.339(5) . ? C30 F21 1.332(5) . ? C30 F19 1.335(5) . ? C30 F20 1.345(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 N5 Mo1 N1 92.01(13) 2_575 . ? N5 Mo1 N4 174.54(12) 2_575 . ? N1 Mo1 N4 90.30(13) . . ? N5 Mo1 N2 89.01(13) 2_575 2_575 ? N1 Mo1 N2 175.01(12) . 2_575 ? N4 Mo1 N2 88.27(13) . 2_575 ? N5 Mo1 Mo1 92.31(9) 2_575 2_575 ? N1 Mo1 Mo1 91.94(9) . 2_575 ? N4 Mo1 Mo1 92.56(9) . 2_575 ? N2 Mo1 Mo1 92.90(9) 2_575 2_575 ? C39 B1 C31 113.3(3) . . ? C39 B1 C23 103.0(3) . . ? C31 B1 C23 113.0(3) . . ? C1 N1 C2 118.9(3) . . ? C1 N1 Mo1 119.9(3) . . ? C2 N1 Mo1 121.2(3) . . ? C1 N2 C7 120.1(3) . . ? C1 N2 Mo1 118.2(3) . 2_575 ? C7 N2 Mo1 121.7(3) . 2_575 ? C1 N3 C4 122.4(4) . . ? C1 N3 C5 120.3(4) . . ? C4 N3 C5 117.2(4) . . ? C12 N4 C13 119.0(3) . . ? C12 N4 Mo1 119.0(3) . . ? C13 N4 Mo1 122.0(3) . . ? C12 N5 C18 117.6(3) . . ? C12 N5 Mo1 119.7(3) . 2_575 ? C18 N5 Mo1 122.7(3) . 2_575 ? C12 N6 C16 122.7(3) . . ? C12 N6 C15 120.7(4) . . ? C16 N6 C15 116.5(4) . . ? C44 C39 C40 116.0(4) . . ? C44 C39 B1 122.7(3) . . ? C40 C39 B1 120.7(4) . . ? C32 C31 C36 116.0(4) . . ? C32 C31 B1 121.0(3) . . ? C36 C31 B1 122.6(3) . . ? C28 C23 C24 116.1(3) . . ? C28 C23 B1 121.9(3) . . ? C24 C23 B1 121.5(3) . . ? N2 C1 N3 122.0(4) . . ? N2 C1 N1 117.0(3) . . ? N3 C1 N1 121.0(4) . . ? N1 C2 C3 113.8(4) . . ? C2 C3 C4 106.0(4) . . ? C2 C3 C9 110.6(4) . . ? C4 C3 C9 111.0(5) . . ? C2 C3 C8 109.6(4) . . ? C4 C3 C8 109.0(4) . . ? C9 C3 C8 110.5(4) . . ? N3 C4 C3 112.0(4) . . ? N3 C5 C6 111.4(4) . . ? C7 C6 C5 107.1(4) . . ? C7 C6 C11 111.3(4) . . ? C5 C6 C11 109.6(4) . . ? C7 C6 C10 109.9(4) . . ? C5 C6 C10 109.6(5) . . ? C11 C6 C10 109.3(5) . . ? N2 C7 C6 114.3(4) . . ? N6 C12 N4 122.2(4) . . ? N6 C12 N5 121.4(4) . . ? N4 C12 N5 116.4(3) . . ? N4 C13 C14 113.8(3) . . ? C15 C14 C13 105.7(4) . . ? C15 C14 C19 110.8(4) . . ? C13 C14 C19 109.6(4) . . ? C15 C14 C20 110.5(4) . . ? C13 C14 C20 110.3(4) . . ? C19 C14 C20 109.9(4) . . ? N6 C15 C14 110.8(4) . . ? N6 C16 C17 112.8(3) . . ? C18 C17 C16 106.5(4) . . ? C18 C17 C22 110.6(3) . . ? C16 C17 C22 109.9(3) . . ? C18 C17 C21 110.6(3) . . ? C16 C17 C21 109.9(4) . . ? C22 C17 C21 109.3(3) . . ? N5 C18 C17 112.7(3) . . ? C50 C49 C53 117.7(4) . . ? C51 C50 C49 118.3(4) . . ? C50 C51 C52 120.9(4) . . ? C50 C51 C54 119.4(4) . . ? C52 C51 C54 119.7(4) . . ? F3C C54 F3 74.6(8) . . ? F3C C54 F1B 66.7(8) . . ? F3 C54 F1B 122.3(8) . . ? F3C C54 F2B 128.9(9) . . ? F3 C54 F2B 66.1(6) . . ? F1B C54 F2B 108.8(6) . . ? F3C C54 F2C 109.4(9) . . ? F1B C54 F2C 128.0(8) . . ? F3C C54 F2 129.6(9) . . ? F3 C54 F2 105.9(6) . . ? F1B C54 F2 72.2(6) . . ? F2C C54 F2 74.8(6) . . ? F3 C54 F1 105.0(6) . . ? F2B C54 F1 130.2(8) . . ? F2C C54 F1 131.5(7) . . ? F2 C54 F1 103.0(6) . . ? F3C C54 F1C 108.6(9) . . ? F3 C54 F1C 128.8(8) . . ? F2B C54 F1C 75.5(8) . . ? F2C C54 F1C 105.1(8) . . ? F1 C54 F1C 75.1(7) . . ? F1B C54 F3B 104.0(6) . . ? F2B C54 F3B 103.6(6) . . ? F2C C54 F3B 75.1(6) . . ? F2 C54 F3B 136.4(7) . . ? F1 C54 F3B 75.4(5) . . ? F1C C54 F3B 139.0(8) . . ? F3C C54 C51 112.2(7) . . ? F3 C54 C51 116.0(6) . . ? F1B C54 C51 117.6(6) . . ? F2B C54 C51 113.6(7) . . ? F2C C54 C51 111.5(6) . . ? F2 C54 C51 112.0(6) . . ? F1 C54 C51 113.8(5) . . ? F1C C54 C51 109.7(6) . . ? F3B C54 C51 107.9(6) . . ? F4C C53 F5B 120.4(9) . . ? F4C C53 F6C 115.0(9) . . ? F5B C53 F6C 45.5(6) . . ? F4C C53 F6 88.6(8) . . ? F5B C53 F6 76.2(5) . . ? F5B C53 F4B 111.6(6) . . ? F6C C53 F4B 135.5(7) . . ? F6 C53 F4B 119.8(6) . . ? F5B C53 F4 122.0(7) . . ? F6C C53 F4 130.5(7) . . ? F6 C53 F4 106.5(5) . . ? F4C C53 F5 109.5(9) . . ? F6C C53 F5 75.8(6) . . ? F6 C53 F5 104.3(6) . . ? F4B C53 F5 87.4(7) . . ? F4 C53 F5 102.3(6) . . ? F4C C53 F6B 67.5(8) . . ? F5B C53 F6B 106.5(5) . . ? F6C C53 F6B 64.6(6) . . ? F4B C53 F6B 101.7(5) . . ? F4 C53 F6B 84.8(6) . . ? F5 C53 F6B 131.7(7) . . ? F4C C53 C49 122.0(8) . . ? F5B C53 C49 116.1(6) . . ? F6C C53 C49 113.0(5) . . ? F6 C53 C49 117.2(4) . . ? F4B C53 C49 111.5(5) . . ? F4 C53 C49 113.1(5) . . ? F5 C53 C49 112.1(7) . . ? F6B C53 C49 108.2(5) . . ? F4C C53 F5C 101.5(8) . . ? F6C C53 F5C 89.1(9) . . ? F6 C53 F5C 115.8(9) . . ? F4B C53 F5C 75.6(7) . . ? F4 C53 F5C 91.6(7) . . ? F6B C53 F5C 139.9(9) . . ? C49 C53 F5C 109.8(7) . . ? C39 C44 C43 121.7(4) . . ? C42 C43 C44 120.8(4) . . ? C42 C43 C46 118.4(4) . . ? C44 C43 C46 120.8(4) . . ? C43 C42 C41 118.7(4) . . ? C42 C41 C40 120.4(4) . . ? C42 C41 C45 118.4(4) . . ? C40 C41 C45 121.2(4) . . ? C41 C40 C39 122.4(4) . . ? F8C C45 F7C 102.4(15) . . ? F8C C45 F7B 111.5(11) . . ? F7C C45 F7B 77.2(12) . . ? F8C C45 F9 47.4(12) . . ? F7C C45 F9 127.6(12) . . ? F7B C45 F9 78.6(6) . . ? F8C C45 F8B 72.4(13) . . ? F7B C45 F8B 108.9(6) . . ? F9 C45 F8B 114.9(8) . . ? F8C C45 F8 59.7(13) . . ? F7C C45 F8 57.4(12) . . ? F7B C45 F8 126.5(8) . . ? F9 C45 F8 106.5(7) . . ? F8C C45 F9C 97.6(13) . . ? F7C C45 F9C 106.0(12) . . ? F9 C45 F9C 54.0(8) . . ? F8B C45 F9C 131.6(7) . . ? F8 C45 F9C 142.5(10) . . ? F8C C45 F7 121.3(12) . . ? F7C C45 F7 47.7(12) . . ? F9 C45 F7 105.7(6) . . ? F8B C45 F7 83.6(5) . . ? F8 C45 F7 103.3(6) . . ? F9C C45 F7 61.0(8) . . ? F7C C45 F9B 131.7(12) . . ? F7B C45 F9B 105.8(5) . . ? F8B C45 F9B 102.5(5) . . ? F8 C45 F9B 87.7(8) . . ? F9C C45 F9B 80.9(8) . . ? F7 C45 F9B 130.6(6) . . ? F8C C45 C41 125.2(11) . . ? F7C C45 C41 114.3(11) . . ? F7B C45 C41 115.3(5) . . ? F9 C45 C41 118.0(6) . . ? F8B C45 C41 115.4(6) . . ? F8 C45 C41 108.6(9) . . ? F9C C45 C41 108.9(6) . . ? F7 C45 C41 113.6(5) . . ? F9B C45 C41 107.6(5) . . ? F11 C46 F12 108.7(5) . . ? F11 C46 F10 105.3(5) . . ? F12 C46 F10 104.8(4) . . ? F11 C46 C43 114.0(4) . . ? F12 C46 C43 112.5(4) . . ? F10 C46 C43 110.9(4) . . ? C33 C32 C31 122.3(4) . . ? C32 C33 C34 120.7(4) . . ? C32 C33 C37 120.9(4) . . ? C34 C33 C37 118.4(4) . . ? C35 C34 C33 118.3(4) . . ? C34 C35 C36 120.9(4) . . ? C34 C35 C38 118.9(4) . . ? C36 C35 C38 120.2(4) . . ? C31 C36 C35 121.7(4) . . ? F15 C38 F13 106.4(4) . . ? F15 C38 F14 106.2(4) . . ? F13 C38 F14 105.2(4) . . ? F15 C38 C35 113.8(4) . . ? F13 C38 C35 112.4(4) . . ? F14 C38 C35 112.2(4) . . ? F16B C37 F17B 110.0(9) . . ? F16B C37 F17 116.1(9) . . ? F17B C37 F17 82.4(7) . . ? F16B C37 F16 84.8(7) . . ? F17 C37 F16 107.7(7) . . ? F16B C37 F18B 104.5(10) . . ? F17B C37 F18B 106.7(8) . . ? F16 C37 F18B 130.1(8) . . ? F17B C37 F18 126.4(7) . . ? F17 C37 F18 105.9(6) . . ? F16 C37 F18 103.4(6) . . ? F18B C37 F18 89.3(8) . . ? F16B C37 C33 115.5(9) . . ? F17B C37 C33 112.8(5) . . ? F17 C37 C33 115.4(5) . . ? F16 C37 C33 113.1(4) . . ? F18B C37 C33 106.6(8) . . ? F18 C37 C33 110.5(5) . . ? C23 C28 C27 122.4(4) . . ? C26 C27 C28 120.3(4) . . ? C26 C27 C30 120.0(4) . . ? C28 C27 C30 119.6(4) . . ? C27 C26 C25 118.6(4) . . ? C24 C25 C26 120.7(4) . . ? C24 C25 C29 121.5(4) . . ? C26 C25 C29 117.8(4) . . ? C25 C24 C23 121.9(4) . . ? F23 C29 F22 108.0(4) . . ? F23 C29 F24 105.0(4) . . ? F22 C29 F24 104.0(4) . . ? F23 C29 C25 113.2(4) . . ? F22 C29 C25 113.7(4) . . ? F24 C29 C25 112.2(4) . . ? F21 C30 F19 106.7(4) . . ? F21 C30 F20 104.9(3) . . ? F19 C30 F20 105.9(3) . . ? F21 C30 C27 113.4(3) . . ? F19 C30 C27 113.3(4) . . ? F20 C30 C27 112.0(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.108 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.093 #===END of CIF for Compound 3 ====================== data_4 _database_code_depnum_ccdc_archive 'CCDC 645815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H112 Mo2 N12' _chemical_formula_sum 'C60 H112 Mo2 N12' _chemical_formula_weight 1193.50 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2621(19) _cell_length_b 14.365(2) _cell_length_c 20.885(4) _cell_angle_alpha 97.180(3) _cell_angle_beta 100.508(3) _cell_angle_gamma 103.563(3) _cell_volume 3179.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4717 _cell_measurement_theta_min 2.640 _cell_measurement_theta_max 25.1355 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9129 _exptl_absorpt_correction_T_max 0.9677 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SAMRT' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18699 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11060 _reflns_number_gt 7499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11060 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 0.57134(3) 0.72469(2) 0.733073(14) 0.01884(10) Uani 1 1 d . . . Mo2 Mo 0.72355(3) 0.71041(2) 0.694793(14) 0.01855(10) Uani 1 1 d . . . N1 N 0.5973(3) 0.8732(2) 0.71790(14) 0.0226(7) Uani 1 1 d . . . N8 N 0.6982(3) 0.5632(2) 0.70964(14) 0.0212(7) Uani 1 1 d . . . N2 N 0.7692(3) 0.8586(2) 0.67795(14) 0.0230(7) Uani 1 1 d . . . N4 N 0.4431(3) 0.6765(2) 0.63902(14) 0.0217(7) Uani 1 1 d . . . N7 N 0.5308(3) 0.5797(2) 0.75266(14) 0.0212(7) Uani 1 1 d . . . N5 N 0.6124(3) 0.6673(2) 0.59532(13) 0.0212(7) Uani 1 1 d . . . N11 N 0.8521(3) 0.7610(2) 0.79019(14) 0.0226(7) Uani 1 1 d . . . C34 C 0.6056(4) 0.5247(3) 0.73854(17) 0.0221(9) Uani 1 1 d . . . N10 N 0.6846(3) 0.7796(2) 0.83212(14) 0.0229(7) Uani 1 1 d . . . C37 C 0.7816(4) 0.5061(3) 0.69109(18) 0.0259(9) Uani 1 1 d . . . H37A H 0.8640 0.5503 0.6943 0.031 Uiso 1 1 calc R . . H37B H 0.7492 0.4744 0.6447 0.031 Uiso 1 1 calc R . . C4 C 0.6948(4) 0.9133(3) 0.69363(17) 0.0237(9) Uani 1 1 d . . . C35 C 0.6660(4) 0.3712(3) 0.73416(18) 0.0265(9) Uani 1 1 d . . . H35A H 0.6229 0.3371 0.6893 0.032 Uiso 1 1 calc R . . H35B H 0.6709 0.3224 0.7627 0.032 Uiso 1 1 calc R . . N3 N 0.7245(3) 1.0128(2) 0.68980(15) 0.0282(8) Uani 1 1 d . . . C7 C 0.8751(3) 0.8966(3) 0.64890(18) 0.0262(9) Uani 1 1 d . . . H7A H 0.8506 0.8729 0.6011 0.031 Uiso 1 1 calc R . . H7B H 0.9441 0.8697 0.6666 0.031 Uiso 1 1 calc R . . C49 C 0.8069(4) 0.7947(3) 0.84045(17) 0.0232(9) Uani 1 1 d . . . C19 C 0.4909(4) 0.6611(3) 0.58589(17) 0.0223(9) Uani 1 1 d . . . C31 C 0.4204(4) 0.5381(3) 0.7773(2) 0.0320(10) Uani 1 1 d . . . H31A H 0.3496 0.5104 0.7395 0.038 Uiso 1 1 calc R . . H31B H 0.3999 0.5906 0.8042 0.038 Uiso 1 1 calc R . . C33 C 0.4811(4) 0.3865(3) 0.77740(18) 0.0294(10) Uani 1 1 d . . . H33A H 0.4976 0.3363 0.8029 0.035 Uiso 1 1 calc R . . H33B H 0.4160 0.3548 0.7377 0.035 Uiso 1 1 calc R . . C3 C 0.6331(4) 1.0667(3) 0.69672(19) 0.0305(10) Uani 1 1 d . . . H3A H 0.5726 1.0550 0.6545 0.037 Uiso 1 1 calc R . . H3B H 0.6752 1.1364 0.7078 0.037 Uiso 1 1 calc R . . C5 C 0.8086(4) 1.0453(3) 0.6473(2) 0.0325(10) Uani 1 1 d . . . H5A H 0.8339 1.1166 0.6549 0.039 Uiso 1 1 calc R . . H5B H 0.7647 1.0223 0.6009 0.039 Uiso 1 1 calc R . . C52 C 0.9863(3) 0.7743(3) 0.79588(17) 0.0299(10) Uani 1 1 d . . . H52A H 1.0164 0.8263 0.7719 0.036 Uiso 1 1 calc R . . H52B H 0.9993 0.7144 0.7737 0.036 Uiso 1 1 calc R . . N9 N 0.5955(3) 0.4344(2) 0.75801(15) 0.0271(8) Uani 1 1 d . . . C16 C 0.3088(3) 0.6592(3) 0.63270(18) 0.0272(9) Uani 1 1 d . . . H16A H 0.2934 0.7027 0.6685 0.033 Uiso 1 1 calc R . . H16B H 0.2745 0.5923 0.6384 0.033 Uiso 1 1 calc R . . C1 C 0.5073(4) 0.9271(3) 0.73031(19) 0.0295(10) Uani 1 1 d . . . H1A H 0.4687 0.9031 0.7656 0.035 Uiso 1 1 calc R . . H1B H 0.4410 0.9144 0.6903 0.035 Uiso 1 1 calc R . . C22 C 0.6695(4) 0.6545(3) 0.53896(17) 0.0269(9) Uani 1 1 d . . . H22A H 0.6706 0.5862 0.5291 0.032 Uiso 1 1 calc R . . H22B H 0.7566 0.6940 0.5510 0.032 Uiso 1 1 calc R . . N12 N 0.8876(3) 0.8406(2) 0.90139(14) 0.0276(8) Uani 1 1 d . . . N6 N 0.4154(3) 0.6461(2) 0.52260(14) 0.0303(8) Uani 1 1 d . . . C17 C 0.2383(4) 0.6748(3) 0.56639(18) 0.0280(9) Uani 1 1 d . . . C12 C 1.0031(4) 1.0388(3) 0.6104(2) 0.0418(11) Uani 1 1 d . . . H12A H 0.9507 1.0140 0.5658 0.050 Uiso 1 1 calc R . . H12B H 1.0257 1.1100 0.6163 0.050 Uiso 1 1 calc R . . C18 C 0.2809(3) 0.6166(3) 0.51338(18) 0.0297(10) Uani 1 1 d . . . H18A H 0.2538 0.5472 0.5153 0.036 Uiso 1 1 calc R . . H18B H 0.2421 0.6264 0.4697 0.036 Uiso 1 1 calc R . . C36 C 0.7976(4) 0.4282(3) 0.73325(18) 0.0272(9) Uani 1 1 d . . . C2 C 0.5642(4) 1.0374(3) 0.75034(19) 0.0282(9) Uani 1 1 d . . . C23 C 0.0965(4) 0.6306(3) 0.5588(2) 0.0382(11) Uani 1 1 d . . . H23A H 0.0536 0.6350 0.5145 0.046 Uiso 1 1 calc R . . H23B H 0.0826 0.5614 0.5615 0.046 Uiso 1 1 calc R . . C20 C 0.4661(4) 0.6263(3) 0.46540(17) 0.0302(10) Uani 1 1 d . . . H20A H 0.4176 0.6445 0.4273 0.036 Uiso 1 1 calc R . . H20B H 0.4585 0.5564 0.4552 0.036 Uiso 1 1 calc R . . C50 C 1.0193(4) 0.8780(3) 0.90177(19) 0.0341(10) Uani 1 1 d . . . H50A H 1.0675 0.8989 0.9475 0.041 Uiso 1 1 calc R . . H50B H 1.0305 0.9346 0.8795 0.041 Uiso 1 1 calc R . . C8 C 0.4628(4) 1.0921(3) 0.7493(2) 0.0389(11) Uani 1 1 d . . . H8A H 0.5038 1.1620 0.7588 0.047 Uiso 1 1 calc R . . H8B H 0.4106 1.0772 0.7045 0.047 Uiso 1 1 calc R . . C42 C 0.8611(4) 0.3575(3) 0.7013(2) 0.0394(11) Uani 1 1 d . . . H42A H 0.8725 0.3107 0.7307 0.047 Uiso 1 1 calc R . . H42B H 0.8040 0.3210 0.6599 0.047 Uiso 1 1 calc R . . C48 C 0.8378(4) 0.8998(3) 0.94489(18) 0.0324(10) Uani 1 1 d . . . H48A H 0.8271 0.9573 0.9261 0.039 Uiso 1 1 calc R . . H48B H 0.8968 0.9221 0.9878 0.039 Uiso 1 1 calc R . . C21 C 0.6033(4) 0.6821(3) 0.47671(18) 0.0307(10) Uani 1 1 d . . . C6 C 0.9238(4) 1.0075(3) 0.66068(19) 0.0295(10) Uani 1 1 d . . . C46 C 0.6265(4) 0.8115(3) 0.88477(17) 0.0304(10) Uani 1 1 d . . . H46A H 0.5544 0.7586 0.8859 0.037 Uiso 1 1 calc R . . H46B H 0.5947 0.8667 0.8736 0.037 Uiso 1 1 calc R . . C38 C 0.3068(4) 0.4059(3) 0.8300(2) 0.0426(12) Uani 1 1 d . . . H38A H 0.2517 0.3753 0.7868 0.051 Uiso 1 1 calc R . . H38B H 0.3184 0.3538 0.8546 0.051 Uiso 1 1 calc R . . C51 C 1.0670(4) 0.7994(3) 0.86643(18) 0.0290(10) Uani 1 1 d . . . C32 C 0.4350(4) 0.4593(3) 0.81872(18) 0.0285(9) Uani 1 1 d . . . C57 C 1.2044(4) 0.8429(3) 0.8653(2) 0.0433(12) Uani 1 1 d . . . H57A H 1.2103 0.9015 0.8453 0.052 Uiso 1 1 calc R . . H57B H 1.2529 0.8629 0.9110 0.052 Uiso 1 1 calc R . . C58 C 1.2636(4) 0.7755(4) 0.8281(2) 0.0585(14) Uani 1 1 d . . . H58A H 1.3500 0.8087 0.8299 0.088 Uiso 1 1 calc R . . H58B H 1.2180 0.7566 0.7824 0.088 Uiso 1 1 calc R . . H58C H 1.2607 0.7179 0.8482 0.088 Uiso 1 1 calc R . . C47 C 0.7118(4) 0.8420(3) 0.95447(18) 0.0326(10) Uani 1 1 d . . . C25 C 0.2709(4) 0.7832(3) 0.56293(19) 0.0363(10) Uani 1 1 d . . . H25A H 0.2466 0.8175 0.5999 0.044 Uiso 1 1 calc R . . H25B H 0.3620 0.8066 0.5694 0.044 Uiso 1 1 calc R . . C29 C 0.6203(4) 0.7925(3) 0.4890(2) 0.0415(12) Uani 1 1 d . . . H29A H 0.5953 0.8101 0.5304 0.050 Uiso 1 1 calc R . . H29B H 0.7097 0.8244 0.4955 0.050 Uiso 1 1 calc R . . C44 C 0.8718(4) 0.4805(3) 0.80299(19) 0.0350(10) Uani 1 1 d . . . H44A H 0.9572 0.5120 0.7997 0.042 Uiso 1 1 calc R . . H44B H 0.8339 0.5321 0.8172 0.042 Uiso 1 1 calc R . . C14 C 0.9965(4) 1.0427(3) 0.7324(2) 0.0378(11) Uani 1 1 d . . . H14A H 1.0669 1.0132 0.7395 0.045 Uiso 1 1 calc R . . H14B H 0.9415 1.0190 0.7616 0.045 Uiso 1 1 calc R . . C59 C 1.0494(4) 0.7092(3) 0.90010(19) 0.0370(11) Uani 1 1 d . . . H59A H 0.9599 0.6842 0.8985 0.044 Uiso 1 1 calc R . . H59B H 1.0752 0.6588 0.8741 0.044 Uiso 1 1 calc R . . C53 C 0.6589(4) 0.9080(3) 0.9982(2) 0.0472(13) Uani 1 1 d . . . H53A H 0.7158 0.9278 1.0419 0.057 Uiso 1 1 calc R . . H53B H 0.6583 0.9669 0.9792 0.057 Uiso 1 1 calc R . . C40 C 0.5309(4) 0.5050(3) 0.88395(18) 0.0415(11) Uani 1 1 d . . . H40A H 0.6092 0.5390 0.8734 0.050 Uiso 1 1 calc R . . H40B H 0.4999 0.5539 0.9080 0.050 Uiso 1 1 calc R . . C27 C 0.6509(4) 0.6457(4) 0.4160(2) 0.0525(14) Uani 1 1 d . . . H27A H 0.6344 0.5747 0.4107 0.063 Uiso 1 1 calc R . . H27B H 0.6022 0.6606 0.3765 0.063 Uiso 1 1 calc R . . C55 C 0.7262(4) 0.7507(3) 0.98295(19) 0.0409(11) Uani 1 1 d . . . H55A H 0.6433 0.7140 0.9867 0.049 Uiso 1 1 calc R . . H55B H 0.7550 0.7098 0.9513 0.049 Uiso 1 1 calc R . . C10 C 0.6545(4) 1.0567(3) 0.8179(2) 0.0425(11) Uani 1 1 d . . . H10A H 0.6062 1.0353 0.8504 0.051 Uiso 1 1 calc R . . H10B H 0.7133 1.0164 0.8152 0.051 Uiso 1 1 calc R . . C24 C 0.0358(4) 0.6764(4) 0.6086(2) 0.0554(14) Uani 1 1 d . . . H24A H -0.0525 0.6429 0.5997 0.083 Uiso 1 1 calc R . . H24B H 0.0452 0.7444 0.6053 0.083 Uiso 1 1 calc R . . H24C H 0.0757 0.6714 0.6529 0.083 Uiso 1 1 calc R . . C39 C 0.2413(4) 0.4686(4) 0.8668(2) 0.0562(14) Uani 1 1 d . . . H39A H 0.1617 0.4288 0.8712 0.084 Uiso 1 1 calc R . . H39B H 0.2270 0.5196 0.8425 0.084 Uiso 1 1 calc R . . H39C H 0.2932 0.4975 0.9104 0.084 Uiso 1 1 calc R . . C43 C 0.9866(5) 0.4014(4) 0.6859(3) 0.0633(15) Uani 1 1 d . . . H43A H 1.0175 0.3501 0.6656 0.095 Uiso 1 1 calc R . . H43B H 1.0456 0.4357 0.7265 0.095 Uiso 1 1 calc R . . H43C H 0.9768 0.4466 0.6557 0.095 Uiso 1 1 calc R . . C13 C 1.1211(5) 1.0059(4) 0.6142(3) 0.0635(15) Uani 1 1 d . . . H13A H 1.1638 1.0297 0.5807 0.095 Uiso 1 1 calc R . . H13B H 1.1003 0.9354 0.6067 0.095 Uiso 1 1 calc R . . H13C H 1.1755 1.0315 0.6576 0.095 Uiso 1 1 calc R . . C54 C 0.5285(4) 0.8639(4) 1.0073(2) 0.0685(17) Uani 1 1 d . . . H54A H 0.5033 0.9112 1.0356 0.103 Uiso 1 1 calc R . . H54B H 0.5282 0.8067 1.0276 0.103 Uiso 1 1 calc R . . H54C H 0.4704 0.8456 0.9646 0.103 Uiso 1 1 calc R . . C26 C 0.2106(5) 0.8113(4) 0.4992(2) 0.0652(16) Uani 1 1 d . . . H26A H 0.2381 0.8812 0.5020 0.098 Uiso 1 1 calc R . . H26B H 0.1202 0.7913 0.4930 0.098 Uiso 1 1 calc R . . H26C H 0.2351 0.7791 0.4620 0.098 Uiso 1 1 calc R . . C45 C 0.8806(5) 0.4190(3) 0.8568(2) 0.0564(14) Uani 1 1 d . . . H45A H 0.9295 0.4598 0.8981 0.085 Uiso 1 1 calc R . . H45B H 0.9208 0.3687 0.8446 0.085 