# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1238 data_mc1505 #--------------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' #--------------------------------------------------------------------------- _chemical_formula_weight 907.10 _chemical_formula_sum 'C20 H40 N4 Nb2 S12 ' _chemical_formula_moiety 'C20 H40 N4 Nb2 S12 ' _chemical_formula_structural 'Nb2 (S2)2 (S2 C N (C2 H5)2)4' #--------------------------------------------------------------------------- _cell_length_a 24.010(3) _cell_length_b 6.957(4) _cell_length_c 21.172(2) _cell_angle_alpha 90 _cell_angle_beta 94.460(9) _cell_angle_gamma 90 _cell_volume 3526(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.2 _cell_measurement_theta_max 16.2 #--------------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1848.00 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.648 #--------------------------------------------------------------------------- _diffrn_ambient_temperature 295.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.19 _diffrn_reflns_number 4479 _reflns_number_total 4372 _reflns_number_observed 2550 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.108 _diffrn_reflns_av_sigmaI/netI 0.103 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.03365 _diffrn_orient_matrix_UB_12 0.01092 _diffrn_orient_matrix_UB_13 -0.03073 _diffrn_orient_matrix_UB_21 -0.02468 _diffrn_orient_matrix_UB_22 -0.02667 _diffrn_orient_matrix_UB_23 0.03491 _diffrn_orient_matrix_UB_31 -0.00206 _diffrn_orient_matrix_UB_32 0.14081 _diffrn_orient_matrix_UB_33 0.00900 #--------------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 160 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 16 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Nb 0 8 -2.073 0.621 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 48 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #--------------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Nb(1) 0.19558(2) 0.25563(8) 0.02484(2) 0.0277(1) Uani d . 1.00 . S(1) 0.23807(5) 0.5254(2) -0.03466(6) 0.0330(4) Uani d . 1.00 . S(2) 0.21379(5) 0.2942(2) -0.08875(6) 0.0347(4) Uani d . 1.00 . S(3) 0.09674(6) 0.3843(2) -0.01179(7) 0.0392(4) Uani d . 1.00 . S(4) 0.13010(5) -0.0111(2) -0.02275(6) 0.0368(4) Uani d . 1.00 . S(5) 0.18623(6) 0.5336(2) 0.10314(6) 0.0410(4) Uani d . 1.00 . S(6) 0.15338(6) 0.1453(2) 0.12932(7) 0.0417(4) Uani d . 1.00 . N(1) 0.0287(2) 0.1179(6) -0.0662(2) 0.035(1) Uani d . 1.00 . N(2) 0.1535(2) 0.4272(7) 0.2155(2) 0.047(2) Uani d . 1.00 . C(1) 0.0789(2) 0.1563(8) -0.0386(2) 0.033(2) Uani d . 1.00 . C(2) 0.1632(2) 0.3765(9) 0.1572(2) 0.038(2) Uani d . 1.00 . C(3) -0.0152(2) 0.266(1) -0.0735(2) 0.046(2) Uani d . 1.00 . C(4) -0.0105(2) 0.4011(10) -0.1274(3) 0.063(2) Uani d . 1.00 . C(5) 0.0146(2) -0.0746(8) -0.0914(2) 0.040(2) Uani d . 1.00 . C(6) 0.0110(3) -0.0801(9) -0.1628(3) 0.061(2) Uani d . 1.00 . C(7) 0.1662(3) 0.622(1) 0.2388(3) 0.067(2) Uani d . 1.00 . C(8) 0.1172(3) 0.726(1) 0.2600(4) 0.123(4) Uani d . 1.00 . C(9) 0.1348(3) 0.289(1) 0.2615(3) 0.063(2) Uani d . 1.00 . C(10) 0.1818(3) 0.208(1) 0.3044(3) 0.116(3) Uani d . 1.00 . H(1) -0.0503 0.2023 -0.0795 0.0556 Uiso calc . 1.00 . H(2) -0.0139 0.3389 -0.0355 0.0556 Uiso calc . 1.00 . H(3) 0.0241 0.4676 -0.1221 0.0762 Uiso calc . 1.00 . H(4) -0.0123 0.3310 -0.1660 0.0762 Uiso calc . 1.00 . H(5) -0.0403 0.4910 -0.1286 0.0762 Uiso calc . 1.00 . H(6) 0.0426 -0.1624 -0.0755 0.0485 Uiso calc . 1.00 . H(7) -0.0204 -0.1121 -0.0774 0.0485 Uiso calc . 1.00 . H(8) -0.0170 0.0072 -0.1791 0.0727 Uiso calc . 1.00 . H(9) 0.0460 -0.0445 -0.1772 0.0727 Uiso calc . 1.00 . H(10) 0.0016 -0.2064 -0.1769 0.0727 Uiso calc . 1.00 . H(11) 0.1936 0.6138 0.2736 0.0800 Uiso calc . 1.00 . H(12) 0.1807 0.6939 0.2056 0.0800 Uiso calc . 1.00 . H(13) 0.1282 0.8500 0.2746 0.1480 Uiso calc . 1.00 . H(14) 0.0896 0.7372 0.2255 0.1480 Uiso calc . 1.00 . H(15) 0.1022 0.6560 0.2934 0.1480 Uiso calc . 1.00 . H(16) 0.1093 0.3513 0.2867 0.0759 Uiso calc . 1.00 . H(17) 0.1166 0.1856 0.2390 0.0759 Uiso calc . 1.00 . H(18) 0.1673 0.1200 0.3331 0.1392 Uiso calc . 1.00 . H(19) 0.2076 0.1444 0.2798 0.1392 Uiso calc . 1.00 . H(20) 0.2003 0.3101 0.3275 0.1392 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb(1) 0.0271(2) 0.0299(3) 0.0262(2) -0.0047(3) 0.0019(2) -0.0017(3) S(1) 0.0342(7) 0.0309(8) 0.0337(7) -0.0026(7) 0.0014(6) 0.0039(6) S(2) 0.0354(7) 0.042(1) 0.0262(6) -0.0043(7) -0.0022(5) 0.0023(6) S(3) 0.0328(8) 0.0329(9) 0.0517(9) -0.0005(7) 0.0010(7) -0.0128(8) S(4) 0.0344(7) 0.0300(8) 0.0453(8) -0.0018(7) -0.0005(6) -0.0054(7) S(5) 0.0517(9) 0.0367(9) 0.0351(8) -0.0106(8) 0.0074(7) -0.0079(7) S(6) 0.0466(9) 0.0404(10) 0.0397(8) -0.0121(8) 0.0136(7) -0.0035(8) N(1) 0.029(2) 0.032(3) 0.042(3) -0.003(2) -0.002(2) -0.002(2) N(2) 0.059(3) 0.051(4) 0.033(3) -0.012(3) 0.016(2) -0.005(3) C(1) 0.033(3) 0.036(3) 0.032(3) -0.001(3) 0.005(2) -0.001(3) C(2) 0.035(3) 0.042(4) 0.038(3) -0.001(3) 0.005(3) -0.003(3) C(3) 0.024(3) 0.054(4) 0.060(3) -0.001(4) -0.001(2) -0.007(4) C(4) 0.058(4) 0.059(5) 0.072(4) 0.013(4) -0.008(4) 0.009(4) C(5) 0.032(3) 0.044(4) 0.045(3) -0.014(3) 0.000(3) -0.004(3) C(6) 0.078(5) 0.052(5) 0.052(4) -0.016(4) 0.011(3) -0.013(4) C(7) 0.089(5) 0.070(5) 0.043(4) -0.007(5) 0.016(4) -0.016(4) C(8) 0.109(7) 0.092(7) 0.162(8) 0.042(6) -0.037(6) -0.051(7) C(9) 0.071(4) 0.076(6) 0.044(4) 0.003(4) 0.018(3) -0.009(4) C(10) 0.140(7) 0.126(9) 0.074(5) -0.035(7) -0.045(5) 0.032(6) #--------------------------------------------------------------------------- _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00001|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 2550 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0424 _refine_ls_wR_factor_obs 0.0269 _refine_ls_goodness_of_fit_obs 1.375 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.52 _refine_diff_density_max 0.47 #--------------------------------------------------------------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb(1) Nb(1) 2.8928(9) 1_555 7_555 Nb(1) S(1) 2.520(1) 1_555 1_555 Nb(1) S(1) 2.520(1) 1_555 7_555 Nb(1) S(2) 2.492(1) 1_555 1_555 Nb(1) S(2) 2.496(1) 1_555 7_555 Nb(1) S(3) 2.598(2) 1_555 1_555 Nb(1) S(4) 2.586(1) 1_555 1_555 Nb(1) S(5) 2.569(2) 1_555 1_555 Nb(1) S(6) 2.619(2) 1_555 1_555 S(1) S(2) 2.033(2) 1_555 1_555 S(2) H(11) 2.987 1_555 4_564 S(3) S(4) 2.880(2) 1_555 1_555 S(3) N(1) 2.671(4) 1_555 1_555 S(3) C(1) 1.727(5) 1_555 1_555 S(3) H(2) 2.683 1_555 1_555 S(3) H(2) 2.997 1_555 3_565 S(3) H(3) 2.863 1_555 1_555 S(4) N(1) 2.689(4) 1_555 1_555 S(4) C(1) 1.708(5) 1_555 1_555 S(4) H(6) 2.531 1_555 1_555 S(5) S(6) 2.881(2) 1_555 1_555 S(5) N(2) 2.668(5) 1_555 1_555 S(5) C(2) 1.705(6) 1_555 1_555 S(5) H(12) 2.452 1_555 1_555 S(6) N(2) 2.679(5) 1_555 1_555 S(6) C(2) 1.723(6) 1_555 1_555 S(6) H(17) 2.564 1_555 1_555 N(1) C(1) 1.325(5) 1_555 1_555 N(1) C(3) 1.472(7) 1_555 1_555 N(1) C(4) 2.502(7) 1_555 1_555 N(1) C(5) 1.471(6) 1_555 1_555 N(1) C(6) 2.475(7) 1_555 1_555 N(1) H(1) 1.983 1_555 1_555 N(1) H(2) 1.983 1_555 1_555 N(1) H(3) 2.704 1_555 1_555 N(1) H(4) 2.704 1_555 1_555 N(1) H(6) 1.991 1_555 1_555 N(1) H(7) 1.991 1_555 1_555 N(1) H(8) 2.665 1_555 1_555 N(1) H(9) 2.670 1_555 1_555 N(2) C(2) 1.324(6) 1_555 1_555 N(2) C(7) 1.468(8) 1_555 1_555 N(2) C(8) 2.466(10) 1_555 1_555 N(2) C(9) 1.463(7) 1_555 1_555 N(2) C(10) 2.474(9) 1_555 1_555 N(2) H(11) 1.984 1_555 1_555 N(2) H(12) 1.984 1_555 1_555 N(2) H(14) 2.665 1_555 1_555 N(2) H(15) 2.661 1_555 1_555 N(2) H(16) 1.982 1_555 1_555 N(2) H(17) 1.982 1_555 1_555 N(2) H(19) 2.671 1_555 1_555 N(2) H(20) 2.670 1_555 1_555 C(1) C(3) 2.443(7) 1_555 1_555 C(1) C(5) 2.438(7) 1_555 1_555 C(1) H(2) 2.569 1_555 1_555 C(1) H(6) 2.486 1_555 1_555 C(1) H(7) 2.936 1_555 3_555 C(2) C(7) 2.428(8) 1_555 1_555 C(2) C(9) 2.439(8) 1_555 1_555 C(2) H(12) 2.457 1_555 1_555 C(2) H(17) 2.515 1_555 1_555 C(3) C(4) 1.492(8) 1_555 1_555 C(3) C(5) 2.510(9) 1_555 1_555 C(3) H(1) 0.950 1_555 1_555 C(3) H(2) 0.950 1_555 1_555 C(3) H(3) 2.018 1_555 1_555 C(3) H(4) 2.018 1_555 1_555 C(3) H(5) 2.018 1_555 1_555 C(3) H(7) 2.632 1_555 1_555 C(3) H(8) 2.867 1_555 1_555 C(4) H(1) 2.001 1_555 1_555 C(4) H(2) 2.001 1_555 1_555 C(4) H(3) 0.950 1_555 1_555 C(4) H(4) 0.950 1_555 1_555 C(4) H(5) 0.950 1_555 1_555 C(4) H(8) 2.950 1_555 1_555 C(4) H(10) 2.947 1_555 1_565 C(4) H(14) 2.869 1_555 3_565 C(5) C(6) 1.508(7) 1_555 1_555 C(5) H(1) 2.502 1_555 1_555 C(5) H(6) 0.950 1_555 1_555 C(5) H(7) 0.950 1_555 1_555 C(5) H(8) 2.033 1_555 1_555 C(5) H(9) 2.033 1_555 1_555 C(5) H(10) 2.033 1_555 1_555 C(6) H(4) 2.913 1_555 1_555 C(6) H(6) 2.024 1_555 1_555 C(6) H(7) 2.024 1_555 1_555 C(6) H(8) 0.950 1_555 1_555 C(6) H(9) 0.950 1_555 1_555 C(6) H(10) 0.950 1_555 1_555 C(7) C(8) 1.477(9) 1_555 1_555 C(7) C(9) 2.50(1) 1_555 1_555 C(7) H(11) 0.950 1_555 1_555 C(7) H(12) 0.950 1_555 1_555 C(7) H(13) 2.005 1_555 1_555 C(7) H(14) 2.005 1_555 1_555 C(7) H(15) 2.005 1_555 1_555 C(7) H(16) 2.581 1_555 1_555 C(7) H(20) 2.945 1_555 1_555 C(8) H(11) 1.992 1_555 1_555 C(8) H(12) 1.992 1_555 1_555 C(8) H(13) 0.950 1_555 1_555 C(8) H(14) 0.950 1_555 1_555 C(8) H(15) 0.950 1_555 1_555 C(8) H(16) 2.675 1_555 1_555 C(9) C(10) 1.500(8) 1_555 1_555 C(9) H(11) 2.666 1_555 1_555 C(9) H(15) 2.771 1_555 1_555 C(9) H(16) 0.950 1_555 1_555 C(9) H(17) 0.950 1_555 1_555 C(9) H(18) 2.026 1_555 1_555 C(9) H(19) 2.026 1_555 1_555 C(9) H(20) 2.026 1_555 1_555 C(10) H(11) 2.913 1_555 1_555 C(10) H(13) 2.855 1_555 1_545 C(10) H(16) 2.015 1_555 1_555 C(10) H(17) 2.015 1_555 1_555 C(10) H(18) 0.950 1_555 1_555 C(10) H(19) 0.950 1_555 1_555 C(10) H(20) 0.950 1_555 1_555 #--------------------------------------------------------------------------- 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_2 _geom_angle_site_symmetry_3 Nb(1) Nb(1) S(1) 54.98(3) 7_555 1_555 1_555 Nb(1) Nb(1) S(1) 54.96(3) 7_555 1_555 7_555 Nb(1) Nb(1) S(2) 54.61(3) 7_555 1_555 1_555 Nb(1) Nb(1) S(2) 54.49(3) 7_555 1_555 7_555 Nb(1) Nb(1) S(3) 136.96(4) 7_555 1_555 1_555 Nb(1) Nb(1) S(4) 112.21(4) 7_555 1_555 1_555 Nb(1) Nb(1) S(5) 112.45(4) 7_555 1_555 1_555 Nb(1) Nb(1) S(6) 135.97(4) 7_555 1_555 1_555 S(1) Nb(1) S(1) 109.94(4) 1_555 1_555 7_555 S(1) Nb(1) S(2) 47.87(4) 1_555 1_555 1_555 S(1) Nb(1) S(2) 90.26(4) 1_555 1_555 7_555 S(1) Nb(1) S(3) 89.44(5) 1_555 1_555 1_555 S(1) Nb(1) S(4) 126.68(4) 1_555 1_555 1_555 S(1) Nb(1) S(5) 79.68(5) 1_555 1_555 1_555 S(1) Nb(1) S(6) 147.03(5) 1_555 1_555 1_555 S(1) Nb(1) S(2) 90.34(5) 7_555 1_555 1_555 S(1) Nb(1) S(2) 47.83(4) 7_555 1_555 7_555 S(1) Nb(1) S(3) 148.08(5) 7_555 1_555 1_555 S(1) Nb(1) S(4) 80.60(5) 7_555 1_555 1_555 S(1) Nb(1) S(5) 128.12(5) 7_555 1_555 1_555 S(1) Nb(1) S(6) 89.23(5) 7_555 1_555 1_555 S(2) Nb(1) S(2) 109.10(3) 1_555 1_555 7_555 S(2) Nb(1) S(3) 84.24(5) 1_555 1_555 1_555 S(2) Nb(1) S(4) 81.27(4) 1_555 1_555 1_555 S(2) Nb(1) S(5) 124.92(5) 1_555 1_555 1_555 S(2) Nb(1) S(6) 162.78(5) 1_555 1_555 1_555 S(2) Nb(1) S(3) 161.35(5) 7_555 1_555 1_555 S(2) Nb(1) S(4) 126.14(5) 7_555 1_555 1_555 S(2) Nb(1) S(5) 82.59(5) 7_555 1_555 1_555 S(2) Nb(1) S(6) 83.09(5) 7_555 1_555 1_555 S(3) Nb(1) S(4) 67.50(5) 1_555 1_555 1_555 S(3) Nb(1) S(5) 79.02(5) 1_555 1_555 1_555 S(3) Nb(1) S(6) 87.06(5) 1_555 1_555 1_555 S(4) Nb(1) S(5) 135.32(5) 1_555 1_555 1_555 S(4) Nb(1) S(6) 81.67(5) 