Uiso 1 1 calc R . . H45C H 0.7972 0.3890 0.8621 0.085 Uiso 1 1 calc R . . C9 C 0.3775(5) 1.0704(4) 0.7973(3) 0.0643(15) Uani 1 1 d . . . H9A H 0.3165 1.1082 0.7923 0.096 Uiso 1 1 calc R . . H9B H 0.4271 1.0875 0.8423 0.096 Uiso 1 1 calc R . . H9C H 0.3344 1.0017 0.7881 0.096 Uiso 1 1 calc R . . C15 C 1.0475(5) 1.1534(3) 0.7530(3) 0.0683(17) Uani 1 1 d . . . H15A H 1.0919 1.1690 0.7990 0.102 Uiso 1 1 calc R . . H15B H 0.9785 1.1835 0.7475 0.102 Uiso 1 1 calc R . . H15C H 1.1044 1.1777 0.7255 0.102 Uiso 1 1 calc R . . C30 C 0.5484(5) 0.8341(4) 0.4350(2) 0.0691(17) Uani 1 1 d . . . H30A H 0.5663 0.9040 0.4481 0.104 Uiso 1 1 calc R . . H30B H 0.4593 0.8052 0.4289 0.104 Uiso 1 1 calc R . . H30C H 0.5741 0.8195 0.3939 0.104 Uiso 1 1 calc R . . C60 C 1.1197(5) 0.7244(4) 0.9710(2) 0.0755(18) Uani 1 1 d . . . H60A H 1.1019 0.6635 0.9874 0.113 Uiso 1 1 calc R . . H60B H 1.0934 0.7726 0.9978 0.113 Uiso 1 1 calc R . . H60C H 1.2088 0.7468 0.9734 0.113 Uiso 1 1 calc R . . C41 C 0.5602(5) 0.4354(4) 0.9296(2) 0.0772(18) Uani 1 1 d . . . H41A H 0.6205 0.4715 0.9693 0.116 Uiso 1 1 calc R . . H41B H 0.5949 0.3882 0.9073 0.116 Uiso 1 1 calc R . . H41C H 0.4840 0.4020 0.9413 0.116 Uiso 1 1 calc R . . C11 C 0.7294(5) 1.1612(3) 0.8433(2) 0.0771(19) Uani 1 1 d . . . H11A H 0.7836 1.1658 0.8860 0.116 Uiso 1 1 calc R . . H11B H 0.6727 1.2019 0.8479 0.116 Uiso 1 1 calc R . . H11C H 0.7797 1.1831 0.8123 0.116 Uiso 1 1 calc R . . C56 C 0.8150(5) 0.7682(4) 1.0498(2) 0.0768(19) Uani 1 1 d . . . H56A H 0.8171 0.7063 1.0633 0.115 Uiso 1 1 calc R . . H56B H 0.7865 0.8071 1.0822 0.115 Uiso 1 1 calc R . . H56C H 0.8984 0.8024 1.0466 0.115 Uiso 1 1 calc R . . C28 C 0.7896(5) 0.6884(5) 0.4189(2) 0.0795(19) Uani 1 1 d . . . H28A H 0.8111 0.6607 0.3792 0.119 Uiso 1 1 calc R . . H28B H 0.8392 0.6733 0.4574 0.119 Uiso 1 1 calc R . . H28C H 0.8067 0.7584 0.4220 0.119 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 0.0192(2) 0.01933(18) 0.01836(18) 0.00460(13) 0.00510(14) 0.00428(15) Mo2 0.0187(2) 0.01918(18) 0.01834(18) 0.00494(13) 0.00497(14) 0.00458(15) N1 0.0216(18) 0.0176(16) 0.0300(18) 0.0062(13) 0.0077(14) 0.0053(14) N8 0.0199(18) 0.0201(16) 0.0240(17) 0.0053(13) 0.0068(14) 0.0041(14) N2 0.0196(18) 0.0206(17) 0.0305(18) 0.0087(14) 0.0077(14) 0.0046(15) N4 0.0170(17) 0.0280(18) 0.0214(16) 0.0051(13) 0.0046(13) 0.0076(14) N7 0.0162(17) 0.0222(17) 0.0276(17) 0.0098(13) 0.0072(14) 0.0050(14) N5 0.0210(18) 0.0275(17) 0.0184(16) 0.0078(13) 0.0062(14) 0.0096(15) N11 0.0191(17) 0.0250(18) 0.0210(16) 0.0026(14) 0.0013(13) 0.0038(15) C34 0.026(2) 0.0173(19) 0.0200(19) 0.0039(15) 0.0010(17) 0.0031(18) N10 0.0219(19) 0.0247(17) 0.0220(17) 0.0035(13) 0.0030(14) 0.0074(15) C37 0.027(2) 0.023(2) 0.029(2) 0.0065(17) 0.0095(18) 0.0051(18) C4 0.024(2) 0.024(2) 0.023(2) 0.0104(17) 0.0017(17) 0.0048(18) C35 0.031(2) 0.020(2) 0.030(2) 0.0044(17) 0.0071(18) 0.0084(19) N3 0.028(2) 0.0212(17) 0.042(2) 0.0147(15) 0.0147(16) 0.0100(15) C7 0.022(2) 0.026(2) 0.031(2) 0.0076(17) 0.0079(17) 0.0026(18) C49 0.027(2) 0.023(2) 0.018(2) 0.0031(16) 0.0043(17) 0.0037(18) C19 0.025(2) 0.023(2) 0.019(2) 0.0063(16) 0.0031(17) 0.0064(17) C31 0.031(3) 0.028(2) 0.040(2) 0.0129(19) 0.0113(19) 0.007(2) C33 0.033(3) 0.024(2) 0.031(2) 0.0068(17) 0.0117(19) 0.0021(19) C3 0.031(3) 0.027(2) 0.036(2) 0.0116(18) 0.0066(19) 0.010(2) C5 0.030(3) 0.027(2) 0.042(3) 0.0142(19) 0.011(2) 0.005(2) C52 0.020(2) 0.044(3) 0.023(2) 0.0038(18) 0.0068(17) 0.0034(19) N9 0.029(2) 0.0221(17) 0.0339(19) 0.0121(14) 0.0117(15) 0.0065(15) C16 0.018(2) 0.037(2) 0.027(2) 0.0082(18) 0.0037(17) 0.0062(19) C1 0.025(2) 0.026(2) 0.040(2) 0.0046(18) 0.0098(19) 0.0104(19) C22 0.027(2) 0.034(2) 0.020(2) 0.0052(17) 0.0050(17) 0.0088(19) N12 0.0246(19) 0.0284(18) 0.0244(17) -0.0028(14) 0.0044(15) 0.0009(15) N6 0.0197(19) 0.050(2) 0.0211(17) 0.0025(15) 0.0034(14) 0.0113(17) C17 0.020(2) 0.037(2) 0.025(2) 0.0016(17) 0.0021(17) 0.0078(19) C12 0.039(3) 0.034(2) 0.057(3) 0.020(2) 0.023(2) 0.002(2) C18 0.020(2) 0.040(2) 0.023(2) -0.0016(18) -0.0039(17) 0.0085(19) C36 0.029(2) 0.027(2) 0.030(2) 0.0085(17) 0.0091(18) 0.0115(19) C2 0.028(2) 0.018(2) 0.037(2) 0.0015(17) 0.0072(19) 0.0052(18) C23 0.023(2) 0.055(3) 0.034(2) 0.005(2) 0.0025(19) 0.009(2) C20 0.032(3) 0.037(2) 0.019(2) 0.0008(17) 0.0017(18) 0.008(2) C50 0.026(2) 0.036(2) 0.031(2) 0.0026(19) -0.0023(19) 0.000(2) C8 0.044(3) 0.027(2) 0.054(3) 0.012(2) 0.019(2) 0.015(2) C42 0.044(3) 0.034(2) 0.050(3) 0.013(2) 0.018(2) 0.021(2) C48 0.038(3) 0.029(2) 0.025(2) -0.0021(17) 0.0018(19) 0.006(2) C21 0.027(2) 0.045(3) 0.021(2) 0.0111(18) 0.0072(17) 0.006(2) C6 0.028(2) 0.026(2) 0.034(2) 0.0098(18) 0.0066(18) 0.0038(19) C46 0.029(2) 0.037(2) 0.026(2) 0.0008(18) 0.0088(18) 0.010(2) C38 0.036(3) 0.045(3) 0.053(3) 0.025(2) 0.021(2) 0.007(2) C51 0.022(2) 0.034(2) 0.024(2) 0.0038(18) 0.0003(17) -0.0008(19) C32 0.026(2) 0.034(2) 0.030(2) 0.0155(18) 0.0123(18) 0.0048(19) C57 0.020(2) 0.054(3) 0.046(3) 0.006(2) 0.001(2) -0.003(2) C58 0.032(3) 0.080(4) 0.061(3) -0.005(3) 0.016(2) 0.016(3) C47 0.035(3) 0.039(2) 0.020(2) 0.0003(18) 0.0056(18) 0.006(2) C25 0.036(3) 0.042(3) 0.038(2) 0.010(2) 0.009(2) 0.020(2) C29 0.034(3) 0.048(3) 0.040(3) 0.023(2) 0.000(2) 0.003(2) C44 0.028(2) 0.037(2) 0.038(2) 0.0061(19) 0.0035(19) 0.009(2) C14 0.031(3) 0.030(2) 0.048(3) 0.007(2) 0.002(2) 0.006(2) C59 0.037(3) 0.035(2) 0.037(2) 0.0072(19) 0.003(2) 0.009(2) C53 0.045(3) 0.063(3) 0.030(2) -0.011(2) 0.008(2) 0.017(3) C40 0.044(3) 0.054(3) 0.024(2) 0.000(2) 0.009(2) 0.010(2) C27 0.045(3) 0.092(4) 0.023(2) 0.008(2) 0.012(2) 0.021(3) C55 0.041(3) 0.052(3) 0.029(2) 0.011(2) 0.011(2) 0.007(2) C10 0.051(3) 0.036(3) 0.040(3) 0.009(2) 0.011(2) 0.009(2) C24 0.034(3) 0.076(4) 0.061(3) 0.009(3) 0.022(2) 0.016(3) C39 0.043(3) 0.069(4) 0.069(3) 0.025(3) 0.033(3) 0.017(3) C43 0.060(4) 0.066(4) 0.086(4) 0.017(3) 0.043(3) 0.038(3) C13 0.051(4) 0.073(4) 0.082(4) 0.026(3) 0.038(3) 0.021(3) C54 0.046(3) 0.107(5) 0.050(3) -0.009(3) 0.016(3) 0.024(3) C26 0.090(4) 0.068(4) 0.050(3) 0.023(3) 0.012(3) 0.041(3) C45 0.058(3) 0.060(3) 0.044(3) 0.022(2) -0.006(2) 0.008(3) C9 0.058(4) 0.077(4) 0.078(4) 0.024(3) 0.036(3) 0.037(3) C15 0.062(4) 0.041(3) 0.084(4) -0.005(3) -0.013(3) 0.009(3) C30 0.070(4) 0.056(3) 0.073(4) 0.035(3) -0.008(3) 0.006(3) C60 0.086(5) 0.080(4) 0.053(3) 0.028(3) -0.007(3) 0.016(3) C41 0.090(5) 0.113(5) 0.036(3) 0.027(3) 0.006(3) 0.040(4) C11 0.101(5) 0.044(3) 0.059(3) -0.007(3) -0.013(3) -0.003(3) C56 0.079(4) 0.093(5) 0.053(3) 0.038(3) -0.001(3) 0.010(4) C28 0.052(4) 0.141(6) 0.051(3) 0.016(3) 0.031(3) 0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.0599(5) . ? Mo1 N7 2.133(3) . ? Mo1 N4 2.140(3) . ? Mo1 N1 2.156(3) . ? Mo1 N10 2.165(3) . ? Mo2 N8 2.137(3) . ? Mo2 N5 2.152(3) . ? Mo2 N2 2.158(3) . ? Mo2 N11 2.165(3) . ? N1 C4 1.332(5) . ? N1 C1 1.452(5) . ? N8 C34 1.341(5) . ? N8 C37 1.455(5) . ? N2 C4 1.331(5) . ? N2 C7 1.459(4) . ? N4 C19 1.335(4) . ? N4 C16 1.452(4) . ? N7 C34 1.329(5) . ? N7 C31 1.459(5) . ? N5 C19 1.326(4) . ? N5 C22 1.453(4) . ? N11 C49 1.333(5) . ? N11 C52 1.459(5) . ? C34 N9 1.393(4) . ? N10 C49 1.318(5) . ? N10 C46 1.458(5) . ? C37 C36 1.531(5) . ? C4 N3 1.406(4) . ? C35 N9 1.439(5) . ? C35 C36 1.520(5) . ? N3 C3 1.442(5) . ? N3 C5 1.451(5) . ? C7 C6 1.530(5) . ? C49 N12 1.403(4) . ? C19 N6 1.396(4) . ? C31 C32 1.529(5) . ? C33 N9 1.463(5) . ? C33 C32 1.516(5) . ? C3 C2 1.522(5) . ? C5 C6 1.514(5) . ? C52 C51 1.534(5) . ? C16 C17 1.535(5) . ? C1 C2 1.534(5) . ? C22 C21 1.522(5) . ? N12 C48 1.443(5) . ? N12 C50 1.452(5) . ? N6 C20 1.440(5) . ? N6 C18 1.444(5) . ? C17 C18 1.518(5) . ? C17 C25 1.528(5) . ? C17 C23 1.545(5) . ? C12 C13 1.505(6) . ? C12 C6 1.541(5) . ? C36 C42 1.528(5) . ? C36 C44 1.540(5) . ? C2 C8 1.529(5) . ? C2 C10 1.533(5) . ? C23 C24 1.511(6) . ? C20 C21 1.525(5) . ? C50 C51 1.527(6) . ? C8 C9 1.521(6) . ? C42 C43 1.515(6) . ? C48 C47 1.528(5) . ? C21 C29 1.534(5) . ? C21 C27 1.544(5) . ? C6 C14 1.530(5) . ? C46 C47 1.539(5) . ? C38 C39 1.514(6) . ? C38 C32 1.542(5) . ? C51 C57 1.533(5) . ? C51 C59 1.540(5) . ? C32 C40 1.536(5) . ? C57 C58 1.514(6) . ? C47 C53 1.528(6) . ? C47 C55 1.536(6) . ? C25 C26 1.527(5) . ? C29 C30 1.532(5) . ? C44 C45 1.518(5) . ? C14 C15 1.534(5) . ? C59 C60 1.510(5) . ? C53 C54 1.513(6) . ? C40 C41 1.514(6) . ? C27 C28 1.525(6) . ? C55 C56 1.516(6) . ? C10 C11 1.514(6) . ? 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 Mo2 Mo1 N7 93.38(8) . . ? Mo2 Mo1 N4 93.51(8) . . ? N7 Mo1 N4 90.18(11) . . ? Mo2 Mo1 N1 92.33(9) . . ? N7 Mo1 N1 174.27(12) . . ? N4 Mo1 N1 89.84(11) . . ? Mo2 Mo1 N10 92.73(9) . . ? N7 Mo1 N10 91.19(11) . . ? N4 Mo1 N10 173.51(12) . . ? N1 Mo1 N10 88.15(11) . . ? Mo1 Mo2 N8 92.48(8) . . ? Mo1 Mo2 N5 92.36(8) . . ? N8 Mo2 N5 92.53(11) . . ? Mo1 Mo2 N2 93.66(8) . . ? N8 Mo2 N2 173.69(12) . . ? N5 Mo2 N2 88.65(11) . . ? Mo1 Mo2 N11 92.94(9) . . ? N8 Mo2 N11 90.55(11) . . ? N5 Mo2 N11 173.74(12) . . ? N2 Mo2 N11 87.71(11) . . ? C4 N1 C1 120.3(3) . . ? C4 N1 Mo1 118.5(3) . . ? C1 N1 Mo1 121.1(2) . . ? C34 N8 C37 120.2(3) . . ? C34 N8 Mo2 118.6(2) . . ? C37 N8 Mo2 121.2(2) . . ? C4 N2 C7 121.3(3) . . ? C4 N2 Mo2 117.2(2) . . ? C7 N2 Mo2 121.5(2) . . ? C19 N4 C16 120.7(3) . . ? C19 N4 Mo1 117.5(3) . . ? C16 N4 Mo1 121.8(2) . . ? C34 N7 C31 119.6(3) . . ? C34 N7 Mo1 118.3(2) . . ? C31 N7 Mo1 122.0(2) . . ? C19 N5 C22 120.1(3) . . ? C19 N5 Mo2 118.2(2) . . ? C22 N5 Mo2 121.4(2) . . ? C49 N11 C52 121.3(3) . . ? C49 N11 Mo2 117.2(3) . . ? C52 N11 Mo2 120.5(2) . . ? N7 C34 N8 117.1(3) . . ? N7 C34 N9 121.5(3) . . ? N8 C34 N9 121.1(3) . . ? C49 N10 C46 122.1(3) . . ? C49 N10 Mo1 117.9(2) . . ? C46 N10 Mo1 119.4(2) . . ? N8 C37 C36 114.5(3) . . ? N2 C4 N1 118.3(3) . . ? N2 C4 N3 120.6(3) . . ? N1 C4 N3 120.9(4) . . ? N9 C35 C36 111.3(3) . . ? C4 N3 C3 119.4(3) . . ? C4 N3 C5 117.2(3) . . ? C3 N3 C5 115.9(3) . . ? N2 C7 C6 115.7(3) . . ? N10 C49 N11 118.2(3) . . ? N10 C49 N12 121.2(3) . . ? N11 C49 N12 120.5(4) . . ? N5 C19 N4 118.1(3) . . ? N5 C19 N6 121.8(3) . . ? N4 C19 N6 120.0(3) . . ? N7 C31 C32 114.6(3) . . ? N9 C33 C32 111.0(3) . . ? N3 C3 C2 111.5(3) . . ? N3 C5 C6 111.1(3) . . ? N11 C52 C51 116.1(3) . . ? C34 N9 C35 119.8(3) . . ? C34 N9 C33 119.3(3) . . ? C35 N9 C33 115.9(3) . . ? N4 C16 C17 114.4(3) . . ? N1 C1 C2 113.9(3) . . ? N5 C22 C21 114.2(3) . . ? C49 N12 C48 115.9(3) . . ? C49 N12 C50 117.4(3) . . ? C48 N12 C50 115.4(3) . . ? C19 N6 C20 119.8(3) . . ? C19 N6 C18 119.8(3) . . ? C20 N6 C18 116.8(3) . . ? C18 C17 C25 111.8(3) . . ? C18 C17 C16 105.7(3) . . ? C25 C17 C16 109.4(3) . . ? C18 C17 C23 107.8(3) . . ? C25 C17 C23 112.7(3) . . ? C16 C17 C23 109.2(3) . . ? C13 C12 C6 116.2(4) . . ? N6 C18 C17 110.7(3) . . ? C35 C36 C42 107.7(3) . . ? C35 C36 C37 106.0(3) . . ? C42 C36 C37 110.9(3) . . ? C35 C36 C44 111.7(3) . . ? C42 C36 C44 112.6(3) . . ? C37 C36 C44 107.7(3) . . ? C3 C2 C8 107.1(3) . . ? C3 C2 C10 111.4(3) . . ? C8 C2 C10 113.3(3) . . ? C3 C2 C1 105.3(3) . . ? C8 C2 C1 111.6(3) . . ? C10 C2 C1 108.0(3) . . ? C24 C23 C17 116.3(3) . . ? N6 C20 C21 111.6(3) . . ? N12 C50 C51 110.0(3) . . ? C9 C8 C2 116.3(4) . . ? C43 C42 C36 116.7(4) . . ? N12 C48 C47 110.5(3) . . ? C22 C21 C20 105.7(3) . . ? C22 C21 C29 108.4(3) . . ? C20 C21 C29 111.7(3) . . ? C22 C21 C27 110.8(4) . . ? C20 C21 C27 106.6(3) . . ? C29 C21 C27 113.4(4) . . ? C5 C6 C14 111.4(3) . . ? C5 C6 C7 105.7(3) . . ? C14 C6 C7 108.7(3) . . ? C5 C6 C12 107.8(3) . . ? C14 C6 C12 112.8(4) . . ? C7 C6 C12 110.3(3) . . ? N10 C46 C47 115.8(3) . . ? C39 C38 C32 115.6(4) . . ? C50 C51 C57 108.4(3) . . ? C50 C51 C52 104.6(3) . . ? C57 C51 C52 110.1(3) . . ? C50 C51 C59 110.8(3) . . ? C57 C51 C59 112.2(3) . . ? C52 C51 C59 110.5(3) . . ? C33 C32 C31 105.9(3) . . ? C33 C32 C40 110.8(3) . . ? C31 C32 C40 109.5(3) . . ? C33 C32 C38 107.8(3) . . ? C31 C32 C38 110.2(3) . . ? C40 C32 C38 112.4(3) . . ? C58 C57 C51 114.9(4) . . ? C53 C47 C48 109.3(3) . . ? C53 C47 C55 112.5(3) . . ? C48 C47 C55 110.3(4) . . ? C53 C47 C46 109.8(3) . . ? C48 C47 C46 105.3(3) . . ? C55 C47 C46 109.4(3) . . ? C26 C25 C17 116.2(3) . . ? C30 C29 C21 116.8(4) . . ? C45 C44 C36 117.2(3) . . ? C6 C14 C15 115.2(3) . . ? C60 C59 C51 116.2(4) . . ? C54 C53 C47 115.7(4) . . ? C41 C40 C32 116.1(4) . . ? C28 C27 C21 115.3(4) . . ? C56 C55 C47 116.0(4) . . ? C11 C10 C2 115.8(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.906 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.085 #===END of CIF for Compound 4 ============================= data_5twoDMSO _database_code_depnum_ccdc_archive 'CCDC 645816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H112 N12 Mo2, C32 H12 B F24, 2(C2 H6 O S)' _chemical_formula_sum 'C96 H136 B F24 Mo2 N12 O2 S2' _chemical_formula_weight 2212.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 21.2869(10) _cell_length_b 21.2869(10) _cell_length_c 23.846(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10805.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6044 _cell_measurement_theta_min 2.3035 _cell_measurement_theta_max 24.982 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4596 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8836 _exptl_absorpt_correction_T_max 0.9409 _exptl_absorpt_process_details SADABS _exptl_special_details ; Not all hydrogen atoms were included in refinement because of disorder. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32124 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9533 _reflns_number_gt 4728 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+33.7395P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9533 _refine_ls_number_parameters 818 _refine_ls_number_restraints 236 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.2447 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.010 _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 0.2500 0.2500 0.42935(5) 0.0572(4) Uani 1 4 d S . . Mo2 Mo 0.2500 0.2500 0.34066(5) 0.0542(3) Uani 1 4 d S . . N1 N 0.3141(2) 0.3270(2) 0.4322(2) 0.0554(14) Uani 1 1 d . . . N2 N 0.3150(2) 0.3254(2) 0.3362(2) 0.0523(13) Uani 1 1 d . . . N3 N 0.3745(3) 0.4020(3) 0.3828(2) 0.0631(15) Uani 1 1 d . . . C1 C 0.3356(3) 0.3510(3) 0.3845(3) 0.0548(16) Uani 1 1 d . . . C2 C 0.3356(4) 0.3533(3) 0.4855(3) 0.069(2) Uani 1 1 d . A . H2A H 0.3713 0.3284 0.4989 0.083 Uiso 1 1 calc R . . H2B H 0.3018 0.3492 0.5131 0.083 Uiso 1 1 calc R . . C3 C 0.3553(4) 0.4214(4) 0.4826(3) 0.076(2) Uani 1 1 d D . . C4 C 0.4013(4) 0.4265(4) 0.4341(3) 0.081(2) Uani 1 1 d . A . H4A H 0.4129 0.4707 0.4286 0.097 Uiso 1 1 calc R . . H4B H 0.4396 0.4031 0.4431 0.097 Uiso 1 1 calc R . . C5 C 0.4029(3) 0.4234(4) 0.3309(3) 0.071(2) Uani 1 1 d . . . H5A H 0.4414 0.3995 0.3239 0.085 Uiso 1 1 calc R . . H5B H 0.4143 0.4678 0.3345 0.085 Uiso 1 1 calc R . . C6 C 0.3587(3) 0.4155(3) 0.2816(3) 0.0599(18) Uani 1 1 d . . . C7 C 0.3387(3) 0.3474(3) 0.2826(3) 0.0617(18) Uani 1 1 d . . . H7A H 0.3059 0.3412 0.2543 0.074 Uiso 1 1 calc R . . H7B H 0.3747 0.3213 0.2719 0.074 Uiso 1 1 calc R . . C8 C 0.3981(8) 0.4378(18) 0.5329(6) 0.090(6) Uani 0.546(13) 1 d PD A 1 H8A H 0.4358 0.4114 0.5318 0.109 Uiso 0.546(13) 1 calc PR A 1 H8B H 0.4114 0.4818 0.5301 0.109 Uiso 0.546(13) 1 calc PR A 1 C9 C 0.3645(12) 0.4277(17) 0.5879(7) 0.237(13) Uani 0.546(13) 1 d PD A 1 H9A H 0.3927 0.4372 0.6187 0.356 Uiso 0.546(13) 1 calc PR A 1 H9B H 0.3509 0.3843 0.5906 0.356 Uiso 0.546(13) 1 calc PR A 1 H9C H 0.3281 0.4551 0.5898 0.356 Uiso 0.546(13) 1 calc PR A 1 C8B C 0.3714(10) 0.445(2) 0.5417(7) 0.090(6) Uani 0.454(13) 1 d PD A 2 H8BA H 0.3518 0.4858 0.5472 0.109 Uiso 0.454(13) 1 calc PR A 2 H8BB H 0.3526 0.4156 0.5689 0.109 Uiso 0.454(13) 1 calc PR A 2 C9B C 0.4402(10) 0.450(2) 0.5546(11) 0.237(13) Uani 0.454(13) 1 d PD A 2 H9BA H 0.4456 0.4725 0.5899 0.356 Uiso 0.454(13) 1 calc PR A 2 H9BB H 0.4608 0.4737 0.5249 0.356 Uiso 0.454(13) 1 calc PR A 2 H9BC H 0.4586 0.4089 0.5575 0.356 Uiso 0.454(13) 1 calc PR A 2 C10 C 0.2965(5) 0.4608(4) 0.4705(4) 0.097(3) Uani 1 1 d D A . C11 C 0.3027(8) 0.5292(5) 0.4566(6) 0.131(5) Uani 0.729(11) 1 d PD A 1 H11A H 0.2613 0.5470 0.4506 0.196 Uiso 0.729(11) 1 calc PR A 1 H11B H 0.3277 0.5340 0.4229 0.196 Uiso 0.729(11) 1 calc PR A 1 H11C H 0.3231 0.5508 0.4875 0.196 Uiso 0.729(11) 1 calc PR A 1 C11B C 0.2563(17) 0.4780(17) 0.5204(11) 0.131(5) Uani 0.271(11) 1 d PD A 2 H11D H 0.2202 0.5020 0.5079 0.196 Uiso 0.271(11) 1 calc PR A 2 H11E H 0.2808 0.5031 0.5465 0.196 Uiso 0.271(11) 1 calc PR A 2 H11F H 0.2421 0.4400 0.5390 0.196 Uiso 0.271(11) 1 calc PR A 2 C12 C 0.3946(4) 0.4314(4) 0.2283(3) 0.078(2) Uani 1 1 d . . . H12A H 0.4310 0.4033 0.2258 0.093 Uiso 1 1 calc R . . H12B H 0.4107 0.4744 0.2319 0.093 Uiso 1 1 calc R . . C13 C 0.3579(4) 0.4270(5) 0.1729(3) 0.105(3) Uani 1 1 d . . . H13A H 0.3853 0.4380 0.1420 0.158 Uiso 1 1 calc R . . H13B H 0.3226 0.4557 0.1739 0.158 Uiso 1 1 calc R . . H13C H 0.3427 0.3844 0.1679 0.158 Uiso 1 1 calc R . . C14 C 0.3005(4) 0.4573(3) 0.2883(3) 0.072(2) Uani 1 1 d . . . H14A H 0.2713 0.4478 0.2577 0.086 Uiso 1 1 calc R . . H14B H 0.2796 0.4459 0.3235 0.086 Uiso 1 1 calc R . . C15 C 0.3119(5) 0.5277(4) 0.2888(4) 0.110(3) Uani 1 1 d . . . H15A H 0.2723 0.5495 0.2935 0.166 Uiso 1 1 calc R . . H15B H 0.3311 0.5403 0.2537 0.166 Uiso 1 1 calc R . . H15C H 0.3397 0.5383 0.3197 0.166 Uiso 1 1 calc R . . Mo3 Mo 0.2500 0.7500 1.04437(4) 0.0574(3) Uani 1 2 d S . . N4 N 0.1852(2) 0.6739(2) 1.0476(2) 0.0561(14) Uani 1 1 d . . . N5 N 0.1859(2) 0.6736(2) 0.9514(2) 0.0558(13) Uani 1 1 d . . . N6 N 0.1244(3) 0.5987(3) 0.9997(2) 0.0658(16) Uani 1 1 d . . . C16 C 0.1639(3) 0.6498(3) 0.9991(3) 0.0592(18) Uani 1 1 d . . . C17 C 0.1581(4) 0.6537(3) 1.1007(3) 0.073(2) Uani 1 1 d . . . H17A H 0.1214 0.6799 1.1088 0.087 Uiso 1 1 calc R . . H17B H 0.1889 0.6608 1.1306 0.087 Uiso 1 1 calc R . . C18 C 0.1383(4) 0.5852(4) 1.1018(3) 0.078(2) Uani 1 1 d . B . C19 C 0.0961(3) 0.5760(4) 1.0514(3) 0.082(2) Uani 1 1 d . . . H19A H 0.0866 0.5312 1.0474 0.098 Uiso 1 1 calc R . . H19B H 0.0564 0.5982 1.0577 0.098 Uiso 1 1 calc R . . C20 C 0.0941(3) 0.5786(4) 0.9482(3) 0.076(2) Uani 1 1 d . . . H20A H 0.0570 0.6048 0.9414 0.092 Uiso 1 1 calc R . . H20B H 0.0800 0.5350 0.9523 0.092 Uiso 1 1 calc R . . C21 C 0.1384(3) 0.5834(3) 0.8982(3) 0.0627(18) Uani 1 1 d . C . C22 C 0.1620(3) 0.6508(3) 0.8981(3) 0.0659(19) Uani 1 1 d . . . H22A H 0.1954 0.6544 0.8700 0.079 Uiso 1 1 calc R . . H22B H 0.1275 0.6782 0.8862 0.079 Uiso 1 1 calc R . . C23 C 0.0978(5) 0.5723(5) 1.1550(4) 0.125(4) Uani 1 1 d D . . C24 C 0.1344(7) 0.5758(8) 1.2101(5) 0.154(7) Uani 0.759(11) 1 d PD B 1 H24A H 0.1066 0.5661 1.2411 0.231 Uiso 0.759(11) 1 calc PR B 1 H24B H 0.1512 0.6178 1.2148 0.231 Uiso 0.759(11) 1 calc PR B 1 H24C H 0.1686 0.5458 1.2092 0.231 Uiso 0.759(11) 1 calc PR B 1 C24B C 0.0437(15) 0.5268(16) 1.1524(17) 0.14(2) Uani 0.241(11) 1 d PD B 2 H24D H 0.0255 0.5222 1.1894 0.211 Uiso 0.241(11) 1 calc PR B 2 H24E H 0.0588 0.4863 1.1394 0.211 Uiso 0.241(11) 1 calc PR B 2 H24F H 0.0122 0.5425 1.1266 0.211 Uiso 0.241(11) 1 calc PR B 2 C25 C 0.1980(4) 0.5450(4) 1.0963(4) 0.094(3) Uani 1 1 d D . . C26 C 0.1920(6) 0.4744(4) 1.1008(8) 0.157(8) Uani 0.759(11) 1 d PD B 1 H26A H 0.2333 0.4554 1.0978 0.235 Uiso 0.759(11) 1 calc PR B 1 H26B H 0.1654 0.4590 1.0707 0.235 Uiso 0.759(11) 1 calc PR B 1 H26C H 0.1735 0.4635 1.1366 0.235 Uiso 0.759(11) 1 calc PR B 1 C26B C 0.2229(17) 0.540(2) 1.1550(8) 0.121(17) Uani 0.241(11) 1 d PD B 2 H26D H 0.2607 0.5144 1.1550 0.182 Uiso 0.241(11) 1 calc PR B 2 H26E H 0.1915 0.5204 1.1788 0.182 Uiso 0.241(11) 1 calc PR B 2 H26F H 0.2327 0.5815 1.1692 0.182 Uiso 0.241(11) 1 calc PR B 2 C27 C 0.1005(4) 0.5710(4) 0.8438(4) 0.084(2) Uani 1 1 d D . . C28 C 0.1368(8) 0.5726(8) 0.7921(7) 0.093(4) Uani 0.469(10) 1 d PD C 1 H28A H 0.1094 0.5637 0.7606 0.140 Uiso 0.469(10) 1 calc PR C 1 H28B H 0.1698 0.5413 0.7938 0.140 Uiso 0.469(10) 1 calc PR C 1 H28C H 0.1553 0.6139 0.7875 0.140 Uiso 0.469(10) 1 calc PR C 1 C28A C 0.0705(7) 0.5098(6) 0.8396(7) 0.093(4) Uani 0.531(10) 1 d PD C 2 H28D H 0.0492 0.5064 0.8038 0.140 Uiso 0.531(10) 1 calc PR C 2 H28E H 0.0403 0.5052 0.8697 0.140 Uiso 0.531(10) 1 calc PR C 2 H28F H 0.1021 0.4771 0.8425 0.140 Uiso 0.531(10) 1 calc PR C 2 C29 C 0.1940(3) 0.5382(3) 0.9062(3) 0.071(2) Uani 1 1 d D . . C30 C 0.1826(9) 0.4714(6) 0.9082(8) 0.097(4) Uani 0.462(9) 1 d PD C 1 H30A H 0.2223 0.4493 0.9122 0.145 Uiso 0.462(9) 1 calc PR C 1 H30B H 0.1622 0.4582 0.8738 0.145 Uiso 0.462(9) 1 calc PR C 1 H30C H 0.1558 0.4617 0.9399 0.145 Uiso 0.462(9) 1 calc PR C 1 C30A C 0.2318(7) 0.5272(7) 0.8567(6) 0.097(4) Uani 0.538(9) 1 d PD C 2 H30D H 0.2650 0.4977 0.8655 0.145 Uiso 0.538(9) 1 calc PR C 2 H30E H 0.2500 0.5666 0.8443 0.145 Uiso 0.538(9) 1 calc PR C 2 H30F H 0.2055 0.5101 0.8272 0.145 Uiso 0.538(9) 1 calc PR C 2 B1 B 0.2500 0.2500 0.8576(7) 0.054(4) Uani 1 4 d S . . C31 C 0.2326(4) 0.3087(3) 0.9025(3) 0.058(2) Uani 0.522(2) 1 d PGD D 1 C32 C 0.1715(3) 0.3165(4) 0.9219(4) 0.057(2) Uani 0.522(2) 1 d PGD D 1 C33 C 0.1588(3) 0.3604(4) 0.9636(4) 0.068(3) Uani 0.522(2) 1 d PGD D 1 C34 C 0.2071(4) 0.3965(4) 0.9858(3) 0.075(3) Uani 0.522(2) 1 d PGD D 1 C35 C 0.2682(4) 0.3888(4) 0.9663(4) 0.069(3) Uani 0.522(2) 1 d PGD D 1 C36 C 0.2809(3) 0.3449(4) 0.9247(4) 0.059(3) Uani 0.522(2) 1 d PGD D 1 C37 C 0.3186(5) 0.4286(5) 0.9892(5) 0.081(5) Uani 0.522(2) 1 d PD . . F1 F 0.3401(17) 0.4023(19) 1.0356(10) 0.142(8) Uani 0.2610(11) 1 d PD D -1 F2 F 0.3671(13) 0.4321(14) 0.9543(13) 0.144(7) Uani 0.2610(11) 1 d PD D -1 F3 F 0.3043(17) 0.4874(7) 1.0020(14) 0.139(6) Uani 0.2610(11) 1 d PD D -1 F1A F 0.3567(15) 0.3931(18) 1.0194(12) 0.142(8) Uani 0.2610(11) 1 d PD D -2 F2A F 0.3532(14) 0.4548(13) 0.9497(12) 0.144(7) Uani 0.2610(11) 1 d PD D -2 F3A F 0.2991(17) 0.4740(9) 1.0224(13) 0.139(6) Uani 0.2610(11) 1 d PD D -2 C38 C 0.0940(4) 0.3688(5) 0.9841(5) 0.072(4) Uani 0.522(2) 1 d PD . . F4 F 0.0553(11) 0.3212(9) 0.9757(12) 0.176(9) Uani 0.2610(11) 1 d PD D -1 F5 F 0.0934(10) 0.3787(13) 1.0387(6) 0.115(4) Uani 0.2610(11) 1 d PD D -1 F6 F 0.0659(9) 0.4183(9) 0.9620(11) 0.138(7) Uani 0.2610(11) 1 d PD D -1 F4A F 0.0748(14) 0.3218(9) 1.0160(11) 0.176(9) Uani 0.2610(11) 1 d PD D -2 F5A F 0.0830(9) 0.4202(8) 1.0131(10) 0.115(4) Uani 0.2610(11) 1 d PD D -2 F6A F 0.0542(10) 0.3705(13) 0.9415(8) 0.138(7) Uani 0.2610(11) 1 d PD D -2 C39 C 0.2313(4) 0.3101(3) 0.8154(3) 0.058(2) Uani 0.478(2) 1 d PG D 2 C40 C 0.1697(3) 0.3178(4) 0.7974(4) 0.057(2) Uani 0.478(2) 1 d PG D 2 C41 C 0.1549(3) 0.3656(4) 0.7599(4) 0.068(3) Uani 0.478(2) 1 d PGD D 2 C42 C 0.2016(4) 0.4056(4) 0.7404(4) 0.075(3) Uani 0.478(2) 1 d PG D 2 C43 C 0.2632(4) 0.3978(4) 0.7584(4) 0.069(3) Uani 0.478(2) 1 d PGD D 2 C44 C 0.2781(3) 0.3501(4) 0.7959(4) 0.059(3) Uani 0.478(2) 1 d PG D 2 C46 C 0.3136(5) 0.4404(5) 0.7394(6) 0.072(4) Uani 0.478(2) 1 d PD . . F7 F 0.3394(13) 0.4697(13) 0.7827(9) 0.142(8) Uani 0.2390(11) 1 d PD D -1 F8 F 0.3604(10) 0.4113(13) 0.7142(12) 0.144(7) Uani 0.2390(11) 1 d PD D -1 F9 F 0.2957(11) 0.4855(9) 0.7050(10) 0.139(6) Uani 0.2390(11) 1 d PD D -1 F7A F 0.3738(7) 0.4322(14) 0.7491(13) 0.142(8) Uani 0.2390(11) 1 d PD D -2 F8A F 0.3069(12) 0.4348(15) 0.6843(7) 0.144(7) Uani 0.2390(11) 1 d PD D -2 F9A F 0.3023(11) 0.5005(7) 0.7499(13) 0.139(6) Uani 0.2390(11) 1 d PD D -2 C45 C 0.0886(5) 0.3730(5) 0.7431(6) 0.081(5) Uani 0.478(2) 1 d PD . . F10 F 0.0810(15) 0.3381(11) 0.6980(10) 0.176(9) Uani 0.2390(11) 1 d PD D -1 F11 F 0.0679(11) 0.4294(7) 0.7280(10) 0.115(4) Uani 0.2390(11) 1 d PD D -1 F12 F 0.0454(10) 0.3529(10) 0.7787(10) 0.138(7) Uani 0.2390(11) 1 d PD D -1 F10A F 0.0546(13) 0.3294(11) 0.7178(12) 0.176(9) Uani 0.2390(11) 1 d PD D -2 F11A F 0.0858(10) 0.4219(8) 0.7090(9) 0.115(4) Uani 0.2390(11) 1 d PD D -2 F12A F 0.0542(10) 0.3895(10) 0.7869(8) 0.138(7) Uani 0.2390(11) 1 d PD D -2 B2 B 0.7500 0.2500 0.5000 0.21(2) Uani 1 4 d SD . . C51 C 0.7783(15) 0.1966(10) 0.4567(9) 0.175(8) Uani 0.264(10) 1 d PD E 1 C52 C 0.7270(14) 0.158(2) 0.445(2) 0.193(9) Uani 0.264(10) 1 d PD E 1 C53 C 0.7322(16) 0.111(2) 0.405(3) 0.185(8) Uani 0.264(10) 1 d PD . 1 C54 C 0.789(2) 0.100(2) 0.379(2) 0.197(9) Uani 0.264(10) 1 d PD E 1 C55 C 0.8402(18) 0.139(2) 0.390(2) 0.184(8) Uani 0.264(10) 1 d PD . 1 C56 C 0.8362(14) 0.1836(19) 0.432(2) 0.193(8) Uani 0.264(10) 1 d PD E 1 C57 C 0.6968(19) 0.070(2) 0.3670(18) 0.267(18) Uani 0.264(10) 1 d PD . . F13 F 0.699(3) 0.046(3) 0.3158(18) 0.341(18) Uani 0.132(5) 1 d PD . -1 F14 F 0.637(2) 0.053(3) 0.367(4) 0.288(15) Uani 0.132(5) 1 d PD . -1 F15 F 0.708(3) 0.012(3) 0.384(4) 0.255(9) Uani 0.132(5) 1 d PD . -1 F13A F 0.673(4) 0.062(3) 0.316(2) 0.341(18) Uani 0.132(5) 1 d PD . -2 F14A F 0.638(3) 0.079(3) 0.383(4) 0.288(15) Uani 0.132(5) 1 d PD . -2 F15A F 0.685(4) 0.0091(19) 0.374(4) 0.255(9) Uani 0.132(5) 1 d PD . -2 C58 C 0.8913(13) 0.1272(17) 0.3491(12) 0.198(12) Uani 0.264(10) 1 d PD . . F16 F 0.942(3) 0.131(4) 0.381(3) 0.148(5) Uani 0.132(5) 1 d PD . -1 F17 F 0.906(4) 0.075(2) 0.323(3) 0.200(9) Uani 0.132(5) 1 d PD . -1 F18 F 0.909(4) 0.167(3) 0.309(2) 0.196(9) Uani 0.132(5) 1 d PD E -1 F16A F 0.944(3) 0.148(4) 0.372(3) 0.148(5) Uani 0.132(5) 1 d PDU . -2 F17A F 0.911(5) 0.069(2) 0.338(3) 0.200(9) Uani 0.132(5) 1 d PD . -2 F18A F 0.900(4) 0.151(3) 0.2984(15) 0.196(9) Uani 0.132(5) 1 d PD E -2 C51B C 0.7407(6) 0.3093(3) 0.4559(3) 0.175(8) Uani 0.736(10) 1 d PGD E 2 C52B C 0.7877(4) 0.3492(7) 0.4366(8) 0.193(9) Uani 0.736(10) 1 d PGD E 2 C53B C 0.7731(8) 0.3973(7) 0.3994(8) 0.185(8) Uani 0.736(10) 1 d PGD . 2 C54B C 0.7116(10) 0.4055(6) 0.3814(5) 0.197(9) Uani 0.736(10) 1 d PG E 2 C55B C 0.6646(7) 0.3656(8) 0.4006(8) 0.184(8) Uani 0.736(10) 1 d PGD . 2 C56B C 0.6791(5) 0.3175(6) 0.4378(7) 0.193(8) Uani 0.736(10) 1 d PGD E 2 C57B C 0.8264(6) 0.4369(7) 0.3819(8) 0.267(18) Uani 0.736(10) 1 d PD . . F13B F 0.8619(17) 0.3967(9) 0.3542(18) 0.341(18) Uani 0.368(5) 1 d PD . -1 F14B F 0.8682(17) 0.4551(10) 0.4197(16) 0.288(15) Uani 0.368(5) 1 d PD E -1 F15B F 0.8021(12) 0.4925(9) 0.3703(11) 0.255(9) Uani 0.368(5) 1 d PD . -1 F13C F 0.8518(18) 0.4252(12) 0.3325(12) 0.341(18) Uani 0.368(5) 1 d PD . -2 F14C F 0.8767(14) 0.4278(11) 0.4134(19) 0.288(15) Uani 0.368(5) 1 d PD E -2 F15C F 0.8270(12) 0.4987(7) 0.3801(11) 0.255(9) Uani 0.368(5) 1 d PD . -2 C58B C 0.5983(6) 0.3770(5) 0.3855(6) 0.198(12) Uani 0.736(10) 1 d PD . . F16B F 0.5593(10) 0.3702(10) 0.4285(8) 0.148(5) Uani 0.368(5) 1 d PD E -1 F17B F 0.5785(18) 0.4273(13) 0.3579(14) 0.200(9) Uani 0.368(5) 1 d PD . -1 F18B F 0.5881(13) 0.3283(12) 0.3522(12) 0.196(9) Uani 0.368(5) 1 d PD . -1 F16C F 0.5646(10) 0.4016(10) 0.4266(8) 0.148(5) Uani 0.368(5) 1 d PD E -2 F17C F 0.602(2) 0.4210(13) 0.3464(11) 0.200(9) Uani 0.368(5) 1 d PD . -2 F18C F 0.5640(12) 0.3311(15) 0.3639(17) 0.196(9) Uani 0.368(5) 1 d PD . -2 O1 O 0.2500 0.2500 0.5502(4) 0.085(3) Uani 1 4 d SD . . S1 S 0.2779(4) 0.2552(15) 0.6075(3) 0.097(4) Uani 0.25 1 d PD . . C1S C 0.2345(15) 0.3145(13) 0.6465(11) 0.181(12) Uani 0.50 1 d PD . . O2 O 0.2500 0.7500 0.1736(5) 0.151(4) Uani 1 2 d SD . . S2 S 0.2283(3) 0.7378(3) 0.2322(4) 0.156(3) Uani 0.50 1 d PD . . C2S C 0.2259(9) 0.8059(7) 0.2777(8) 0.260(10) Uani 1 1 d D . . S3 S 0.2528(16) 0.2762(12) 0.1314(7) 0.171(16) Uani 0.25 1 d PD . . O3 O 0.2500 0.2500 0.1894(8) 0.171(7) Uani 1 4 d SD . . C3S C 0.1891(12) 0.2443(17) 0.0894(16) 0.224(18) Uani 0.50 1 d PD . . 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 0.0581(5) 0.0581(5) 0.0555(7) 0.000 0.000 0.000 Mo2 0.0546(5) 0.0546(5) 0.0533(7) 0.000 0.000 0.000 N1 0.060(3) 0.059(3) 0.047(3) 0.002(3) -0.006(3) -0.003(3) N2 0.057(3) 0.057(3) 0.044(3) 0.001(3) 0.003(3) -0.002(3) N3 0.060(4) 0.074(4) 0.055(3) -0.004(3) 0.000(3) -0.016(3) C1 0.049(4) 0.056(4) 0.059(4) -0.002(3) -0.004(3) 0.001(3) C2 0.083(5) 0.069(5) 0.057(4) 0.006(4) -0.016(4) -0.011(4) C3 0.094(6) 0.085(6) 0.047(4) -0.003(4) -0.004(4) -0.020(5) C4 0.075(5) 0.101(6) 0.067(5) -0.004(4) -0.016(4) -0.020(5) C5 0.057(4) 0.075(5) 0.081(5) -0.006(4) 0.000(4) -0.017(4) C6 0.059(4) 0.062(4) 0.059(4) -0.005(3) 0.009(3) -0.009(3) C7 0.062(4) 0.064(4) 0.059(4) -0.002(3) 0.001(3) -0.005(3) C8 0.085(16) 0.127(12) 0.060(8) -0.028(7) 0.015(9) -0.046(16) C9 0.21(2) 0.42(4) 0.084(13) -0.095(19) -0.046(13) -0.04(3) C8B 0.085(16) 0.127(12) 0.060(8) -0.028(7) 0.015(9) -0.046(16) C9B 0.21(2) 0.42(4) 0.084(13) -0.095(19) -0.046(13) -0.04(3) C10 0.138(8) 0.077(6) 0.078(6) -0.001(5) 0.014(6) 0.024(6) C11 0.183(15) 0.096(10) 0.113(11) -0.008(8) 0.001(10) 0.020(10) C11B 0.183(15) 0.096(10) 0.113(11) -0.008(8) 0.001(10) 0.020(10) C12 0.072(5) 0.086(6) 0.076(5) -0.003(4) 0.014(4) -0.017(4) C13 0.120(8) 0.119(8) 0.075(6) 0.005(5) 0.003(5) -0.038(6) C14 0.076(5) 0.072(5) 0.068(5) 0.006(4) 0.002(4) -0.002(4) C15 0.138(9) 0.063(5) 0.130(8) 0.007(5) 0.028(7) 0.008(5) Mo3 0.0478(5) 0.0509(5) 0.0734(6) 0.000 0.000 0.0005(4) N4 0.044(3) 0.049(3) 0.075(4) 0.002(3) 0.009(3) 0.000(2) N5 0.054(3) 0.045(3) 0.068(4) 0.004(3) -0.007(3) -0.003(3) N6 0.054(3) 0.066(4) 0.078(4) 0.005(3) -0.003(3) -0.014(3) C16 0.047(4) 0.048(4) 0.082(5) 0.005(4) -0.007(4) 0.005(3) C17 0.070(5) 0.063(5) 0.085(5) 0.000(4) 0.021(4) -0.006(4) C18 0.069(5) 0.080(5) 0.085(6) -0.003(4) 0.013(4) -0.022(4) C19 0.059(5) 0.088(6) 0.098(6) 0.002(5) 0.017(5) -0.025(4) C20 0.053(4) 0.072(5) 0.104(6) 0.003(5) -0.010(4) -0.009(4) C21 0.056(4) 0.051(4) 0.081(5) 0.009(4) -0.017(4) -0.007(3) C22 0.061(4) 0.053(4) 0.084(5) 0.007(4) -0.015(4) 0.002(3) C23 0.148(10) 0.148(10) 0.079(7) 0.005(6) 0.030(7) -0.078(8) C24 0.199(18) 0.170(15) 0.094(11) 0.008(10) 0.025(11) -0.081(13) C24B 0.25(6) 0.08(3) 0.09(3) 0.02(2) 0.01(3) 0.01(4) C25 0.101(7) 0.061(5) 0.119(7) 0.010(5) -0.007(6) 0.007(5) C26 0.091(10) 0.081(9) 0.30(2) 0.041(12) -0.021(12) 0.008(7) C26B 0.07(3) 0.16(4) 0.13(4) -0.01(3) 0.01(2) 0.03(3) C27 0.087(6) 0.075(5) 0.089(6) 0.006(5) -0.031(5) -0.019(4) C28 0.094(9) 0.082(8) 0.103(10) 0.000(7) -0.040(8) -0.008(7) C28A 0.094(9) 0.082(8) 0.103(10) 0.000(7) -0.040(8) -0.008(7) C29 0.067(5) 0.059(5) 0.086(5) -0.002(4) -0.006(4) 0.013(4) C30 0.091(9) 0.082(9) 0.117(10) -0.017(7) -0.030(8) 0.009(7) C30A 0.091(9) 0.082(9) 0.117(10) -0.017(7) -0.030(8) 0.009(7) B1 0.043(5) 0.043(5) 0.076(10) 0.000 0.000 0.000 C31 0.053(5) 0.048(5) 0.073(6) 0.000(4) -0.001(5) 0.006(4) C32 0.051(6) 0.048(6) 0.071(6) 0.002(5) 0.002(5) -0.001(5) C33 0.061(6) 0.061(6) 0.083(7) 0.009(5) -0.005(5) 0.006(5) C34 0.078(7) 0.058(6) 0.091(8) 0.012(6) -0.005(6) 0.004(6) C35 0.062(6) 0.056(6) 0.089(7) 0.007(5) -0.007(5) 0.003(5) C36 0.052(6) 0.045(6) 0.079(7) 0.004(5) 0.000(5) 0.002(5) C37 0.073(10) 0.061(8) 0.110(10) -0.009(8) -0.028(9) 0.032(7) F1 0.110(16) 0.140(15) 0.176(15) 0.021(12) -0.042(11) -0.036(10) F2 0.123(14) 0.164(17) 0.144(11) -0.013(11) -0.012(9) -0.082(12) F3 0.104(8) 0.088(8) 0.23(2) -0.040(10) 0.002(10) -0.024(7) F1A 0.110(16) 0.140(15) 0.176(15) 0.021(12) -0.042(11) -0.036(10) F2A 0.123(14) 0.164(17) 0.144(11) -0.013(11) -0.012(9) -0.082(12) F3A 0.104(8) 0.088(8) 0.23(2) -0.040(10) 0.002(10) -0.024(7) C38 0.068(8) 0.057(7) 0.091(9) 0.034(7) 0.019(7) -0.006(6) F4 0.114(17) 0.095(12) 0.32(3) -0.015(14) 0.047(16) 0.030(10) F5 0.066(7) 0.111(9) 0.168(13) 0.015(8) 0.002(7) 0.023(6) F6 0.057(7) 0.111(13) 0.245(16) 0.077(13) 0.010(8) 0.013(9) F4A 0.114(17) 0.095(12) 0.32(3) -0.015(14) 0.047(16) 0.030(10) F5A 0.066(7) 0.111(9) 0.168(13) 0.015(8) 0.002(7) 0.023(6) F6A 0.057(7) 0.111(13) 0.245(16) 0.077(13) 0.010(8) 0.013(9) C39 0.053(5) 0.048(5) 0.073(6) 0.000(4) -0.001(5) 0.006(4) C40 0.051(6) 0.048(6) 0.071(6) 0.002(5) 0.002(5) -0.001(5) C41 0.061(6) 0.061(6) 0.083(7) 0.009(5) -0.005(5) 0.006(5) C42 0.078(7) 0.058(6) 0.091(8) 0.012(6) -0.005(6) 0.004(6) C43 0.062(6) 0.056(6) 0.089(7) 0.007(5) -0.007(5) 0.003(5) C44 0.052(6) 0.045(6) 0.079(7) 0.004(5) 0.000(5) 0.002(5) C46 0.068(8) 0.057(7) 0.091(9) 0.034(7) 0.019(7) -0.006(6) F7 0.110(16) 0.140(15) 0.176(15) 0.021(12) -0.042(11) -0.036(10) F8 0.123(14) 0.164(17) 0.144(11) -0.013(11) -0.012(9) -0.082(12) F9 0.104(8) 0.088(8) 0.23(2) -0.040(10) 0.002(10) -0.024(7) F7A 0.110(16) 0.140(15) 0.176(15) 0.021(12) -0.042(11) -0.036(10) F8A 0.123(14) 0.164(17) 0.144(11) -0.013(11) -0.012(9) -0.082(12) F9A 0.104(8) 0.088(8) 0.23(2) -0.040(10) 0.002(10) -0.024(7) C45 0.073(10) 0.061(8) 0.110(10) -0.009(8) -0.028(9) 0.032(7) F10 0.114(17) 0.095(12) 0.32(3) -0.015(14) 0.047(16) 0.030(10) F11 0.066(7) 0.111(9) 0.168(13) 0.015(8) 0.002(7) 0.023(6) F12 0.057(7) 0.111(13) 0.245(16) 0.077(13) 0.010(8) 0.013(9) F10A 0.114(17) 0.095(12) 0.32(3) -0.015(14) 0.047(16) 0.030(10) F11A 0.066(7) 0.111(9) 0.168(13) 0.015(8) 0.002(7) 0.023(6) F12A 0.057(7) 0.111(13) 0.245(16) 0.077(13) 0.010(8) 0.013(9) B2 0.071(10) 0.071(10) 0.50(8) 0.000 0.000 0.000 C51 0.065(10) 0.056(7) 0.41(2) -0.033(15) 0.015(13) -0.003(7) C52 0.114(12) 0.046(7) 0.42(3) -0.011(17) 0.068(19) 0.000(8) C53 0.111(11) 0.078(10) 0.37(2) -0.045(19) 0.07(2) -0.006(8) C54 0.131(12) 0.091(10) 0.37(3) -0.096(19) 0.01(3) 0.025(9) C55 0.103(10) 0.081(9) 0.37(3) -0.07(2) 0.00(2) 0.019(8) C56 0.093(11) 0.068(7) 0.42(3) -0.040(19) -0.003(18) 0.027(8) C57 0.060(15) 0.125(17) 0.62(6) -0.05(3) 0.03(2) 0.035(13) F13 0.21(2) 0.049(15) 0.76(5) -0.04(2) 0.23(3) -0.030(16) F14 0.161(12) 0.078(17) 0.62(4) 0.15(2) -0.082(18) -0.053(14) F15 0.084(15) 0.101(7) 0.58(3) 0.014(18) 0.07(2) -0.038(8) F13A 0.21(2) 0.049(15) 0.76(5) -0.04(2) 0.23(3) -0.030(16) F14A 0.161(12) 0.078(17) 0.62(4) 0.15(2) -0.082(18) -0.053(14) F15A 0.084(15) 0.101(7) 0.58(3) 0.014(18) 0.07(2) -0.038(8) C58 0.21(2) 0.075(11) 0.31(4) -0.017(17) 0.04(2) 0.007(13) F16 0.138(6) 0.153(7) 0.155(6) 0.002(5) -0.009(4) 0.009(5) F17 0.14(2) 0.131(8) 0.33(2) -0.029(15) -0.05(2) 0.024(8) F18 0.110(15) 0.144(10) 0.34(3) -0.083(12) -0.041(14) 0.010(10) F16A 0.138(6) 0.153(7) 0.155(6) 0.002(5) -0.009(4) 0.009(5) F17A 0.14(2) 0.131(8) 0.33(2) -0.029(15) -0.05(2) 0.024(8) F18A 0.110(15) 0.144(10) 0.34(3) -0.083(12) -0.041(14) 0.010(10) C51B 0.065(10) 0.056(7) 0.41(2) -0.033(15) 0.015(13) -0.003(7) C52B 0.114(12) 0.046(7) 0.42(3) -0.011(17) 0.068(19) 0.000(8) C53B 0.111(11) 0.078(10) 0.37(2) -0.045(19) 0.07(2) -0.006(8) C54B 0.131(12) 0.091(10) 0.37(3) -0.096(19) 0.01(3) 0.025(9) C55B 0.103(10) 0.081(9) 0.37(3) -0.07(2) 0.00(2) 0.019(8) C56B 0.093(11) 0.068(7) 0.42(3) -0.040(19) -0.003(18) 0.027(8) C57B 0.060(15) 0.125(17) 0.62(6) -0.05(3) 0.03(2) 0.035(13) F13B 0.21(2) 0.049(15) 0.76(5) -0.04(2) 0.23(3) -0.030(16) F14B 0.161(12) 0.078(17) 0.62(4) 0.15(2) -0.082(18) -0.053(14) F15B 0.084(15) 0.101(7) 0.58(3) 0.014(18) 0.07(2) -0.038(8) F13C 0.21(2) 0.049(15) 0.76(5) -0.04(2) 0.23(3) -0.030(16) F14C 0.161(12) 0.078(17) 0.62(4) 0.15(2) -0.082(18) -0.053(14) F15C 