1_555 1_555 1_555 S(5) Nb(1) S(6) 67.46(5) 1_555 1_555 1_555 Nb(1) S(1) Nb(1) 70.06(4) 1_555 1_555 7_555 Nb(1) S(1) S(2) 65.35(5) 1_555 1_555 1_555 Nb(1) S(1) S(2) 65.45(5) 7_555 1_555 1_555 Nb(1) S(2) Nb(1) 70.90(3) 1_555 1_555 7_555 Nb(1) S(2) S(1) 66.78(5) 1_555 1_555 1_555 Nb(1) S(2) H(11) 159.62(5) 1_555 1_555 4_564 Nb(1) S(2) S(1) 66.72(5) 7_555 1_555 1_555 Nb(1) S(2) H(11) 128.87(5) 7_555 1_555 4_564 S(1) S(2) H(11) 113.44(6) 1_555 1_555 4_564 Nb(1) S(3) S(4) 56.05(4) 1_555 1_555 1_555 Nb(1) S(3) N(1) 113.8(1) 1_555 1_555 1_555 Nb(1) S(3) C(1) 88.8(2) 1_555 1_555 1_555 Nb(1) S(3) H(2) 152.06(7) 1_555 1_555 1_555 Nb(1) S(3) H(2) 137.44(5) 1_555 1_555 3_565 Nb(1) S(3) H(3) 142.91(6) 1_555 1_555 1_555 S(4) S(3) N(1) 57.8(1) 1_555 1_555 1_555 S(4) S(3) C(1) 32.8(2) 1_555 1_555 1_555 S(4) S(3) H(2) 98.64(5) 1_555 1_555 1_555 S(4) S(3) H(2) 146.81(6) 1_555 1_555 3_565 S(4) S(3) H(3) 106.46(5) 1_555 1_555 1_555 N(1) S(3) C(1) 25.0(2) 1_555 1_555 1_555 N(1) S(3) H(2) 43.48(9) 1_555 1_555 1_555 N(1) S(3) H(2) 101.0(1) 1_555 1_555 3_565 N(1) S(3) H(3) 58.36(9) 1_555 1_555 1_555 C(1) S(3) H(2) 67.3(2) 1_555 1_555 1_555 C(1) S(3) H(2) 123.0(2) 1_555 1_555 3_565 C(1) S(3) H(3) 78.4(2) 1_555 1_555 1_555 H(2) S(3) H(2) 57.64(3) 1_555 1_555 3_565 H(2) S(3) H(3) 48.68(2) 1_555 1_555 1_555 H(2) S(3) H(3) 76.37(3) 3_565 1_555 1_555 Nb(1) S(4) S(3) 56.45(4) 1_555 1_555 1_555 Nb(1) S(4) N(1) 113.6(1) 1_555 1_555 1_555 Nb(1) S(4) C(1) 89.6(2) 1_555 1_555 1_555 Nb(1) S(4) H(6) 158.33(6) 1_555 1_555 1_555 S(3) S(4) N(1) 57.2(1) 1_555 1_555 1_555 S(3) S(4) C(1) 33.3(2) 1_555 1_555 1_555 S(3) S(4) H(6) 101.91(5) 1_555 1_555 1_555 N(1) S(4) C(1) 24.0(2) 1_555 1_555 1_555 N(1) S(4) H(6) 44.72(10) 1_555 1_555 1_555 C(1) S(4) H(6) 68.7(2) 1_555 1_555 1_555 Nb(1) S(5) S(6) 57.10(4) 1_555 1_555 1_555 Nb(1) S(5) N(2) 114.4(1) 1_555 1_555 1_555 Nb(1) S(5) C(2) 90.0(2) 1_555 1_555 1_555 Nb(1) S(5) H(12) 157.96(7) 1_555 1_555 1_555 S(6) S(5) N(2) 57.6(1) 1_555 1_555 1_555 S(6) S(5) C(2) 33.0(2) 1_555 1_555 1_555 S(6) S(5) H(12) 102.81(5) 1_555 1_555 1_555 N(2) S(5) C(2) 24.6(2) 1_555 1_555 1_555 N(2) S(5) H(12) 45.3(1) 1_555 1_555 1_555 C(2) S(5) H(12) 69.8(2) 1_555 1_555 1_555 Nb(1) S(6) S(5) 55.44(4) 1_555 1_555 1_555 Nb(1) S(6) N(2) 112.4(1) 1_555 1_555 1_555 Nb(1) S(6) C(2) 87.9(2) 1_555 1_555 1_555 Nb(1) S(6) H(17) 156.40(7) 1_555 1_555 1_555 S(5) S(6) N(2) 57.2(1) 1_555 1_555 1_555 S(5) S(6) C(2) 32.6(2) 1_555 1_555 1_555 S(5) S(6) H(17) 100.98(6) 1_555 1_555 1_555 N(2) S(6) C(2) 24.6(2) 1_555 1_555 1_555 N(2) S(6) H(17) 44.3(1) 1_555 1_555 1_555 C(2) S(6) H(17) 68.6(2) 1_555 1_555 1_555 S(3) N(1) S(4) 64.98(10) 1_555 1_555 1_555 S(3) N(1) C(1) 33.4(3) 1_555 1_555 1_555 S(3) N(1) C(3) 88.3(3) 1_555 1_555 1_555 S(3) N(1) C(4) 82.5(2) 1_555 1_555 1_555 S(3) N(1) C(5) 154.6(3) 1_555 1_555 1_555 S(3) N(1) C(6) 143.4(2) 1_555 1_555 1_555 S(3) N(1) H(1) 113.7(2) 1_555 1_555 1_555 S(3) N(1) H(2) 68.6(1) 1_555 1_555 1_555 S(3) N(1) H(3) 64.4(1) 1_555 1_555 1_555 S(3) N(1) H(4) 97.5(1) 1_555 1_555 1_555 S(3) N(1) H(6) 128.4(2) 1_555 1_555 1_555 S(3) N(1) H(7) 161.0(2) 1_555 1_555 1_555 S(3) N(1) H(8) 141.5(2) 1_555 1_555 1_555 S(3) N(1) H(9) 122.8(2) 1_555 1_555 1_555 S(4) N(1) C(1) 31.6(3) 1_555 1_555 1_555 S(4) N(1) C(3) 153.0(3) 1_555 1_555 1_555 S(4) N(1) C(4) 137.2(2) 1_555 1_555 1_555 S(4) N(1) C(5) 89.8(3) 1_555 1_555 1_555 S(4) N(1) C(6) 100.9(2) 1_555 1_555 1_555 S(4) N(1) H(1) 167.7(2) 1_555 1_555 1_555 S(4) N(1) H(2) 128.5(2) 1_555 1_555 1_555 S(4) N(1) H(3) 117.1(2) 1_555 1_555 1_555 S(4) N(1) H(4) 135.7(2) 1_555 1_555 1_555 S(4) N(1) H(6) 63.4(1) 1_555 1_555 1_555 S(4) N(1) H(7) 106.5(2) 1_555 1_555 1_555 S(4) N(1) H(8) 120.6(2) 1_555 1_555 1_555 S(4) N(1) H(9) 87.8(1) 1_555 1_555 1_555 C(1) N(1) C(3) 121.6(5) 1_555 1_555 1_555 C(1) N(1) C(4) 111.3(4) 1_555 1_555 1_555 C(1) N(1) C(5) 121.3(4) 1_555 1_555 1_555 C(1) N(1) C(6) 124.7(4) 1_555 1_555 1_555 C(1) N(1) H(1) 146.0(4) 1_555 1_555 1_555 C(1) N(1) H(2) 100.0(3) 1_555 1_555 1_555 C(1) N(1) H(3) 91.0(3) 1_555 1_555 1_555 C(1) N(1) H(4) 119.9(3) 1_555 1_555 1_555 C(1) N(1) H(6) 95.0(3) 1_555 1_555 1_555 C(1) N(1) H(7) 136.4(4) 1_555 1_555 1_555 C(1) N(1) H(8) 138.7(3) 1_555 1_555 1_555 C(1) N(1) H(9) 106.0(3) 1_555 1_555 1_555 C(3) N(1) C(4) 32.7(3) 1_555 1_555 1_555 C(3) N(1) C(5) 117.1(4) 1_555 1_555 1_555 C(3) N(1) C(6) 103.1(3) 1_555 1_555 1_555 C(3) N(1) H(1) 27.1(2) 1_555 1_555 1_555 C(3) N(1) H(2) 27.1(2) 1_555 1_555 1_555 C(3) N(1) H(3) 47.2(3) 1_555 1_555 1_555 C(3) N(1) H(4) 47.2(2) 1_555 1_555 1_555 C(3) N(1) H(6) 143.0(3) 1_555 1_555 1_555 C(3) N(1) H(7) 97.8(3) 1_555 1_555 1_555 C(3) N(1) H(8) 82.3(3) 1_555 1_555 1_555 C(3) N(1) H(9) 111.3(3) 1_555 1_555 1_555 C(4) N(1) C(5) 117.6(3) 1_555 1_555 1_555 C(4) N(1) C(6) 88.7(2) 1_555 1_555 1_555 C(4) N(1) H(1) 51.4(2) 1_555 1_555 1_555 C(4) N(1) H(2) 51.4(2) 1_555 1_555 1_555 C(4) N(1) H(3) 20.6(1) 1_555 1_555 1_555 C(4) N(1) H(4) 20.6(2) 1_555 1_555 1_555 C(4) N(1) H(6) 141.2(2) 1_555 1_555 1_555 C(4) N(1) H(7) 112.1(2) 1_555 1_555 1_555 C(4) N(1) H(8) 69.6(2) 1_555 1_555 1_555 C(4) N(1) H(9) 87.4(2) 1_555 1_555 1_555 C(5) N(1) C(6) 34.3(3) 1_555 1_555 1_555 C(5) N(1) H(1) 91.6(3) 1_555 1_555 1_555 C(5) N(1) H(2) 135.6(3) 1_555 1_555 1_555 C(5) N(1) H(3) 131.3(3) 1_555 1_555 1_555 C(5) N(1) H(4) 99.0(3) 1_555 1_555 1_555 C(5) N(1) H(6) 26.9(2) 1_555 1_555 1_555 C(5) N(1) H(7) 26.9(2) 1_555 1_555 1_555 C(5) N(1) H(8) 49.1(2) 1_555 1_555 1_555 C(5) N(1) H(9) 48.9(2) 1_555 1_555 1_555 C(6) N(1) H(1) 86.9(2) 1_555 1_555 1_555 C(6) N(1) H(2) 130.0(2) 1_555 1_555 1_555 C(6) N(1) H(3) 98.1(2) 1_555 1_555 1_555 C(6) N(1) H(4) 68.3(2) 1_555 1_555 1_555 C(6) N(1) H(6) 52.6(2) 1_555 1_555 1_555 C(6) N(1) H(7) 52.6(2) 1_555 1_555 1_555 C(6) N(1) H(8) 20.9(2) 1_555 1_555 1_555 C(6) N(1) H(9) 20.8(1) 1_555 1_555 1_555 H(1) N(1) H(2) 46.04(10) 1_555 1_555 1_555 H(1) N(1) H(3) 70.5(1) 1_555 1_555 1_555 H(1) N(1) H(4) 56.03(10) 1_555 1_555 1_555 H(1) N(1) H(6) 116.2(2) 1_555 1_555 1_555 H(1) N(1) H(7) 70.7(1) 1_555 1_555 1_555 H(1) N(1) H(8) 68.7(1) 1_555 1_555 1_555 H(1) N(1) H(9) 102.3(2) 1_555 1_555 1_555 H(2) N(1) H(3) 56.0(1) 1_555 1_555 1_555 H(2) N(1) H(4) 70.5(1) 1_555 1_555 1_555 H(2) N(1) H(6) 152.4(2) 1_555 1_555 1_555 H(2) N(1) H(7) 110.3(2) 1_555 1_555 1_555 H(2) N(1) H(8) 109.3(2) 1_555 1_555 1_555 H(2) N(1) H(9) 137.4(2) 1_555 1_555 1_555 H(3) N(1) H(4) 33.35(5) 1_555 1_555 1_555 H(3) N(1) H(6) 147.1(2) 1_555 1_555 1_555 H(3) N(1) H(7) 131.9(2) 1_555 1_555 1_555 H(3) N(1) H(8) 82.4(1) 1_555 1_555 1_555 H(3) N(1) H(9) 90.0(1) 1_555 1_555 1_555 H(4) N(1) H(6) 120.9(2) 1_555 1_555 1_555 H(4) N(1) H(7) 99.9(1) 1_555 1_555 1_555 H(4) N(1) H(8) 50.04(7) 1_555 1_555 1_555 H(4) N(1) H(9) 67.39(9) 1_555 1_555 1_555 H(6) N(1) H(7) 45.85(10) 1_555 1_555 1_555 H(6) N(1) H(8) 71.8(1) 1_555 1_555 1_555 H(6) N(1) H(9) 57.3(1) 1_555 1_555 1_555 H(7) N(1) H(8) 57.48(10) 1_555 1_555 1_555 H(7) N(1) H(9) 71.7(1) 1_555 1_555 1_555 H(8) N(1) H(9) 33.81(5) 1_555 1_555 1_555 S(5) N(2) S(6) 65.2(1) 1_555 1_555 1_555 S(5) N(2) C(2) 32.4(3) 1_555 1_555 1_555 S(5) N(2) C(7) 88.6(3) 1_555 1_555 1_555 S(5) N(2) C(8) 104.1(3) 1_555 1_555 1_555 S(5) N(2) C(9) 154.4(4) 1_555 1_555 1_555 S(5) N(2) C(10) 140.0(3) 1_555 1_555 1_555 S(5) N(2) H(11) 102.0(2) 1_555 1_555 1_555 S(5) N(2) H(12) 61.6(1) 1_555 1_555 1_555 S(5) N(2) H(14) 93.3(2) 1_555 1_555 1_555 S(5) N(2) H(15) 124.7(2) 1_555 1_555 1_555 S(5) N(2) H(16) 164.7(2) 1_555 1_555 1_555 S(5) N(2) H(17) 128.9(2) 1_555 1_555 1_555 S(5) N(2) H(19) 119.6(2) 1_555 1_555 1_555 S(5) N(2) H(20) 138.0(2) 1_555 1_555 1_555 S(6) N(2) C(2) 32.8(3) 1_555 1_555 1_555 S(6) N(2) C(7) 153.5(4) 1_555 1_555 1_555 S(6) N(2) C(8) 153.4(3) 1_555 1_555 1_555 S(6) N(2) C(9) 89.3(3) 1_555 1_555 1_555 S(6) N(2) C(10) 93.1(3) 1_555 1_555 1_555 S(6) N(2) H(11) 151.1(2) 1_555 1_555 1_555 S(6) N(2) H(12) 126.6(2) 1_555 1_555 1_555 S(6) N(2) H(14) 132.6(2) 1_555 1_555 1_555 S(6) N(2) H(15) 152.1(2) 1_555 1_555 1_555 S(6) N(2) H(16) 110.5(2) 1_555 1_555 1_555 S(6) N(2) H(17) 64.7(1) 1_555 1_555 1_555 S(6) N(2) H(19) 77.4(1) 1_555 1_555 1_555 S(6) N(2) H(20) 111.1(2) 1_555 1_555 1_555 C(2) N(2) C(7) 120.8(5) 1_555 1_555 1_555 C(2) N(2) C(8) 132.3(5) 1_555 1_555 1_555 C(2) N(2) C(9) 122.1(5) 1_555 1_555 1_555 C(2) N(2) C(10) 119.3(5) 1_555 1_555 1_555 C(2) N(2) H(11) 129.8(4) 1_555 1_555 1_555 C(2) N(2) H(12) 93.8(4) 1_555 1_555 1_555 C(2) N(2) H(14) 115.7(4) 1_555 1_555 1_555 C(2) N(2) H(15) 149.5(4) 1_555 1_555 1_555 C(2) N(2) H(16) 141.6(4) 1_555 1_555 1_555 C(2) N(2) H(17) 97.1(4) 1_555 1_555 1_555 C(2) N(2) H(19) 99.5(4) 1_555 1_555 1_555 C(2) N(2) H(20) 130.9(4) 1_555 1_555 1_555 C(7) N(2) C(8) 33.2(4) 1_555 1_555 1_555 C(7) N(2) C(9) 116.8(5) 1_555 1_555 1_555 C(7) N(2) C(10) 106.0(4) 1_555 1_555 1_555 C(7) N(2) H(11) 27.0(3) 1_555 1_555 1_555 C(7) N(2) H(12) 27.0(3) 1_555 1_555 1_555 C(7) N(2) H(14) 48.0(3) 1_555 1_555 1_555 C(7) N(2) H(15) 48.1(3) 1_555 1_555 1_555 C(7) N(2) H(16) 95.8(4) 1_555 1_555 1_555 C(7) N(2) H(17) 141.7(4) 1_555 1_555 1_555 C(7) N(2) H(19) 115.5(4) 1_555 1_555 1_555 C(7) N(2) H(20) 85.5(3) 1_555 1_555 1_555 C(8) N(2) C(9) 99.5(4) 1_555 1_555 1_555 C(8) N(2) C(10) 108.2(3) 1_555 1_555 1_555 C(8) N(2) H(11) 51.8(2) 1_555 1_555 1_555 C(8) N(2) H(12) 51.8(3) 1_555 1_555 1_555 C(8) N(2) H(14) 20.9(2) 1_555 1_555 1_555 C(8) N(2) H(15) 20.9(2) 1_555 1_555 1_555 C(8) N(2) H(16) 73.0(3) 1_555 1_555 1_555 C(8) N(2) H(17) 116.1(3) 1_555 1_555 1_555 C(8) N(2) H(19) 126.7(3) 1_555 1_555 1_555 C(8) N(2) H(20) 93.2(2) 1_555 1_555 1_555 C(9) N(2) C(10) 33.9(3) 1_555 1_555 1_555 C(9) N(2) H(11) 100.2(3) 1_555 1_555 1_555 C(9) N(2) H(12) 143.7(4) 1_555 1_555 1_555 C(9) N(2) H(14) 105.8(3) 1_555 1_555 1_555 C(9) N(2) H(15) 78.6(3) 1_555 1_555 1_555 C(9) N(2) H(16) 27.0(3) 1_555 1_555 1_555 C(9) N(2) H(17) 27.0(3) 1_555 1_555 1_555 C(9) N(2) H(19) 48.6(3) 1_555 1_555 1_555 C(9) N(2) H(20) 48.6(3) 1_555 1_555 1_555 C(10) N(2) H(11) 80.8(2) 1_555 1_555 1_555 C(10) N(2) H(12) 125.6(3) 1_555 1_555 1_555 C(10) N(2) H(14) 124.3(3) 1_555 1_555 1_555 C(10) N(2) H(15) 90.6(2) 1_555 1_555 1_555 C(10) N(2) H(16) 52.4(2) 1_555 1_555 1_555 C(10) N(2) H(17) 52.4(2) 1_555 1_555 1_555 C(10) N(2) H(19) 20.8(2) 1_555 1_555 1_555 C(10) N(2) H(20) 20.8(2) 1_555 1_555 1_555 H(11) N(2) H(12) 46.0(1) 1_555 1_555 1_555 H(11) N(2) H(14) 71.1(2) 1_555 1_555 1_555 H(11) N(2) H(15) 56.7(1) 1_555 1_555 1_555 H(11) N(2) H(16) 88.1(2) 1_555 1_555 1_555 H(11) N(2) H(17) 127.2(2) 1_555 1_555 1_555 H(11) N(2) H(19) 88.5(2) 1_555 1_555 1_555 H(11) N(2) H(20) 60.0(1) 1_555 1_555 1_555 H(12) N(2) H(14) 56.5(1) 1_555 1_555 1_555 H(12) N(2) H(15) 71.2(1) 1_555 1_555 1_555 H(12) N(2) H(16) 122.0(2) 1_555 1_555 1_555 H(12) N(2) H(17) 167.8(3) 1_555 1_555 1_555 H(12) N(2) H(19) 126.3(2) 1_555 1_555 1_555 H(12) N(2) H(20) 105.1(2) 1_555 1_555 1_555 H(14) N(2) H(15) 33.87(6) 1_555 1_555 1_555 H(14) N(2) H(16) 79.0(2) 1_555 1_555 1_555 H(14) N(2) H(17) 113.2(2) 1_555 1_555 1_555 H(14) N(2) H(19) 144.7(2) 1_555 1_555 1_555 H(14) N(2) H(20) 112.4(2) 1_555 1_555 1_555 H(15) N(2) H(16) 52.2(1) 1_555 1_555 1_555 H(15) N(2) H(17) 96.6(2) 1_555 1_555 1_555 H(15) N(2) H(19) 110.8(2) 1_555 1_555 1_555 H(15) N(2) H(20) 79.4(1) 1_555 1_555 1_555 H(16) N(2) H(17) 46.1(1) 1_555 1_555 1_555 H(16) N(2) H(19) 71.6(1) 1_555 1_555 1_555 H(16) N(2) H(20) 57.1(1) 1_555 1_555 1_555 H(17) N(2) H(19) 57.1(1) 1_555 1_555 1_555 H(17) N(2) H(20) 71.6(1) 1_555 1_555 1_555 H(19) N(2) H(20) 33.77(6) 1_555 1_555 1_555 S(3) C(1) S(4) 113.9(3) 1_555 1_555 1_555 S(3) C(1) N(1) 121.6(4) 1_555 1_555 1_555 S(3) C(1) C(3) 90.8(3) 1_555 1_555 1_555 S(3) C(1) C(5) 152.6(3) 1_555 1_555 1_555 S(3) C(1) H(2) 74.4(2) 1_555 1_555 1_555 S(3) C(1) H(6) 173.9(3) 1_555 1_555 1_555 S(3) C(1) H(7) 86.8(2) 1_555 1_555 3_555 S(4) C(1) N(1) 124.4(4) 1_555 1_555 1_555 S(4) C(1) C(3) 155.0(3) 1_555 1_555 1_555 S(4) C(1) C(5) 93.5(3) 1_555 1_555 1_555 S(4) C(1) H(2) 160.9(3) 1_555 1_555 1_555 S(4) C(1) H(6) 71.5(2) 1_555 1_555 1_555 S(4) C(1) H(7) 98.5(2) 1_555 1_555 3_555 N(1) C(1) C(3) 30.9(3) 1_555 1_555 1_555 N(1) C(1) C(5) 31.1(3) 1_555 1_555 1_555 N(1) C(1) H(2) 49.5(3) 1_555 1_555 1_555 N(1) C(1) H(6) 52.9(3) 1_555 1_555 1_555 N(1) C(1) H(7) 82.6(3) 1_555 1_555 3_555 C(3) C(1) C(5) 61.9(2) 1_555 1_555 1_555 C(3) C(1) H(2) 21.7(1) 1_555 1_555 1_555 C(3) C(1) H(6) 83.7(2) 1_555 1_555 1_555 C(3) C(1) H(7) 78.2(2) 1_555 1_555 3_555 C(5) C(1) H(2) 79.6(2) 1_555 1_555 1_555 C(5) C(1) H(6) 22.2(1) 1_555 1_555 1_555 C(5) C(1) H(7) 89.3(2) 1_555 1_555 3_555 H(2) C(1) H(6) 99.6(2) 1_555 1_555 1_555 H(2) C(1) H(7) 63.9(1) 1_555 1_555 3_555 H(6) C(1) H(7) 89.5(2) 1_555 1_555 3_555 S(5) C(2) S(6) 114.3(3) 1_555 1_555 1_555 S(5) C(2) N(2) 123.1(5) 1_555 1_555 1_555 S(5) C(2) C(7) 91.9(3) 1_555 1_555 1_555 S(5) C(2) C(9) 153.6(4) 1_555 1_555 1_555 S(5) C(2) H(12) 69.5(2) 1_555 1_555 1_555 S(5) C(2) H(17) 170.4(3) 1_555 1_555 1_555 S(6) C(2) N(2) 122.6(5) 1_555 1_555 1_555 S(6) C(2) C(7) 153.7(4) 1_555 1_555 1_555 S(6) C(2) C(9) 92.0(3) 1_555 1_555 1_555 S(6) C(2) H(12) 175.0(3) 1_555 1_555 1_555 S(6) C(2) H(17) 71.7(2) 1_555 1_555 1_555 N(2) C(2) C(7) 31.3(3) 1_555 1_555 1_555 N(2) C(2) C(9) 30.5(3) 1_555 1_555 1_555 N(2) C(2) H(12) 53.7(3) 1_555 1_555 1_555 N(2) C(2) H(17) 51.4(3) 1_555 1_555 1_555 C(7) C(2) C(9) 61.7(3) 1_555 1_555 1_555 C(7) C(2) H(12) 22.4(2) 1_555 1_555 1_555 C(7) C(2) H(17) 82.6(2) 1_555 1_555 1_555 C(9) C(2) H(12) 84.1(2) 1_555 1_555 1_555 C(9) C(2) H(17) 22.0(2) 1_555 1_555 1_555 H(12) C(2) H(17) 104.9(2) 1_555 1_555 1_555 N(1) C(3) C(1) 27.5(2) 1_555 1_555 1_555 N(1) C(3) C(4) 115.2(4) 1_555 1_555 1_555 N(1) C(3) C(5) 31.4(2) 1_555 1_555 1_555 N(1) C(3) H(1) 108.0(6) 1_555 1_555 1_555 N(1) C(3) H(2) 108.0(5) 1_555 1_555 1_555 N(1) C(3) H(3) 100.4(3) 1_555 1_555 1_555 N(1) C(3) H(4) 100.4(3) 1_555 1_555 1_555 N(1) C(3) H(5) 141.5(4) 1_555 1_555 1_555 N(1) C(3) H(7) 48.5(3) 1_555 1_555 1_555 N(1) C(3) H(8) 67.1(3) 1_555 1_555 1_555 C(1) C(3) C(4) 107.8(4) 1_555 1_555 1_555 C(1) C(3) C(5) 58.9(2) 1_555 1_555 1_555 C(1) C(3) H(1) 133.2(6) 1_555 1_555 1_555 C(1) C(3) H(2) 86.7(3) 1_555 1_555 1_555 C(1) C(3) H(3) 85.0(2) 1_555 1_555 1_555 C(1) C(3) H(4) 105.2(2) 1_555 1_555 1_555 C(1) C(3) H(5) 130.2(3) 1_555 1_555 1_555 C(1) C(3) H(7) 74.9(2) 1_555 1_555 1_555 C(1) C(3) H(8) 89.9(2) 1_555 1_555 1_555 C(4) C(3) C(5) 116.1(4) 1_555 1_555 1_555 C(4) C(3) H(1) 108.0(5) 1_555 1_555 1_555 C(4) C(3) H(2) 108.0(6) 1_555 1_555 1_555 C(4) C(3) H(3) 26.3(3) 1_555 1_555 1_555 C(4) C(3) H(4) 26.3(3) 1_555 1_555 1_555 C(4) C(3) H(5) 26.3(3) 1_555 1_555 1_555 C(4) C(3) H(7) 127.8(4) 1_555 1_555 1_555 C(4) C(3) H(8) 78.2(3) 1_555 1_555 1_555 C(5) C(3) H(1) 78.6(4) 1_555 1_555 1_555 C(5) C(3) H(2) 130.0(5) 1_555 1_555 1_555 C(5) C(3) H(3) 115.4(3) 1_555 1_555 1_555 C(5) C(3) H(4) 91.9(2) 1_555 1_555 1_555 C(5) C(3) H(5) 136.2(3) 1_555 1_555 1_555 C(5) C(3) H(7) 21.1(1) 1_555 1_555 1_555 C(5) C(3) H(8) 43.8(2) 1_555 1_555 1_555 H(1) C(3) H(2) 109.5(5) 1_555 1_555 1_555 H(1) C(3) H(3) 134.4(5) 1_555 1_555 1_555 H(1) C(3) H(4) 94.1(3) 1_555 1_555 1_555 H(1) C(3) H(5) 93.5(4) 1_555 1_555 1_555 H(1) C(3) H(7) 59.5(4) 1_555 1_555 1_555 H(1) C(3) H(8) 69.2(3) 1_555 1_555 1_555 H(2) C(3) H(3) 94.1(5) 1_555 1_555 1_555 H(2) C(3) H(4) 134.4(6) 1_555 1_555 1_555 H(2) C(3) H(5) 93.5(5) 1_555 1_555 1_555 H(2) C(3) H(7) 124.1(5) 1_555 1_555 1_555 H(2) C(3) H(8) 173.5(5) 1_555 1_555 1_555 H(3) C(3) H(4) 45.2(1) 1_555 1_555 1_555 H(3) C(3) H(5) 45.2(1) 1_555 1_555 1_555 H(3) C(3) H(7) 134.6(3) 1_555 1_555 1_555 H(3) C(3) H(8) 91.0(2) 1_555 1_555 1_555 H(4) C(3) H(5) 45.2(1) 1_555 1_555 1_555 H(4) C(3) H(7) 101.5(2) 1_555 1_555 1_555 H(4) C(3) H(8) 51.9(1) 1_555 1_555 1_555 H(5) C(3) H(7) 138.2(2) 1_555 1_555 1_555 H(5) C(3) H(8) 92.9(2) 1_555 1_555 1_555 H(7) C(3) H(8) 49.6(1) 1_555 1_555 1_555 N(1) C(4) C(3) 32.2(3) 1_555 1_555 1_555 N(1) C(4) H(1) 50.8(2) 1_555 1_555 1_555 N(1) C(4) H(2) 50.8(2) 1_555 1_555 1_555 N(1) C(4) H(3) 91.8(4) 1_555 1_555 1_555 N(1) C(4) H(4) 91.8(4) 1_555 1_555 1_555 N(1) C(4) H(5) 141.6(5) 1_555 1_555 1_555 N(1) C(4) H(8) 57.8(2) 1_555 1_555 1_555 N(1) C(4) H(10) 150.5(3) 1_555 1_555 1_565 N(1) C(4) H(14) 108.2(2) 1_555 1_555 3_565 C(3) C(4) H(1) 26.8(2) 1_555 1_555 1_555 C(3) C(4) H(2) 26.8(3) 1_555 1_555 1_555 C(3) C(4) H(3) 109.5(5) 1_555 1_555 1_555 C(3) C(4) H(4) 109.5(6) 1_555 1_555 1_555 C(3) C(4) H(5) 109.5(6) 1_555 1_555 1_555 C(3) C(4) H(8) 72.1(3) 1_555 1_555 1_555 C(3) C(4) H(10) 150.8(4) 1_555 1_555 1_565 C(3) C(4) H(14) 104.9(4) 1_555 1_555 3_565 H(1) C(4) H(2) 45.6(1) 1_555 1_555 1_555 H(1) C(4) H(3) 136.3(5) 1_555 1_555 1_555 H(1) C(4) H(4) 95.2(5) 1_555 1_555 1_555 H(1) C(4) H(5) 94.5(5) 1_555 1_555 1_555 H(1) C(4) H(8) 62.1(2) 1_555 1_555 1_555 H(1) C(4) H(10) 152.2(3) 1_555 1_555 1_565 H(1) C(4) H(14) 79.7(2) 1_555 1_555 3_565 H(2) C(4) H(3) 95.2(4) 1_555 1_555 1_555 H(2) C(4) H(4) 136.3(6) 1_555 1_555 1_555 H(2) C(4) H(5) 94.6(5) 1_555 1_555 1_555 H(2) C(4) H(8) 98.9(2) 1_555 1_555 1_555 H(2) C(4) H(10) 123.9(3) 1_555 1_555 1_565 H(2) C(4) H(14) 123.8(3) 1_555 1_555 3_565 H(3) C(4) H(4) 109.5(6) 1_555 1_555 1_555 H(3) C(4) H(5) 109.5(7) 1_555 1_555 1_555 H(3) C(4) H(8) 121.1(5) 1_555 1_555 1_555 H(3) C(4) H(10) 58.8(3) 1_555 1_555 1_565 H(3) C(4) H(14) 140.6(5) 1_555 1_555 3_565 H(4) C(4) H(5) 109.5(6) 1_555 1_555 1_555 H(4) C(4) H(8) 37.5(3) 1_555 1_555 1_555 H(4) C(4) H(10) 99.8(4) 1_555 1_555 1_565 H(4) C(4) H(14) 38.9(3) 1_555 1_555 3_565 H(5) C(4) H(8) 125.8(5) 1_555 1_555 1_555 H(5) C(4) H(10) 58.4(4) 1_555 1_555 1_565 H(5) C(4) H(14) 75.4(3) 1_555 1_555 3_565 H(8) C(4) H(10) 137.1(2) 1_555 1_555 1_565 H(8) C(4) H(14) 53.6(1) 1_555 1_555 3_565 H(10) C(4) H(14) 97.6(2) 1_565 1_555 3_565 N(1) C(5) C(1) 27.7(2) 1_555 1_555 1_555 N(1) C(5) C(3) 31.5(2) 1_555 1_555 1_555 N(1) C(5) C(6) 112.3(5) 1_555 1_555 1_555 N(1) C(5) H(1) 52.4(2) 1_555 1_555 1_555 N(1) C(5) H(6) 108.8(4) 1_555 1_555 1_555 N(1) C(5) H(7) 108.8(5) 1_555 1_555 1_555 N(1) C(5) H(8) 97.8(3) 1_555 1_555 1_555 N(1) C(5) H(9) 98.0(3) 1_555 1_555 1_555 N(1) C(5) H(10) 138.5(4) 1_555 1_555 1_555 C(1) C(5) C(3) 59.1(2) 1_555 1_555 1_555 C(1) C(5) C(6) 117.5(4) 1_555 1_555 1_555 C(1) C(5) H(1) 79.8(2) 1_555 1_555 1_555 C(1) C(5) H(6) 81.8(3) 1_555 1_555 1_555 C(1) C(5) H(7) 125.6(4) 1_555 1_555 1_555 C(1) C(5) H(8) 114.4(3) 1_555 1_555 1_555 C(1) C(5) H(9) 94.4(2) 1_555 1_555 1_555 C(1) C(5) H(10) 139.0(3) 1_555 1_555 1_555 C(3) C(5) C(6) 100.4(4) 1_555 1_555 1_555 C(3) C(5) H(1) 21.8(1) 1_555 1_555 1_555 C(3) C(5) H(6) 139.1(4) 1_555 1_555 1_555 C(3) C(5) H(7) 86.7(4) 1_555 1_555 1_555 C(3) C(5) H(8) 77.5(2) 1_555 1_555 1_555 C(3) C(5) H(9) 99.7(3) 1_555 1_555 1_555 C(3) C(5) H(10) 122.3(3) 1_555 1_555 1_555 C(6) C(5) H(1) 97.6(4) 1_555 1_555 1_555 C(6) C(5) H(6) 108.8(5) 1_555 1_555 1_555 C(6) C(5) H(7) 108.8(5) 1_555 1_555 1_555 C(6) C(5) H(8) 26.1(3) 1_555 1_555 1_555 C(6) C(5) H(9) 26.1(3) 1_555 1_555 1_555 C(6) C(5) H(10) 26.1(3) 1_555 1_555 1_555 H(1) C(5) H(6) 152.7(4) 1_555 1_555 1_555 H(1) C(5) H(7) 66.8(3) 1_555 1_555 1_555 H(1) C(5) H(8) 71.7(2) 1_555 1_555 1_555 H(1) C(5) H(9) 106.7(2) 1_555 1_555 1_555 H(1) C(5) H(10) 112.5(2) 1_555 1_555 1_555 H(6) C(5) H(7) 109.5(6) 1_555 1_555 1_555 H(6) C(5) H(8) 134.9(5) 1_555 1_555 1_555 H(6) C(5) H(9) 94.6(4) 1_555 1_555 1_555 H(6) C(5) H(10) 94.6(4) 1_555 1_555 1_555 H(7) C(5) H(8) 94.9(3) 1_555 1_555 1_555 H(7) C(5) H(9) 134.9(4) 1_555 1_555 1_555 H(7) C(5) H(10) 94.3(3) 1_555 1_555 1_555 H(8) C(5) H(9) 44.9(1) 1_555 1_555 1_555 H(8) C(5) H(10) 44.9(1) 1_555 1_555 1_555 H(9) C(5) H(10) 44.9(1) 1_555 1_555 1_555 N(1) C(6) C(5) 33.4(3) 1_555 1_555 1_555 N(1) C(6) H(4) 59.6(2) 1_555 1_555 1_555 N(1) C(6) H(6) 51.4(2) 1_555 1_555 1_555 N(1) C(6) H(7) 51.4(2) 1_555 1_555 1_555 N(1) C(6) H(8) 90.9(4) 1_555 1_555 1_555 N(1) C(6) H(9) 91.3(4) 1_555 1_555 1_555 N(1) C(6) H(10) 142.8(5) 1_555 1_555 1_555 C(5) C(6) H(4) 89.7(4) 1_555 1_555 1_555 C(5) C(6) H(6) 26.4(3) 1_555 1_555 1_555 C(5) C(6) H(7) 26.4(2) 1_555 1_555 1_555 C(5) C(6) H(8) 109.5(6) 1_555 1_555 1_555 C(5) C(6) H(9) 109.5(5) 1_555 1_555 1_555 C(5) C(6) H(10) 109.5(6) 1_555 1_555 1_555 H(4) C(6) H(6) 110.9(2) 1_555 1_555 1_555 H(4) C(6) H(7) 92.6(2) 1_555 1_555 1_555 H(4) C(6) H(8) 40.1(3) 1_555 1_555 1_555 H(4) C(6) H(9) 84.8(4) 1_555 1_555 1_555 H(4) C(6) H(10) 149.4(5) 1_555 1_555 1_555 H(6) C(6) H(7) 45.1(1) 1_555 1_555 1_555 H(6) C(6) H(8) 135.9(5) 1_555 1_555 1_555 H(6) C(6) H(9) 95.1(4) 1_555 1_555 1_555 H(6) C(6) H(10) 95.1(4) 1_555 1_555 1_555 H(7) C(6) H(8) 95.4(4) 1_555 1_555 1_555 H(7) C(6) H(9) 135.9(5) 1_555 1_555 1_555 H(7) C(6) H(10) 94.8(4) 1_555 1_555 1_555 H(8) C(6) H(9) 109.5(6) 1_555 1_555 1_555 H(8) C(6) H(10) 109.5(6) 1_555 1_555 1_555 H(9) C(6) H(10) 109.5(6) 1_555 1_555 1_555 N(2) C(7) C(2) 27.9(3) 1_555 1_555 1_555 N(2) C(7) C(8) 113.8(6) 1_555 1_555 1_555 N(2) C(7) C(9) 31.5(3) 1_555 1_555 1_555 N(2) C(7) H(11) 108.4(7) 1_555 1_555 1_555 N(2) C(7) H(12) 108.4(5) 1_555 1_555 1_555 N(2) C(7) H(13) 140.3(5) 1_555 1_555 1_555 N(2) C(7) H(14) 99.1(4) 1_555 1_555 1_555 N(2) C(7) H(15) 98.9(4) 1_555 1_555 1_555 N(2) C(7) H(16) 49.8(3) 1_555 1_555 1_555 N(2) C(7) H(20) 64.7(3) 1_555 1_555 1_555 C(2) C(7) C(8) 125.4(5) 1_555 1_555 1_555 C(2) C(7) C(9) 59.4(3) 1_555 1_555 1_555 C(2) C(7) H(11) 119.2(6) 1_555 1_555 1_555 C(2) C(7) H(12) 80.5(4) 1_555 1_555 1_555 C(2) C(7) H(13) 146.8(4) 1_555 1_555 1_555 C(2) C(7) H(14) 101.9(3) 1_555 1_555 1_555 C(2) C(7) H(15) 120.8(3) 1_555 1_555 1_555 C(2) C(7) H(16) 77.2(3) 1_555 1_555 1_555 C(2) C(7) H(20) 85.8(3) 1_555 1_555 1_555 C(8) C(7) C(9) 97.8(5) 1_555 1_555 1_555 C(8) C(7) H(11) 108.4(6) 1_555 1_555 1_555 C(8) C(7) H(12) 108.4(8) 1_555 1_555 1_555 C(8) C(7) H(13) 26.5(4) 1_555 1_555 1_555 C(8) C(7) H(14) 26.5(3) 1_555 1_555 1_555 C(8) C(7) H(15) 26.5(4) 1_555 1_555 1_555 C(8) C(7) H(16) 77.2(5) 1_555 1_555 1_555 C(8) C(7) H(20) 110.8(5) 1_555 1_555 1_555 C(9) C(7) H(11) 89.7(5) 1_555 1_555 1_555 C(9) C(7) H(12) 139.8(5) 1_555 1_555 1_555 C(9) C(7) H(13) 120.6(3) 1_555 1_555 1_555 C(9) C(7) H(14) 96.4(3) 1_555 1_555 1_555 C(9) C(7) H(15) 75.1(3) 1_555 1_555 1_555 C(9) C(7) H(16) 21.5(1) 1_555 1_555 1_555 C(9) C(7) H(20) 42.7(2) 1_555 1_555 1_555 H(11) C(7) H(12) 109.5(7) 1_555 1_555 1_555 H(11) C(7) H(13) 93.7(4) 1_555 1_555 1_555 H(11) C(7) H(14) 134.9(5) 1_555 1_555 1_555 H(11) C(7) H(15) 94.4(4) 1_555 1_555 1_555 H(11) C(7) H(16) 90.4(4) 1_555 1_555 1_555 H(11) C(7) H(20) 47.1(4) 1_555 1_555 1_555 H(12) C(7) H(13) 93.9(5) 1_555 