0.084(15) 0.101(7) 0.58(3) 0.014(18) 0.07(2) -0.038(8) C58B 0.21(2) 0.075(11) 0.31(4) -0.017(17) 0.04(2) 0.007(13) F16B 0.138(6) 0.153(7) 0.155(6) 0.002(5) -0.009(4) 0.009(5) F17B 0.14(2) 0.131(8) 0.33(2) -0.029(15) -0.05(2) 0.024(8) F18B 0.110(15) 0.144(10) 0.34(3) -0.083(12) -0.041(14) 0.010(10) F16C 0.138(6) 0.153(7) 0.155(6) 0.002(5) -0.009(4) 0.009(5) F17C 0.14(2) 0.131(8) 0.33(2) -0.029(15) -0.05(2) 0.024(8) F18C 0.110(15) 0.144(10) 0.34(3) -0.083(12) -0.041(14) 0.010(10) O1 0.081(5) 0.081(5) 0.093(8) 0.000 0.000 0.000 S1 0.070(6) 0.134(10) 0.088(5) 0.01(2) -0.001(5) -0.012(8) C1S 0.18(3) 0.19(3) 0.17(2) -0.12(2) 0.01(2) -0.03(2) O2 0.102(8) 0.133(10) 0.220(14) 0.000 0.000 -0.001(7) S2 0.121(6) 0.101(5) 0.247(9) 0.009(5) -0.016(6) -0.040(4) C2S 0.211(18) 0.177(16) 0.39(3) -0.048(18) 0.036(18) 0.038(14) S3 0.17(3) 0.098(16) 0.248(15) -0.065(19) 0.11(2) -0.10(2) O3 0.178(12) 0.178(12) 0.157(17) 0.000 0.000 0.000 C3S 0.14(2) 0.19(3) 0.34(5) -0.06(3) -0.13(3) 0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.1147(17) . ? Mo1 N1 2.133(5) 2 ? Mo1 N1 2.133(5) . ? Mo1 N1 2.133(5) 3 ? Mo1 N1 2.133(5) 4 ? Mo2 N2 2.122(5) 2 ? Mo2 N2 2.122(5) 3 ? Mo2 N2 2.122(5) . ? Mo2 N2 2.122(5) 4 ? N1 C1 1.327(8) . ? N1 C2 1.463(8) . ? N2 C1 1.347(8) . ? N2 C7 1.451(8) . ? N3 C1 1.367(8) . ? N3 C4 1.446(8) . ? N3 C5 1.451(8) . ? C2 C3 1.512(10) . ? C3 C4 1.520(10) . ? C3 C10 1.533(12) . ? C3 C8B 1.533(10) . ? C3 C8 1.548(9) . ? C5 C6 1.515(9) . ? C6 C7 1.513(9) . ? C6 C12 1.520(9) . ? C6 C14 1.535(9) . ? C8 C9 1.510(10) . ? C8B C9B 1.501(10) . ? C10 C11 1.499(8) . ? C10 C11B 1.512(10) . ? C12 C13 1.537(10) . ? C14 C15 1.518(10) . ? Mo3 Mo3 2.1160(19) 7_567 ? Mo3 N5 2.126(5) 8_667 ? Mo3 N5 2.126(5) 7_567 ? Mo3 N4 2.129(5) 2_565 ? Mo3 N4 2.129(5) . ? N4 C16 1.344(8) . ? N4 C17 1.455(8) . ? N5 C16 1.330(8) . ? N5 C22 1.453(8) . ? N5 Mo3 2.126(5) 7_567 ? N6 C16 1.377(8) . ? N6 C20 1.452(9) . ? N6 C19 1.453(9) . ? C17 C18 1.517(10) . ? C18 C19 1.514(11) . ? C18 C25 1.538(11) . ? C18 C23 1.560(11) . ? C20 C21 1.523(10) . ? C21 C22 1.519(9) . ? C21 C29 1.538(9) . ? C21 C27 1.552(10) . ? C23 C24B 1.506(10) . ? C23 C24 1.528(9) . ? C25 C26B 1.500(10) . ? C25 C26 1.513(8) . ? C27 C28A 1.452(13) . ? C27 C28 1.454(13) . ? C29 C30 1.444(13) . ? C29 C30A 1.446(13) . ? B1 C39 1.675(11) 3 ? B1 C39 1.675(11) 2 ? B1 C39 1.675(11) . ? B1 C39 1.675(11) 4 ? B1 C31 1.688(12) 3 ? B1 C31 1.688(12) 4 ? B1 C31 1.688(12) . ? B1 C31 1.688(12) 2 ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C36 0.836(15) 3 ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 C38 1.474(7) . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 C37 1.473(8) . ? C36 C32 0.836(15) 4 ? C37 F4A 0.65(3) 4 ? C37 C38 1.179(17) 4 ? C37 F3A 1.316(6) . ? C37 F2A 1.320(6) . ? C37 F1 1.321(6) . ? C37 F1A 1.323(6) . ? C37 F3 1.323(6) . ? C37 F2 1.327(6) . ? C37 F6A 1.63(3) 4 ? C37 F5 1.80(2) 4 ? F1 C38 1.38(3) 4 ? F2 C38 0.90(3) 4 ? F1A C38 0.92(3) 4 ? F2A C38 1.36(3) 4 ? C38 F2 0.90(3) 3 ? C38 F1A 0.92(3) 3 ? C38 C37 1.179(17) 3 ? C38 F5A 1.316(6) . ? C38 F5 1.320(6) . ? C38 F6 1.320(6) . ? C38 F4 1.322(6) . ? C38 F6A 1.322(6) . ? C38 F4A 1.322(6) . ? C38 F2A 1.36(3) 3 ? C38 F1 1.38(3) 3 ? F4 C37 0.47(3) 3 ? F5 C37 1.80(2) 3 ? F4A C37 0.65(3) 3 ? F6A C37 1.63(3) 3 ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C44 0.946(17) 3 ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C41 C45 1.476(8) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C43 C46 1.475(7) . ? C44 C40 0.946(16) 4 ? C46 F10A 0.62(4) 4 ? C46 F10 1.21(3) 4 ? C46 F12 1.29(3) 4 ? C46 F7A 1.316(6) . ? C46 F9 1.318(6) . ? C46 F8 1.319(6) . ? C46 F9A 1.325(6) . ? C46 F8A 1.325(6) . ? C46 F7 1.327(6) . ? C46 C45 1.410(19) 4 ? F7 C45 1.72(3) 4 ? F8 C45 0.74(3) 4 ? F7A C45 0.47(3) 4 ? C45 F8 0.74(3) 3 ? C45 F10 1.317(6) . ? C45 F10A 1.321(6) . ? C45 F11A 1.321(6) . ? C45 F12 1.322(6) . ? C45 F12A 1.323(6) . ? C45 F11 1.327(6) . ? C45 C46 1.410(19) 3 ? C45 F7 1.72(3) 3 ? F10 C46 1.21(3) 3 ? F12 C46 1.29(3) 3 ? F10A C46 0.62(3) 3 ? B2 C51 1.650(6) 8_656 ? B2 C51 1.650(6) . ? B2 C51 1.650(6) 2_655 ? B2 C51 1.650(6) 7_666 ? B2 C51B 1.656(5) 8_656 ? B2 C51B 1.656(5) 2_655 ? B2 C51B 1.656(5) . ? B2 C51B 1.656(5) 7_666 ? C51 C52 1.3905(19) . ? C51 C56 1.391(2) . ? C52 C53 1.390(2) . ? C53 C54 1.390(2) . ? C53 C57 1.474(8) . ? C53 C57B 1.70(3) 2_655 ? C54 C55 1.391(2) . ? C55 C58B 1.36(4) 2_655 ? C55 C56 1.391(2) . ? C55 C58 1.476(8) . ? C57 C57B 0.62(5) 2_655 ? C57 C53B 1.23(4) 2_655 ? C57 F13 1.321(6) . ? C57 F14 1.321(6) . ? C57 F15A 1.321(6) . ? C57 F15 1.322(6) . ? C57 F13A 1.322(6) . ? C57 F14A 1.323(6) . ? C57 F15B 1.32(6) 2_655 ? C57 F13C 1.33(5) 2_655 ? C57 F13B 1.47(6) 2_655 ? F13 C57B 1.71(5) 2_655 ? F14 C57B 0.88(5) 2_655 ? F15 C57B 1.32(6) 2_655 ? F13A C57B 1.56(6) 2_655 ? F14A C57B 0.82(5) 2_655 ? F15A C57B 1.19(5) 2_655 ? C58 C58B 0.90(4) 2_655 ? C58 F17C 1.04(5) 2_655 ? C58 F18B 1.05(5) 2_655 ? C58 F16A 1.322(6) . ? C58 F17 1.323(6) . ? C58 F17A 1.323(6) . ? C58 F16 1.323(6) . ? C58 F18 1.323(6) . ? C58 F18A 1.324(6) . ? C58 F17B 1.34(4) 2_655 ? C58 F18C 1.35(5) 2_655 ? F16 C58B 0.89(6) 2_655 ? F17 C58B 1.82(5) 2_655 ? F16A C58B 1.09(7) 2_655 ? F17A C58B 1.62(6) 2_655 ? C51B C52B 1.3900 . ? C51B C56B 1.3900 . ? C52B C53B 1.3900 . ? C53B C57 1.23(3) 2_655 ? C53B C54B 1.3900 . ? C53B C57B 1.473(8) . ? C54B C55B 1.3900 . ? C55B C56B 1.3900 . ? C55B C58B 1.476(8) . ? C57B C57 0.62(5) 2_655 ? C57B F14A 0.82(5) 2_655 ? C57B F14 0.88(5) 2_655 ? C57B F15A 1.19(5) 2_655 ? C57B F15C 1.315(6) . ? C57B F15 1.32(6) 2_655 ? C57B F13B 1.319(6) . ? C57B F14C 1.321(6) . ? C57B F13C 1.321(6) . ? C57B F15B 1.321(6) . ? C57B F14B 1.323(6) . ? F13B C57 1.47(6) 2_655 ? F15B C57 1.32(6) 2_655 ? F13C C57 1.33(5) 2_655 ? F15C C57 1.57(5) 2_655 ? C58B F16 0.89(6) 2_655 ? C58B C58 0.90(4) 2_655 ? C58B F16A 1.09(7) 2_655 ? C58B F18B 1.322(6) . ? C58B F18C 1.323(6) . ? C58B F16C 1.325(6) . ? C58B F17C 1.324(6) . ? C58B F17B 1.326(6) . ? C58B F16B 1.327(6) . ? C58B C55 1.36(4) 2_655 ? C58B F17A 1.62(6) 2_655 ? F17B C58 1.34(4) 2_655 ? F18B C58 1.05(5) 2_655 ? F17C C58 1.04(5) 2_655 ? F18C C58 1.35(5) 2_655 ? O1 S1 1.494(5) 2 ? O1 S1 1.494(5) . ? O1 S1 1.494(5) 3 ? O1 S1 1.494(5) 4 ? S1 S1 0.853(12) 4 ? S1 S1 0.853(12) 3 ? S1 S1 1.207(17) 2 ? S1 C1S 1.232(19) 4 ? S1 C1S 1.77(4) 2 ? S1 C1S 1.818(5) . ? S1 C1S 2.22(2) 3 ? C1S S1 1.232(19) 3 ? C1S S1 1.77(4) 2 ? C1S S1 2.22(2) 4 ? O2 S2 1.494(5) 2_565 ? O2 S2 1.494(5) . ? S2 S2 1.059(12) 2_565 ? S2 C2S 1.730(14) 2_565 ? S2 C2S 1.812(5) . ? C2S S2 1.730(14) 2_565 ? S3 S3 0.79(3) 3 ? S3 S3 0.79(3) 4 ? S3 S3 1.12(5) 2 ? S3 C3S 1.26(2) 4 ? S3 O3 1.493(5) . ? S3 C3S 1.65(5) 2 ? S3 C3S 1.817(5) . ? S3 C3S 2.11(4) 3 ? O3 S3 1.493(5) 3 ? O3 S3 1.493(5) 2 ? O3 S3 1.493(5) 4 ? C3S S3 1.26(2) 3 ? C3S S3 1.65(5) 2 ? C3S S3 2.11(4) 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 Mo2 Mo1 N1 91.81(14) . 2 ? Mo2 Mo1 N1 91.81(14) . . ? N1 Mo1 N1 176.4(3) 2 . ? Mo2 Mo1 N1 91.81(14) . 3 ? N1 Mo1 N1 89.943(9) 2 3 ? N1 Mo1 N1 89.943(9) . 3 ? Mo2 Mo1 N1 91.81(14) . 4 ? N1 Mo1 N1 89.943(9) 2 4 ? N1 Mo1 N1 89.943(9) . 4 ? N1 Mo1 N1 176.4(3) 3 4 ? Mo1 Mo2 N2 92.86(13) . 2 ? Mo1 Mo2 N2 92.86(13) . 3 ? N2 Mo2 N2 89.857(14) 2 3 ? Mo1 Mo2 N2 92.86(13) . . ? N2 Mo2 N2 174.3(3) 2 . ? N2 Mo2 N2 89.857(14) 3 . ? Mo1 Mo2 N2 92.86(13) . 4 ? N2 Mo2 N2 89.857(14) 2 4 ? N2 Mo2 N2 174.3(3) 3 4 ? N2 Mo2 N2 89.857(14) . 4 ? C1 N1 C2 119.3(6) . . ? C1 N1 Mo1 119.3(4) . . ? C2 N1 Mo1 121.5(4) . . ? C1 N2 C7 120.7(5) . . ? C1 N2 Mo2 118.3(4) . . ? C7 N2 Mo2 120.9(4) . . ? C1 N3 C4 120.1(6) . . ? C1 N3 C5 121.8(6) . . ? C4 N3 C5 116.4(6) . . ? N1 C1 N2 117.7(6) . . ? N1 C1 N3 122.7(6) . . ? N2 C1 N3 119.5(6) . . ? N1 C2 C3 114.5(6) . . ? C2 C3 C4 106.4(7) . . ? C2 C3 C10 107.9(7) . . ? C4 C3 C10 110.2(7) . . ? C2 C3 C8B 109.1(19) . . ? C4 C3 C8B 122.2(11) . . ? C10 C3 C8B 100.4(15) . . ? C2 C3 C8 110.1(15) . . ? C4 C3 C8 101.2(8) . . ? C10 C3 C8 120.2(14) . . ? N3 C4 C3 111.3(6) . . ? N3 C5 C6 111.7(5) . . ? C7 C6 C5 105.6(6) . . ? C7 C6 C12 111.7(6) . . ? C5 C6 C12 108.2(6) . . ? C7 C6 C14 109.1(6) . . ? C5 C6 C14 110.8(6) . . ? C12 C6 C14 111.4(6) . . ? N2 C7 C6 114.9(5) . . ? C9 C8 C3 111.2(13) . . ? C9B C8B C3 115.7(16) . . ? C11 C10 C11B 89.3(16) . . ? C11 C10 C3 120.0(10) . . ? C11B C10 C3 116.5(17) . . ? C6 C12 C13 116.7(6) . . ? C15 C14 C6 116.3(7) . . ? Mo3 Mo3 N5 92.73(15) 7_567 8_667 ? Mo3 Mo3 N5 92.73(15) 7_567 7_567 ? N5 Mo3 N5 174.5(3) 8_667 7_567 ? Mo3 Mo3 N4 92.10(16) 7_567 2_565 ? N5 Mo3 N4 89.47(19) 8_667 2_565 ? N5 Mo3 N4 90.33(19) 7_567 2_565 ? Mo3 Mo3 N4 92.10(16) 7_567 . ? N5 Mo3 N4 90.33(19) 8_667 . ? N5 Mo3 N4 89.47(19) 7_567 . ? N4 Mo3 N4 175.8(3) 2_565 . ? C16 N4 C17 120.2(6) . . ? C16 N4 Mo3 118.5(4) . . ? C17 N4 Mo3 120.9(5) . . ? C16 N5 C22 119.9(6) . . ? C16 N5 Mo3 118.4(5) . 7_567 ? C22 N5 Mo3 121.5(4) . 7_567 ? C16 N6 C20 119.7(6) . . ? C16 N6 C19 121.7(6) . . ? C20 N6 C19 115.8(6) . . ? N5 C16 N4 118.2(6) . . ? N5 C16 N6 121.7(7) . . ? N4 C16 N6 119.9(6) . . ? N4 C17 C18 114.1(6) . . ? C19 C18 C17 106.0(7) . . ? C19 C18 C25 110.5(7) . . ? C17 C18 C25 107.7(6) . . ? C19 C18 C23 107.2(7) . . ? C17 C18 C23 109.7(7) . . ? C25 C18 C23 115.3(8) . . ? N6 C19 C18 112.6(6) . . ? N6 C20 C21 111.5(6) . . ? C22 C21 C20 105.6(6) . . ? C22 C21 C29 109.7(6) . . ? C20 C21 C29 109.8(6) . . ? C22 C21 C27 109.3(6) . . ? C20 C21 C27 108.7(6) . . ? C29 C21 C27 113.4(6) . . ? N5 C22 C21 115.4(6) . . ? C24B C23 C24 117.2(17) . . ? C24B C23 C18 120.1(18) . . ? C24 C23 C18 114.1(9) . . ? C26B C25 C26 83.8(19) . . ? C26B C25 C18 104.7(16) . . ? C26 C25 C18 118.5(8) . . ? C28A C27 C28 101.4(11) . . ? C28A C27 C21 116.0(8) . . ? C28 C27 C21 115.4(9) . . ? C30 C29 C30A 87.8(11) . . ? C30 C29 C21 119.4(9) . . ? C30A C29 C21 115.3(9) . . ? C39 B1 C39 68.9(6) 3 2 ? C39 B1 C39 68.9(6) 3 . ? C39 B1 C39 106.2(11) 2 . ? C39 B1 C39 106.2(11) 3 4 ? C39 B1 C39 68.9(6) 2 4 ? C39 B1 C39 68.9(6) . 4 ? C39 B1 C31 76.3(4) 3 3 ? C39 B1 C31 112.9(4) 2 3 ? C39 B1 C31 111.9(4) . 3 ? C39 B1 C31 177.4(10) 4 3 ? C39 B1 C31 177.4(10) 3 4 ? C39 B1 C31 111.9(4) 2 4 ? C39 B1 C31 112.9(4) . 4 ? C39 B1 C31 76.3(4) 4 4 ? C31 B1 C31 101.2(10) 3 4 ? C39 B1 C31 112.9(4) 3 . ? C39 B1 C31 177.4(10) 2 . ? C39 B1 C31 76.3(4) . . ? C39 B1 C31 111.9(4) 4 . ? C31 B1 C31 66.2(6) 3 . ? C31 B1 C31 66.2(6) 4 . ? C39 B1 C31 111.9(4) 3 2 ? C39 B1 C31 76.3(4) 2 2 ? C39 B1 C31 177.4(10) . 2 ? C39 B1 C31 112.9(4) 4 2 ? C31 B1 C31 66.2(6) 3 2 ? C31 B1 C31 66.2(6) 4 2 ? C31 B1 C31 101.2(10) . 2 ? C32 C31 C36 120.0 . . ? C32 C31 B1 120.3(5) . . ? C36 C31 B1 119.3(5) . . ? C36 C31 C36 137.4(2) . 3 ? B1 C31 C36 98.2(4) . 3 ? C32 C31 C31 70.0(6) . 3 ? C36 C31 C31 147.1(4) . 3 ? B1 C31 C31 56.9(3) . 3 ? C32 C31 C31 151.5(4) . 4 ? C36 C31 C31 67.2(5) . 4 ? B1 C31 C31 56.9(3) . 4 ? C36 C31 C31 129.6(2) 3 4 ? C31 C31 C31 90.0 3 4 ? C32 C31 C32 140.8(3) . 4 ? B1 C31 C32 96.5(4) . 4 ? C36 C31 C32 148.4 3 4 ? C31 C31 C32 130.2(2) 3 4 ? C36 C32 C33 118.1(4) 3 . ? C36 C32 C31 108.0(7) 3 . ? C33 C32 C31 120.0 . . ? C33 C32 C31 148.5(3) . 3 ? C31 C32 C31 66.3(5) . 3 ? C33 C32 C35 80.7(5) . 3 ? C31 C32 C35 137.0(5) . 3 ? C31 C32 C35 77.4(6) 3 3 ? C34 C33 C32 120.0 . . ? C34 C33 C38 119.9(8) . . ? C32 C33 C38 120.1(8) . . ? C34 C33 C36 134.3(3) . 3 ? C38 C33 C36 103.2(9) . 3 ? C33 C34 C35 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 C37 120.6(8) . . ? C34 C35 C37 119.3(8) . . ? C34 C35 C32 138.6(3) . 4 ? C37 C35 C32 101.3(8) . 4 ? C32 C36 C35 120.9(5) 4 . ? C32 C36 C31 114.2(7) 4 . ? C35 C36 C31 120.0 . . ? C32 C36 C31 46.3(5) 4 4 ? C35 C36 C31 151.1(3) . 4 ? C31 C36 C31 68.3(5) . 4 ? C35 C36 C33 81.7(5) . 4 ? C31 C36 C33 144.0(5) . 4 ? C31 C36 C33 79.6(6) 4 4 ? F4A C37 C38 87.8(19) 4 4 ? F4A C37 F3A 61(3) 4 . ? C38 C37 F3A 130.4(19) 4 . ? F4A C37 F2A 134(3) 4 . ? C38 C37 F2A 65.9(17) 4 . ? F3A C37 F2A 107.2(9) . . ? C38 C37 F1 66.4(16) 4 . ? F3A C37 F1 85(3) . . ? F2A C37 F1 126(3) . . ? F4A C37 F1A 48(2) 4 . ? F3A C37 F1A 106.6(9) . . ? F2A C37 F1A 106.7(9) . . ? F4A C37 F3 84(3) 4 . ? C38 C37 F3 128.3(17) 4 . ? F2A C37 F3 84(2) . . ? F1 C37 F3 106.7(9) . . ? F1A C37 F3 124(4) . . ? F4A C37 F2 123(2) 4 . ? F3A C37 F2 125(3) . . ? F1 C37 F2 106.2(9) . . ? F1A C37 F2 84(2) . . ? F3 C37 F2 105.7(9) . . ? F4A C37 C35 112(3) 4 . ? C38 C37 C35 112.8(10) 4 . ? F3A C37 C35 114.6(19) . . ? F2A C37 C35 112.7(19) . . ? F1 C37 C35 109(2) . . ? F1A C37 C35 109(2) . . ? F3 C37 C35 117.5(19) . . ? F2 C37 C35 111(2) . . ? F4A C37 F6A 130(2) 4 4 ? C38 C37 F6A 53.3(10) 4 4 ? F3A C37 F6A 118.0(17) . 4 ? F1 C37 F6A 116.4(18) . 4 ? F1A C37 F6A 95.3(17) . 4 ? F3 C37 F6A 96.1(15) . 4 ? C35 C37 F6A 111.4(12) . 4 ? C38 C37 F5 47.1(8) 4 4 ? F3A C37 F5 91.2(19) . 4 ? F2A C37 F5 100(2) . 4 ? F3 C37 F5 105(2) . 4 ? F2 C37 F5 82.7(16) . 4 ? C35 C37 F5 127.6(11) . 4 ? F6A C37 F5 91.9(11) 4 4 ? C37 F1 C38 51.8(10) . 4 ? C38 F2 C37 60.3(12) 4 . ? C38 F1A C37 60.2(12) 4 . ? C37 F2A C38 52.1(10) . 4 ? F2 C38 F1A 153(3) 3 3 ? F2 C38 C37 78.0(16) 3 3 ? F1A C38 C37 76.9(15) 3 3 ? F2 C38 F5A 110(3) 3 . ? F1A C38 F5A 79(3) 3 . ? C37 C38 F5A 128.8(13) 3 . ? F2 C38 F5 141(3) 3 . ? C37 C38 F5 92.1(14) 3 . ? F5A C38 F5 49.1(11) . . ? F2 C38 F6 56(2) 3 . ? F1A C38 F6 136(3) 3 . ? C37 C38 F6 125.4(13) 3 . ? F5A C38 F6 57.8(11) . . ? F5 C38 F6 105.2(9) . . ? F2 C38 F4 57.6(19) 3 . ? F1A C38 F4 96.3(19) 3 . ? F5A C38 F4 127.4(19) . . ? F5 C38 F4 105.3(9) . . ? F6 C38 F4 105.6(9) . . ? F1A C38 F6A 154(2) 3 . ? C37 C38 F6A 81.0(14) 3 . ? F5A C38 F6A 105.5(9) . . ? F5 C38 F6A 138.3(17) . . ? F6 C38 F6A 51.8(11) . . ? F4 C38 F6A 60.4(12) . . ? F2 C38 F4A 103(2) 3 . ? F1A C38 F4A 49.8(19) 3 . ? F5A C38 F4A 105.7(9) . . ? F5 C38 F4A 63.1(13) . . ? F6 C38 F4A 133.9(19) . . ? F4 C38 F4A 46.7(13) . . ? F6A C38 F4A 105.4(9) . . ? F1A C38 F2A 135(2) 3 3 ? C37 C38 F2A 62.0(11) 3 3 ? F5A C38 F2A 112.6(19) . 3 ? F5 C38 F2A 128.6(18) . 3 ? F6 C38 F2A 67.0(16) . 3 ? F4A C38 F2A 85.8(17) . 3 ? F2 C38 F1 136(2) 3 3 ? C37 C38 F1 61.8(11) 3 3 ? F5A C38 F1 85(2) . 3 ? F6 C38 F1 137(2) . 3 ? F4 C38 F1 80.2(15) . 3 ? F6A C38 F1 137.3(17) . 3 ? F2A C38 F1 118.2(18) 3 3 ? F2 C38 C33 108(3) 3 . ? F1A C38 C33 89(3) 3 . ? C37 C38 C33 107.8(9) 3 . ? F5A C38 C33 116.2(12) . . ? F5 C38 C33 110.9(13) . . ? F6 C38 C33 112.9(11) . . ? F4 C38 C33 116.0(16) . . ? F6A C38 C33 110.4(14) . . ? F4A C38 C33 112.8(16) . . ? F2A C38 C33 118.9(18) 3 . ? F1 C38 C33 101(2) 3 . ? C37 F4 C38 62(2) 3 . ? C37 F4A C38 63.0(16) 3 . ? C38 F6A C37 45.7(8) . 3 ? C40 C39 C44 120.0 . . ? C40 C39 B1 120.0(5) . . ? C44 C39 B1 119.9(5) . . ? C40 C39 C39 70.5(6) . 3 ? C44 C39 C39 151.1(5) . 3 ? B1 C39 C39 55.6(3) . 3 ? C40 C39 C39 152.9(5) . 4 ? C44 C39 C39 69.5(6) . 4 ? B1 C39 C39 55.6(3) . 4 ? C39 C39 C39 90.0 3 4 ? C44 C39 C44 141.6(3) . 3 ? B1 C39 C44 95.1(4) . 3 ? C39 C39 C44 129.4(2) 4 3 ? C40 C39 C40 143.2(3) . 4 ? B1 C39 C40 94.4(4) . 4 ? C39 C39 C40 129.6(2) 3 4 ? C44 C39 C40 152.0 3 4 ? C44 C40 C39 109.0(7) 3 . ? C44 C40 C41 122.0(4) 3 . ? C39 C40 C41 120.0 . . ? C39 C40 C39 67.0(5) . 3 ? C41 C40 C39 152.5(4) . 3 ? C42 C41 C40 120.0 . . ? C42 C41 C45 121.9(7) . . ? C40 C41 C45 118.1(7) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 C46 121.1(8) . . ? C44 C43 C46 118.9(8) . . ? C40 C44 C43 123.5(5) 4 . ? C40 C44 C39 110.9(7) 4 . ? C43 C44 C39 120.0 . . ? C43 C44 C39 153.7(4) . 4 ? C39 C44 C39 67.7(5) . 4 ? F10A C46 F12 102(3) 4 4 ? F10 C46 F12 113.6(14) 4 4 ? F10A C46 F7A 69(2) 4 . ? F10 C46 F7A 70.8(15) 4 . ? F10A C46 F9 61(2) 4 . ? F10 C46 F9 84(2) 4 . ? F12 C46 F9 117.8(18) 4 . ? F7A C46 F9 119(2) . . ? F10A C46 F8 45(2) 4 . ? F12 C46 F8 87.1(15) 4 . ? F9 C46 F8 106.1(10) . . ? F10A C46 F9A 95(3) 4 . ? F10 C46 F9A 127(2) 4 . ? F12 C46 F9A 75.8(18) 4 . ? F7A C46 F9A 105.8(10) . . ? F9 C46 F9A 50.4(12) . . ? F8 C46 F9A 133(2) . . ? F12 C46 F8A 143.9(15) 4 . ? F7A C46 F8A 105.5(9) . . ? F9 C46 F8A 54.5(12) . . ? F8 C46 F8A 65.6(13) . . ? F9A C46 F8A 104.7(9) . . ? F10A C46 F7 110(3) 4 . ? F10 C46 F7 129.4(17) 4 . ? F7A C46 F7 61.3(12) . . ? F9 C46 F7 105.2(9) . . ? F8 C46 F7 105.2(10) . . ? F9A C46 F7 58.3(11) . . ? F8A C46 F7 149.1(19) . . ? F10A C46 C45 68.9(16) 4 4 ? F10 C46 C45 59.8(9) 4 4 ? F12 C46 C45 58.4(10) 4 4 ? F9 C46 C45 128.0(14) . 4 ? F9A C46 C45 125.0(13) . 4 ? F8A C46 C45 96.8(15) . 4 ? F7 C46 C45 77.6(14) . 4 ? F10A C46 C43 139(4) 4 . ? F10 C46 C43 109.6(18) 4 . ? F12 C46 C43 113.0(15) 4 . ? F7A C46 C43 124.9(17) . . ? F9 C46 C43 115.5(14) . . ? F8 C46 C43 113.6(17) . . ? F9A C46 C43 113.8(14) . . ? F8A C46 C43 99.9(14) . . ? F7 C46 C43 110.5(17) . . ? C45 C46 C43 111.3(10) 4 . ? C46 F7 C45 53.4(9) . 4 ? C45 F8 C46 81.2(18) 4 . ? C45 F7A C46 92(3) 4 . ? F8 C45 F10A 47(2) 3 . ? F8 C45 F11A 73(2) 3 . ? F10 C45 F11A 86.3(18) . . ? F10A C45 F11A 104.3(9) . . ? F8 C45 F12 119(2) 3 . ? F10 C45 F12 104.9(9) . . ? F10A C45 F12 71.7(15) . . ? F11A C45 F12 128.2(16) . . ? F8 C45 F12A 147(3) 3 . ? F10 C45 F12A 136.6(18) . . ? F10A C45 F12A 104.1(9) . . ? F11A C45 F12A 104.6(9) . . ? F8 C45 F11 94(3) 3 . ? F10 C45 F11 104.3(9) . . ? F10A C45 F11 109(2) . . ? F12 C45 F11 103.6(9) . . ? F12A C45 F11 77.9(13) . . ? F8 C45 C46 67.6(14) 3 3 ? F10 C45 C46 52.4(15) . 3 ? F11A C45 C46 130.4(15) . 3 ? F12 C45 C46 56.4(14) . 3 ? F12A C45 C46 92.6(14) . 3 ? F11 C45 C46 130.5(15) . 3 ? F8 C45 C41 102(3) 3 . ? F10 C45 C41 106.2(18) . . ? F10A C45 C41 124.9(17) . . ? F11A C45 C41 107.1(13) . . ? F12 C45 C41 117.1(15) . . ? F12A C45 C41 110.0(14) . . ? F11 C45 C41 119.2(15) . . ? C46 C45 C41 109.8(9) 3 . ? F8 C45 F7 111(2) 3 3 ? F10 C45 F7 97.2(16) . 3 ? F10A C45 F7 64.1(15) . 3 ? F11A C45 F7 129.4(14) . 3 ? F11 C45 F7 106.6(15) . 3 ? C46 C45 F7 49.0(8) 3 3 ? C41 C45 F7 119.8(13) . 3 ? C46 F10 C45 67.8(13) 3 . ? C46 F12 C45 65.3(11) 3 . ? C46 F10A C45 85(2) 3 . ? C51 B2 C51 113.1(10) 8_656 . ? C51 B2 C51 113.1(10) 8_656 2_655 ? C51 B2 C51 102.4(18) . 2_655 ? C51 B2 C51 102.4(18) 8_656 7_666 ? C51 B2 C51 113.1(10) . 7_666 ? C51 B2 C51 113.1(10) 2_655 7_666 ? C51 B2 C51B 99.8(8) 8_656 8_656 ? C51 B2 C51B 126.5(12) . 8_656 ? C51 B2 C51B 101.7(12) 2_655 8_656 ? C51 B2 C51B 126.5(12) 8_656 2_655 ? C51 B2 C51B 99.8(8) 2_655 2_655 ? C51 B2 C51B 101.7(12) 7_666 2_655 ? C51B B2 C51B 113.9(2) 8_656 2_655 ? C51 B2 C51B 101.7(12) 8_656 . ? C51 B2 C51B 99.8(8) . . ? C51 B2 C51B 126.5(12) 7_666 . ? C51B B2 C51B 113.9(2) 8_656 . ? C51B B2 C51B 101.0(4) 2_655 . ? C51 B2 C51B 101.7(12) . 7_666 ? C51 B2 C51B 126.5(12) 2_655 7_666 ? C51 B2 C51B 99.8(8) 7_666 7_666 ? C51B B2 C51B 101.0(4) 8_656 7_666 ? C51B B2 C51B 113.9(2) 2_655 7_666 ? C51B B2 C51B 113.9(2) . 7_666 ? C52 C51 C56 119.7(3) . . ? C52 C51 B2 104(2) . . ? C56 C51 B2 136(2) . . ? C53 C52 C51 119.9(3) . . ? C52 C53 C54 120.1(3) . . ? C52 C53 C57 145(3) . . ? C54 C53 C57 94(3) . . ? C52 C53 C57B 127(2) . 2_655 ? C54 C53 C57B 113(2) . 2_655 ? C53 C54 C55 119.8(3) . . ? C58B C55 C56 107(3) 2_655 . ? C58B C55 C54 126(3) 2_655 . ? C56 C55 C54 119.7(4) . . ? C56 C55 C58 130(3) . . ? C54 C55 C58 110(3) . . ? C55 C56 C51 119.8(3) . . ? C57B C57 C53B 100(5) 2_655 2_655 ? C57B C57 F13 118(5) 2_655 . ? C53B C57 F13 141(5) 2_655 . ? C53B C57 F14 131(5) 2_655 . ? F13 C57 F14 86(3) . . ? C57B C57 F15A 64(5) 2_655 . ? C53B C57 F15A 125(6) 2_655 . ? F13 C57 F15A 76(6) . . ? F14 C57 F15A 64(5) . . ? C57B C57 F15 76(5) 2_655 . ? C53B C57 F15 104(6) 2_655 . ? F13 C57 F15 86(3) . . ? F14 C57 F15 86(3) . . ? C57B C57 F13A 101(5) 2_655 . ? C53B C57 F13A 148(5) 2_655 . ? F14 C57 F13A 66(6) . . ? F15A C57 F13A 86(3) . . ? F15 C57 F13A 104(6) . . ? C53B C57 F14A 103(7) 2_655 . ? F13 C57 F14A 111(6) . . ? F15A C57 F14A 86(3) . . ? F15 C57 F14A 102(4) . . ? F13A C57 F14A 86(3) . . ? C57B C57 F15B 76(5) 2_655 2_655 ? C53B C57 F15B 122(4) 2_655 2_655 ? F13 C57 F15B 71(3) . 2_655 ? F14 C57 F15B 76(4) . 2_655 ? F13A C57 F15B 86(4) . 2_655 ? F14A C57 F15B 98(4) . 2_655 ? C57B C57 F13C 76(4) 2_655 2_655 ? C53B C57 F13C 139(4) 2_655 2_655 ? F13 C57 F13C 59(4) . 2_655 ? F15A C57 F13C 91(5) . 2_655 ? F15 C57 F13C 114(4) . 2_655 ? F14A C57 F13C 56(5) . 2_655 ? F15B C57 F13C 98(3) 2_655 2_655 ? C57B C57 F13B 64(5) 2_655 2_655 ? C53B C57 F13B 107(4) 2_655 2_655 ? F13 C57 F13B 91(4) . 2_655 ? F14 C57 F13B 46(3) . 2_655 ? F15A C57 F13B 110(4) . 2_655 ? F15 C57 F13B 132(4) . 2_655 ? F13A C57 F13B 63(4) . 2_655 ? F15B C57 F13B 121(3) 2_655 2_655 ? C57B C57 C53 101(4) 2_655 . ? F13 C57 C53 141(5) . . ? F14 C57 C53 131(5) . . ? F15A C57 C53 127(6) . . ? F15 C57 C53 106(6) . . ? F13A C57 C53 147(6) . . ? F14A C57 C53 102(6) . . ? F15B C57 C53 123(4) 2_655 . ? F13C C57 C53 137(5) 2_655 . ? F13B C57 C53 106(4) 2_655 . ? C58B C58 F17C 86(4) 2_655 2_655 ? C58B C58 F18B 85(3) 2_655 2_655 ? F17C C58 F18B 148(5) 2_655 2_655 ? C58B C58 F16A 55(4) 2_655 . ? F17C C58 F16A 105(6) 2_655 . ? F18B C58 F16A 46(3) 2_655 . ? C58B C58 F17 108(4) 2_655 . ? F18B C58 F17 134(5) 2_655 . ? F16A C58 F17 106(8) . . ? C58B C58 F17A 91(4) 2_655 . ? F18B C58 F17A 136(5) 2_655 . ? F16A C58 F17A 97.6(19) . . ? F17C C58 F16 90(4) 2_655 . ? F18B C58 F16 64(4) 2_655 . ? F17 C58 F16 97.4(19) . . ? F17A C58 F16 85(7) . . ? C58B C58 F18 133(4) 2_655 . ? F17C C58 F18 123(5) 2_655 . ? F18B C58 F18 50(3) 2_655 . ? F16A C58 F18 80(5) . . ? F17 C58 F18 97.4(19) . . ? F17A C58 F18 111(7) . . ? F16 C58 F18 97.2(19) . . ? C58B C58 F18A 152(5) 2_655 . ? F17C C58 F18A 107(4) 2_655 . ? F18B C58 F18A 70(3) 2_655 . ? F16A C58 F18A 97.3(19) . . ? F17 C58 F18A 81(5) . . ? F17A C58 F18A 97.3(19) . . ? F16 C58 F18A 112(6) . . ? C58B C58 F17B 69(3) 2_655 2_655 ? F18B C58 F17B 125(3) 2_655 2_655 ? F16A C58 F17B 80(5) . 2_655 ? F16 C58 F17B 65(3) . 2_655 ? F18 C58 F17B 121(5) . 2_655 ? F18A C58 F17B 114(4) . 2_655 ? C58B C58 F18C 69(3) 2_655 2_655 ? F17C C58 F18C 125(4) 2_655 2_655 ? F17 C58 F18C 121(5) . 2_655 ? F17A C58 F18C 116(5) . 2_655 ? F18 C58 F18C 64(3) . 2_655 ? F18A C58 F18C 84(3) . 2_655 ? F17B C58 F18C 101(3) 2_655 2_655 ? C58B C58 C55 64(3) 2_655 . ? F17C C58 C55 108(3) 2_655 . ? F18B C58 C55 96(3) 2_655 . ? F16A C58 C55 107(5) . . ? F17 C58 C55 129(5) . . ? F17A C58 C55 121(6) . . ? F16 C58 C55 103(5) . . ? F18 C58 C55 125(6) . . ? F18A C58 C55 130(5) . . ? F17B C58 C55 114(4) 2_655 . ? F18C C58 C55 104(3) 2_655 . ? C52B C51B C56B 120.0 . . ? C52B C51B B2 126.1(9) . . ? C56B C51B B2 113.9(9) . . ? C53B C52B C51B 120.0 . . ? C57 C53B C52B 135(2) 2_655 . ? C57 C53B C54B 103(2) 2_655 . ? C52B C53B C54B 120.0 . . ? C52B C53B C57B 115.5(14) . . ? C54B C53B C57B 124.5(14) . . ? C53B C54B C55B 120.0 . . ? C56B C55B C54B 120.0 . . ? C56B C55B C58B 119.3(14) . . ? C54B C55B C58B 120.5(13) . . ? C56B C55B C58 132.6(16) . 2_655 ? C54B C55B C58 102.0(17) . 2_655 ? C55B C56B C51B 120.0 . . ? C57 C57B F14A 131(9) 2_655 2_655 ? C57 C57B F14 121(8) 2_655 2_655 ? F14A C57B F14 46(7) 2_655 2_655 ? C57 C57B F15A 88(5) 2_655 2_655 ? F14A C57B F15A 126(7) 2_655 2_655 ? F14 C57B F15A 84(7) 2_655 2_655 ? C57 C57B F15C 102(5) 2_655 . ? F14A C57B F15C 113(6) 2_655 . ? F14 C57B F15C 75(4) 2_655 . ? C57 C57B F15 77(5) 2_655 2_655 ? F14A C57B F15 147(6) 2_655 2_655 ? F14 C57B F15 108(6) 2_655 2_655 ? C57 C57B F13B 91(6) 2_655 . ? F14 C57B F13B 56(4) 2_655 . ? F15A C57B F13B 132(5) 2_655 . ? F15C C57B F13B 128.7(17) . . ? F15 C57B F13B 151(5) 2_655 . ? C57 C57B F14C 159(5) 2_655 . ? F14 C57B F14C 63(6) 2_655 . ? F15A C57B F14C 113(4) 2_655 . ? F15C C57B F14C 99.0(11) . . ? F15 C57B F14C 123(4) 2_655 . ? F13B C57B F14C 74(3) . . ? C57 C57B F13C 77(5) 2_655 . ? F14A C57B F13C 66(8) 2_655 . ? F14 C57B F13C 47(5) 2_655 . ? F15A C57B F13C 98(5) 2_655 . ? F15C C57B F13C 98.9(11) . . ? F15 C57B F13C 115(4) 2_655 . ? F14C C57B F13C 98.5(11) . . ? C57 C57B F15B 77(5) 2_655 . ? F14A C57B F15B 137(7) 2_655 . ? F14 C57B F15B 93(5) 2_655 . ? F13B C57B F15B 134(2) . . ? F14C C57B F15B 124.6(15) . . ? F13C C57B F15B 98.2(10) . . ? C57 C57B F14B 170(6) 2_655 . ? F14A C57B F14B 58(5) 2_655 . ? F14 C57B F14B 67(6) 2_655 . ? F15A C57B F14B 88(4) 2_655 . ? F15C C57B F14B 74.0(15) . . ? F15 C57B F14B 96(4) 2_655 . ? F13B C57B F14B 98.4(11) . . ? F13C C57B F14B 113(4) . . ? F15B C57B F14B 98.3(10) . . ? C57 C57B C53B 55(3) 2_655 . ? F14A C57B C53B 118(7) 2_655 . ? F14 C57B C53B 159(4) 2_655 . ? F15A C57B C53B 116(4) 2_655 . ? F15C C57B C53B 126.1(15) . . ? F15 C57B C53B 92(4) 2_655 . ? F13B C57B C53B 102.2(18) . . ? F14C C57B C53B 112(2) . . ? F13C C57B C53B 117(2) . . ? F15B C57B C53B 105.7(16) . . ? F14B C57B C53B 119(3) . . ? F16 C58B C58 96(4) 2_655 2_655 ? C58 C58B F16A 83(4) 2_655 2_655 ? F16 C58B F18B 67(5) 2_655 . ? C58 C58B F18B 52(3) 2_655 . ? F16A C58B F18B 46(4) 2_655 . ? C58 C58B F18C 72(3) 2_655 . ? F16 C58B F16C 69(4) 2_655 . ? C58 C58B F16C 152(3) 2_655 . ? F16A C58B F16C 88(4) 2_655 . ? F18B C58B F16C 131.7(19) . . ? F18C C58B F16C 106.2(10) . . ? F16 C58B F17C 97(6) 2_655 . ? C58 C58B F17C 51(3) 2_655 . ? F16A C58B F17C 101(6) 2_655 . ? F18B C58B F17C 98(3) . . ? F18C C58B F17C 106.5(10) . . ? F16C C58B F17C 106.1(10) . . ? F16 C58B F17B 78(5) 2_655 . ? C58 C58B F17B 71(3) 2_655 . ? F16A C58B F17B 89(5) 2_655 . ? F18B C58B F17B 106.4(10) . . ? F18C C58B F17B 103(4) . . ? F16C C58B F17B 82.8(18) . . ? F16 C58B F16B 58(4) 2_655 . ? C58 C58B F16B 153(3) 2_655 . ? F16A C58B F16B 70(3) 2_655 . ? F18B C58B F16B 106.0(10) . . ? F18C C58B F16B 83(2) . . ? F17C C58B F16B 131(2) . . ? F17B C58B F16B 105.7(10) . . ? F16 C58B C55 154(6) 2_655 2_655 ? C58 C58B C55 79(3) 2_655 2_655 ? F16A C58B C55 133(5) 2_655 2_655 ? F18B C58B C55 90(3) . 2_655 ? F18C C58B C55 112(3) . 2_655 ? F16C C58B C55 125(3) . 2_655 ? F17C C58B C55 100(3) . 2_655 ? F17B C58B C55 123(2) . 2_655 ? F16B C58B C55 121(2) . 2_655 ? F16 C58B C55B 158(6) 2_655 . ? C58 C58B C55B 89.2(19) 2_655 . ? F16A C58B C55B 141(5) 2_655 . ? F18B C58B C55B 100.1(18) . . ? F18C C58B C55B 120(2) . . ? F16C C58B C55B 113.7(17) . . ? F17C C58B C55B 103(2) . . ? F17B C58B C55B 124(2) . . ? F16B C58B C55B 113.0(18) . . ? F16 C58B F17A 86(9) 2_655 2_655 ? C58 C58B F17A 55(3) 2_655 2_655 ? F16A C58B F17A 93(5) 2_655 2_655 ? F18B C58B F17A 97(4) . 2_655 ? F18C C58B F17A 101(5) . 2_655 ? F16C C58B F17A 100(3) . 2_655 ? F16B C58B F17A 123(4) . 2_655 ? C55 C58B F17A 110(4) 2_655 2_655 ? C55B C58B F17A 114(4) . 2_655 ? S1 O1 S1 47.6(7) 2 . ? S1 O1 S1 47.6(7) 3 4 ? S1 S1 S1 90.00(2) 4 3 ? S1 S1 S1 45.000(5) 4 2 ? S1 S1 S1 45.000(16) 3 2 ? S1 S1 C1S 120(2) 4 4 ? S1 S1 C1S 115(3) 3 4 ? S1 S1 C1S 130.8(17) 2 4 ? S1 S1 O1 73.4(2) 4 . ? S1 S1 O1 73.4(2) 3 . ? S1 S1 O1 66.2(4) 2 . ? C1S S1 O1 162.6(16) 4 . ? S1 S1 C1S 110.5(16) 3 2 ? S1 S1 C1S 72.5(17) 2 2 ? C1S S1 C1S 81.2(17) 4 2 ? O1 S1 C1S 111.0(15) . 2 ? S1 S1 C1S 107(2) 4 . ? S1 S1 C1S 68(2) 2 . ? C1S S1 C1S 79.2(19) 4 . ? O1 S1 C1S 108.6(13) . . ? C1S S1 C1S 103.7(19) 2 . ? S1 S1 C1S 48.4(15) 4 3 ? S1 S1 C1S 51.7(16) 3 3 ? C1S S1 C1S 106(2) 4 3 ? O1 S1 C1S 91.0(9) . 3 ? C1S S1 C1S 58.8(8) 2 3 ? C1S S1 C1S 58.3(9) . 3 ? S1 C1S C1S 63.5(15) 3 3 ? S1 C1S C1S 71.0(5) . 3 ? S1 C1S C1S 61.2(12) 3 4 ? S1 C1S C1S 71.9(8) 2 4 ? C1S C1S C1S 90.000(3) 3 4 ? C1S C1S S1 49.3(7) 3 4 ? C1S C1S S1 50.8(7) 4 4 ? S2 S2 O2 69.2(3) 2_565 . ? S2 S2 C2S 76.9(8) 2_565 2_565 ? O2 S2 C2S 120.4(8) . 2_565 ? S2 S2 C2S 68.4(8) 2_565 . ? O2 S2 C2S 115.5(8) . . ? C2S S2 C2S 94.0(14) 2_565 . ? S3 S3 S3 90.00(2) 3 4 ? S3 S3 S3 45.000(7) 3 2 ? S3 S3 S3 45.000(18) 4 2 ? S3 S3 C3S 105(3) 3 4 ? S3 S3 C3S 123(3) 4 4 ? S3 S3 C3S 124.6(18) 2 4 ? S3 S3 O3 74.6(6) 3 . ? S3 S3 O3 74.6(6) 4 . ? S3 S3 O3 67.9(9) 2 . ? C3S S3 O3 162(4) 4 . ? S3 S3 C3S 115(3) 3 2 ? S3 S3 C3S 47(3) 4 2 ? S3 S3 C3S 79(3) 2 2 ? C3S S3 C3S 77(3) 4 2 ? O3 S3 C3S 120(2) . 2 ? S3 S3 C3S 100.2(19) 4 . ? S3 S3 C3S 63(2) 2 . ? C3S S3 C3S 71(2) 4 . ? O3 S3 C3S 110.0(16) . . ? C3S S3 C3S 97(3) 2 . ? S3 S3 C3S 58(2) 3 3 ? S3 S3 C3S 45(2) 4 3 ? C3S S3 C3S 98(3) 4 3 ? O3 S3 C3S 96.5(16) . 3 ? C3S S3 C3S 57.1(15) 2 3 ? C3S S3 C3S 55.3(11) . 3 ? S3 C3S C3S 61(2) 3 4 ? S3 C3S C3S 74.1(8) 2 4 ? S3 C3S C3S 68.9(12) 3 3 ? S3 C3S C3S 70.4(13) . 3 ? C3S C3S C3S 90.000(7) 4 3 ? C3S C3S S3 54.3(9) 4 4 ? C3S C3S S3 48.8(9) 3 4 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.907 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.077 #===END of CIF for Compound 5.2DMSO ====================== data_SIHCL _database_code_depnum_ccdc_archive 'CCDC 645817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cl N3 O2' _chemical_formula_sum 'C10 H22 Cl N3 O2' _chemical_formula_weight 251.76 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 18.8345(16) _cell_length_b 8.1735(7) _cell_length_c 17.4200(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2681.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 2687 _cell_measurement_theta_min 2.1625 _cell_measurement_theta_max 27.063 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.278 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8876 _exptl_absorpt_correction_T_max 0.9811 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9015 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.52 _reflns_number_total 1592 _reflns_number_gt 1234 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+3.2499P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1592 _refine_ls_number_parameters 76 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Cl1 Cl 0.5000 0.12354(9) 0.31661(3) 0.0389(2) Uani 1 2 d S . . O1 O 0.37994(7) 0.15296(16) 0.43364(7) 0.0370(3) Uani 1 1 d . . . H1A H 0.4114 0.1565 0.4003 0.055 Uiso 1 1 calc R . . N1 N 0.5000 0.3223(2) 0.62552(11) 0.0217(4) Uani 1 2 d S . . H1B H 0.5000 0.2595 0.5824 0.026 Uiso 1 2 calc SR . . H1C H 0.5000 0.2543 0.6669 0.026 Uiso 1 2 calc SR . . C1 C 0.43451(8) 0.42703(19) 0.62693(9) 0.0218(3) Uani 1 1 d . . . H1D H 0.4359 0.5015 0.5829 0.026 Uiso 1 1 calc R . . H1E H 0.4353 0.4940 0.6736 0.026 Uiso 1 1 calc R . . C2 C 0.36452(8) 0.3313(2) 0.62464(9) 0.0222(3) Uani 1 1 d . . . N2 N 0.40212(7) 0.24138(17) 0.49852(8) 0.0267(3) Uani 1 1 d . . . C5 C 0.35754(9) 0.2117(2) 0.69237(10) 0.0319(4) Uani 1 1 d . . . H5A H 0.3953 0.1311 0.6898 0.048 Uiso 1 1 calc R . . H5B H 0.3119 0.1568 0.6898 0.048 Uiso 1 1 calc R . . H5C H 0.3610 0.2716 0.7403 0.048 Uiso 1 1 calc R . . C3 C 0.35551(8) 0.2386(2) 0.55050(9) 0.0255(3) Uani 1 1 d . . . H3A H 0.3140 0.1769 0.5428 0.031 Uiso 1 1 calc R . . C4 C 0.30445(9) 0.4589(2) 0.62929(11) 0.0335(4) Uani 1 1 d . . . H4A H 0.3086 0.5348 0.5867 0.050 Uiso 1 1 calc R . . H4B H 0.3081 0.5184 0.6773 0.050 Uiso 1 1 calc R . . H4C H 0.2589 0.4039 0.6268 0.050 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0313(3) 0.0628(5) 0.0227(3) -0.0082(3) 0.000 0.000 O1 0.0382(7) 0.0457(8) 0.0271(6) -0.0123(6) 0.0046(5) -0.0094(6) N1 0.0179(9) 0.0225(9) 0.0246(9) 0.0029(7) 0.000 0.000 C1 0.0178(7) 0.0235(8) 0.0240(7) -0.0008(6) -0.0006(6) 0.0029(6) C2 0.0173(7) 0.0271(8) 0.0224(7) -0.0004(6) 0.0003(6) 0.0004(6) N2 0.0297(7) 0.0276(7) 0.0228(6) -0.0053(5) -0.0003(6) -0.0024(6) C5 0.0268(8) 0.0416(10) 0.0273(8) 0.0065(8) 0.0006(7) -0.0075(8) C3 0.0216(8) 0.0281(8) 0.0268(8) -0.0001(7) -0.0018(6) -0.0033(6) C4 0.0199(8) 0.0401(10) 0.0404(10) -0.0064(8) -0.0010(7) 0.0050(7) _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 Cl1 O1 3.0540(13) . ? O1 N2 1.4050(17) . ? N1 C1 1.5018(17) . ? C1 C2 1.533(2) . ? C2 C3 1.507(2) . ? C2 C5 1.538(2) . ? C2 C4 1.541(2) . ? N2 C3 1.261(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 O1 Cl1 O1 95.53(5) 12_655 . ? N2 O1 Cl1 110.94(8) . . ? C1 N1 C1 110.44(16) . 12_655 ? C1 N1 N2 68.12(8) . . ? C1 N1 N2 130.71(12) 12_655 . ? C1 N1 N2 130.71(12) . 12_655 ? C1 N1 N2 68.12(8) 12_655 12_655 ? N2 N1 N2 77.21(7) . 12_655 ? N1 C1 C2 114.51(13) . . ? C3 C2 C1 112.07(13) . . ? C3 C2 C5 109.14(13) . . ? C1 C2 C5 112.20(13) . . ? C3 C2 C4 107.63(13) . . ? C1 C2 C4 106.54(13) . . ? C5 C2 C4 109.10(14) . . ? C3 N2 O1 111.18(13) . . ? C3 N2 N1 84.31(10) . . ? O1 N2 N1 154.54(10) . . ? N2 C3 C2 121.85(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.329 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.048 #===END CIF for SI.HCl=========================================== data_SI _database_code_depnum_ccdc_archive 'CCDC 645818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H21 N3 O2' _chemical_formula_sum 'C10 H21 N3 O2' _chemical_formula_weight 215.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(2)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y, x+1/2, z+1/2' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y, -x-1/2, -z-1/2' '-y-1/2, x, -z-1/2' _cell_length_a 19.4244(18) _cell_length_b 19.4244(18) _cell_length_c 6.8427(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2581.