1_555 1_555 H(12) C(7) H(14) 94.2(5) 1_555 1_555 1_555 H(12) C(7) H(15) 134.9(6) 1_555 1_555 1_555 H(12) C(7) H(16) 155.5(5) 1_555 1_555 1_555 H(12) C(7) H(20) 139.3(6) 1_555 1_555 1_555 H(13) C(7) H(14) 45.5(2) 1_555 1_555 1_555 H(13) C(7) H(15) 45.5(2) 1_555 1_555 1_555 H(13) C(7) H(16) 99.2(3) 1_555 1_555 1_555 H(13) C(7) H(20) 117.0(2) 1_555 1_555 1_555 H(14) C(7) H(15) 45.5(2) 1_555 1_555 1_555 H(14) C(7) H(16) 80.7(2) 1_555 1_555 1_555 H(14) C(7) H(20) 126.2(3) 1_555 1_555 1_555 H(15) C(7) H(16) 53.6(2) 1_555 1_555 1_555 H(15) C(7) H(20) 84.7(2) 1_555 1_555 1_555 H(16) C(7) H(20) 48.8(1) 1_555 1_555 1_555 N(2) C(8) C(7) 33.0(4) 1_555 1_555 1_555 N(2) C(8) H(11) 51.5(2) 1_555 1_555 1_555 N(2) C(8) H(12) 51.5(2) 1_555 1_555 1_555 N(2) C(8) H(13) 142.5(7) 1_555 1_555 1_555 N(2) C(8) H(14) 91.4(5) 1_555 1_555 1_555 N(2) C(8) H(15) 91.2(6) 1_555 1_555 1_555 N(2) C(8) H(16) 45.1(2) 1_555 1_555 1_555 C(7) C(8) H(11) 26.9(3) 1_555 1_555 1_555 C(7) C(8) H(12) 26.9(3) 1_555 1_555 1_555 C(7) C(8) H(13) 109.5(8) 1_555 1_555 1_555 C(7) C(8) H(14) 109.5(8) 1_555 1_555 1_555 C(7) C(8) H(15) 109.5(8) 1_555 1_555 1_555 C(7) C(8) H(16) 70.2(5) 1_555 1_555 1_555 H(11) C(8) H(12) 45.8(2) 1_555 1_555 1_555 H(11) C(8) H(13) 94.5(5) 1_555 1_555 1_555 H(11) C(8) H(14) 136.4(7) 1_555 1_555 1_555 H(11) C(8) H(15) 95.2(5) 1_555 1_555 1_555 H(11) C(8) H(16) 70.7(3) 1_555 1_555 1_555 H(12) C(8) H(13) 94.7(7) 1_555 1_555 1_555 H(12) C(8) H(14) 94.9(6) 1_555 1_555 1_555 H(12) C(8) H(15) 136.4(7) 1_555 1_555 1_555 H(12) C(8) H(16) 94.9(3) 1_555 1_555 1_555 H(13) C(8) H(14) 109.5(9) 1_555 1_555 1_555 H(13) C(8) H(15) 109.5(8) 1_555 1_555 1_555 H(13) C(8) H(16) 147.2(6) 1_555 1_555 1_555 H(14) C(8) H(15) 109.5(8) 1_555 1_555 1_555 H(14) C(8) H(16) 100.9(6) 1_555 1_555 1_555 H(15) C(8) H(16) 46.3(4) 1_555 1_555 1_555 N(2) C(9) C(2) 27.4(3) 1_555 1_555 1_555 N(2) C(9) C(7) 31.7(3) 1_555 1_555 1_555 N(2) C(9) C(10) 113.2(6) 1_555 1_555 1_555 N(2) C(9) H(11) 47.1(3) 1_555 1_555 1_555 N(2) C(9) H(15) 70.3(3) 1_555 1_555 1_555 N(2) C(9) H(16) 108.5(6) 1_555 1_555 1_555 N(2) C(9) H(17) 108.5(5) 1_555 1_555 1_555 N(2) C(9) H(18) 139.4(5) 1_555 1_555 1_555 N(2) C(9) H(19) 98.6(4) 1_555 1_555 1_555 N(2) C(9) H(20) 98.6(4) 1_555 1_555 1_555 C(2) C(9) C(7) 58.9(2) 1_555 1_555 1_555 C(2) C(9) C(10) 113.1(5) 1_555 1_555 1_555 C(2) C(9) H(11) 72.1(2) 1_555 1_555 1_555 C(2) C(9) H(15) 95.4(3) 1_555 1_555 1_555 C(2) C(9) H(16) 129.3(6) 1_555 1_555 1_555 C(2) C(9) H(17) 83.5(4) 1_555 1_555 1_555 C(2) C(9) H(18) 134.8(3) 1_555 1_555 1_555 C(2) C(9) H(19) 90.0(2) 1_555 1_555 1_555 C(2) C(9) H(20) 110.5(3) 1_555 1_555 1_555 C(7) C(9) C(10) 103.9(5) 1_555 1_555 1_555 C(7) C(9) H(11) 20.9(2) 1_555 1_555 1_555 C(7) C(9) H(15) 44.4(2) 1_555 1_555 1_555 C(7) C(9) H(16) 84.3(5) 1_555 1_555 1_555 C(7) C(9) H(17) 137.8(5) 1_555 1_555 1_555 C(7) C(9) H(18) 125.4(3) 1_555 1_555 1_555 C(7) C(9) H(19) 103.3(3) 1_555 1_555 1_555 C(7) C(9) H(20) 80.5(3) 1_555 1_555 1_555 C(10) C(9) H(11) 83.7(4) 1_555 1_555 1_555 C(10) C(9) H(15) 114.2(5) 1_555 1_555 1_555 C(10) C(9) H(16) 108.5(6) 1_555 1_555 1_555 C(10) C(9) H(17) 108.5(7) 1_555 1_555 1_555 C(10) C(9) H(18) 26.2(3) 1_555 1_555 1_555 C(10) C(9) H(19) 26.2(3) 1_555 1_555 1_555 C(10) C(9) H(20) 26.2(4) 1_555 1_555 1_555 H(11) C(9) H(15) 49.6(1) 1_555 1_555 1_555 H(11) C(9) H(16) 85.3(4) 1_555 1_555 1_555 H(11) C(9) H(17) 155.5(5) 1_555 1_555 1_555 H(11) C(9) H(18) 104.5(2) 1_555 1_555 1_555 H(11) C(9) H(19) 87.8(2) 1_555 1_555 1_555 H(11) C(9) H(20) 59.7(2) 1_555 1_555 1_555 H(15) C(9) H(16) 40.0(3) 1_555 1_555 1_555 H(15) C(9) H(17) 133.7(5) 1_555 1_555 1_555 H(15) C(9) H(18) 116.9(2) 1_555 1_555 1_555 H(15) C(9) H(19) 131.8(3) 1_555 1_555 1_555 H(15) C(9) H(20) 89.0(2) 1_555 1_555 1_555 H(16) C(9) H(17) 109.5(6) 1_555 1_555 1_555 H(16) C(9) H(18) 94.1(4) 1_555 1_555 1_555 H(16) C(9) H(19) 134.8(5) 1_555 1_555 1_555 H(16) C(9) H(20) 94.6(4) 1_555 1_555 1_555 H(17) C(9) H(18) 94.1(5) 1_555 1_555 1_555 H(17) C(9) H(19) 94.5(5) 1_555 1_555 1_555 H(17) C(9) H(20) 134.8(6) 1_555 1_555 1_555 H(18) C(9) H(19) 45.0(1) 1_555 1_555 1_555 H(18) C(9) H(20) 45.0(1) 1_555 1_555 1_555 H(19) C(9) H(20) 45.0(1) 1_555 1_555 1_555 N(2) C(10) C(9) 32.9(3) 1_555 1_555 1_555 N(2) C(10) H(11) 42.2(2) 1_555 1_555 1_555 N(2) C(10) H(13) 106.1(3) 1_555 1_555 1_545 N(2) C(10) H(16) 51.2(2) 1_555 1_555 1_555 N(2) C(10) H(17) 51.2(2) 1_555 1_555 1_555 N(2) C(10) H(18) 142.4(6) 1_555 1_555 1_555 N(2) C(10) H(19) 91.4(5) 1_555 1_555 1_555 N(2) C(10) H(20) 91.3(6) 1_555 1_555 1_555 C(9) C(10) H(11) 65.5(4) 1_555 1_555 1_555 C(9) C(10) H(13) 83.5(4) 1_555 1_555 1_545 C(9) C(10) H(16) 26.6(3) 1_555 1_555 1_555 C(9) C(10) H(17) 26.6(3) 1_555 1_555 1_555 C(9) C(10) H(18) 109.5(7) 1_555 1_555 1_555 C(9) C(10) H(19) 109.5(6) 1_555 1_555 1_555 C(9) C(10) H(20) 109.5(8) 1_555 1_555 1_555 H(11) C(10) H(13) 147.8(2) 1_555 1_555 1_545 H(11) C(10) H(16) 65.1(2) 1_555 1_555 1_555 H(11) C(10) H(17) 90.3(3) 1_555 1_555 1_555 H(11) C(10) H(18) 144.8(7) 1_555 1_555 1_555 H(11) C(10) H(19) 104.6(6) 1_555 1_555 1_555 H(11) C(10) H(20) 49.1(4) 1_555 1_555 1_555 H(13) C(10) H(16) 91.2(3) 1_545 1_555 1_555 H(13) C(10) H(17) 57.7(2) 1_545 1_555 1_555 H(13) C(10) H(18) 52.7(4) 1_545 1_555 1_555 H(13) C(10) H(19) 76.7(5) 1_545 1_555 1_555 H(13) C(10) H(20) 161.6(6) 1_545 1_555 1_555 H(16) C(10) H(17) 45.3(2) 1_555 1_555 1_555 H(16) C(10) H(18) 94.8(6) 1_555 1_555 1_555 H(16) C(10) H(19) 136.0(5) 1_555 1_555 1_555 H(16) C(10) H(20) 95.2(7) 1_555 1_555 1_555 H(17) C(10) H(18) 94.8(5) 1_555 1_555 1_555 H(17) C(10) H(19) 95.2(5) 1_555 1_555 1_555 H(17) C(10) H(20) 136.0(7) 1_555 1_555 1_555 H(18) C(10) H(19) 109.5(9) 1_555 1_555 1_555 H(18) C(10) H(20) 109.5(7) 1_555 1_555 1_555 H(19) C(10) H(20) 109.5(8) 1_555 1_555 1_555 #--------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Nb(1) Nb(1) 2.8928(9) 1_555 7_555 Nb(1) S(1) 2.520(1) 1_555 1_555 Nb(1) S(1) 2.520(1) 1_555 7_555 Nb(1) S(3) 2.598(2) 1_555 1_555 Nb(1) S(4) 2.586(1) 1_555 1_555 Nb(1) S(5) 2.569(2) 1_555 1_555 Nb(1) S(6) 2.619(2) 1_555 1_555 S(3) S(4) 2.880(2) 1_555 1_555 S(3) N(1) 2.671(4) 1_555 1_555 S(4) N(1) 2.689(4) 1_555 1_555 S(5) S(6) 2.881(2) 1_555 1_555 S(5) N(2) 2.668(5) 1_555 1_555 S(6) N(2) 2.679(5) 1_555 1_555 N(1) C(4) 2.502(7) 1_555 1_555 C(3) C(5) 2.510(9) 1_555 1_555 S(1) S(1) 3.482(3) 1_555 7_565 N(1) C(5) 3.583(6) 1_555 3_555 #--------------------------------------------------------------------------- #===END # data for [Nb2 S2 (acac)4] 2H2Cl2 data_2 #------------------------------------------------------------------------------ _audit_creation_date 'Thu May 7 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ' May 7 1998' #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92 (Altomare, A. et al. 1994)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_formula_weight 816.23 _chemical_formula_sum 'C22 H32 Cl4 Nb2 O8 S2 ' _chemical_formula_structural '[Nb2 S2 (CH3 CO CH CO CH3)4] (CH2CL2)2' #------------------------------------------------------------------------------ _cell_length_a 9.00(2) _cell_length_b 11.15(3) _cell_length_c 8.868(6) _cell_angle_alpha 101.5(1) _cell_angle_beta 95.69(10) _cell_angle_gamma 73.3(2) _cell_volume 834(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 14 _cell_measurement_theta_min 3.8 _cell_measurement_theta_max 7.9 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 410.00 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.444 #------------------------------------------------------------------------------ _diffrn_special_details ; voltage and current for X-ray generation: 46 kV, 260 mA scan width (\w): ( 1.785 + 0.30tan\w) deg with a fractional offset 0.5. scan speed (\w): 16 deg/min background-count time: 25% of the peak-scan time on each side Weak reflections ( I < 10.0\s(I) ) were rescanned one more time, and the counts were accumulated. Linear correction for decay (1.86%) was applied. Only part of reflections could be measured due to the trouble in the computer system controlling the diffractometer. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.86 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 2 -2 1 1 2 2 2 -1 _diffrn_reflns_number 967 _reflns_number_total 798 _reflns_number_observed 784 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.038 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 2 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 22.45 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.07497 _diffrn_orient_matrix_UB_12 0.05305 _diffrn_orient_matrix_UB_13 0.02333 _diffrn_orient_matrix_UB_21 -0.02042 _diffrn_orient_matrix_UB_22 0.01562 _diffrn_orient_matrix_UB_23 0.11204 _diffrn_orient_matrix_UB_31 0.08630 _diffrn_orient_matrix_UB_32 -0.07746 _diffrn_orient_matrix_UB_33 0.01316 #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined isotropically, and hydrogen atoms were not included in the refinements. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + (1/4)(0.019|Fo|)^2^]' _refine_ls_hydrogen_treatment 'Hydrogen atoms were not included.' _refine_ls_extinction_method none _refine_ls_number_reflns 784 _refine_ls_number_parameters 77 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0737 _refine_ls_wR_factor_obs 0.0778 _refine_ls_goodness_of_fit_obs 3.900 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -0.55 _refine_diff_density_max 0.56 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Nb 0 2 -2.073 0.621 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 2 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 22 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O 0 8 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 4 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Nb 0.0317(5) 0.6049(2) -0.0503(2) 0.0344(7) Uiso d . 1.00 . Cl(1) 0.107(1) 0.9412(6) -0.3222(7) 0.078(2) Uiso d . 1.00 . Cl(2) 0.368(2) 1.0381(8) -0.3365(8) 0.109(3) Uiso d . 1.00 . S 0.182(1) 0.3870(5) -0.0913(5) 0.039(2) Uiso d . 1.00 . O(1) -0.066(3) 0.590(1) -0.263(1) 0.037(4) Uiso d . 1.00 . O(2) -0.067(3) 0.805(1) -0.052(1) 0.036(4) Uiso d . 1.00 . O(3) 0.232(4) 0.646(1) -0.151(2) 0.056(6) Uiso d . 1.00 . O(4) 0.140(4) 0.671(1) 0.140(2) 0.044(6) Uiso d . 1.00 . C(1) -0.222(4) 0.605(2) -0.504(2) 0.046(7) Uiso d . 1.00 . C(2) -0.168(4) 0.672(2) -0.343(2) 0.045(7) Uiso d . 1.00 . C(3) -0.226(4) 0.806(2) -0.298(2) 0.052(7) Uiso d . 1.00 . C(4) -0.166(4) 0.863(2) -0.148(2) 0.056(7) Uiso d . 1.00 . C(5) -0.237(4) 1.011(2) -0.104(2) 0.051(7) Uiso d . 1.00 . C(6) 0.477(5) 0.662(2) -0.212(2) 0.062(8) Uiso d . 1.00 . C(7) 0.381(6) 0.655(2) -0.100(3) 0.08(1) Uiso d . 1.00 . C(8) 0.407(5) 0.672(2) 0.067(2) 0.047(7) Uiso d . 1.00 . C(9) 0.272(5) 0.679(2) 0.169(2) 0.031(8) Uiso d . 1.00 . C(10) 0.341(4) 0.702(2) 0.348(2) 0.050(7) Uiso d . 1.00 . C(11) 0.166(6) 1.077(2) -0.326(2) 0.064(9) Uiso d . 1.00 . #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb Nb 2.880(5) 1_555 2_747 Nb S 2.393(7) 1_555 1_555 Nb S 2.37(1) 1_555 2_747 Nb O(1) 1.99(1) 1_555 1_555 Nb O(2) 2.15(1) 1_555 1_555 Nb O(3) 2.29(3) 1_555 1_555 Nb O(4) 1.98(2) 1_555 1_555 Cl(1) C(11) 1.75(3) 1_555 1_555 Cl(2) C(11) 1.75(4) 1_555 1_555 O(1) C(2) 1.35(3) 1_555 1_555 O(2) C(4) 1.30(3) 1_555 1_555 O(3) C(7) 1.39(5) 1_555 1_555 O(4) C(9) 1.22(5) 1_555 1_555 C(1) C(2) 1.57(3) 1_555 1_555 C(2) C(3) 1.42(2) 1_555 1_555 C(3) C(4) 1.47(3) 1_555 1_555 C(4) C(5) 1.57(3) 1_555 1_555 C(6) C(7) 1.41(5) 1_555 1_555 C(7) C(8) 1.45(3) 1_555 1_555 C(8) C(9) 1.56(5) 1_555 1_555 C(9) C(10) 1.64(3) 1_555 1_555 #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 Nb Nb S 52.4(3) 2_747 1_555 1_555 Nb Nb S 53.1(2) 2_747 1_555 2_747 Nb Nb O(1) 100.6(5) 2_747 1_555 1_555 Nb Nb O(2) 141.1(6) 2_747 1_555 1_555 Nb Nb O(3) 138.1(5) 2_747 1_555 1_555 Nb Nb O(4) 99.0(5) 2_747 1_555 1_555 S Nb S 105.6(3) 1_555 1_555 2_747 S Nb O(1) 93.1(4) 1_555 1_555 1_555 S Nb O(2) 166.2(6) 1_555 1_555 1_555 S Nb O(3) 86.3(5) 1_555 1_555 1_555 S Nb O(4) 99.7(5) 1_555 1_555 1_555 S Nb O(1) 99.8(7) 2_747 1_555 1_555 S Nb O(2) 88.0(6) 2_747 1_555 1_555 S Nb O(3) 165.7(4) 2_747 1_555 1_555 S Nb O(4) 91.1(8) 2_747 1_555 1_555 O(1) Nb O(2) 82.0(5) 1_555 1_555 1_555 O(1) Nb O(3) 87.2(8) 1_555 1_555 1_555 O(1) Nb O(4) 160.3(6) 1_555 1_555 1_555 O(2) Nb O(3) 80.5(7) 1_555 1_555 1_555 O(2) Nb O(4) 82.0(6) 1_555 1_555 1_555 O(3) Nb O(4) 78.9(9) 1_555 1_555 1_555 Nb S Nb 74.4(3) 1_555 1_555 2_747 Nb O(1) C(2) 134(1) 1_555 1_555 1_555 Nb O(2) C(4) 130(1) 1_555 1_555 1_555 Nb O(3) C(7) 136(1) 1_555 1_555 1_555 Nb O(4) C(9) 133(2) 1_555 1_555 1_555 O(1) C(2) C(1) 113(1) 1_555 1_555 1_555 O(1) C(2) C(3) 127(2) 1_555 1_555 1_555 C(1) C(2) C(3) 119(2) 1_555 1_555 1_555 C(2) C(3) C(4) 116(2) 1_555 1_555 1_555 O(2) C(4) C(3) 127(1) 1_555 1_555 1_555 O(2) C(4) C(5) 118(1) 1_555 1_555 1_555 C(3) C(4) C(5) 113(2) 1_555 1_555 1_555 O(3) C(7) C(6) 116(2) 1_555 1_555 1_555 O(3) C(7) C(8) 114(3) 1_555 1_555 1_555 C(6) C(7) C(8) 128(4) 1_555 1_555 1_555 C(7) C(8) C(9) 119(3) 1_555 1_555 1_555 O(4) C(9) C(8) 132(2) 1_555 1_555 1_555 O(4) C(9) C(10) 121(2) 1_555 1_555 1_555 C(8) C(9) C(10) 106(3) 1_555 1_555 1_555 Cl(1) C(11) Cl(2) 110(1) 1_555 1_555 1_555 #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(4) 3.42(4) 1_555 1_555 S C(8) 3.56(4) 1_555 2_847 O(1) C(1) 3.42(3) 1_555 2_746 O(2) C(11) 3.45(3) 1_555 2_757 O(4) C(11) 3.58(4) 1_555 2_757 C(2) C(6) 3.54(6) 1_555 1_455 C(5) C(8) 3.39(3) 1_555 2_757 C(5) C(9) 3.54(3) 1_555 2_757 #------------------------------------------------------------------------------ #===END # data for [[Nb2S(Te2)(dtc)4]CHCl3 data_3 #------------------------------------------------------------------------------ _audit_creation_date 'Wed May 6 20:07:35 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record 'May 7 1998' #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92 (Altomare, A. et al. 1994)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_formula_weight 1185.49 _chemical_formula_sum 'C21 H41 Cl3 N4 Nb2 S9 Te2 ' _chemical_formula_structural '[Nb2 S (Te2) (S2 C N (C2H5)2)4] C H Cl3' #------------------------------------------------------------------------------ _cell_length_a 13.030(3) _cell_length_b 14.391(5) _cell_length_c 12.053(4) _cell_angle_alpha 97.61(3) _cell_angle_beta 110.81(2) _cell_angle_gamma 78.40(3) _cell_volume 2064(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173.2 _cell_measurement_reflns_used 16 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.907 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1152.00 _exptl_absorpt_coefficient_mu 2.610 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.429 #------------------------------------------------------------------------------ _diffrn_special_details ; voltage and current for X-ray generation: 46 kV, 260 mA scan width (\w): ( 1.60 + 0.30tan\w) deg with a fractional offset 0.5. scan speed (\w): 16 deg/min background-count time: 25% of the peak-scan time on each side Weak reflections ( I < 10.0\s(I) ) were rescanned one more time, and the counts were accumulated. Linear correction for decay (1.65%) was applied. ; _diffrn_ambient_temperature 173.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.65 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 2 1 -2 2 0 -2 1 -1 _diffrn_reflns_number 9893 _reflns_number_total 9476 _reflns_number_observed 3191 _reflns_observed_criterion >2.5sigma(I) _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_av_sigmaI/netI 0.201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.54 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.06968 _diffrn_orient_matrix_UB_12 0.02364 _diffrn_orient_matrix_UB_13 0.01939 _diffrn_orient_matrix_UB_21 0.04324 _diffrn_orient_matrix_UB_22 -0.00691 _diffrn_orient_matrix_UB_23 0.08641 _diffrn_orient_matrix_UB_31 0.01442 _diffrn_orient_matrix_UB_32 0.06669 _diffrn_orient_matrix_UB_33 0.00839 #------------------------------------------------------------------------------ _refine_special_details ; Heavy atoms (Te, Nb, and S) were refined anisotropically, and other non-hydrogen atoms were refined isotropically. Hydrogen atoms were included at the calculated positons but not refined. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + (1/4)(0.004|Fo|)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 3191 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0910 _refine_ls_wR_factor_obs 0.0554 _refine_ls_goodness_of_fit_obs 2.568 _refine_ls_shift/esd_max 0.0078 _refine_ls_shift/esd_mean 0.0005 _refine_diff_density_min -1.53 _refine_diff_density_max 1.97 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 42 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 82 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 8 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 18 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Nb 0 4 -2.073 0.621 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Te 0 4 -0.531 1.675 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 6 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Te(1) 0.9706(2) 0.3393(1) 0.9938(1) 0.0440(7) Uani d . 1.00 . Te(2) 0.8989(2) 0.1793(1) 0.8898(2) 0.0527(8) Uani d . 1.00 . Nb(1) 0.9898(2) 0.2782(2) 0.7667(2) 0.0374(9) Uani d . 1.00 . Nb(2) 0.7723(2) 0.3521(2) 0.7904(2) 0.0374(9) Uani d . 1.00 . Cl(1) 0.823(2) -0.127(2) 0.549(1) 0.35(1) Uani d . 1.00 . Cl(2) 0.722(1) 0.0030(9) 0.666(2) 0.253(9) Uani d . 1.00 . Cl(3) 0.916(2) -0.092(1) 0.817(1) 0.26(1) Uani d . 1.00 . S(1) 0.8155(6) 0.3095(5) 0.6119(5) 0.054(3) Uani d . 1.00 . S(2) 1.1781(6) 0.1697(5) 0.8753(6) 0.056(3) Uani d . 1.00 . S(3) 1.0145(7) 0.1152(5) 0.6523(6) 0.053(3) Uani d . 1.00 . S(4) 1.0743(7) 0.4262(5) 0.8226(6) 0.059(3) Uani d . 1.00 . S(5) 1.0750(6) 0.3122(5) 0.6126(6) 0.047(3) Uani d . 1.00 . S(6) 0.6609(7) 0.3552(6) 0.9307(6) 0.071(3) Uani d . 1.00 . S(7) 0.6133(6) 0.2533(5) 0.7005(6) 0.055(3) Uani d . 1.00 . S(8) 0.7955(6) 0.5229(5) 0.8466(6) 0.051(3) Uani d . 1.00 . S(9) 0.6029(6) 0.4674(5) 0.6654(6) 0.051(3) Uani d . 1.00 . N(1) 1.195(2) -0.003(2) 0.770(2) 0.070(8) Uiso d . 1.00 . N(2) 1.143(2) 0.485(2) 0.661(2) 0.063(7) Uiso d . 1.00 . N(3) 0.486(2) 0.264(1) 0.839(2) 0.050(6) Uiso d . 1.00 . N(4) 0.640(2) 0.648(2) 0.714(2) 0.069(7) Uiso d . 1.00 . C(1) 1.136(3) 0.083(2) 0.768(2) 0.069(9) Uiso d . 1.00 . C(2) 1.105(2) 0.417(2) 0.691(2) 0.038(7) Uiso d . 1.00 . C(3) 0.572(2) 0.290(2) 0.824(2) 0.053(8) Uiso d . 1.00 . C(4) 0.669(2) 0.557(2) 0.739(2) 0.046(7) Uiso d . 1.00 . C(5) 1.295(3) -0.027(2) 0.880(3) 0.09(1) Uiso d . 1.00 . C(6) 1.259(3) -0.074(2) 0.962(3) 0.12(1) Uiso d . 1.00 . C(7) 1.168(4) -0.072(3) 0.649(4) 0.15(2) Uiso d . 1.00 . C(8) 1.143(6) -0.131(5) 0.698(6) 0.36(5) Uiso d . 1.00 . C(9) 1.194(4) 0.568(3) 0.751(3) 0.14(2) Uiso d . 1.00 . C(10) 1.095(6) 0.634(4) 0.710(5) 0.30(3) Uiso d . 1.00 . C(11) 1.160(3) 0.470(2) 0.548(3) 0.08(1) Uiso d . 1.00 . C(12) 1.282(4) 0.437(3) 0.569(3) 0.17(2) Uiso d . 1.00 . C(13) 0.476(3) 0.274(3) 0.961(3) 0.12(1) Uiso d . 1.00 . C(14) 0.405(3) 0.371(3) 0.942(3) 0.10(1) Uiso d . 1.00 . C(15) 0.407(3) 0.207(2) 0.737(3) 0.10(1) Uiso d . 1.00 . C(16) 0.441(3) 0.100(3) 0.762(3) 0.13(1) Uiso d . 1.00 . C(17) 0.722(4) 0.728(3) 0.744(4) 0.15(2) Uiso d . 1.00 . C(18) 0.666(6) 0.766(5) 0.807(5) 0.29(4) Uiso d . 1.00 . C(19) 0.514(4) 0.685(3) 0.620(3) 0.11(1) Uiso d . 1.00 . C(20) 0.437(5) 0.687(4) 0.682(4) 0.24(3) Uiso d . 1.00 . C(21) 0.844(5) -0.066(4) 0.645(5) 0.20(2) Uiso d . 1.00 . H(1) 1.3521 -0.0691 0.8583 0.1072 Uiso calc . 1.00 . H(2) 1.3223 0.0296 0.9190 0.1072 Uiso calc . 1.00 . H(3) 1.2023 -0.0315 0.9841 0.1395 Uiso calc . 1.00 . H(4) 1.2311 -0.1301 0.9227 0.1395 Uiso calc . 1.00 . H(5) 1.3209 -0.0902 1.0318 0.1395 Uiso calc . 1.00 . H(6) 1.1086 -0.0448 0.5844 0.1815 Uiso calc . 1.00 . H(7) 1.2312 -0.0962 0.6253 0.1815 Uiso calc . 1.00 . H(8) 1.0824 -0.1018 0.7235 0.4285 Uiso calc . 1.00 . H(9) 1.1218 -0.1832 0.6422 0.4285 Uiso calc . 1.00 . H(10) 1.2050 -0.1534 0.7641 0.4285 Uiso calc . 1.00 . H(11) 1.2134 0.5552 0.8319 0.1719 Uiso calc . 1.00 . H(12) 1.2553 0.5847 0.7384 0.1719 Uiso calc . 1.00 . H(13) 1.1048 0.6930 0.7537 0.3542 Uiso calc . 1.00 . H(14) 1.0781 0.6410 0.6280 0.3542 Uiso calc . 1.00 . H(15) 1.0358 0.6111 0.7209 0.3542 Uiso calc . 1.00 . H(16) 1.1191 0.4225 0.5002 0.0958 Uiso calc . 1.00 . H(17) 1.1359 0.5272 0.5092 0.0958 Uiso calc . 1.00 . H(18) 1.3054 0.3791 0.6079 0.2024 Uiso calc . 1.00 . H(19) 1.2939 0.4269 0.4951 0.2024 Uiso calc . 1.00 . H(20) 1.3224 0.4839 0.6177 0.2024 Uiso calc . 1.00 . H(21) 0.4398 0.2272 0.9728 0.1425 Uiso calc . 1.00 . H(22) 0.5459 0.2741 1.0232 0.1425 Uiso calc . 1.00 . H(23) 0.4445 0.4134 0.9263 0.1243 Uiso calc . 1.00 . H(24) 0.3385 0.3664 0.8759 0.1243 Uiso calc . 1.00 . H(25) 0.3865 0.3938 1.0111 0.1243 Uiso calc . 1.00 . H(26) 0.3327 0.2285 0.7340 0.1154 Uiso calc . 1.00 . H(27) 0.4140 0.2161 0.6633 0.1154 Uiso calc . 1.00 . H(28) 0.4351 0.0915 0.8359 0.1564 Uiso calc . 1.00 . H(29) 0.3936 0.0644 0.7002 0.1564 Uiso calc . 1.00 . H(30) 0.5162 0.0789 0.7649 0.1564 Uiso calc . 1.00 . H(31) 0.7989 0.7064 0.7850 0.1793 Uiso calc . 1.00 . H(32) 0.7153 0.7625 0.6788 0.1793 Uiso calc . 1.00 . H(33) 0.6907 0.8230 0.8457 0.3518 Uiso calc . 1.00 . H(34) 0.5896 0.7795 0.7585 0.3518 Uiso calc . 1.00 . H(35) 0.6734 0.7236 0.8648 0.3518 Uiso calc . 1.00 . H(36) 0.5103 0.7472 0.5980 0.1307 Uiso calc . 1.00 . H(37) 0.4980 0.6429 0.5512 0.1307 Uiso calc . 1.00 . H(38) 0.4542 0.7291 0.7513 0.2930 Uiso calc . 1.00 . H(39) 0.3631 0.7083 0.6310 0.2930 Uiso calc . 1.00 . H(40) 0.4415 0.6249 0.7040 0.2930 Uiso calc . 