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1723 _cell_measurement_theta_min 2.966 _cell_measurement_theta_max 22.254 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9448 _exptl_absorpt_correction_T_max 0.9972 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14633 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.0647 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2276 _reflns_number_gt 1238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2276 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1289 _refine_ls_R_factor_gt 0.0595 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1561 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 O2 O 1.05807(9) 0.57093(10) 0.1253(3) 0.0423(6) Uani 1 1 d . . . H2A H 1.0817 0.5730 0.2261 0.063 Uiso 1 1 calc R . . N1 N 0.83898(11) 0.51972(11) 0.1732(3) 0.0334(6) Uani 1 1 d . . . H1A H 0.8663 0.5280 0.2711 0.040 Uiso 1 1 calc R . . N3 N 0.99254(11) 0.60084(11) 0.1609(3) 0.0317(6) Uani 1 1 d . . . N2 N 0.91752(11) 0.39569(11) 0.4805(3) 0.0325(6) Uani 1 1 d . . . C1 C 0.79539(14) 0.45926(14) 0.1616(4) 0.0309(7) Uani 1 1 d . . . H1B H 0.8061 0.4340 0.0414 0.037 Uiso 1 1 calc R . . H1C H 0.7472 0.4739 0.1544 0.037 Uiso 1 1 calc R . . O1 O 0.98411(9) 0.36965(11) 0.4442(3) 0.0433(6) Uani 1 1 d . . . H1D H 1.0088 0.3763 0.5415 0.065 Uiso 1 1 calc R . . C3 C 0.87779(14) 0.38676(13) 0.3372(4) 0.0309(7) Uani 1 1 d . . . H3B H 0.8947 0.3638 0.2263 0.037 Uiso 1 1 calc R . . C7 C 0.88180(14) 0.62666(14) 0.0158(4) 0.0301(7) Uani 1 1 d . . . C2 C 0.80450(13) 0.41126(13) 0.3361(4) 0.0289(7) Uani 1 1 d . . . C8 C 0.95428(13) 0.59871(14) 0.0121(4) 0.0308(7) Uani 1 1 d . . . H8A H 0.9713 0.5792 -0.1039 0.037 Uiso 1 1 calc R . . C6 C 0.83262(13) 0.56499(14) 0.0060(4) 0.0308(7) Uani 1 1 d . . . H6A H 0.7852 0.5819 -0.0017 0.037 Uiso 1 1 calc R . . H6B H 0.8421 0.5387 -0.1134 0.037 Uiso 1 1 calc R . . C10 C 0.86854(15) 0.66943(15) 0.1992(5) 0.0439(9) Uani 1 1 d . . . H10A H 0.8750 0.6409 0.3141 0.066 Uiso 1 1 calc R . . H10B H 0.8217 0.6867 0.1969 0.066 Uiso 1 1 calc R . . H10C H 0.9005 0.7078 0.2031 0.066 Uiso 1 1 calc R . . C9 C 0.87148(16) 0.67148(17) -0.1671(5) 0.0501(9) Uani 1 1 d . . . H9A H 0.9023 0.7108 -0.1616 0.075 Uiso 1 1 calc R . . H9B H 0.8242 0.6875 -0.1721 0.075 Uiso 1 1 calc R . . H9C H 0.8815 0.6445 -0.2830 0.075 Uiso 1 1 calc R . . C5 C 0.75801(16) 0.34847(15) 0.3057(5) 0.0471(9) Uani 1 1 d . . . H5A H 0.7702 0.3258 0.1842 0.071 Uiso 1 1 calc R . . H5B H 0.7103 0.3632 0.3002 0.071 Uiso 1 1 calc R . . H5C H 0.7641 0.3166 0.4135 0.071 Uiso 1 1 calc R . . C4 C 0.78547(16) 0.44753(16) 0.5265(4) 0.0412(8) Uani 1 1 d . . . H4A H 0.8148 0.4875 0.5441 0.062 Uiso 1 1 calc R . . H4B H 0.7918 0.4161 0.6352 0.062 Uiso 1 1 calc R . . H4C H 0.7377 0.4620 0.5211 0.062 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0253(11) 0.0569(14) 0.0446(13) -0.0059(11) -0.0017(10) 0.0082(10) N1 0.0391(14) 0.0312(13) 0.0301(13) 0.0049(11) -0.0161(11) -0.0101(11) N3 0.0210(13) 0.0347(14) 0.0394(14) 0.0003(11) -0.0001(12) 0.0026(11) N2 0.0258(13) 0.0339(14) 0.0376(14) 0.0047(12) 0.0033(11) 0.0031(11) C1 0.0275(16) 0.0338(16) 0.0316(16) -0.0015(13) -0.0052(13) 0.0004(12) O1 0.0303(12) 0.0562(14) 0.0433(13) 0.0046(11) -0.0002(10) 0.0116(10) C3 0.0357(17) 0.0270(16) 0.0299(16) 0.0021(13) 0.0023(14) 0.0020(13) C7 0.0256(15) 0.0292(15) 0.0354(16) 0.0062(13) -0.0020(13) -0.0007(12) C2 0.0255(15) 0.0268(15) 0.0343(16) 0.0019(13) -0.0008(13) -0.0035(12) C8 0.0274(15) 0.0335(16) 0.0316(16) 0.0034(13) 0.0013(13) -0.0046(12) C6 0.0262(15) 0.0342(16) 0.0321(16) 0.0027(13) -0.0048(13) 0.0013(12) C10 0.0318(17) 0.0374(18) 0.063(2) -0.0098(16) 0.0000(16) 0.0006(14) C9 0.0419(19) 0.050(2) 0.058(2) 0.0230(18) -0.0103(17) -0.0025(16) C5 0.046(2) 0.0387(19) 0.056(2) 0.0062(16) -0.0060(16) -0.0116(15) C4 0.0366(18) 0.0468(19) 0.0403(18) 0.0033(15) 0.0028(14) 0.0059(15) _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 O2 N3 1.420(3) . ? N1 C6 1.448(3) . ? N1 C1 1.450(3) . ? N3 C8 1.261(3) . ? N2 C3 1.260(3) . ? N2 O1 1.411(3) . ? C1 C2 1.526(4) . ? C3 C2 1.501(4) . ? C7 C8 1.509(4) . ? C7 C10 1.527(4) . ? C7 C6 1.534(4) . ? C7 C9 1.537(4) . ? C2 C4 1.526(4) . ? C2 C5 1.532(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 C6 N1 C1 113.5(2) . . ? C8 N3 O2 112.1(2) . . ? C3 N2 O1 112.1(2) . . ? N1 C1 C2 112.6(2) . . ? N2 C3 C2 122.8(2) . . ? C8 C7 C10 111.5(2) . . ? C8 C7 C6 107.4(2) . . ? C10 C7 C6 110.8(2) . . ? C8 C7 C9 108.2(2) . . ? C10 C7 C9 109.8(2) . . ? C6 C7 C9 109.0(2) . . ? C3 C2 C1 107.9(2) . . ? C3 C2 C4 111.8(2) . . ? C1 C2 C4 111.0(2) . . ? C3 C2 C5 107.9(2) . . ? C1 C2 C5 108.2(2) . . ? C4 C2 C5 109.9(2) . . ? N3 C8 C7 121.6(3) . . ? N1 C6 C7 112.7(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.424 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.050 #===END of CIF for SI ========================================== data_CdSII _database_code_depnum_ccdc_archive 'CCDC 645819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H50 Cd N6, 2(N O3), H2 O' _chemical_formula_sum 'C20 H52 Cd N8 O7' _chemical_formula_weight 629.10 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 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' _cell_length_a 14.8977(10) _cell_length_b 20.0088(14) _cell_length_c 9.9762(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.6110(10) _cell_angle_gamma 90.00 _cell_volume 2947.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8760 _cell_measurement_theta_min 2.5085 _cell_measurement_theta_max 27.541 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6475 _exptl_absorpt_correction_T_max 0.8806 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8357 _diffrn_reflns_av_R_equivalents 0.0131 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4169 _reflns_number_gt 4109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+0.3286P] 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 H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.346(14) _refine_ls_number_reflns 4169 _refine_ls_number_parameters 337 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0152 _refine_ls_R_factor_gt 0.0148 _refine_ls_wR_factor_ref 0.0396 _refine_ls_wR_factor_gt 0.0392 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.004 _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 Cd1 Cd 0.581035(16) 0.716024(5) 0.283975(19) 0.02142(5) Uani 1 1 d . . . N2 N 0.57743(12) 0.59968(8) 0.21050(18) 0.0232(4) Uani 1 1 d . . . H1C H 0.5767 0.5971 0.1183 0.028 Uiso 1 1 calc R . . N7 N 0.28628(13) 0.85043(10) 0.2313(2) 0.0345(5) Uani 1 1 d . . . O3 O 0.29654(13) 0.82096(9) 0.12352(19) 0.0463(4) Uani 1 1 d . . . O2 O 0.34770(16) 0.84834(11) 0.3275(2) 0.0560(6) Uani 1 1 d . . . O1 O 0.21402(13) 0.88112(10) 0.2386(2) 0.0550(5) Uani 1 1 d . . . C3 C 0.49628(18) 0.56647(13) 0.2521(3) 0.0266(6) Uani 1 1 d . . . H1A H 0.4908 0.5795 0.3454 0.032 Uiso 1 1 calc R . . H1B H 0.5054 0.5180 0.2510 0.032 Uiso 1 1 calc R . . C6 C 0.66061(18) 0.56820(14) 0.2812(3) 0.0279(6) Uani 1 1 d . . . H6A H 0.6515 0.5197 0.2825 0.034 Uiso 1 1 calc R . . H6B H 0.6693 0.5837 0.3753 0.034 Uiso 1 1 calc R . . C2 C 0.40736(14) 0.58318(10) 0.1627(2) 0.0270(5) Uani 1 1 d . . . C1 C 0.39612(14) 0.65848(10) 0.1345(2) 0.0272(5) Uani 1 1 d . . . H3A H 0.4334 0.6709 0.0645 0.033 Uiso 1 1 calc R . . H3B H 0.3328 0.6674 0.0986 0.033 Uiso 1 1 calc R . . N1 N 0.4215(2) 0.70129(13) 0.2542(3) 0.0278(6) Uani 1 1 d . . . H2A H 0.4039 0.6817 0.3289 0.033 Uiso 1 1 calc R . . H2B H 0.3934 0.7416 0.2419 0.033 Uiso 1 1 calc R . . N3 N 0.7392(2) 0.70200(13) 0.2982(3) 0.0274(6) Uani 1 1 d . . . H3C H 0.7664 0.7423 0.2906 0.033 Uiso 1 1 calc R . . H3D H 0.7613 0.6838 0.3795 0.033 Uiso 1 1 calc R . . C7 C 0.74718(14) 0.58270(10) 0.2186(2) 0.0271(5) Uani 1 1 d . . . C8 C 0.75831(15) 0.65723(11) 0.1872(2) 0.0293(5) Uani 1 1 d . . . H8A H 0.8204 0.6651 0.1687 0.035 Uiso 1 1 calc R . . H8B H 0.7174 0.6686 0.1052 0.035 Uiso 1 1 calc R . . C5 C 0.3305(2) 0.55677(15) 0.2371(3) 0.0350(7) Uani 1 1 d . . . H5A H 0.2725 0.5669 0.1845 0.052 Uiso 1 1 calc R . . H5B H 0.3339 0.5780 0.3250 0.052 Uiso 1 1 calc R . . H5C H 0.3365 0.5088 0.2486 0.052 Uiso 1 1 calc R . . C10 C 0.82616(19) 0.55831(16) 0.3206(3) 0.0340(7) Uani 1 1 d . . . H10A H 0.8180 0.5113 0.3396 0.051 Uiso 1 1 calc R . . H10B H 0.8281 0.5838 0.4037 0.051 Uiso 1 1 calc R . . H10C H 0.8825 0.5644 0.2833 0.051 Uiso 1 1 calc R . . N5 N 0.58335(12) 0.83467(8) 0.35347(19) 0.0237(4) Uani 1 1 d . . . H4D H 0.5257 0.8498 0.3591 0.028 Uiso 1 1 calc R . . N6 N 0.57711(13) 0.69690(9) 0.51618(19) 0.0270(4) Uani 1 1 d . . . H6C H 0.5485 0.6575 0.5279 0.032 Uiso 1 1 calc R . . H6D H 0.6345 0.6943 0.5602 0.032 Uiso 1 1 calc R . . C9 C 0.74716(19) 0.54448(12) 0.0863(3) 0.0406(6) Uani 1 1 d . . . H9A H 0.6964 0.5591 0.0219 0.061 Uiso 1 1 calc R . . H9B H 0.7418 0.4970 0.1030 0.061 Uiso 1 1 calc R . . H9C H 0.8033 0.5531 0.0499 0.061 Uiso 1 1 calc R . . C16 C 0.63798(17) 0.83454(13) 0.4874(3) 0.0251(6) Uani 1 1 d . . . H16A H 0.6635 0.8793 0.5052 0.030 Uiso 1 1 calc R . . H16B H 0.6887 0.8035 0.4854 0.030 Uiso 1 1 calc R . . C11 C 0.52421(19) 0.82748(13) 0.0573(3) 0.0280(6) Uani 1 1 d . . . H13A H 0.4695 0.8170 0.0979 0.034 Uiso 1 1 calc R . . H13B H 0.5058 0.8363 -0.0391 0.034 Uiso 1 1 calc R . . N4 N 0.58567(14) 0.76853(9) 0.07144(19) 0.0281(4) Uani 1 1 d . . . H5D H 0.6433 0.7818 0.0646 0.034 Uiso 1 1 calc R . . H5E H 0.5684 0.7389 0.0037 0.034 Uiso 1 1 calc R . . C13 C 0.62755(15) 0.87589(10) 0.2580(2) 0.0257(5) Uani 1 1 d . . . H11A H 0.6823 0.8528 0.2383 0.031 Uiso 1 1 calc R . . H11B H 0.6464 0.9183 0.3021 0.031 Uiso 1 1 calc R . . C12 C 0.56799(15) 0.89089(10) 0.1243(2) 0.0268(5) Uani 1 1 d . . . C17 C 0.58645(14) 0.81489(10) 0.6040(2) 0.0255(4) Uani 1 1 d . . . C15 C 0.62842(17) 0.92507(12) 0.0317(2) 0.0383(6) Uani 1 1 d . . . H15A H 0.6556 0.9647 0.0760 0.057 Uiso 1 1 calc R . . H15B H 0.5921 0.9377 -0.0525 0.057 Uiso 1 1 calc R . . H15C H 0.6757 0.8945 0.0130 0.057 Uiso 1 1 calc R . . C18 C 0.52821(15) 0.75246(11) 0.5720(2) 0.0277(5) Uani 1 1 d . . . H18A H 0.5060 0.7372 0.6550 0.033 Uiso 1 1 calc R . . H18B H 0.4755 0.7643 0.5068 0.033 Uiso 1 1 calc R . . C14 C 0.49152(17) 0.93940(11) 0.1497(3) 0.0366(5) Uani 1 1 d . . . H14A H 0.4529 0.9182 0.2083 0.055 Uiso 1 1 calc R . . H14B H 0.4559 0.9508 0.0643 0.055 Uiso 1 1 calc R . . H14C H 0.5177 0.9797 0.1927 0.055 Uiso 1 1 calc R . . C4 C 0.40181(18) 0.54768(11) 0.0259(2) 0.0374(5) Uani 1 1 d . . . H4A H 0.3454 0.5594 -0.0292 0.056 Uiso 1 1 calc R . . H4B H 0.4042 0.4997 0.0400 0.056 Uiso 1 1 calc R . . H4C H 0.4523 0.5615 -0.0198 0.056 Uiso 1 1 calc R . . C20 C 0.65564(16) 0.80280(12) 0.7303(2) 0.0320(5) Uani 1 1 d . . . H20A H 0.6242 0.7888 0.8047 0.048 Uiso 1 1 calc R . . H20B H 0.6886 0.8438 0.7546 0.048 Uiso 1 1 calc R . . H20C H 0.6978 0.7682 0.7113 0.048 Uiso 1 1 calc R . . C19 C 0.52280(18) 0.87167(13) 0.6334(3) 0.0396(6) Uani 1 1 d . . . H19A H 0.4901 0.8587 0.7072 0.059 Uiso 1 1 calc R . . H19B H 0.4801 0.8806 0.5533 0.059 Uiso 1 1 calc R . . H19C H 0.5580 0.9116 0.6584 0.059 Uiso 1 1 calc R . . N8 N 0.35947(15) 0.66188(10) 0.6331(3) 0.0441(6) Uani 1 1 d . . . O4 O 0.4084(4) 0.6266(3) 0.5682(7) 0.0551(14) Uani 0.624(8) 1 d P A 1 O5 O 0.2914(4) 0.6954(3) 0.5564(8) 0.0517(11) Uani 0.624(8) 1 d P A 1 O6 O 0.3604(7) 0.6702(5) 0.7460(8) 0.056(2) Uani 0.624(8) 1 d P A 1 O4A O 0.4266(7) 0.6212(5) 0.6349(11) 0.0551(14) Uani 0.376(8) 1 d P A 2 O5A O 0.3171(7) 0.6793(6) 0.5514(16) 0.0517(11) Uani 0.376(8) 1 d P A 2 O6A O 0.3638(11) 0.6776(9) 0.7715(16) 0.050(4) Uiso 0.376(8) 1 d P A 2 O7 O 0.56012(13) 0.64567(9) 0.8831(2) 0.0463(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02398(7) 0.01903(7) 0.02129(7) -0.00102(8) 0.00314(4) 0.00019(8) N2 0.0261(9) 0.0204(8) 0.0231(9) 0.0029(7) 0.0033(7) 0.0012(7) N7 0.0340(11) 0.0249(10) 0.0451(14) 0.0021(9) 0.0064(9) -0.0044(8) O3 0.0517(11) 0.0461(10) 0.0422(11) -0.0067(9) 0.0098(9) -0.0023(8) O2 0.0509(12) 0.0652(14) 0.0481(13) -0.0005(10) -0.0071(10) -0.0012(11) O1 0.0438(11) 0.0438(10) 0.0798(16) 0.0019(10) 0.0175(10) 0.0094(9) C3 0.0276(13) 0.0190(12) 0.0330(14) 0.0024(10) 0.0030(10) -0.0009(10) C6 0.0290(13) 0.0238(12) 0.0305(14) 0.0042(10) 0.0020(10) 0.0030(10) C2 0.0274(10) 0.0247(10) 0.0278(11) 0.0007(9) -0.0007(9) -0.0040(8) C1 0.0272(11) 0.0255(10) 0.0275(11) -0.0006(9) -0.0020(9) -0.0006(8) N1 0.0282(14) 0.0207(10) 0.0338(15) 0.0019(11) 0.0010(11) -0.0009(11) N3 0.0268(14) 0.0261(11) 0.0293(14) 0.0018(11) 0.0042(10) -0.0017(11) C7 0.0294(11) 0.0256(10) 0.0271(12) 0.0028(9) 0.0065(9) 0.0059(8) C8 0.0292(11) 0.0291(11) 0.0314(12) 0.0022(9) 0.0110(9) 0.0043(9) C5 0.0295(17) 0.0342(16) 0.0393(18) 0.0056(13) -0.0026(13) -0.0040(13) C10 0.0271(17) 0.0358(17) 0.0398(17) 0.0091(12) 0.0075(13) 0.0081(12) N5 0.0198(8) 0.0256(9) 0.0255(9) -0.0023(7) 0.0028(7) -0.0030(7) N6 0.0330(10) 0.0228(8) 0.0255(10) -0.0002(8) 0.0055(8) -0.0020(8) C9 0.0510(15) 0.0345(12) 0.0383(14) -0.0041(11) 0.0139(12) 0.0077(11) C16 0.0274(14) 0.0253(12) 0.0231(12) -0.0019(10) 0.0057(10) -0.0053(10) C11 0.0345(15) 0.0243(12) 0.0224(12) 0.0000(10) -0.0063(10) 0.0006(11) N4 0.0377(11) 0.0225(8) 0.0238(10) -0.0023(7) 0.0035(8) 0.0014(8) C13 0.0289(11) 0.0221(10) 0.0262(12) -0.0005(9) 0.0041(9) -0.0047(9) C12 0.0337(11) 0.0192(10) 0.0272(12) 0.0017(8) 0.0029(9) -0.0030(8) C17 0.0285(11) 0.0266(11) 0.0221(11) -0.0036(9) 0.0062(9) -0.0002(9) C15 0.0474(14) 0.0347(12) 0.0321(13) 0.0058(10) 0.0028(11) -0.0080(11) C18 0.0295(11) 0.0305(12) 0.0244(11) -0.0020(9) 0.0079(9) -0.0020(9) C14 0.0401(13) 0.0244(11) 0.0436(14) 0.0015(10) -0.0011(11) 0.0043(9) C4 0.0477(14) 0.0298(11) 0.0331(13) -0.0056(10) -0.0009(11) -0.0058(10) C20 0.0378(13) 0.0368(12) 0.0216(12) -0.0022(10) 0.0039(10) -0.0038(10) C19 0.0451(14) 0.0377(13) 0.0383(14) -0.0087(11) 0.0141(11) 0.0070(11) N8 0.0340(12) 0.0342(11) 0.0669(19) -0.0027(12) 0.0166(12) -0.0106(9) O4 0.057(2) 0.0396(14) 0.077(4) -0.024(3) 0.039(3) -0.0097(15) O5 0.032(3) 0.052(3) 0.0688(18) 0.007(2) -0.001(3) 0.0130(19) O6 0.073(4) 0.068(4) 0.027(4) -0.001(3) 0.006(3) -0.003(2) O4A 0.057(2) 0.0396(14) 0.077(4) -0.024(3) 0.039(3) -0.0097(15) O5A 0.032(3) 0.052(3) 0.0688(18) 0.007(2) -0.001(3) 0.0130(19) O7 0.0555(11) 0.0454(10) 0.0390(10) -0.0020(8) 0.0095(8) -0.0065(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N6 2.3562(19) . ? Cd1 N3 2.358(3) . ? Cd1 N1 2.375(3) . ? Cd1 N4 2.3755(19) . ? Cd1 N2 2.4391(16) . ? Cd1 N5 2.4720(16) . ? N2 C6 1.483(3) . ? N2 C3 1.486(3) . ? N7 O2 1.236(3) . ? N7 O1 1.250(3) . ? N7 O3 1.253(3) . ? C3 C2 1.533(3) . ? C6 C7 1.533(4) . ? C2 C4 1.531(3) . ? C2 C1 1.538(3) . ? C2 C5 1.539(4) . ? C1 N1 1.478(4) . ? N3 C8 1.481(4) . ? C7 C9 1.526(3) . ? C7 C10 1.530(3) . ? C7 C8 1.537(3) . ? N5 C16 1.469(3) . ? N5 C13 1.479(3) . ? N6 C18 1.478(3) . ? C16 C17 1.528(3) . ? C11 N4 1.488(3) . ? C11 C12 1.539(3) . ? C13 C12 1.531(3) . ? C12 C15 1.534(3) . ? C12 C14 1.543(3) . ? C17 C18 1.530(3) . ? C17 C19 1.533(3) . ? C17 C20 1.538(3) . ? N8 O5A 1.024(13) . ? N8 O6 1.137(8) . ? N8 O4 1.255(6) . ? N8 O4A 1.287(11) . ? N8 O5 1.363(7) . ? N8 O6A 1.409(14) . ? 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 Cd1 N3 94.38(9) . . ? N6 Cd1 N1 87.03(9) . . ? N3 Cd1 N1 165.55(5) . . ? N6 Cd1 N4 163.09(6) . . ? N3 Cd1 N4 87.67(9) . . ? N1 Cd1 N4 95.17(9) . . ? N6 Cd1 N2 97.93(6) . . ? N3 Cd1 N2 83.48(8) . . ? N1 Cd1 N2 82.08(8) . . ? N4 Cd1 N2 98.97(6) . . ? N6 Cd1 N5 83.19(6) . . ? N3 Cd1 N5 96.93(8) . . ? N1 Cd1 N5 97.52(8) . . ? N4 Cd1 N5 79.90(6) . . ? N2 Cd1 N5 178.77(6) . . ? C6 N2 C3 109.68(16) . . ? C6 N2 Cd1 106.18(14) . . ? C3 N2 Cd1 109.21(14) . . ? O2 N7 O1 121.7(2) . . ? O2 N7 O3 119.2(2) . . ? O1 N7 O3 119.0(2) . . ? N2 C3 C2 114.4(2) . . ? N2 C6 C7 114.9(2) . . ? C4 C2 C3 111.0(2) . . ? C4 C2 C1 107.44(18) . . ? C3 C2 C1 112.64(17) . . ? C4 C2 C5 108.4(2) . . ? C3 C2 C5 106.6(2) . . ? C1 C2 C5 110.8(2) . . ? N1 C1 C2 114.21(19) . . ? C1 N1 Cd1 108.51(18) . . ? C8 N3 Cd1 108.47(18) . . ? C9 C7 C10 109.1(2) . . ? C9 C7 C6 110.7(2) . . ? C10 C7 C6 106.4(2) . . ? C9 C7 C8 107.29(19) . . ? C10 C7 C8 110.55(19) . . ? C6 C7 C8 112.71(19) . . ? N3 C8 C7 113.4(2) . . ? C16 N5 C13 110.24(17) . . ? C16 N5 Cd1 103.81(14) . . ? C13 N5 Cd1 110.23(13) . . ? C18 N6 Cd1 109.03(13) . . ? N5 C16 C17 114.8(2) . . ? N4 C11 C12 113.1(2) . . ? C11 N4 Cd1 110.19(15) . . ? N5 C13 C12 114.48(17) . . ? C13 C12 C15 107.08(18) . . ? C13 C12 C11 112.36(18) . . ? C15 C12 C11 110.8(2) . . ? C13 C12 C14 109.59(19) . . ? C15 C12 C14 108.89(19) . . ? C11 C12 C14 108.09(19) . . ? C16 C17 C18 112.31(17) . . ? C16 C17 C19 109.94(19) . . ? C18 C17 C19 107.27(19) . . ? C16 C17 C20 108.34(18) . . ? C18 C17 C20 110.02(18) . . ? C19 C17 C20 108.91(19) . . ? N6 C18 C17 113.48(19) . . ? O5A N8 O6 131.6(9) . . ? O5A N8 O4 96.9(7) . . ? O6 N8 O4 131.5(6) . . ? O5A N8 O4A 128.5(7) . . ? O6 N8 O4A 99.9(7) . . ? O4 N8 O4A 31.6(4) . . ? O5A N8 O5 18.4(9) . . ? O6 N8 O5 113.2(6) . . ? O4 N8 O5 115.3(4) . . ? O4A N8 O5 146.9(5) . . ? O5A N8 O6A 130.3(10) . . ? O6 N8 O6A 4.9(12) . . ? O4 N8 O6A 132.6(8) . . ? O4A N8 O6A 101.1(8) . . ? O5 N8 O6A 112.0(8) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.304 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.038 #===END of CIF for Cd(SII)2(NO3)2.H2O ====================== data_H2TMhppHCO3 _database_code_depnum_ccdc_archive 'CCDC 645820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H22 N3, H1 C1 O3' _chemical_formula_sum 'C12 H23 N3 O3' _chemical_formula_weight 257.33 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' _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 13.853(3) _cell_length_b 15.973(4) _cell_length_c 13.067(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.038(4) _cell_angle_gamma 90.00 _cell_volume 2855.6(11) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3571 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.048 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9657 _exptl_absorpt_correction_T_max 0.9940 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12778 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.79 _reflns_number_total 12845 _reflns_number_gt 5634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12845 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1553 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1218 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _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 O3 O 0.66377(9) 0.07410(7) 0.45921(9) 0.0390(3) Uani 1 1 d . . . H3A H 0.7217 0.0847 0.4825 0.059 Uiso 1 1 calc R . . O1A O 0.97655(10) 0.16481(8) 0.60413(11) 0.0494(4) Uani 1 1 d . . . O3A O 0.84129(10) 0.23171(7) 0.53986(10) 0.0471(4) Uani 1 1 d . . . H3AC H 0.7862 0.2211 0.5075 0.071 Uiso 1 1 calc R . . O2A O 0.84552(10) 0.09185(8) 0.53575(10) 0.0436(4) Uani 1 1 d . . . O2 O 0.66482(10) 0.21319(8) 0.43768(10) 0.0439(4) Uani 1 1 d . . . O1 O 0.53266(10) 0.13779(8) 0.37706(11) 0.0485(4) Uani 1 1 d . . . N3 N 0.43148(11) 0.84367(9) 0.33199(12) 0.0353(4) Uani 1 1 d . . . N3A N 1.08461(11) 0.88051(9) 0.69911(12) 0.0364(4) Uani 1 1 d . . . N2 N 0.56896(12) 0.91464(10) 0.41142(12) 0.0415(4) Uani 1 1 d . . . H2A H 0.5999 0.9621 0.4213 0.050 Uiso 1 1 calc R . . C4 C 0.47711(15) 0.91514(12) 0.36168(14) 0.0334(5) Uani 1 1 d . . . N1 N 0.43418(12) 0.98890(9) 0.33815(12) 0.0389(4) Uani 1 1 d . . . H1A H 