1.00 . H(41) 0.8833 -0.0222 0.6311 0.2435 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Te(1) 0.043(1) 0.049(2) 0.040(1) -0.010(1) 0.0121(10) 0.0031(10) Te(2) 0.064(2) 0.048(2) 0.051(1) -0.019(1) 0.017(1) 0.009(1) Nb(1) 0.037(2) 0.038(2) 0.038(1) -0.003(2) 0.014(1) 0.003(1) Nb(2) 0.031(2) 0.042(2) 0.038(1) -0.005(2) 0.013(1) -0.002(1) Cl(1) 0.33(3) 0.55(3) 0.25(2) -0.26(2) 0.20(2) -0.30(2) Cl(2) 0.20(2) 0.11(1) 0.50(3) -0.02(1) 0.23(2) -0.09(1) Cl(3) 0.37(3) 0.21(2) 0.26(2) -0.07(2) 0.19(2) -0.03(1) S(1) 0.036(5) 0.080(7) 0.042(4) 0.002(5) 0.009(4) 0.023(4) S(2) 0.049(6) 0.045(6) 0.061(5) 0.004(5) 0.009(4) 0.003(4) S(3) 0.062(6) 0.035(5) 0.057(5) -0.001(5) 0.018(4) -0.003(4) S(4) 0.076(7) 0.066(6) 0.049(4) -0.038(6) 0.031(4) -0.012(4) S(5) 0.050(6) 0.042(5) 0.057(5) 0.002(5) 0.034(4) 0.001(4) S(6) 0.061(6) 0.112(8) 0.048(5) -0.030(6) 0.027(4) -0.012(5) S(7) 0.048(6) 0.061(6) 0.056(5) -0.019(5) 0.010(4) 0.002(4) S(8) 0.038(5) 0.046(6) 0.054(4) -0.001(4) 0.000(4) -0.001(4) S(9) 0.036(5) 0.049(6) 0.053(4) 0.003(5) 0.005(4) -0.007(4) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Te(1) Te(2) 2.648(3) 1_555 1_555 Te(1) Nb(1) 2.844(3) 1_555 1_555 Te(1) Nb(2) 2.854(3) 1_555 1_555 Te(2) Nb(1) 2.848(3) 1_555 1_555 Te(2) Nb(2) 2.842(3) 1_555 1_555 Nb(1) Nb(2) 2.920(4) 1_555 1_555 Nb(1) S(1) 2.376(7) 1_555 1_555 Nb(1) S(2) 2.625(8) 1_555 1_555 Nb(1) S(3) 2.581(8) 1_555 1_555 Nb(1) S(4) 2.499(7) 1_555 1_555 Nb(1) S(5) 2.618(7) 1_555 1_555 Nb(2) S(1) 2.387(8) 1_555 1_555 Nb(2) S(6) 2.581(8) 1_555 1_555 Nb(2) S(7) 2.581(7) 1_555 1_555 Nb(2) S(8) 2.511(7) 1_555 1_555 Nb(2) S(9) 2.593(8) 1_555 1_555 Cl(1) C(21) 1.33(6) 1_555 1_555 Cl(2) C(21) 1.78(6) 1_555 1_555 Cl(3) C(21) 2.01(5) 1_555 1_555 S(2) C(1) 1.69(3) 1_555 1_555 S(3) C(1) 1.73(3) 1_555 1_555 S(4) C(2) 1.75(2) 1_555 1_555 S(5) C(2) 1.70(2) 1_555 1_555 S(6) C(3) 1.71(2) 1_555 1_555 S(7) C(3) 1.74(3) 1_555 1_555 S(8) C(4) 1.72(2) 1_555 1_555 S(9) C(4) 1.67(2) 1_555 1_555 N(1) C(1) 1.32(3) 1_555 1_555 N(1) C(5) 1.51(3) 1_555 1_555 N(1) C(7) 1.62(4) 1_555 1_555 N(2) C(2) 1.33(3) 1_555 1_555 N(2) C(9) 1.58(4) 1_555 1_555 N(2) C(11) 1.43(3) 1_555 1_555 N(3) C(3) 1.33(3) 1_555 1_555 N(3) C(13) 1.50(4) 1_555 1_555 N(3) C(15) 1.55(3) 1_555 1_555 N(4) C(4) 1.33(3) 1_555 1_555 N(4) C(17) 1.64(4) 1_555 1_555 N(4) C(19) 1.65(4) 1_555 1_555 C(5) C(6) 1.52(4) 1_555 1_555 C(7) C(8) 1.24(8) 1_555 1_555 C(9) C(10) 1.40(7) 1_555 1_555 C(11) C(12) 1.50(5) 1_555 1_555 C(13) C(14) 1.51(4) 1_555 1_555 C(15) C(16) 1.55(4) 1_555 1_555 C(17) C(18) 1.24(8) 1_555 1_555 C(19) C(20) 1.45(6) 1_555 1_555 #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 Te(2) Te(1) Nb(1) 62.37(7) 1_555 1_555 1_555 Te(2) Te(1) Nb(2) 62.06(7) 1_555 1_555 1_555 Nb(1) Te(1) Nb(2) 61.66(8) 1_555 1_555 1_555 Te(1) Te(2) Nb(1) 62.19(7) 1_555 1_555 1_555 Te(1) Te(2) Nb(2) 62.54(7) 1_555 1_555 1_555 Nb(1) Te(2) Nb(2) 61.76(8) 1_555 1_555 1_555 Te(1) Nb(1) Te(2) 55.44(7) 1_555 1_555 1_555 Te(1) Nb(1) Nb(2) 59.35(8) 1_555 1_555 1_555 Te(1) Nb(1) S(1) 111.5(2) 1_555 1_555 1_555 Te(1) Nb(1) S(2) 88.1(2) 1_555 1_555 1_555 Te(1) Nb(1) S(3) 134.8(2) 1_555 1_555 1_555 Te(1) Nb(1) S(4) 76.4(2) 1_555 1_555 1_555 Te(1) Nb(1) S(5) 143.3(2) 1_555 1_555 1_555 Te(2) Nb(1) Nb(2) 59.01(8) 1_555 1_555 1_555 Te(2) Nb(1) S(1) 91.8(2) 1_555 1_555 1_555 Te(2) Nb(1) S(2) 84.3(2) 1_555 1_555 1_555 Te(2) Nb(1) S(3) 83.6(2) 1_555 1_555 1_555 Te(2) Nb(1) S(4) 131.8(2) 1_555 1_555 1_555 Te(2) Nb(1) S(5) 160.2(2) 1_555 1_555 1_555 Nb(2) Nb(1) S(1) 52.4(2) 1_555 1_555 1_555 Nb(2) Nb(1) S(2) 140.1(2) 1_555 1_555 1_555 Nb(2) Nb(1) S(3) 118.0(2) 1_555 1_555 1_555 Nb(2) Nb(1) S(4) 99.8(2) 1_555 1_555 1_555 Nb(2) Nb(1) S(5) 130.3(2) 1_555 1_555 1_555 S(1) Nb(1) S(2) 153.2(3) 1_555 1_555 1_555 S(1) Nb(1) S(3) 85.4(3) 1_555 1_555 1_555 S(1) Nb(1) S(4) 108.8(3) 1_555 1_555 1_555 S(1) Nb(1) S(5) 85.3(2) 1_555 1_555 1_555 S(2) Nb(1) S(3) 67.8(2) 1_555 1_555 1_555 S(2) Nb(1) S(4) 93.2(3) 1_555 1_555 1_555 S(2) Nb(1) S(5) 89.5(3) 1_555 1_555 1_555 S(3) Nb(1) S(4) 139.4(3) 1_555 1_555 1_555 S(3) Nb(1) S(5) 76.7(2) 1_555 1_555 1_555 S(4) Nb(1) S(5) 67.2(2) 1_555 1_555 1_555 Te(1) Nb(2) Te(2) 55.40(7) 1_555 1_555 1_555 Te(1) Nb(2) Nb(1) 58.99(8) 1_555 1_555 1_555 Te(1) Nb(2) S(1) 110.8(2) 1_555 1_555 1_555 Te(1) Nb(2) S(6) 88.4(2) 1_555 1_555 1_555 Te(1) Nb(2) S(7) 134.6(2) 1_555 1_555 1_555 Te(1) Nb(2) S(8) 77.2(2) 1_555 1_555 1_555 Te(1) Nb(2) S(9) 144.5(2) 1_555 1_555 1_555 Te(2) Nb(2) Nb(1) 59.23(8) 1_555 1_555 1_555 Te(2) Nb(2) S(1) 91.7(2) 1_555 1_555 1_555 Te(2) Nb(2) S(6) 86.6(2) 1_555 1_555 1_555 Te(2) Nb(2) S(7) 84.0(2) 1_555 1_555 1_555 Te(2) Nb(2) S(8) 132.6(2) 1_555 1_555 1_555 Te(2) Nb(2) S(9) 158.5(2) 1_555 1_555 1_555 Nb(1) Nb(2) S(1) 52.0(2) 1_555 1_555 1_555 Nb(1) Nb(2) S(6) 141.7(2) 1_555 1_555 1_555 Nb(1) Nb(2) S(7) 119.8(2) 1_555 1_555 1_555 Nb(1) Nb(2) S(8) 98.4(2) 1_555 1_555 1_555 Nb(1) Nb(2) S(9) 131.6(2) 1_555 1_555 1_555 S(1) Nb(2) S(6) 155.3(2) 1_555 1_555 1_555 S(1) Nb(2) S(7) 87.5(2) 1_555 1_555 1_555 S(1) Nb(2) S(8) 106.5(3) 1_555 1_555 1_555 S(1) Nb(2) S(9) 86.2(2) 1_555 1_555 1_555 S(6) Nb(2) S(7) 67.8(2) 1_555 1_555 1_555 S(6) Nb(2) S(8) 92.5(3) 1_555 1_555 1_555 S(6) Nb(2) S(9) 86.4(3) 1_555 1_555 1_555 S(7) Nb(2) S(8) 138.7(3) 1_555 1_555 1_555 S(7) Nb(2) S(9) 74.6(2) 1_555 1_555 1_555 S(8) Nb(2) S(9) 68.0(2) 1_555 1_555 1_555 Nb(1) S(1) Nb(2) 75.6(2) 1_555 1_555 1_555 Nb(1) S(2) C(1) 87(1) 1_555 1_555 1_555 Nb(1) S(3) C(1) 88(1) 1_555 1_555 1_555 Nb(1) S(4) C(2) 92.6(8) 1_555 1_555 1_555 Nb(1) S(5) C(2) 89.7(9) 1_555 1_555 1_555 Nb(2) S(6) C(3) 89(1) 1_555 1_555 1_555 Nb(2) S(7) C(3) 89.0(9) 1_555 1_555 1_555 Nb(2) S(8) C(4) 89.5(9) 1_555 1_555 1_555 Nb(2) S(9) C(4) 87.9(10) 1_555 1_555 1_555 C(1) N(1) C(5) 117(2) 1_555 1_555 1_555 C(1) N(1) C(7) 118(2) 1_555 1_555 1_555 C(5) N(1) C(7) 122(2) 1_555 1_555 1_555 C(2) N(2) C(9) 123(2) 1_555 1_555 1_555 C(2) N(2) C(11) 116(2) 1_555 1_555 1_555 C(9) N(2) C(11) 118(2) 1_555 1_555 1_555 C(3) N(3) C(13) 119(2) 1_555 1_555 1_555 C(3) N(3) C(15) 120(2) 1_555 1_555 1_555 C(13) N(3) C(15) 119(2) 1_555 1_555 1_555 C(4) N(4) C(17) 127(2) 1_555 1_555 1_555 C(4) N(4) C(19) 119(2) 1_555 1_555 1_555 C(17) N(4) C(19) 112(2) 1_555 1_555 1_555 S(2) C(1) S(3) 116(1) 1_555 1_555 1_555 S(2) C(1) N(1) 121(2) 1_555 1_555 1_555 S(3) C(1) N(1) 121(2) 1_555 1_555 1_555 S(4) C(2) S(5) 110(1) 1_555 1_555 1_555 S(4) C(2) N(2) 122(1) 1_555 1_555 1_555 S(5) C(2) N(2) 127(2) 1_555 1_555 1_555 S(6) C(3) S(7) 113(1) 1_555 1_555 1_555 S(6) C(3) N(3) 123(2) 1_555 1_555 1_555 S(7) C(3) N(3) 123(1) 1_555 1_555 1_555 S(8) C(4) S(9) 114(1) 1_555 1_555 1_555 S(8) C(4) N(4) 118(1) 1_555 1_555 1_555 S(9) C(4) N(4) 127(2) 1_555 1_555 1_555 N(1) C(5) C(6) 108(2) 1_555 1_555 1_555 N(1) C(5) H(1) 109(2) 1_555 1_555 1_555 N(1) C(5) H(2) 109(2) 1_555 1_555 1_555 C(6) C(5) H(1) 109(3) 1_555 1_555 1_555 C(6) C(5) H(2) 109(2) 1_555 1_555 1_555 H(1) C(5) H(2) 109(3) 1_555 1_555 1_555 C(5) C(6) H(3) 109(3) 1_555 1_555 1_555 C(5) C(6) H(4) 109(3) 1_555 1_555 1_555 C(5) C(6) H(5) 109(3) 1_555 1_555 1_555 H(3) C(6) H(4) 109(3) 1_555 1_555 1_555 H(3) C(6) H(5) 109(3) 1_555 1_555 1_555 H(4) C(6) H(5) 109(3) 1_555 1_555 1_555 N(1) C(7) C(8) 91(4) 1_555 1_555 1_555 N(1) C(7) H(6) 113(4) 1_555 1_555 1_555 N(1) C(7) H(7) 113(3) 1_555 1_555 1_555 C(8) C(7) H(6) 113(6) 1_555 1_555 1_555 C(8) C(7) H(7) 113(6) 1_555 1_555 1_555 H(6) C(7) H(7) 109(4) 1_555 1_555 1_555 C(7) C(8) H(8) 109(7) 1_555 1_555 1_555 C(7) C(8) H(9) 109(7) 1_555 1_555 1_555 C(7) C(8) H(10) 109(7) 1_555 1_555 1_555 H(8) C(8) H(9) 109(7) 1_555 1_555 1_555 H(8) C(8) H(10) 109(7) 1_555 1_555 1_555 H(9) C(8) H(10) 109(7) 1_555 1_555 1_555 N(2) C(9) C(10) 93(3) 1_555 1_555 1_555 N(2) C(9) H(11) 113(3) 1_555 1_555 1_555 N(2) C(9) H(12) 113(3) 1_555 1_555 1_555 C(10) C(9) H(11) 113(5) 1_555 1_555 1_555 C(10) C(9) H(12) 113(4) 1_555 1_555 1_555 H(11) C(9) H(12) 109(4) 1_555 1_555 1_555 C(9) C(10) H(13) 109(5) 1_555 1_555 1_555 C(9) C(10) H(14) 109(6) 1_555 1_555 1_555 C(9) C(10) H(15) 109(5) 1_555 1_555 1_555 H(13) C(10) H(14) 109(5) 1_555 1_555 1_555 H(13) C(10) H(15) 109(6) 1_555 1_555 1_555 H(14) C(10) H(15) 109(6) 1_555 1_555 1_555 N(2) C(11) C(12) 108(2) 1_555 1_555 1_555 N(2) C(11) H(16) 109(2) 1_555 1_555 1_555 N(2) C(11) H(17) 109(3) 1_555 1_555 1_555 C(12) C(11) H(16) 109(3) 1_555 1_555 1_555 C(12) C(11) H(17) 109(3) 1_555 1_555 1_555 H(16) C(11) H(17) 109(2) 1_555 1_555 1_555 C(11) C(12) H(18) 109(4) 1_555 1_555 1_555 C(11) C(12) H(19) 109(3) 1_555 1_555 1_555 C(11) C(12) H(20) 109(4) 1_555 1_555 1_555 H(18) C(12) H(19) 109(4) 1_555 1_555 1_555 H(18) C(12) H(20) 109(3) 1_555 1_555 1_555 H(19) C(12) H(20) 109(4) 1_555 1_555 1_555 N(3) C(13) C(14) 93(2) 1_555 1_555 1_555 N(3) C(13) H(21) 113(3) 1_555 1_555 1_555 N(3) C(13) H(22) 113(3) 1_555 1_555 1_555 C(14) C(13) H(21) 113(3) 1_555 1_555 1_555 C(14) C(13) H(22) 113(3) 1_555 1_555 1_555 H(21) C(13) H(22) 109(3) 1_555 1_555 1_555 C(13) C(14) H(23) 109(3) 1_555 1_555 1_555 C(13) C(14) H(24) 109(3) 1_555 1_555 1_555 C(13) C(14) H(25) 109(3) 1_555 1_555 1_555 H(23) C(14) H(24) 109(3) 1_555 1_555 1_555 H(23) C(14) H(25) 109(3) 1_555 1_555 1_555 H(24) C(14) H(25) 109(3) 1_555 1_555 1_555 N(3) C(15) C(16) 108(2) 1_555 1_555 1_555 N(3) C(15) H(26) 109(2) 1_555 1_555 1_555 N(3) C(15) H(27) 109(2) 1_555 1_555 1_555 C(16) C(15) H(26) 109(3) 1_555 1_555 1_555 C(16) C(15) H(27) 109(3) 1_555 1_555 1_555 H(26) C(15) H(27) 109(3) 1_555 1_555 1_555 C(15) C(16) H(28) 109(3) 1_555 1_555 1_555 C(15) C(16) H(29) 109(3) 1_555 1_555 1_555 C(15) C(16) H(30) 109(3) 1_555 1_555 1_555 H(28) C(16) H(29) 109(3) 1_555 1_555 1_555 H(28) C(16) H(30) 109(3) 1_555 1_555 1_555 H(29) C(16) H(30) 109(3) 1_555 1_555 1_555 N(4) C(17) C(18) 82(4) 1_555 1_555 1_555 N(4) C(17) H(31) 115(3) 1_555 1_555 1_555 N(4) C(17) H(32) 115(3) 1_555 1_555 1_555 C(18) C(17) H(31) 115(5) 1_555 1_555 1_555 C(18) C(17) H(32) 115(6) 1_555 1_555 1_555 H(31) C(17) H(32) 109(4) 1_555 1_555 1_555 C(17) C(18) H(33) 109(7) 1_555 1_555 1_555 C(17) C(18) H(34) 109(6) 1_555 1_555 1_555 C(17) C(18) H(35) 109(6) 1_555 1_555 1_555 H(33) C(18) H(34) 109(6) 1_555 1_555 1_555 H(33) C(18) H(35) 109(5) 1_555 1_555 1_555 H(34) C(18) H(35) 109(6) 1_555 1_555 1_555 N(4) C(19) C(20) 106(3) 1_555 1_555 1_555 N(4) C(19) H(36) 110(3) 1_555 1_555 1_555 N(4) C(19) H(37) 110(3) 1_555 1_555 1_555 C(20) C(19) H(36) 110(4) 1_555 1_555 1_555 C(20) C(19) H(37) 110(4) 1_555 1_555 1_555 H(36) C(19) H(37) 109(3) 1_555 1_555 1_555 C(19) C(20) H(38) 109(5) 1_555 1_555 1_555 C(19) C(20) H(39) 109(4) 1_555 1_555 1_555 C(19) C(20) H(40) 109(5) 1_555 1_555 1_555 H(38) C(20) H(39) 109(5) 1_555 1_555 1_555 H(38) C(20) H(40) 109(4) 1_555 1_555 1_555 H(39) C(20) H(40) 109(5) 1_555 1_555 1_555 Cl(1) C(21) Cl(2) 113(3) 1_555 1_555 1_555 Cl(1) C(21) Cl(3) 129(4) 1_555 1_555 1_555 Cl(1) C(21) H(41) 105(5) 1_555 1_555 1_555 Cl(2) C(21) Cl(3) 93(3) 1_555 1_555 1_555 Cl(2) C(21) H(41) 106(4) 1_555 1_555 1_555 Cl(3) C(21) H(41) 106(4) 1_555 1_555 1_555 #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) S(5) 3.42(2) 1_555 2_756 C(8) C(10) 3.59(8) 1_555 1_545 #------------------------------------------------------------------------------ #===END # data for [Nb2(Se2)2(dtc)4] 2CHCl3 data_4 #------------------------------------------------------------------------------ _audit_creation_date 'Sun May 11 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record 'May 11 1998' #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SIR92 (Altomare, A. et al. 1994)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_formula_weight 1333.45 _chemical_formula_sum 'C22 H42 Cl6 N4 Nb2 S8 Se4 ' _chemical_formula_structural '[Nb2 (Se2)2 (S2 C N (C2 H5)2)4] (C H Cl3)2' #------------------------------------------------------------------------------ _cell_length_a 10.899(5) _cell_length_b 12.42(1) _cell_length_c 17.406(5) _cell_angle_alpha 90 _cell_angle_beta 104.25(3) _cell_angle_gamma 90 _cell_volume 2282(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.8 _cell_measurement_theta_max 17.5 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.300 _exptl_crystal_density_diffrn 2.649 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1300.00 _exptl_absorpt_coefficient_mu 4.431 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.461 #------------------------------------------------------------------------------ _diffrn_special_details ; voltage and current for X-ray generation: 50 kV, 200 mA. scan width (\w): ( 1.313 + 0.30tan\w) deg with a fractional offset 0.5. scan speed (\w): 16 deg/min background-count time: 25% of the peak-scan time on each side Weak reflections ( I < 10.0\s(I) ) were rescanned one more time, and the counts were accumulated. Linear correction for decay (10.35%) was applied. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 -3 2 0 -4 3 -1 -4 _diffrn_standards_decay_% -10.35 _diffrn_reflns_number 7261 _reflns_number_total 6934 _reflns_number_observed 2981 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.121 _diffrn_reflns_av_sigmaI/netI 0.144 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 29.99 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.08424 _diffrn_orient_matrix_UB_12 -0.02241 _diffrn_orient_matrix_UB_13 -0.00778 _diffrn_orient_matrix_UB_21 -0.00018 _diffrn_orient_matrix_UB_22 -0.06400 _diffrn_orient_matrix_UB_23 0.03485 _diffrn_orient_matrix_UB_31 -0.04318 _diffrn_orient_matrix_UB_32 -0.04345 _diffrn_orient_matrix_UB_33 -0.04732 #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were included at the calculated positons but not refined. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + (1/4)(0.005|Fo|)^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 2981 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0787 _refine_ls_wR_factor_obs 0.0488 _refine_ls_goodness_of_fit_obs 2.534 _refine_ls_shift/esd_max 0.0065 _refine_ls_shift/esd_mean 0.0006 _refine_diff_density_min -1.56 _refine_diff_density_max 1.42 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 63 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 123 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 12 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 24 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Se 0 12 -0.093 2.226 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Nb 0 6 -2.073 0.621 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Cl 0 9 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Nb 0.4963(1) -0.05109(10) 0.57665(6) 0.0343(4) Uani d . 1.00 . Se(1) 0.7045(1) 0.0138(1) 0.53902(7) 0.0480(5) Uani d . 1.00 . Se(2) 0.6092(1) -0.1367(1) 0.47308(7) 0.0430(4) Uani d . 1.00 . Cl(1) 0.3243(5) -0.2927(5) 0.8519(3) 0.124(2) Uani d . 1.00 . Cl(2) 0.5691(6) -0.2081(6) 0.8964(3) 0.204(3) Uani d . 1.00 . Cl(3) 0.5258(6) -0.3865(5) 0.7989(3) 0.152(3) Uani d . 1.00 . S(1) 0.5864(3) 0.0681(3) 0.6993(2) 0.047(1) Uani d . 1.00 . S(2) 0.6564(3) -0.1527(3) 0.6893(2) 0.049(1) Uani d . 1.00 . S(3) 0.3263(3) -0.0797(3) 0.6573(2) 0.049(1) Uani d . 1.00 . S(4) 0.4008(3) -0.2435(3) 0.5621(2) 0.046(1) Uani d . 1.00 . N(1) 0.770(1) -0.0272(9) 0.8153(6) 0.052(4) Uani d . 1.00 . N(2) 0.200(1) -0.2642(9) 0.6265(6) 0.050(4) Uani d . 1.00 . C(1) 0.681(1) -0.0383(9) 0.7424(7) 0.038(4) Uani d . 1.00 . C(2) 0.296(1) -0.2031(10) 0.6170(6) 0.034(4) Uani d . 1.00 . C(3) 0.788(1) 0.075(1) 0.8567(7) 0.060(5) Uani d . 1.00 . C(4) 0.732(2) 0.076(1) 0.9256(9) 0.115(8) Uani d . 1.00 . C(5) 0.848(1) -0.120(1) 0.8464(7) 0.059(5) Uani d . 1.00 . C(6) 0.978(1) -0.109(2) 0.841(1) 0.111(8) Uani d . 1.00 . C(7) 0.103(1) -0.220(1) 0.6622(8) 0.061(6) Uani d . 1.00 . C(8) -0.002(2) -0.170(2) 0.6025(9) 0.112(8) Uani d . 1.00 . C(9) 0.181(1) -0.371(1) 0.5944(8) 0.072(6) Uani d . 1.00 . C(10) 0.202(2) -0.457(1) 0.6497(9) 0.132(9) Uani d . 1.00 . C(11) 0.460(1) -0.268(1) 0.8266(7) 0.065(6) Uani d . 1.00 . H(1) 0.8757 0.0889 0.8743 0.0716 Uiso calc . 1.00 . H(2) 0.7486 0.1296 0.8209 0.0716 Uiso calc . 1.00 . H(3) 0.7459 0.1451 0.9504 0.1381 Uiso calc . 1.00 . H(4) 0.6439 0.0629 0.9088 0.1381 Uiso calc . 1.00 . H(5) 0.7711 0.0225 0.9623 0.1381 Uiso calc . 1.00 . H(6) 0.8476 -0.1281 0.9007 0.0706 Uiso calc . 1.00 . H(7) 0.8119 -0.1816 0.8176 0.0706 Uiso calc . 1.00 . H(8) 1.0238 -0.1718 0.8622 0.1330 Uiso calc . 1.00 . H(9) 0.9794 -0.1015 0.7868 0.1330 Uiso calc . 1.00 . H(10) 1.0150 -0.0477 0.8697 0.1330 Uiso calc . 1.00 . H(11) 0.0704 -0.2761 0.6882 0.0731 Uiso calc . 1.00 . H(12) 0.1411 -0.1665 0.6998 0.0731 Uiso calc . 1.00 . H(13) 0.0292 -0.1126 0.5766 0.1347 Uiso calc . 1.00 . H(14) -0.0409 -0.2223 0.5645 0.1347 Uiso calc . 1.00 . H(15) -0.0635 -0.1424 0.6281 0.1347 Uiso calc . 1.00 . H(16) 0.0963 -0.3759 0.5638 0.0863 Uiso calc . 1.00 . H(17) 0.2373 -0.3805 0.5609 0.0863 Uiso calc . 1.00 . H(18) 0.1461 -0.4506 0.6835 0.1581 Uiso calc . 1.00 . H(19) 0.1872 -0.5238 0.6220 0.1581 Uiso calc . 1.00 . H(20) 0.2871 -0.4551 0.6806 0.1581 Uiso calc . 1.00 . H(21) 0.4413 -0.2213 0.7818 0.0778 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb 0.0360(7) 0.0340(7) 0.0325(6) 0.0068(7) 0.0078(6) 0.0005(6) Se(1) 0.0403(9) 0.057(1) 0.0449(8) 0.0070(9) 0.0070(7) 0.0049(8) Se(2) 0.0479(9) 0.0415(10) 0.0418(7) 0.0149(9) 0.0153(7) 0.0013(7) Cl(1) 0.083(4) 0.172(6) 0.126(4) -0.022(4) 0.044(3) 0.019(4) Cl(2) 0.184(6) 0.34(1) 0.092(4) -0.169(7) 0.046(4) -0.087(5) Cl(3) 0.167(6) 0.118(6) 0.179(5) 0.044(5) 0.061(5) 0.016(4) S(1) 0.058(3) 0.039(2) 0.041(2) 0.004(2) 0.005(2) -0.003(2) S(2) 0.058(3) 0.043(2) 0.040(2) 0.012(2) 0.001(2) 0.003(2) S(3) 0.057(3) 0.048(3) 0.049(2) 0.006(2) 0.024(2) 0.004(2) S(4) 0.048(2) 0.043(2) 0.049(2) 0.007(2) 0.018(2) 0.000(2) N(1) 0.051(8) 0.056(10) 0.040(7) 0.003(7) -0.003(6) 0.004(6) N(2) 0.061(9) 0.040(9) 0.054(7) -0.008(8) 0.023(7) -0.015(6) C(1) 0.040(8) 0.013(7) 0.063(8) 0.005(7) 0.016(7) 0.003(6) C(2) 0.050(9) 0.025(8) 0.027(6) 0.008(7) 0.008(7) 0.001(5) C(3) 0.07(1) 0.06(1) 0.040(8) -0.010(10) 0.000(8) -0.010(8) C(4) 0.19(2) 0.08(1) 0.10(1) -0.03(2) 0.07(1) -0.02(1) C(5) 0.06(1) 0.06(1) 0.040(8) 0.02(1) -0.006(8) 0.030(8) C(6) 0.05(1) 0.12(2) 0.15(2) 0.01(1) 0.01(1) 0.05(1) C(7) 0.05(1) 0.07(1) 0.063(10) 0.010(10) 0.025(9) 0.000(9) C(8) 0.06(1) 0.18(2) 0.10(1) 0.04(1) 0.02(1) -0.02(1) C(9) 0.08(1) 0.10(2) 0.050(9) 0.01(1) 0.030(9) 0.011(10) C(10) 0.23(2) 0.08(2) 0.08(1) 0.00(2) 0.04(2) 0.02(1) C(11) 0.08(1) 0.07(1) 0.047(9) -0.02(1) 0.017(9) 0.007(8) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb Nb 2.974(2) 1_555 3_656 Nb Se(1) 2.639(2) 1_555 1_555 Nb Se(1) 2.625(2) 1_555 3_656 Nb Se(2) 2.644(2) 1_555 1_555 Nb Se(2) 2.649(2) 1_555 3_656 Nb S(1) 2.585(3) 1_555 1_555 Nb S(2) 2.607(4) 1_555 1_555 Nb S(3) 2.609(4) 1_555 1_555 Nb S(4) 2.593(4) 1_555 1_555 Se(1) Se(2) 2.303(2) 1_555 1_555 Cl(1) C(11) 1.67(1) 1_555 1_555 Cl(2) C(11) 1.65(1) 1_555 1_555 Cl(3) C(11) 1.76(2) 1_555 1_555 S(1) C(1) 1.73(1) 1_555 1_555 S(2) C(1) 1.68(1) 1_555 1_555 S(3) C(2) 1.68(1) 1_555 1_555 S(4) C(2) 1.73(1) 1_555 1_555 N(1) C(1) 1.40(1) 1_555 1_555 N(1) C(3) 1.45(2) 1_555 1_555 N(1) C(5) 1.45(1) 1_555 1_555 N(2) C(2) 1.34(1) 1_555 1_555 N(2) C(7) 1.46(2) 1_555 1_555 N(2) C(9) 1.43(2) 1_555 1_555 C(3) C(4) 1.47(2) 1_555 1_555 C(5) C(6) 1.45(2) 1_555 1_555 C(7) C(8) 1.48(2) 1_555 1_555 C(9) C(10) 1.42(2) 1_555 1_555 #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 Nb Nb Se(1) 55.37(5) 3_656 1_555 1_555 Nb Nb Se(1) 55.82(5) 3_656 1_555 3_656 Nb Nb Se(2) 55.91(4) 3_656 1_555 1_555 Nb Nb Se(2) 55.73(5) 3_656 1_555 3_656 Nb Nb S(1) 114.1(1) 3_656 1_555 1_555 Nb Nb S(2) 136.1(1) 3_656 1_555 1_555 Nb Nb S(3) 136.11(10) 3_656 1_555 1_555 Nb Nb S(4) 113.85(9) 3_656 1_555 1_555 Se(1) Nb Se(1) 111.20(6) 1_555 1_555 3_656 Se(1) Nb Se(2) 51.68(5) 1_555 1_555 1_555 Se(1) Nb Se(2) 88.91(6) 1_555 1_555 3_656 Se(1) Nb S(1) 81.66(9) 1_555 1_555 1_555 Se(1) Nb S(2) 82.93(10) 1_555 1_555 1_555 Se(1) Nb S(3) 160.58(9) 1_555 1_555 1_555 Se(1) Nb S(4) 127.31(9) 1_555 1_555 1_555 Se(1) Nb Se(2) 89.33(6) 3_656 1_555 1_555 Se(1) Nb Se(2) 51.77(5) 3_656 1_555 3_656 Se(1) Nb S(1) 127.47(10) 3_656 1_555 1_555 Se(1) Nb S(2) 160.0(1) 3_656 1_555 1_555 Se(1) Nb S(3) 82.43(9) 3_656 1_555 1_555 Se(1) Nb S(4) 81.30(9) 3_656 1_555 1_555 Se(2) Nb Se(2) 111.64(5) 1_555 1_555 3_656 Se(2) Nb S(1) 130.34(10) 1_555 1_555 1_555 Se(2) Nb S(2) 88.86(9) 1_555 1_555 1_555 Se(2) Nb S(3) 145.46(10) 1_555 1_555 1_555 Se(2) Nb S(4) 78.81(8) 1_555 1_555 1_555 Se(2) Nb S(1) 79.18(9) 3_656 1_555 1_555 Se(2) Nb S(2) 145.90(10) 3_656 1_555 1_555 Se(2) Nb S(3) 89.25(9) 3_656 1_555 1_555 Se(2) Nb S(4) 130.35(9) 3_656 1_555 1_555 S(1) Nb S(2) 66.9(1) 1_555 1_555 1_555 S(1) Nb S(3) 79.0(1) 1_555 1_555 1_555 S(1) Nb S(4) 132.1(1) 1_555 1_555 1_555 S(2) Nb S(3) 87.8(1) 1_555 1_555 1_555 S(2) Nb S(4) 78.8(1) 1_555 1_555 1_555 S(3) Nb S(4) 66.8(1) 1_555 1_555 1_555 Nb Se(1) Nb 68.80(6) 1_555 1_555 3_656 Nb Se(1) Se(2) 64.27(6) 1_555 1_555 1_555 Nb Se(1) Se(2) 64.67(5) 3_656 1_555 1_555 Nb Se(2) Nb 68.36(5) 1_555 1_555 3_656 Nb Se(2) Se(1) 64.05(6) 1_555 1_555 1_555 Nb Se(2) Se(1) 63.56(6) 3_656 1_555 1_555 Nb S(1) C(1) 89.2(4) 1_555 1_555 1_555 Nb S(2) C(1) 89.5(4) 1_555 1_555 1_555 Nb S(3) C(2) 89.4(4) 1_555 1_555 1_555 Nb S(4) C(2) 88.9(4) 1_555 1_555 1_555 C(1) N(1) C(3) 120(1) 1_555 1_555 1_555 C(1) N(1) C(5) 118(1) 1_555 1_555 1_555 C(3) N(1) C(5) 121(1) 1_555 1_555 1_555 C(2) N(2) C(7) 120(1) 1_555 1_555 1_555 C(2) N(2) C(9) 121(1) 1_555 1_555 1_555 C(7) N(2) C(9) 117(1) 1_555 1_555 1_555 S(1) C(1) S(2) 114.2(7) 1_555 1_555 1_555 S(1) C(1) N(1) 121.6(9) 1_555 1_555 1_555 S(2) C(1) N(1) 124.2(9) 1_555 1_555 1_555 S(3) C(2) S(4) 114.0(8) 1_555 1_555 1_555 S(3) C(2) N(2) 122.9(10) 1_555 1_555 1_555 S(4) C(2) N(2) 123.1(10) 1_555 1_555 1_555 N(1) C(3) C(4) 112(1) 1_555 1_555 1_555 N(1) C(3) H(1) 108(1) 1_555 1_555 1_555 N(1) C(3) H(2) 108(1) 1_555 1_555 1_555 C(4) C(3) H(1) 108(1) 1_555 1_555 1_555 C(4) C(3) H(2) 108(1) 1_555 1_555 1_555 H(1) C(3) H(2) 109(1) 1_555 1_555 1_555 C(3) C(4) H(3) 109(1) 1_555 1_555 1_555 C(3) C(4) H(4) 109(1) 1_555 1_555 1_555 C(3) C(4) H(5) 109(1) 1_555 1_555 1_555 H(3) C(4) H(4) 109(1) 1_555 1_555 1_555 H(3) C(4) H(5) 109(1) 1_555 1_555 1_555 H(4) C(4) H(5) 109(1) 1_555 1_555 1_555 N(1) C(5) C(6) 113(1) 1_555 1_555 1_555 N(1) C(5) H(6) 108(1) 1_555 1_555 1_555 N(1) C(5) H(7) 108(1) 1_555 1_555 1_555 C(6) C(5) H(6) 108(1) 1_555 1_555 1_555 C(6) C(5) H(7) 108(1) 1_555 1_555 1_555 H(6) C(5) H(7) 109(1) 1_555 1_555 1_555 C(5) C(6) H(8) 109(1) 1_555 1_555 1_555 C(5) C(6) H(9) 109(1) 1_555 1_555 1_555 C(5) C(6) H(10) 109(1) 1_555 1_555 1_555 H(8) C(6) H(9) 109(1) 1_555 1_555 1_555 H(8) C(6) H(10) 109(1) 1_555 1_555 1_555 H(9) C(6) H(10) 109(1) 1_555 1_555 1_555 N(2) C(7) C(8) 112(1) 1_555 1_555 1_555 N(2) C(7) H(11) 108(1) 1_555 1_555 1_555 N(2) C(7) H(12) 108(1) 1_555 1_555 1_555 C(8) C(7) H(11) 108(1) 1_555 1_555 1_555 C(8) C(7) H(12) 108(1) 1_555 1_555 1_555 H(11) C(7) H(12) 109(1) 1_555 1_555 1_555 C(7) C(8) H(13) 109(1) 1_555 1_555 1_555 C(7) C(8) H(14) 109(1) 1_555 1_555 1_555 C(7) C(8) H(15) 109(1) 1_555 1_555 1_555 H(13) C(8) H(14) 109(1) 1_555 1_555 1_555 H(13) C(8) H(15) 109(1) 1_555 1_555 1_555 H(14) C(8) H(15) 109(1) 1_555 1_555 1_555 N(2) C(9) C(10) 116(1) 1_555 1_555 1_555 N(2) C(9) H(16) 107(1) 1_555 1_555 1_555 N(2) C(9) H(17) 107(1) 1_555 1_555 1_555 C(10) C(9) H(16) 107(1) 1_555 1_555 1_555 C(10) C(9) H(17) 107(1) 1_555 1_555 1_555 H(16) C(9) H(17) 109(1) 1_555 1_555 1_555 C(9) C(10) H(18) 109(1) 1_555 1_555 1_555 C(9) C(10) H(19) 109(1) 1_555 1_555 1_555 C(9) C(10) H(20) 109(1) 1_555 1_555 1_555 H(18) C(10) H(19) 109(1) 1_555 1_555 1_555 H(18) C(10) H(20) 109(1) 1_555 1_555 1_555 H(19) C(10) H(20) 109(2) 1_555 1_555 1_555 Cl(1) C(11) Cl(2) 114.4(8) 1_555 1_555 1_555 Cl(1) C(11) Cl(3) 111.3(9) 1_555 1_555 1_555 Cl(1) C(11) H(21) 107(1) 1_555 1_555 1_555 Cl(2) C(11) Cl(3) 108.0(9) 1_555 1_555 1_555 Cl(2) C(11) H(21) 107(1) 1_555 1_555 1_555 Cl(3) C(11) H(21) 107(1) 1_555 1_555 1_555 #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(2) C(9) 3.50(1) 1_555 4_545 Cl(2) C(5) 3.53(2) 1_555 1_555 S(2) C(3) 3.56(1) 1_555 2_646 #------------------------------------------------------------------------------ #===END # data for [Nb2 (S2)2 (dtc)4] data_5 #------------------------------------------------------------------------------ _audit_creation_date 'Sun May 3 22:50:29 1998' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ' May 7 1998' #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _chemical_formula_weight 710.49 _chemical_formula_sum 'C20 H28 Nb2 O8 S4 ' _chemical_formula_moiety 'C20 H28 Nb2 O8 S4 ' _chemical_formula_structural '[Nb2 (S2)2 (CH3 CO CH CO CH3)4]' #------------------------------------------------------------------------------ _cell_length_a 23.923(3) _cell_length_b 7.868(3) _cell_length_c 17.819(3) _cell_angle_alpha 90 _cell_angle_beta 121.036(8) _cell_angle_gamma 90 _cell_volume 2873(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.6 _cell_measurement_theta_max 13.8 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1432.00 _exptl_absorpt_coefficient_mu 1.127 _exptl_absorpt_correction_type '\DF (DIFABS; Walker & Stuart, 1983)' _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.734 #------------------------------------------------------------------------------ _diffrn_special_details ; voltage and current for X-ray generation: : 50 kV, 200 mA scan width (\w): ( 1.103 + 0.30tan\w) deg with a fractional offset 0.5. scan speed (\w): 16 deg/min background-count time: 25% of the peak-scan time on each side Weak reflections ( I < 10.0\s(I) ) were rescanned (maximum of 3 scans), and the counts were accumulated. No decay was observed. ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -8 0 6 -5 -1 5 -2 0 4 _diffrn_standards_decay_% 0.11 _diffrn_reflns_number 3634 _reflns_number_total 3547 _reflns_number_observed 1917 _reflns_observed_criterion >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.111 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.00879 _diffrn_orient_matrix_UB_12 -0.08194 _diffrn_orient_matrix_UB_13 0.04778 _diffrn_orient_matrix_UB_21 0.00980 _diffrn_orient_matrix_UB_22 0.09704 _diffrn_orient_matrix_UB_23 0.04123 _diffrn_orient_matrix_UB_31 -0.04698 _diffrn_orient_matrix_UB_32 0.00491 _diffrn_orient_matrix_UB_33 -0.01753 #------------------------------------------------------------------------------ _refine_special_details ; All non-hydrogen atoms were refined anisotropically, and hydrogen atoms were refined isotropically. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + (1/4)(0.003|Fo|)^2^]' _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 1917 _refine_ls_number_parameters 210 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0396 _refine_ls_wR_factor_obs 0.0243 _refine_ls_goodness_of_fit_obs 1.327 _refine_ls_shift/esd_max 0.0292 _refine_ls_shift/esd_mean 0.0016 _refine_diff_density_min -0.50 _refine_diff_density_max 0.46 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 80 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 112 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; O 0 32 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Nb 0 8 -2.073 0.621 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 16 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Nb 0.19218(2) 0.24843(8) 0.00704(3) 0.0314(1) Uani d . 1.00 . S(1) 0.19172(6) 0.2765(2) -0.13499(8) 0.0421(4) Uani d . 1.00 . S(2) 0.21560(7) 0.0431(2) -0.08023(9) 0.0393(4) Uani d . 1.00 . O(1) 0.1461(2) 0.4904(4) -0.0422(2) 0.042(1) Uani d . 1.00 . O(2) 0.0935(2) 0.1674(4) -0.0706(2) 0.046(1) Uani d . 1.00 . O(3) 0.1671(2) 0.3272(4) 0.1004(2) 0.043(1) Uani d . 1.00 . O(4) 0.1907(2) 0.0058(4) 0.0606(2) 0.039(1) Uani d . 1.00 . C(1) 0.0764(5) 0.719(1) -0.1126(7) 0.079(3) Uani d . 1.00 . C(2) 0.0882(3) 0.5318(8) -0.0924(4) 0.057(2) Uani d . 1.00 . C(3) 0.0360(4) 0.418(1) -0.1296(7) 0.110(3) Uani d . 1.00 . C(4) 0.0406(3) 0.244(1) -0.1157(4) 0.074(2) Uani d . 1.00 . C(5) -0.0210(5) 0.139(2) -0.156(1) 0.133(5) Uani d . 1.00 . C(6) 0.1411(6) 0.353(1) 0.2102(8) 0.078(4) Uani d . 1.00 . C(7) 0.1595(2) 0.2476(9) 0.1554(3) 0.045(2) Uani d . 1.00 . C(8) 0.1660(3) 0.0718(8) 0.1682(4) 0.054(2) Uani d . 1.00 . C(9) 0.1800(2) -0.0401(7) 0.1189(3) 0.036(2) Uani d . 1.00 . C(10) 0.1805(5) -0.226(1) 0.1350(6) 0.064(3) Uani d . 1.00 . H(1) 0.061(3) 0.739(9) -0.077(3) 0.06(2) Uiso calc . 1.00 . H(2) 0.097(3) 0.754(10) -0.141(4) 0.08(2) Uiso calc . 1.00 . H(3) 0.039(3) 0.73(1) -0.162(4) 0.16(4) Uiso calc . 1.00 . H(4) -0.001(3) 0.465(7) -0.166(3) 0.05(2) Uiso calc . 1.00 . H(5) -0.060(3) 0.20(1) -0.173(5) 0.14(3) Uiso calc . 1.00 . H(6) -0.016(5) 0.10(1) -0.204(6) 0.16(6) Uiso calc . 1.00 . H(7) -0.020(3) 0.042(8) -0.116(4) 0.08(2) Uiso calc . 1.00 . H(8) 0.158(3) 0.448(8) 0.224(4) 0.08(3) Uiso calc . 1.00 . H(9) 0.103(3) 0.412(8) 0.177(4) 0.07(2) Uiso calc . 1.00 . H(10) 0.138(3) 0.290(9) 0.248(4) 0.12(3) Uiso calc . 1.00 . H(11) 0.159(3) 0.028(7) 0.209(3) 0.06(2) Uiso calc . 1.00 . H(12) 0.190(2) -0.248(8) 0.188(3) 0.06(2) Uiso calc . 1.00 . H(13) 0.154(3) -0.287(9) 0.087(4) 0.10(3) Uiso calc . 1.00 . H(14) 0.217(3) -0.264(10) 0.136(4) 0.09(3) Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Nb 0.0313(2) 0.0311(2) 0.0323(2) 0.0011(3) 0.0169(2) 0.0015(3) S(1) 0.0417(8) 0.0495(10) 0.0291(7) -0.0013(8) 0.0140(6) 0.0027(7) S(2) 0.0417(9) 0.0405(8) 0.0367(8) -0.0048(7) 0.0210(7) -0.0065(7) O(1) 0.044(2) 0.033(2) 0.046(2) 0.008(2) 0.020(2) 0.004(2) O(2) 0.031(2) 0.040(2) 0.060(3) -0.001(2) 0.018(2) 0.000(2) O(3) 0.057(3) 0.034(2) 0.055(3) 0.007(2) 0.040(2) 0.004(2) O(4) 0.048(2) 0.033(2) 0.043(2) 0.002(2) 0.029(2) 0.001(2) C(1) 0.088(7) 0.056(6) 0.085(7) 0.026(5) 0.039(6) 0.020(5) C(2) 0.057(4) 0.036(3) 0.076(5) 0.013(4) 0.032(4) 0.007(3) C(3) 0.036(5) 0.054(5) 0.174(10) 0.017(4) 0.007(6) 0.018(6) C(4) 0.034(3) 0.059(4) 0.112(6) 0.004(5) 0.025(4) -0.001(6) C(5) 0.029(5) 0.083(8) 0.23(2) -0.007(5) 0.029(8) 0.018(10) C(6) 0.123(9) 0.051(5) 0.112(8) 0.003(6) 0.098(8) -0.006(5) C(7) 0.047(3) 0.047(3) 0.052(3) -0.005(4) 0.034(3) -0.013(4) C(8) 0.078(5) 0.051(4) 0.054(4) -0.007(4) 0.049(4) 0.001(3) C(9) 0.030(3) 0.043(3) 0.033(3) -0.001(3) 0.014(3) 0.003(3) C(10) 0.103(7) 0.042(5) 0.063(5) 0.001(4) 0.054(5) 0.006(4) #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Nb Nb 2.9039(9) 1_555 7_555 Nb S(1) 2.535(1) 1_555 1_555 Nb S(1) 2.534(1) 1_555 7_555 Nb S(2) 2.498(1) 1_555 1_555 Nb S(2) 2.508(2) 1_555 7_555 Nb O(1) 2.147(4) 1_555 1_555 Nb O(2) 2.127(4) 1_555 1_555 Nb O(3) 2.131(3) 1_555 1_555 Nb O(4) 2.143(3) 1_555 1_555 S(1) S(2) 2.019(2) 1_555 1_555 O(1) C(2) 1.245(6) 1_555 1_555 O(2) C(4) 1.250(7) 1_555 1_555 O(3) C(7) 1.252(6) 1_555 1_555 O(4) C(9) 1.245(5) 1_555 1_555 C(1) C(2) 1.507(10) 1_555 1_555 C(2) C(3) 1.394(9) 1_555 1_555 C(3) C(4) 1.39(1) 1_555 1_555 C(4) C(5) 1.51(1) 1_555 1_555 C(6) C(7) 1.508(9) 1_555 1_555 C(7) C(8) 1.398(9) 1_555 1_555 C(8) C(9) 1.400(7) 1_555 1_555 C(9) C(10) 1.487(9) 1_555 1_555 #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 Nb Nb S(1) 55.04(3) 7_555 1_555 1_555 Nb Nb S(1) 55.06(3) 7_555 1_555 7_555 Nb Nb S(2) 54.71(4) 7_555 1_555 1_555 Nb Nb S(2) 54.39(4) 7_555 1_555 7_555 Nb Nb O(1) 105.6(1) 7_555 1_555 1_555 Nb Nb O(2) 137.2(1) 7_555 1_555 1_555 Nb Nb O(3) 136.8(1) 7_555 1_555 1_555 Nb Nb O(4) 106.33(9) 7_555 1_555 1_555 S(1) Nb S(1) 110.10(4) 1_555 1_555 7_555 S(1) Nb S(2) 47.30(5) 1_555 1_555 1_555 S(1) Nb S(2) 90.69(5) 1_555 1_555 7_555 S(1) Nb O(1) 77.17(10) 1_555 1_555 1_555 S(1) Nb O(2) 86.8(1) 1_555 1_555 1_555 S(1) Nb O(3) 153.67(10) 1_555 1_555 1_555 S(1) Nb O(4) 122.00(10) 1_555 1_555 1_555 S(1) Nb S(2) 90.94(5) 7_555 1_555 1_555 S(1) Nb S(2) 47.21(5) 7_555 1_555 7_555 S(1) Nb O(1) 122.0(1) 7_555 1_555 1_555 S(1) Nb O(2) 153.6(1) 7_555 1_555 1_555 S(1) Nb O(3) 86.5(1) 7_555 1_555 1_555 S(1) Nb O(4) 78.00(10) 7_555 1_555 1_555 S(2) Nb S(2) 109.10(4) 1_555 1_555 7_555 S(2) Nb O(1) 123.49(10) 1_555 1_555 1_555 S(2) Nb O(2) 86.0(1) 1_555 1_555 1_555 S(2) Nb O(3) 156.60(10) 1_555 1_555 1_555 S(2) Nb O(4) 76.21(9) 1_555 1_555 1_555 S(2) Nb O(1) 76.2(1) 7_555 1_555 1_555 S(2) Nb O(2) 156.6(1) 7_555 1_555 1_555 S(2) Nb O(3) 86.0(1) 7_555 1_555 1_555 S(2) Nb O(4) 124.26(10) 7_555 1_555 1_555 O(1) Nb O(2) 80.6(1) 1_555 1_555 1_555 O(1) Nb O(3) 76.7(1) 1_555 1_555 1_555 O(1) Nb O(4) 148.1(1) 1_555 1_555 1_555 O(2) Nb O(3) 86.0(1) 1_555 1_555 1_555 O(2) Nb O(4) 75.8(1) 1_555 1_555 1_555 O(3) Nb O(4) 80.5(1) 1_555 1_555 1_555 Nb S(1) Nb 69.90(4) 1_555 1_555 7_555 Nb S(1) S(2) 65.40(5) 1_555 1_555 1_555 Nb S(1) S(2) 65.73(6) 7_555 1_555 1_555 Nb S(2) Nb 70.90(4) 1_555 1_555 7_555 Nb S(2) S(1) 67.30(6) 1_555 1_555 1_555 Nb S(2) S(1) 67.06(6) 7_555 1_555 1_555 Nb O(1) C(2) 132.2(4) 1_555 1_555 1_555 Nb O(2) C(4) 133.6(5) 1_555 1_555 1_555 Nb O(3) C(7) 132.7(4) 1_555 1_555 1_555 Nb O(4) C(9) 133.5(3) 1_555 1_555 1_555 C(2) C(1) H(1) 95(4) 1_555 1_555 1_555 C(2) C(1) H(2) 109(4) 1_555 1_555 1_555 C(2) C(1) H(3) 109(7) 1_555 1_555 1_555 H(1) C(1) H(2) 150(6) 1_555 1_555 1_555 H(1) C(1) H(3) 96(6) 1_555 1_555 1_555 H(2) C(1) H(3) 87(5) 1_555 1_555 1_555 O(1) C(2) C(1) 115.4(7) 1_555 1_555 1_555 O(1) C(2) C(3) 124.5(6) 1_555 1_555 1_555 C(1) C(2) C(3) 120.1(7) 1_555 1_555 1_555 C(2) C(3) C(4) 125.4(7) 1_555 1_555 1_555 C(2) C(3) H(4) 113(3) 1_555 1_555 1_555 C(4) C(3) H(4) 121(3) 1_555 1_555 1_555 O(2) C(4) C(3) 123.5(7) 1_555 1_555 1_555 O(2) C(4) C(5) 117.2(8) 1_555 1_555 1_555 C(3) C(4) C(5) 119.3(7) 1_555 1_555 1_555 C(4) C(5) H(5) 113(5) 1_555 1_555 1_555 C(4) C(5) H(6) 94(5) 1_555 1_555 1_555 C(4) C(5) H(7) 113(3) 1_555 1_555 1_555 H(5) C(5) H(6) 115(8) 1_555 1_555 1_555 H(5) C(5) H(7) 107(6) 1_555 1_555 1_555 H(6) C(5) H(7) 112(7) 1_555 1_555 1_555 C(7) C(6) H(8) 116(5) 1_555 1_555 1_555 C(7) C(6) H(9) 113(4) 1_555 1_555 1_555 C(7) C(6) H(10) 111(4) 1_555 1_555 1_555 H(8) C(6) H(9) 84(5) 1_555 1_555 1_555 H(8) C(6) H(10) 120(6) 1_555 1_555 1_555 H(9) C(6) H(10) 108(6) 1_555 1_555 1_555 O(3) C(7) C(6) 116.1(7) 1_555 1_555 1_555 O(3) C(7) C(8) 125.0(5) 1_555 1_555 1_555 C(6) C(7) C(8) 118.9(6) 1_555 1_555 1_555 C(7) C(8) C(9) 124.2(5) 1_555 1_555 1_555 C(7) C(8) H(11) 117(3) 1_555 1_555 1_555 C(9) C(8) H(11) 118(3) 1_555 1_555 1_555 O(4) C(9) C(8) 124.0(5) 1_555 1_555 1_555 O(4) C(9) C(10) 117.4(5) 1_555 1_555 1_555 C(8) C(9) C(10) 118.6(5) 1_555 1_555 1_555 C(9) C(10) H(12) 112(4) 1_555 1_555 1_555 C(9) C(10) H(13) 114(4) 1_555 1_555 1_555 C(9) C(10) H(14) 104(4) 1_555 1_555 1_555 H(12) C(10) H(13) 125(6) 1_555 1_555 1_555 H(12) C(10) H(14) 101(5) 1_555 1_555 1_555 H(13) C(10) H(14) 92(5) 1_555 1_555 1_555 #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) C(10) 3.598(9) 1_555 1_565 O(2) C(1) 3.588(9) 1_555 1_545 O(3) C(10) 3.556(9) 1_555 1_565 #------------------------------------------------------------------------------