0.4679 1.0345 0.3526 0.047 Uiso 1 1 calc R . . C4A C 1.04111(15) 0.94991(12) 0.65731(14) 0.0349(5) Uani 1 1 d . . . C5A C 1.18676(14) 0.88068(12) 0.74763(15) 0.0399(5) Uani 1 1 d . . . H5AA H 1.2278 0.8655 0.6959 0.048 Uiso 1 1 calc R . . H5AB H 1.1964 0.8384 0.8026 0.048 Uiso 1 1 calc R . . N2A N 1.08770(11) 1.02326(9) 0.66571(12) 0.0378(4) Uani 1 1 d . . . H2AA H 1.0554 1.0684 0.6449 0.045 Uiso 1 1 calc R . . C12 C 0.61750(15) 0.14545(12) 0.42261(14) 0.0335(5) Uani 1 1 d . . . N1A N 0.94891(12) 0.94838(9) 0.61045(12) 0.0421(4) Uani 1 1 d . . . H1AA H 0.9214 0.9957 0.5898 0.051 Uiso 1 1 calc R . . C12A C 0.89055(16) 0.16062(12) 0.56137(14) 0.0344(5) Uani 1 1 d . . . C3 C 0.33087(14) 0.84278(11) 0.27799(14) 0.0389(5) Uani 1 1 d . . . H3B H 0.2863 0.8363 0.3288 0.047 Uiso 1 1 calc R . . H3C H 0.3218 0.7945 0.2312 0.047 Uiso 1 1 calc R . . C2 C 0.30501(14) 0.92258(12) 0.21579(14) 0.0382(5) Uani 1 1 d . . . C5 C 0.47547(14) 0.76264(11) 0.36407(15) 0.0420(5) Uani 1 1 d . . . H5A H 0.4516 0.7205 0.3117 0.050 Uiso 1 1 calc R . . H5B H 0.4548 0.7457 0.4294 0.050 Uiso 1 1 calc R . . C3A C 1.03543(14) 0.79940(11) 0.68287(16) 0.0431(5) Uani 1 1 d . . . H3AA H 1.0600 0.7622 0.7407 0.052 Uiso 1 1 calc R . . H3AB H 1.0512 0.7740 0.6192 0.052 Uiso 1 1 calc R . . C7A C 1.19055(14) 1.03004(11) 0.70849(15) 0.0402(5) Uani 1 1 d . . . H7AA H 1.2042 1.0864 0.7367 0.048 Uiso 1 1 calc R . . H7AB H 1.2300 1.0213 0.6534 0.048 Uiso 1 1 calc R . . C6A C 1.21873(14) 0.96579(12) 0.79359(14) 0.0391(5) Uani 1 1 d . . . C1 C 0.33311(15) 0.99549(12) 0.28931(15) 0.0412(5) Uani 1 1 d . . . H1B H 0.3235 1.0482 0.2508 0.049 Uiso 1 1 calc R . . H1C H 0.2907 0.9960 0.3427 0.049 Uiso 1 1 calc R . . C7 C 0.61985(15) 0.83861(12) 0.44990(16) 0.0472(5) Uani 1 1 d . . . H7A H 0.6065 0.8265 0.5199 0.057 Uiso 1 1 calc R . . H7B H 0.6905 0.8466 0.4537 0.057 Uiso 1 1 calc R . . C8 C 0.36170(16) 0.92671(12) 0.12395(15) 0.0491(6) Uani 1 1 d . . . H8A H 0.4313 0.9260 0.1495 0.074 Uiso 1 1 calc R . . H8B H 0.3449 0.9779 0.0853 0.074 Uiso 1 1 calc R . . H8C H 0.3446 0.8789 0.0790 0.074 Uiso 1 1 calc R . . C2A C 0.92532(15) 0.80707(12) 0.67452(16) 0.0432(5) Uani 1 1 d . . . C6 C 0.58646(15) 0.76505(12) 0.37850(16) 0.0432(5) Uani 1 1 d . . . C9 C 0.19464(15) 0.92360(13) 0.17760(16) 0.0524(6) Uani 1 1 d . . . H9A H 0.1600 0.9209 0.2365 0.079 Uiso 1 1 calc R . . H9B H 0.1769 0.8757 0.1329 0.079 Uiso 1 1 calc R . . H9C H 0.1771 0.9748 0.1392 0.079 Uiso 1 1 calc R . . C9A C 0.89837(16) 0.83404(13) 0.77909(17) 0.0559(6) Uani 1 1 d . . . H9AA H 0.9203 0.7918 0.8309 0.084 Uiso 1 1 calc R . . H9AB H 0.8280 0.8404 0.7726 0.084 Uiso 1 1 calc R . . H9AC H 0.9297 0.8870 0.7999 0.084 Uiso 1 1 calc R . . C11A C 1.16737(16) 0.98474(14) 0.88702(15) 0.0550(6) Uani 1 1 d . . . H11A H 1.0971 0.9847 0.8651 0.082 Uiso 1 1 calc R . . H11B H 1.1879 1.0392 0.9152 0.082 Uiso 1 1 calc R . . H11C H 1.1846 0.9422 0.9397 0.082 Uiso 1 1 calc R . . C10A C 1.32985(15) 0.96563(14) 0.82732(16) 0.0543(6) Uani 1 1 d . . . H10A H 1.3617 0.9536 0.7680 0.081 Uiso 1 1 calc R . . H10B H 1.3474 0.9231 0.8799 0.081 Uiso 1 1 calc R . . H10C H 1.3507 1.0201 0.8554 0.081 Uiso 1 1 calc R . . C1A C 0.89153(15) 0.87273(12) 0.59177(16) 0.0462(5) Uani 1 1 d . . . H1AB H 0.8979 0.8503 0.5234 0.055 Uiso 1 1 calc R . . H1AC H 0.8224 0.8857 0.5921 0.055 Uiso 1 1 calc R . . C8A C 0.87990(17) 0.72267(13) 0.64098(19) 0.0646(7) Uani 1 1 d . . . H8AA H 0.8980 0.7069 0.5749 0.097 Uiso 1 1 calc R . . H8AB H 0.8093 0.7267 0.6342 0.097 Uiso 1 1 calc R . . H8AC H 0.9034 0.6807 0.6925 0.097 Uiso 1 1 calc R . . C10 C 0.62118(16) 0.77620(13) 0.27352(17) 0.0581(7) Uani 1 1 d . . . H10D H 0.5953 0.8282 0.2419 0.087 Uiso 1 1 calc R . . H10E H 0.5981 0.7297 0.2285 0.087 Uiso 1 1 calc R . . H10F H 0.6920 0.7778 0.2837 0.087 Uiso 1 1 calc R . . C11 C 0.62627(18) 0.68343(13) 0.4298(2) 0.0700(7) Uani 1 1 d . . . H11D H 0.6037 0.6772 0.4960 0.105 Uiso 1 1 calc R . . H11E H 0.6971 0.6847 0.4405 0.105 Uiso 1 1 calc R . . H11F H 0.6032 0.6366 0.3853 0.105 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 O3 0.0418(9) 0.0277(7) 0.0460(8) 0.0014(6) 0.0023(7) -0.0015(6) O1A 0.0413(10) 0.0404(9) 0.0628(10) -0.0004(7) -0.0035(8) 0.0013(7) O3A 0.0464(9) 0.0296(8) 0.0633(10) -0.0020(7) 0.0024(7) 0.0047(7) O2A 0.0465(9) 0.0281(8) 0.0531(9) 0.0020(6) -0.0020(7) 0.0029(7) O2 0.0476(9) 0.0259(7) 0.0576(9) 0.0054(6) 0.0069(7) -0.0021(7) O1 0.0418(10) 0.0380(9) 0.0621(10) 0.0013(7) -0.0027(8) 0.0001(7) N3 0.0394(10) 0.0274(9) 0.0403(10) -0.0032(7) 0.0102(8) -0.0039(8) N3A 0.0368(11) 0.0312(9) 0.0429(10) 0.0097(7) 0.0119(8) 0.0054(8) N2 0.0432(12) 0.0322(10) 0.0483(11) -0.0043(8) 0.0045(9) -0.0055(8) C4 0.0414(13) 0.0294(11) 0.0319(11) -0.0035(9) 0.0133(10) -0.0043(10) N1 0.0462(12) 0.0254(9) 0.0457(11) -0.0033(7) 0.0089(9) -0.0032(8) C4A 0.0389(13) 0.0330(12) 0.0348(12) 0.0055(9) 0.0124(10) 0.0046(10) C5A 0.0409(13) 0.0386(12) 0.0424(12) 0.0117(9) 0.0135(10) 0.0108(10) N2A 0.0385(11) 0.0289(9) 0.0453(10) 0.0066(7) 0.0046(8) 0.0032(8) C12 0.0427(14) 0.0281(11) 0.0319(11) 0.0024(9) 0.0125(10) 0.0045(10) N1A 0.0429(12) 0.0289(9) 0.0522(11) 0.0092(8) 0.0002(9) 0.0019(8) C12A 0.0435(14) 0.0294(11) 0.0320(11) 0.0013(9) 0.0117(10) 0.0041(10) C3 0.0439(14) 0.0362(12) 0.0383(12) -0.0013(9) 0.0121(10) -0.0053(10) C2 0.0459(14) 0.0362(11) 0.0332(11) -0.0002(9) 0.0086(10) -0.0033(10) C5 0.0486(14) 0.0295(11) 0.0509(14) -0.0016(9) 0.0176(11) 0.0011(10) C3A 0.0518(14) 0.0288(12) 0.0519(14) 0.0071(9) 0.0183(11) 0.0022(10) C7A 0.0411(14) 0.0361(12) 0.0454(13) 0.0007(10) 0.0127(10) -0.0001(10) C6A 0.0381(13) 0.0455(13) 0.0346(12) 0.0020(10) 0.0082(10) 0.0078(10) C1 0.0498(15) 0.0363(12) 0.0382(12) 0.0015(9) 0.0087(10) 0.0025(10) C7 0.0474(14) 0.0425(13) 0.0505(14) -0.0030(11) 0.0040(11) 0.0068(11) C8 0.0637(16) 0.0473(13) 0.0393(13) 0.0000(10) 0.0170(11) -0.0056(11) C2A 0.0432(14) 0.0363(12) 0.0532(14) 0.0088(10) 0.0169(11) -0.0030(10) C6 0.0434(14) 0.0368(12) 0.0509(14) -0.0063(10) 0.0119(11) 0.0032(10) C9 0.0516(15) 0.0543(14) 0.0497(14) 0.0020(11) 0.0036(11) 0.0000(12) C9A 0.0509(15) 0.0574(15) 0.0650(16) 0.0149(12) 0.0264(12) 0.0063(12) C11A 0.0600(16) 0.0685(16) 0.0379(13) 0.0004(11) 0.0123(11) 0.0110(12) C10A 0.0491(15) 0.0607(15) 0.0525(15) -0.0013(11) 0.0062(11) 0.0071(12) C1A 0.0454(14) 0.0404(13) 0.0530(14) 0.0024(10) 0.0089(11) -0.0035(11) C8A 0.0650(17) 0.0431(14) 0.0870(19) 0.0083(12) 0.0157(14) -0.0131(12) C10 0.0488(15) 0.0606(15) 0.0704(17) -0.0216(12) 0.0265(13) -0.0079(12) C11 0.0668(18) 0.0465(15) 0.096(2) -0.0028(13) 0.0112(15) 0.0170(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 O3 C12 1.357(2) . ? O1A C12A 1.236(2) . ? O3A C12A 1.332(2) . ? O2A C12A 1.281(2) . ? O2 C12 1.264(2) . ? O1 C12 1.237(2) . ? N3 C4 1.333(2) . ? N3 C3 1.460(2) . ? N3 C5 1.464(2) . ? N3A C4A 1.337(2) . ? N3A C5A 1.457(2) . ? N3A C3A 1.464(2) . ? N2 C4 1.335(2) . ? N2 C7 1.454(2) . ? C4 N1 1.334(2) . ? N1 C1 1.448(2) . ? C4A N1A 1.327(2) . ? C4A N2A 1.334(2) . ? C5A C6A 1.524(3) . ? N2A C7A 1.450(2) . ? N1A C1A 1.446(2) . ? C3 C2 1.524(2) . ? C2 C1 1.521(2) . ? C2 C9 1.532(3) . ? C2 C8 1.535(2) . ? C5 C6 1.520(3) . ? C3A C2A 1.517(3) . ? C7A C6A 1.519(3) . ? C6A C10A 1.533(3) . ? C6A C11A 1.537(2) . ? C7 C6 1.526(3) . ? C2A C8A 1.523(3) . ? C2A C1A 1.526(3) . ? C2A C9A 1.534(3) . ? C6 C11 1.529(3) . ? C6 C10 1.534(3) . ? 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 C4 N3 C3 121.48(17) . . ? C4 N3 C5 121.13(17) . . ? C3 N3 C5 116.92(15) . . ? C4A N3A C5A 121.40(17) . . ? C4A N3A C3A 120.34(18) . . ? C5A N3A C3A 117.58(15) . . ? C4 N2 C7 123.15(17) . . ? N3 C4 N1 121.04(19) . . ? N3 C4 N2 120.58(18) . . ? N1 C4 N2 118.30(18) . . ? C4 N1 C1 122.07(16) . . ? N1A C4A N2A 118.19(17) . . ? N1A C4A N3A 120.84(18) . . ? N2A C4A N3A 120.90(19) . . ? N3A C5A C6A 112.06(15) . . ? C4A N2A C7A 122.05(16) . . ? O1 C12 O2 126.14(18) . . ? O1 C12 O3 116.53(17) . . ? O2 C12 O3 117.33(19) . . ? C4A N1A C1A 123.85(17) . . ? O1A C12A O2A 124.05(18) . . ? O1A C12A O3A 118.35(18) . . ? O2A C12A O3A 117.60(19) . . ? N3 C3 C2 112.10(15) . . ? C1 C2 C3 106.74(16) . . ? C1 C2 C9 109.93(16) . . ? C3 C2 C9 108.75(16) . . ? C1 C2 C8 110.45(15) . . ? C3 C2 C8 110.28(15) . . ? C9 C2 C8 110.60(17) . . ? N3 C5 C6 112.38(15) . . ? N3A C3A C2A 112.27(15) . . ? N2A C7A C6A 110.83(15) . . ? C7A C6A C5A 106.80(16) . . ? C7A C6A C10A 110.04(16) . . ? C5A C6A C10A 109.17(16) . . ? C7A C6A C11A 110.54(16) . . ? C5A C6A C11A 110.29(16) . . ? C10A C6A C11A 109.95(17) . . ? N1 C1 C2 110.88(15) . . ? N2 C7 C6 110.35(17) . . ? C3A C2A C8A 108.34(16) . . ? C3A C2A C1A 107.42(15) . . ? C8A C2A C1A 109.73(18) . . ? C3A C2A C9A 109.96(18) . . ? C8A C2A C9A 110.96(16) . . ? C1A C2A C9A 110.34(16) . . ? C5 C6 C7 107.38(16) . . ? C5 C6 C11 108.73(17) . . ? C7 C6 C11 109.57(18) . . ? C5 C6 C10 110.20(18) . . ? C7 C6 C10 110.48(16) . . ? C11 C6 C10 110.41(17) . . ? N1A C1A C2A 110.82(17) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.79 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.276 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.065 #===END of CIF for [H2TMhpp][HCO3] ========================== data_SIIIHCL _database_code_depnum_ccdc_archive 'CCDC 645821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H32 Cl N3 O3' _chemical_formula_sum 'C14 H32 Cl N3 O3' _chemical_formula_weight 325.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.5762(9) _cell_length_b 21.295(4) _cell_length_c 6.6890(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1791.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 245 _cell_measurement_theta_min 9.085 _cell_measurement_theta_max 20.815 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9156 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Nonius FAST' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9093 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.34 _reflns_number_total 1673 _reflns_number_gt 1556 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+1.0837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1673 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0438 _refine_ls_R_factor_gt 0.0406 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _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 Cl1 Cl 0.64553(4) 0.2500 0.10337(8) 0.0281(2) Uani 1 2 d S . . N1 N 0.87788(14) 0.2500 0.8360(3) 0.0188(4) Uani 1 2 d S . . H1A H 0.8158 0.2500 0.7662 0.023 Uiso 1 2 calc SR . . H1E H 0.8621 0.2500 0.9688 0.023 Uiso 1 2 calc SR . . O1 O 0.67369(10) 0.34898(6) 0.43865(19) 0.0332(3) Uani 1 1 d . . . H1B H 0.6587 0.3198 0.3612 0.050 Uiso 1 1 calc R . . N2 N 0.76501(11) 0.33305(7) 0.5495(2) 0.0258(3) Uani 1 1 d . . . C1 C 0.94182(12) 0.30738(6) 0.7844(2) 0.0204(3) Uani 1 1 d . . . H1C H 0.9659 0.3034 0.6456 0.024 Uiso 1 1 calc R . . H1D H 1.0053 0.3080 0.8692 0.024 Uiso 1 1 calc R . . C4 C 0.84893(15) 0.38069(8) 1.0259(3) 0.0282(4) Uani 1 1 d . . . H4A H 0.7915 0.3510 1.0551 0.034 Uiso 1 1 calc R . . H4B H 0.9087 0.3702 1.1139 0.034 Uiso 1 1 calc R . . C6 C 0.96707(14) 0.42168(8) 0.7487(3) 0.0285(4) Uani 1 1 d . . . H6A H 0.9322 0.4628 0.7564 0.034 Uiso 1 1 calc R . . H6B H 1.0244 0.4214 0.8479 0.034 Uiso 1 1 calc R . . C3 C 0.79031(12) 0.37584(7) 0.6700(2) 0.0236(4) Uani 1 1 d . . . H3A H 0.7487 0.4125 0.6748 0.028 Uiso 1 1 calc R . . C2 C 0.88486(12) 0.37049(7) 0.8069(2) 0.0205(3) Uani 1 1 d . . . C7 C 1.01636(16) 0.41491(9) 0.5420(3) 0.0404(5) Uani 1 1 d . . . H7A H 1.0667 0.4487 0.5200 0.061 Uiso 1 1 calc R . . H7B H 0.9609 0.4168 0.4414 0.061 Uiso 1 1 calc R . . H7C H 1.0529 0.3749 0.5329 0.061 Uiso 1 1 calc R . . C5 C 0.81033(16) 0.44653(8) 1.0792(3) 0.0355(4) Uani 1 1 d . . . H5A H 0.7896 0.4477 1.2188 0.053 Uiso 1 1 calc R . . H5B H 0.7497 0.4573 0.9963 0.053 Uiso 1 1 calc R . . H5C H 0.8671 0.4765 1.0564 0.053 Uiso 1 1 calc R . . O2 O 0.90984(14) 0.2500 0.2485(2) 0.0328(4) Uani 1 2 d S . . 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 Cl1 0.0226(3) 0.0340(3) 0.0277(3) 0.000 -0.0041(2) 0.000 N1 0.0217(9) 0.0160(9) 0.0187(9) 0.000 0.0020(7) 0.000 O1 0.0267(6) 0.0427(7) 0.0302(6) -0.0072(5) -0.0090(5) 0.0058(5) N2 0.0223(7) 0.0277(7) 0.0273(7) -0.0019(6) -0.0047(5) 0.0019(6) C1 0.0202(7) 0.0182(8) 0.0227(8) -0.0005(6) 0.0008(6) -0.0024(6) C4 0.0402(10) 0.0219(8) 0.0225(9) -0.0026(6) 0.0016(7) 0.0014(7) C6 0.0285(9) 0.0198(8) 0.0372(9) 0.0034(7) -0.0018(7) -0.0045(7) C3 0.0232(8) 0.0215(8) 0.0261(8) -0.0013(6) 0.0007(6) 0.0037(6) C2 0.0238(8) 0.0171(8) 0.0205(8) -0.0003(6) 0.0000(6) -0.0010(6) C7 0.0389(11) 0.0306(9) 0.0517(12) 0.0103(9) 0.0168(9) -0.0028(8) C5 0.0450(11) 0.0275(9) 0.0340(9) -0.0096(7) 0.0041(8) 0.0029(8) O2 0.0308(9) 0.0442(10) 0.0235(9) 0.000 -0.0015(7) 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 Cl1 O1 3.0981(13) . ? N1 C1 1.5030(17) . ? N1 C1 1.5030(17) 7_565 ? O1 N2 1.4085(18) . ? N2 C3 1.258(2) . ? C1 C2 1.530(2) . ? C4 C5 1.526(2) . ? C4 C2 1.549(2) . ? C6 C7 1.522(3) . ? C6 C2 1.552(2) . ? C3 C2 1.505(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 C1 N1 C1 108.77(16) . 7_565 ? N2 O1 Cl1 108.08(9) . . ? C3 N2 O1 111.67(13) . . ? N1 C1 C2 116.16(13) . . ? C5 C4 C2 116.27(14) . . ? C7 C6 C2 115.64(14) . . ? N2 C3 C2 122.35(15) . . ? C3 C2 C1 112.11(13) . . ? C3 C2 C4 109.54(13) . . ? C1 C2 C4 110.67(13) . . ? C3 C2 C6 108.69(13) . . ? C1 C2 C6 106.28(13) . . ? C4 C2 C6 109.46(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.539 _refine_diff_density_min -0.253 _refine_diff_density_rms 0.054 #===END of CIF for SIII.HCl ================================= data_CdSIV2NO3EtOH _database_code_depnum_ccdc_archive 'CCDC 645822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H66 Cd N6, 2(N O3), C2 H6 O' _chemical_formula_sum 'C30 H72 Cd N8 O7' _chemical_formula_weight 769.36 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' Cd Cd -0.8075 1.2024 '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 10.351(2) _cell_length_b 12.056(3) _cell_length_c 16.131(4) _cell_angle_alpha 78.651(5) _cell_angle_beta 77.981(6) _cell_angle_gamma 84.069(6) _cell_volume 1926.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 5935 _cell_measurement_theta_min 2.568 _cell_measurement_theta_max 27.4785 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7103 _exptl_absorpt_correction_T_max 0.8745 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10220 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10220 _reflns_number_gt 9680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.2679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10220 _refine_ls_number_parameters 421 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _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 Cd1 Cd 0.31907(2) 0.045248(18) 0.271371(13) 0.02504(7) Uani 1 1 d . . . N8 N 0.4276(2) 0.1529(2) 0.94667(16) 0.0325(6) Uani 1 1 d . . . N1 N 0.5037(2) 0.0853(2) 0.16122(15) 0.0299(6) Uani 1 1 d . . . H1A H 0.5314 0.0200 0.1406 0.036 Uiso 1 1 calc R . . H1D H 0.4748 0.1353 0.1178 0.036 Uiso 1 1 calc R . . N2 N 0.3638(2) 0.23830(19) 0.28994(15) 0.0255(5) Uani 1 1 d . . . H2A H 0.3372 0.2911 0.2462 0.031 Uiso 1 1 calc R . . N3 N 0.1198(2) 0.0930(2) 0.35837(16) 0.0305(6) Uani 1 1 d . . . H3A H 0.0566 0.0481 0.3544 0.037 Uiso 1 1 calc R . . H3C H 0.1299 0.0803 0.4143 0.037 Uiso 1 1 calc R . . N4 N 0.4512(2) -0.0421(2) 0.36850(16) 0.0309(6) Uani 1 1 d . . . H4A H 0.5111 0.0063 0.3717 0.037 Uiso 1 1 calc R . . H4C H 0.4002 -0.0609 0.4218 0.037 Uiso 1 1 calc R . . N5 N 0.2724(2) -0.15477(18) 0.28144(15) 0.0234(5) Uani 1 1 d . . . H5D H 0.3301 -0.1835 0.2380 0.028 Uiso 1 1 calc R . . N6 N 0.2011(2) 0.0686(2) 0.15817(15) 0.0292(5) Uani 1 1 d . . . H6A H 0.1796 0.1441 0.1441 0.035 Uiso 1 1 calc R . . H6C H 0.2588 0.0486 0.1119 0.035 Uiso 1 1 calc R . . N7 N 0.7795(3) 0.0259(3) 0.41993(15) 0.0380(6) Uani 1 1 d . . . C1 C 0.6224(3) 0.1310(3) 0.1770(2) 0.0331(7) Uani 1 1 d . . . H1B H 0.6912 0.1342 0.1248 0.040 Uiso 1 1 calc R . . H1C H 0.6561 0.0777 0.2231 0.040 Uiso 1 1 calc R . . C29 C 0.8551(4) 0.6028(4) 0.0315(3) 0.0660(11) Uani 1 1 d . . . H29A H 0.8846 0.5323 0.0649 0.099 Uiso 1 1 calc R . . H29B H 0.7815 0.6388 0.0667 0.099 Uiso 1 1 calc R . . H29C H 0.9273 0.6528 0.0130 0.099 Uiso 1 1 calc R . . C2 C 0.6010(3) 0.2489(2) 0.20208(19) 0.0288(6) Uani 1 1 d . . . C30 C 0.8117(4) 0.5788(3) -0.0462(3) 0.0540(10) Uani 1 1 d . . . H30A H 0.8858 0.5408 -0.0809 0.065 Uiso 1 1 calc R . . H30B H 0.7398 0.5272 -0.0272 0.065 Uiso 1 1 calc R . . C3 C 0.5055(3) 0.2504(2) 0.28830(19) 0.0288(6) Uani 1 1 d . . . H3B H 0.5353 0.1890 0.3311 0.035 Uiso 1 1 calc R . . H3D H 0.5126 0.3220 0.3067 0.035 Uiso 1 1 calc R . . C4 C 0.5545(3) 0.3370(3) 0.1291(2) 0.0351(7) Uani 1 1 d . . . H4B H 0.6216 0.3365 0.0765 0.042 Uiso 1 1 calc R . . H4D H 0.4728 0.3127 0.1185 0.042 Uiso 1 1 calc R . . C5 C 0.5287(4) 0.4586(3) 0.1450(2) 0.0491(9) Uani 1 1 d . . . H5A H 0.5002 0.5067 0.0955 0.074 Uiso 1 1 calc R . . H5B H 0.6094 0.4851 0.1536 0.074 Uiso 1 1 calc R . . H5C H 0.4601 0.4613 0.1958 0.074 Uiso 1 1 calc R . . C6 C 0.7362(3) 0.2770(3) 0.2178(2) 0.0374(7) Uani 1 1 d . . . H6B H 0.7245 0.3509 0.2360 0.045 Uiso 1 1 calc R . . H6D H 0.7598 0.2205 0.2659 0.045 Uiso 1 1 calc R . . C7 C 0.8523(3) 0.2804(3) 0.1418(2) 0.0464(9) Uani 1 1 d . . . H7A H 0.9310 0.2987 0.1588 0.070 Uiso 1 1 calc R . . H7B H 0.8321 0.3377 0.0941 0.070 Uiso 1 1 calc R . . H7C H 0.8677 0.2070 0.1242 0.070 Uiso 1 1 calc R . . C8 C 0.2851(3) 0.2613(3) 0.37326(19) 0.0326(7) Uani 1 1 d . . . H8A H 0.3236 0.3228 0.3897 0.039 Uiso 1 1 calc R . . H8B H 0.2925 0.1936 0.4174 0.039 Uiso 1 1 calc R . . C9 C 0.1371(3) 0.2943(3) 0.3732(2) 0.0307(7) Uani 1 1 d . . . C10 C 0.0767(3) 0.2134(2) 0.33218(19) 0.0294(7) Uani 1 1 d . . . H10A H -0.0200 0.2224 0.3481 0.035 Uiso 1 1 calc R . . H10B H 0.1010 0.2343 0.2693 0.035 Uiso 1 1 calc R . . C11 C 0.0633(3) 0.2859(3) 0.4679(2) 0.0425(8) Uani 1 1 d . . . H11A H -0.0289 0.3144 0.4677 0.051 Uiso 1 1 calc R . . H11B H 0.0625 0.2057 0.4948 0.051 Uiso 1 1 calc R . . C12 C 0.1191(4) 0.3494(4) 0.5243(3) 0.0780(15) Uani 1 1 d . . . H12A H 0.0655 0.3384 0.5819 0.117 Uiso 1 1 calc R . . H12B H 0.1179 0.4297 0.4998 0.117 Uiso 1 1 calc R . . H12C H 0.2094 0.3206 0.5270 0.117 Uiso 1 1 calc R . . C13 C 0.1233(3) 0.4158(3) 0.3211(2) 0.0438(8) Uani 1 1 d . . . H13A H 0.1548 0.4679 0.3510 0.053 Uiso 1 1 calc R . . H13B H 0.1820 0.4188 0.2647 0.053 Uiso 1 1 calc R . . C14 C -0.0157(4) 0.4595(3) 0.3066(3) 0.0526(10) Uani 1 1 d . . . H14A H -0.0129 0.5359 0.2734 0.079 Uiso 1 1 calc R . . H14B H -0.0748 0.4599 0.3618 0.079 Uiso 1 1 calc R . . H14C H -0.0476 0.4103 0.2753 0.079 Uiso 1 1 calc R . . C15 C 0.5218(3) -0.1462(2) 0.33972(19) 0.0275(6) Uani 1 1 d . . . H15A H 0.6058 -0.1607 0.3602 0.033 Uiso 1 1 calc R . . H15B H 0.5423 -0.1332 0.2766 0.033 Uiso 1 1 calc R . . C16 C 0.4414(3) -0.2507(2) 0.37260(18) 0.0258(6) Uani 1 1 d . . . C17 C 0.2949(3) -0.2228(2) 0.36540(18) 0.0284(6) Uani 1 1 d . . . H17A H 0.2517 -0.2941 0.3754 0.034 Uiso 1 1 calc R . . H17B H 0.2518 -0.1813 0.4113 0.034 Uiso 1 1 calc R . . C18 C 0.4485(3) -0.2922(3) 0.46897(19) 0.0358(7) Uani 1 1 d . . . H18A H 0.5398 -0.3204 0.4724 0.043 Uiso 1 1 calc R . . H18B H 0.4287 -0.2266 0.4980 0.043 Uiso 1 1 calc R . . C19 C 0.3580(4) -0.3837(3) 0.5188(2) 0.0563(10) Uani 1 1 d . . . H19A H 0.3713 -0.4026 0.5779 0.085 Uiso 1 1 calc R . . H19B H 0.3782 -0.4507 0.4923 0.085 Uiso 1 1 calc R . . H19C H 0.2667 -0.3566 0.5181 0.085 Uiso 1 1 calc R . . C20 C 0.4998(3) -0.3439(2) 0.3192(2) 0.0327(7) Uani 1 1 d . . . H20A H 0.4599 -0.4150 0.3486 0.039 Uiso 1 1 calc R . . H20B H 0.4729 -0.3234 0.2631 0.039 Uiso 1 1 calc R . . C21 C 0.6501(3) -0.3658(3) 0.3037(2) 0.0430(8) Uani 1 1 d . . . H21A H 0.6760 -0.4255 0.2699 0.065 Uiso 1 1 calc R . . H21B H 0.6783 -0.3888 0.3586 0.065 Uiso 1 1 calc R . . H21C H 0.6913 -0.2970 0.2728 0.065 Uiso 1 1 calc R . . C22 C 0.1356(3) -0.1681(2) 0.27260(19) 0.0262(6) Uani 1 1 d . . . H22A H 0.0748 -0.1318 0.3161 0.031 Uiso 1 1 calc R . . H22B H 0.1209 -0.2492 0.2867 0.031 Uiso 1 1 calc R . . C23 C 0.0965(3) -0.1205(2) 0.18449(19) 0.0266(6) Uani 1 1 d . . . C24 C 0.0796(3) 0.0099(2) 0.1671(2) 0.0302(7) Uani 1 1 d . . . H24A H 0.0441 0.0345 0.1142 0.036 Uiso 1 1 calc R . . H24B H 0.0137 0.0339 0.2145 0.036 Uiso 1 1 calc R . . C25 C -0.0413(3) -0.1642(3) 0.1929(2) 0.0381(8) Uani 1 1 d . . . H25A H -0.0336 -0.2472 0.2068 0.046 Uiso 1 1 calc R . . H25B H -0.1004 -0.1374 0.2419 0.046 Uiso 1 1 calc R . . C26 C -0.1071(4) -0.1293(3) 0.1138(3) 0.0578(11) Uani 1 1 d . . . H26A H -0.1928 -0.1611 0.1262 0.087 Uiso 1 1 calc R . . H26B H -0.0515 -0.1574 0.0651 0.087 Uiso 1 1 calc R . . H26C H -0.1185 -0.0473 0.1002 0.087 Uiso 1 1 calc R . . C27 C 0.1982(3) -0.1618(3) 0.1110(2) 0.0347(7) Uani 1 1 d . . . H27A H 0.1696 -0.1299 0.0565 0.042 Uiso 1 1 calc R . . H27B H 0.2832 -0.1310 0.1087 0.042 Uiso 1 1 calc R . . C28 C 0.2205(4) -0.2896(3) 0.1173(2) 0.0517(9) Uani 1 1 d . . . H28A H 0.2861 -0.3066 0.0682 0.077 Uiso 1 1 calc R . . H28B H 0.1380 -0.3213 0.1177 0.077 Uiso 1 1 calc R . . H28C H 0.2518 -0.3224 0.1701 0.077 Uiso 1 1 calc R . . O6 O 0.3675(2) 0.0666(2) 0.98367(15) 0.0474(6) Uani 1 1 d . . . O7 O 0.7677(2) 0.67912(19) -0.09785(16) 0.0483(6) Uani 1 1 d . . . H7D H 0.7051 0.7116 -0.0686 0.072 Uiso 1 1 calc R . . O5 O 0.4398(2) 0.2274(2) 0.98787(15) 0.0490(6) Uani 1 1 d . . . O4 O 0.4772(2) 0.1627(2) 0.86880(14) 0.0472(6) Uani 1 1 d . . . O3 O 0.8350(3) 0.0092(3) 0.34951(19) 0.0851(10) Uani 1 1 d . A . O2 O 0.8436(3) 0.0439(3) 0.4725(2) 0.0933(12) Uani 1 1 d . A . O1 O 0.6582(3) 0.0389(5) 0.4382(3) 0.0634(19) Uani 0.869(13) 1 d P A 1 O1A O 0.679(2) -0.032(2) 0.4681(14) 0.038(7) Uiso 0.131(13) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.02448(11) 0.02611(10) 0.02490(10) -0.00540(9) -0.00463(10) -0.00211(7) N8 0.0287(14) 0.0439(17) 0.0263(14) -0.0092(12) -0.0099(11) 0.0058(12) N1 0.0313(14) 0.0292(13) 0.0297(14) -0.0105(11) -0.0025(11) -0.0017(10) N2 0.0197(12) 0.0328(13) 0.0251(13) -0.0101(10) -0.0017(9) -0.0023(10) N3 0.0285(13) 0.0318(14) 0.0307(14) -0.0068(11) -0.0014(11) -0.0062(11) N4 0.0348(14) 0.0298(13) 0.0304(14) -0.0076(11) -0.0093(11) -0.0020(11) N5 0.0188(11) 0.0273(12) 0.0234(12) -0.0021(10) -0.0046(10) -0.0020(9) N6 0.0351(14) 0.0253(12) 0.0276(13) -0.0050(10) -0.0072(11) -0.0015(10) N7 0.0320(15) 0.0525(17) 0.0286(13) -0.0026(14) -0.0075(13) -0.0040(12) C1 0.0267(16) 0.0363(17) 0.0372(18) -0.0140(14) -0.0015(13) -0.0016(13) C29 0.058(3) 0.062(3) 0.075(3) -0.004(2) -0.016(2) 0.002(2) C2 0.0231(15) 0.0310(15) 0.0340(17) -0.0110(13) -0.0036(12) -0.0036(12) C30 0.051(2) 0.036(2) 0.071(3) -0.0101(19) -0.005(2) 0.0000(17) C3 0.0224(14) 0.0344(15) 0.0324(17) -0.0129(13) -0.0037(12) -0.0049(12) C4 0.0273(16) 0.0400(18) 0.0382(17) -0.0128(15) 0.0007(14) -0.0063(14) C5 0.058(2) 0.0365(19) 0.051(2) -0.0031(16) -0.0089(18) -0.0068(17) C6 0.0238(16) 0.0427(18) 0.048(2) -0.0127(15) -0.0046(14) -0.0065(13) C7 0.0248(17) 0.048(2) 0.065(2) -0.0132(18) -0.0024(16) -0.0056(15) C8 0.0264(16) 0.0462(18) 0.0296(17) -0.0211(14) -0.0013(12) -0.0036(13) C9 0.0253(16) 0.0360(17) 0.0318(17) -0.0149(14) 0.0002(13) -0.0011(13) C10 0.0239(16) 0.0336(16) 0.0316(17) -0.0101(13) -0.0042(12) 0.0003(12) C11 0.0308(17) 0.061(2) 0.039(2) -0.0250(17) 0.0023(14) -0.0037(16) C12 0.065(3) 0.127(4) 0.054(3) -0.061(3) 0.012(2) -0.025(3) C13 0.0355(18) 0.0370(18) 0.057(2) -0.0172(16) 0.0039(16) -0.0025(14) C14 0.051(2) 0.0374(19) 0.066(3) -0.0095(17) -0.0094(19) 0.0068(16) C15 0.0257(16) 0.0299(15) 0.0272(16) -0.0045(12) -0.0077(12) 0.0002(12) C16 0.0234(15) 0.0283(15) 0.0240(15) 0.0012(12) -0.0065(12) -0.0009(12) C17 0.0252(15) 0.0321(15) 0.0244(15) 0.0031(12) -0.0036(12) -0.0038(12) C18 0.0370(18) 0.0399(18) 0.0288(17) 0.0016(14) -0.0116(14) 0.0011(14) C19 0.049(2) 0.067(3) 0.042(2) 0.0225(19) -0.0106(17) -0.0081(19) C20 0.0361(17) 0.0264(15) 0.0372(18) -0.0056(13) -0.0127(14) 0.0022(13) C21 0.0389(19) 0.0393(18) 0.049(2) -0.0076(15) -0.0087(15) 0.0081(15) C22 0.0234(14) 0.0264(14) 0.0279(15) -0.0036(13) -0.0031(12) -0.0041(11) C23 0.0276(15) 0.0265(15) 0.0277(16) -0.0053(12) -0.0082(12) -0.0039(12) C24 0.0265(16) 0.0316(16) 0.0333(17) -0.0054(13) -0.0088(13) 0.0000(12) C25 0.0329(18) 0.0396(18) 0.046(2) -0.0086(15) -0.0145(15) -0.0038(14) C26 0.052(2) 0.060(2) 0.074(3) -0.005(2) -0.042(2) -0.0129(19) C27 0.0375(19) 0.0363(17) 0.0327(17) -0.0118(14) -0.0075(14) -0.0005(14) C28 0.056(2) 0.045(2) 0.057(2) -0.0251(18) -0.0060(18) 0.0039(17) O6 0.0507(15) 0.0529(15) 0.0353(13) -0.0061(11) 0.0019(11) -0.0126(12) O7 0.0456(14) 0.0407(13) 0.0519(15) -0.0041(11) 0.0001(11) 0.0001(11) O5 0.0549(15) 0.0504(15) 0.0482(15) -0.0270(12) -0.0113(12) 0.0044(12) O4 0.0530(15) 0.0624(16) 0.0259(12) -0.0112(11) 0.0004(10) -0.0118(12) O3 0.091(2) 0.108(3) 0.0569(19) -0.0460(18) 0.0219(16) -0.021(2) O2 0.063(2) 0.160(4) 0.058(2) 0.015(2) -0.0275(16) -0.046(2) O1 0.0263(17) 0.110(5) 0.062(2) -0.037(3) -0.0077(14) -0.0026(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 Cd1 N4 2.320(2) . ? Cd1 N3 2.328(2) . ? Cd1 N1 2.341(2) . ? Cd1 N6 2.358(2) . ? Cd1 N5 2.475(2) . ? Cd1 N2 2.505(2) . ? N8 O4 1.241(3) . ? N8 O5 1.248(3) . ? N8 O6 1.249(3) . ? N1 C1 1.486(4) . ? N2 C8 1.480(3) . ? N2 C3 1.484(3) . ? N3 C10 1.480(4) . ? N4 C15 1.491(4) . ? N5 C22 1.480(3) . ? N5 C17 1.488(3) . ? N6 C24 1.474(4) . ? N7 O3 1.206(3) . ? N7 O1 1.229(4) . ? N7 O2 1.241(4) . ? N7 O1A 1.331(19) . ? C1 C2 1.535(4) . ? C29 C30 1.504(5) . ? C2 C3 1.531(4) . ? C2 C4 1.544(4) . ? C2 C6 1.555(4) . ? C30 O7 1.419(4) . ? C4 C5 1.524(4) . ? C6 C7 1.525(4) . ? C8 C9 1.543(4) . ? C9 C10 1.527(4) . ? C9 C13 1.547(4) . ? C9 C11 1.548(4) . ? C11 C12 1.527(5) . ? C13 C14 1.529(5) . ? C15 C16 1.527(4) . ? C16 C17 1.542(4) . ? C16 C20 1.547(4) . ? C16 C18 1.551(4) . ? C18 C19 1.514(4) . ? C20 C21 1.527(4) . ? C22 C23 1.544(4) . ? C23 C27 1.538(4) . ? C23 C24 1.540(4) . ? C23 C25 1.542(4) . ? C25 C26 1.537(5) . ? C27 C28 1.520(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 N4 Cd1 N3 104.03(8) . . ? N4 Cd1 N1 91.94(9) . . ? N3 Cd1 N1 153.85(9) . . ? N4 Cd1 N6 159.06(8) . . ? N3 Cd1 N6 87.04(9) . . ? N1 Cd1 N6 84.86(8) . . ? N4 Cd1 N5 80.39(8) . . ? N3 Cd1 N5 95.35(8) . . ? N1 Cd1 N5 107.81(8) . . ? N6 Cd1 N5 80.92(8) . . ? N4 Cd1 N2 91.76(8) . . ? N3 Cd1 N2 79.94(8) . . ? N1 Cd1 N2 78.98(8) . . ? N6 Cd1 N2 107.84(8) . . ? N5 Cd1 N2 169.66(7) . . ? O4 N8 O5 120.3(3) . . ? O4 N8 O6 119.3(3) . . ? O5 N8 O6 120.4(3) . . ? C1 N1 Cd1 121.36(18) . . ? C8 N2 C3 108.8(2) . . ? C8 N2 Cd1 108.86(16) . . ? C3 N2 Cd1 113.08(16) . . ? C10 N3 Cd1 110.95(17) . . ? C15 N4 Cd1 109.47(17) . . ? C22 N5 C17 108.5(2) . . ? C22 N5 Cd1 113.09(15) . . ? C17 N5 Cd1 110.19(16) . . ? C24 N6 Cd1 121.76(18) . . ? O3 N7 O1 121.1(3) . . ? O3 N7 O2 120.6(3) . . ? O1 N7 O2 117.7(3) . . ? O3 N7 O1A 123.8(8) . . ? O2 N7 O1A 104.5(9) . . ? N1 C1 C2 115.7(2) . . ? C3 C2 C1 112.7(2) . . ? C3 C2 C4 111.4(2) . . ? C1 C2 C4 110.2(2) . . ? C3 C2 C6 104.8(2) . . ? C1 C2 C6 106.4(2) . . ? C4 C2 C6 111.2(2) . . ? O7 C30 C29 112.1(3) . . ? N2 C3 C2 116.8(2) . . ? C5 C4 C2 116.2(3) . . ? C7 C6 C2 116.5(3) . . ? N2 C8 C9 114.7(2) . . ? C10 C9 C8 111.4(2) . . ? C10 C9 C13 108.9(3) . . ? C8 C9 C13 108.7(3) . . ? C10 C9 C11 107.8(2) . . ? C8 C9 C11 108.2(3) . . ? C13 C9 C11 111.8(3) . . ? N3 C10 C9 113.4(2) . . ? C12 C11 C9 116.5(3) . . ? C14 C13 C9 116.4(3) . . ? N4 C15 C16 112.8(2) . . ? C15 C16 C17 111.5(2) . . ? C15 C16 C20 109.4(2) . . ? C17 C16 C20 108.9(2) . . ? C15 C16 C18 107.9(2) . . ? C17 C16 C18 108.5(2) . . ? C20 C16 C18 110.7(2) . . ? N5 C17 C16 115.1(2) . . ? C19 C18 C16 117.0(3) . . ? C21 C20 C16 116.2(3) . . ? N5 C22 C23 117.8(2) . . ? C27 C23 C24 110.1(2) . . ? C27 C23 C25 112.2(2) . . ? C24 C23 C25 106.8(2) . . ? C27 C23 C22 111.0(2) . . ? C24 C23 C22 112.2(2) . . ? C25 C23 C22 104.4(2) . . ? N6 C24 C23 115.4(2) . . ? C26 C25 C23 116.4(3) . . ? C28 C27 C23 116.0(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.663 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.067 #===END of CIF for Cd(SIV)2(NO3)3.EtOH ==================== data_HTEhpp _database_code_depnum_ccdc_archive 'CCDC 645823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H29 N3' _chemical_formula_sum 'C15 H29 N3' _chemical_formula_weight 251.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.8325(16) _cell_length_b 10.569(3) _cell_length_c 12.505(4) _cell_angle_alpha 93.964(5) _cell_angle_beta 96.108(5) _cell_angle_gamma 97.355(5) _cell_volume 757.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1622 _cell_measurement_theta_min 2.4425 _cell_measurement_theta_max 26.8035 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 280 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9687 _exptl_absorpt_correction_T_max 0.9869 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4418 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2627 _reflns_number_gt 1928 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0889P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2627 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0663 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1601 _refine_ls_wR_factor_gt 0.1493 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N3 N 0.3839(2) 0.48556(12) 0.80135(11) 0.0369(4) Uani 1 1 d . . . N1 N 0.2253(2) 0.59879(12) 0.93598(11) 0.0392(4) Uani 1 1 d . . . H1A H 0.1065 0.6068 0.9713 0.047 Uiso 1 1 calc R . . C3 C 0.5854(3) 0.58365(15) 0.81113(14) 0.0395(4) Uani 1 1 d . . . H3A H 0.6521 0.5841 0.7425 0.047 Uiso 1 1 calc R . . H3B H 0.7037 0.5632 0.8665 0.047 Uiso 1 1 calc R . . C1 C 0.4095(3) 0.70474(15) 0.94546(13) 0.0362(4) Uani 1 1 d . . . H1B H 0.5281 0.6934 1.0044 0.043 Uiso 1 1 calc R . . H1C H 0.3467 0.7842 0.9636 0.043 Uiso 1 1 calc R . . C5 C 0.4145(3) 0.36058(16) 0.75285(14) 0.0399(4) Uani 1 1 d . . . H5A H 0.5087 0.3175 0.8048 0.048 Uiso 1 1 calc R . . H5B H 0.4981 0.3716 0.6894 0.048 Uiso 1 1 calc R . . N2 N 0.0675(2) 0.39190(12) 0.88675(10) 0.0357(4) Uani 1 1 d . . . C2 C 0.5224(3) 0.71621(15) 0.84108(13) 0.0336(4) Uani 1 1 d . . . C4 C 0.2248(3) 0.48729(15) 0.87558(12) 0.0331(4) Uani 1 1 d . . . C7 C 0.0597(3) 0.27132(15) 0.82216(13) 0.0376(4) Uani 1 1 d . . . H7A H -0.1038 0.2357 0.8015 0.045 Uiso 1 1 calc R . . H7B H 0.1305 0.2114 0.8675 0.045 Uiso 1 1 calc R . . C6 C 0.1815(3) 0.27782(15) 0.71931(13) 0.0360(4) Uani 1 1 d . . . C8 C 0.7496(3) 0.81001(16) 0.86227(14) 0.0409(5) Uani 1 1 d . . . H8A H 0.8558 0.7762 0.9157 0.049 Uiso 1 1 calc R . . H8B H 0.8225 0.8128 0.7952 0.049 Uiso 1 1 calc R . . C12 C 0.2258(3) 0.14352(16) 0.67931(15) 0.0486(5) Uani 1 1 d . . . H12A H 0.3137 0.1510 0.6169 0.058 Uiso 1 1 calc R . . H12B H 0.3239 0.1101 0.7364 0.058 Uiso 1 1 calc R . . C10 C 0.3490(3) 0.75759(16) 0.75355(13) 0.0381(4) Uani 1 1 d . . . H10A H 0.2086 0.6943 0.7438 0.046 Uiso 1 1 calc R . . H10B H 0.3040 0.8394 0.7797 0.046 Uiso 1 1 calc R . . C14 C 0.0330(3) 0.33885(16) 0.63356(13) 0.0417(5) Uani 1 1 d . . . H14A H -0.1194 0.2860 0.6183 0.050 Uiso 1 1 calc R . . H14B H 0.0075 0.4232 0.6640 0.050 Uiso 1 1 calc R . . C9 C 0.7241(3) 0.94648(17) 0.90230(17) 0.0540(5) Uani 1 1 d . . . H9A H 0.8760 0.9981 0.9133 0.081 Uiso 1 1 calc R . . H9B H 0.6567 0.9457 0.9700 0.081 Uiso 1 1 calc R . . H9C H 0.6234 0.9825 0.8491 0.081 Uiso 1 1 calc R . . C13 C 0.0093(4) 0.04705(17) 0.64720(16) 0.0597(6) Uani 1 1 d . . . H13A H 0.0542 -0.0349 0.6243 0.089 Uiso 1 1 calc R . . H13B H -0.0861 0.0768 0.5883 0.089 Uiso 1 1 calc R . . H13C H -0.0785 0.0376 0.7085 0.089 Uiso 1 1 calc R . . C15 C 0.1352(4) 0.35533(19) 0.52694(15) 0.0603(6) Uani 1 1 d . . . H15A H 0.0293 0.3943 0.4782 0.091 Uiso 1 1 calc R . . H15B H 0.1571 0.2723 0.4946 0.091 Uiso 1 1 calc R . . H15C H 0.2839 0.4099 0.5403 0.091 Uiso 1 1 calc R . . C11 C 0.4350(4) 0.7729(2) 0.64419(15) 0.0626(6) Uani 1 1 d . . . H11A H 0.3130 0.7986 0.5948 0.094 Uiso 1 1 calc R . . H11B H 0.4763 0.6920 0.6161 0.094 Uiso 1 1 calc R . . H11C H 0.5706 0.8377 0.6518 0.094 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 N3 0.0292(8) 0.0381(8) 0.0453(8) -0.0006(6) 0.0154(6) 0.0050(6) N1 0.0348(8) 0.0379(8) 0.0470(9) -0.0025(6) 0.0221(7) 0.0015(6) C3 0.0298(9) 0.0430(10) 0.0475(10) 0.0062(8) 0.0121(8) 0.0045(8) C1 0.0367(10) 0.0370(9) 0.0343(9) 0.0032(7) 0.0062(7) 0.0007(7) C5 0.0378(10) 0.0446(10) 0.0409(10) 0.0018(7) 0.0127(8) 0.0135(8) N2 0.0346(8) 0.0347(8) 0.0389(8) 0.0014(6) 0.0119(6) 0.0037(6) C2 0.0271(9) 0.0389(9) 0.0365(9) 0.0068(7) 0.0078(7) 0.0051(7) C4 0.0304(9) 0.0391(9) 0.0323(9) 0.0053(7) 0.0077(7) 0.0098(7) C7 0.0407(10) 0.0360(9) 0.0370(10) 0.0026(7) 0.0081(8) 0.0059(8) C6 0.0373(10) 0.0356(9) 0.0375(10) 0.0028(7) 0.0090(7) 0.0107(7) C8 0.0308(10) 0.0469(10) 0.0451(10) 0.0088(8) 0.0059(7) 0.0018(8) C12 0.0589(13) 0.0418(10) 0.0483(11) -0.0003(8) 0.0120(9) 0.0160(9) C10 0.0330(10) 0.0442(10) 0.0380(10) 0.0053(7) 0.0053(7) 0.0063(7) C14 0.0457(11) 0.0419(10) 0.0383(10) 0.0016(7) 0.0057(8) 0.0097(8) C9 0.0468(12) 0.0477(11) 0.0645(13) 0.0050(9) 0.0073(9) -0.0053(9) C13 0.0830(16) 0.0426(11) 0.0538(12) -0.0052(9) 0.0161(11) 0.0087(11) C15 0.0720(15) 0.0687(13) 0.0437(12) 0.0097(9) 0.0122(10) 0.0155(11) C11 0.0564(14) 0.0911(16) 0.0424(12) 0.0179(10) 0.0081(9) 0.0091(11) _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 N3 C4 1.382(2) . ? N3 C3 1.453(2) . ? N3 C5 1.455(2) . ? N1 C4 1.3546(19) . ? N1 C1 1.4384(19) . ? C3 C2 1.525(2) . ? C1 C2 1.528(2) . ? C5 C6 1.520(2) . ? N2 C4 1.2990(19) . ? N2 C7 1.4538(19) . ? C2 C10 1.535(2) . ? C2 C8 1.537(2) . ? C7 C6 1.535(2) . ? C6 C12 1.535(2) . ? C6 C14 1.535(2) . ? C8 C9 1.525(2) . ? C12 C13 1.517(2) . ? C10 C11 1.518(2) . ? C14 C15 1.529(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 C4 N3 C3 120.15(13) . . ? C4 N3 C5 116.66(13) . . ? C3 N3 C5 116.13(12) . . ? C4 N1 C1 124.20(13) . . ? N3 C3 C2 111.83(13) . . ? N1 C1 C2 111.86(12) . . ? N3 C5 C6 111.29(13) . . ? C4 N2 C7 119.72(13) . . ? C3 C2 C1 105.60(12) . . ? C3 C2 C10 111.77(14) . . ? C1 C2 C10 109.41(13) . . ? C3 C2 C8 107.79(13) . . ? C1 C2 C8 109.80(13) . . ? C10 C2 C8 112.24(12) . . ? N2 C4 N1 118.20(13) . . ? N2 C4 N3 124.39(14) . . ? N1 C4 N3 117.28(13) . . ? N2 C7 C6 116.06(13) . . ? C5 C6 C12 108.75(13) . . ? C5 C6 C14 111.03(13) . . ? C12 C6 C14 111.97(14) . . ? C5 C6 C7 105.51(13) . . ? C12 C6 C7 109.99(13) . . ? C14 C6 C7 109.39(14) . . ? C9 C8 C2 115.60(14) . . ? C13 C12 C6 115.31(15) . . ? C11 C10 C2 115.92(14) . . ? C15 C14 C6 115.59(15) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.262 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.040 #===END of CIF for HTEhpp ==================================