# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C9H22CrN10OS6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C9 H22 Cr1 N10 O1 S6' _chemical_formula_moiety 'C9 H22 Cr1 N10 O1 S6' _chemical_compound_source ? _chemical_formula_weight 530.73 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c m n ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x,-y+1/2,z -x,y+1/2,-z -x+1/2,-y+1/2,z+1/2 x+1/2,y+1/2,-z+1/2 x+1/2,-y,-z+1/2 -x+1/2,y,z+1/2 _cell_length_a 9.6828(16) _cell_length_b 14.744(2) _cell_length_c 16.341(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2332.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1420 _cell_measurement_theta_min 5.59 _cell_measurement_theta_max 25.25 _exptl_crystal_description Plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.6495 _exptl_absorpt_correction_T_max 0.7454 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 23173 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_min 2.445 _diffrn_reflns_theta_max 26.853 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.853 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 2613 _reflns_limit_h_min 0 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.42 _refine_diff_density_max 0.33 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 1409 _refine_ls_number_restraints 0 _refine_ls_number_parameters 137 _oxford_refine_ls_R_factor_ref 0.0515 _refine_ls_wR_factor_ref 0.0533 _refine_ls_goodness_of_fit_ref 1.0782 _refine_ls_shift/su_max 0.0002040 _refine_ls_shift/su_mean 0.0000170 # The values computed from all data _oxford_reflns_number_all 2613 _refine_ls_R_factor_all 0.0972 _refine_ls_wR_factor_all 0.0794 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1536 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_gt 0.0562 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 2.23 3.09 2.44 1.16 0.585 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cr1 Cr -0.00794(9) 0.2500 0.63676(5) 0.0458 1.0000 Uani S T . . . . S1 S -0.2856(2) 0.2500 0.39456(12) 0.0811 1.0000 Uani S T . . . . S2 S -0.25239(18) 0.50194(11) 0.75047(10) 0.0927 1.0000 Uani . . . . . . S3 S 0.20383(17) 0.49849(10) 0.50117(9) 0.0820 1.0000 Uani . . . . . . S4 S 0.2269(2) 0.2500 0.89342(11) 0.0763 1.0000 Uani S T . . . . N1 N -0.1308(5) 0.2500 0.5380(3) 0.0555 1.0000 Uani S T . . . . N2 N -0.1247(4) 0.3464(3) 0.6875(2) 0.0609 1.0000 Uani . . . . . . N3 N 0.1067(4) 0.3464(2) 0.5851(2) 0.0573 1.0000 Uani . . . . . . N4 N 0.1116(6) 0.2500 0.7365(3) 0.0603 1.0000 Uani S T . . . . N5 N -0.0010(4) 0.1075(4) 0.3563(3) 0.1049 1.0000 Uani . . . . . . N6 N 0.4984(5) 0.4400(5) 0.4125(6) 0.1833 1.0000 Uani . . . . . . C1 C -0.1952(6) 0.2500 0.4805(4) 0.0560 1.0000 Uani S T . . . . C2 C -0.1769(5) 0.4100(4) 0.7128(3) 0.0651 1.0000 Uani . . . . . . C3 C 0.1463(4) 0.4086(3) 0.5510(3) 0.0584 1.0000 Uani . . . . . . C4 C 0.1590(6) 0.2500 0.8010(4) 0.0604 1.0000 Uani S T . . . . C5 C 0.4984(8) 0.1631(7) 0.6111(5) 0.1547 1.0000 Uani . . . . . . C6 C 0.4989(10) 0.2500 0.6619(7) 0.1199 1.0000 Uani S T . . . . O1 O 0.5086(8) 0.2500 0.7373(4) 0.1391 1.0000 Uani S T . . . . H51 H 0.4628 0.1143 0.6434 0.62(3) 1.0000 Uiso R . . . . . H52 H 0.5894 0.1496 0.5936 0.62(3) 1.0000 Uiso R . . . . . H53 H 0.4418 0.1722 0.5633 0.62(3) 1.0000 Uiso R . . . . . H511 H -0.0642 0.1278 0.3928 0.55(3) 1.0000 Uiso R . . . . . H512 H -0.0436 0.0740 0.3171 0.55(3) 1.0000 Uiso R . . . . . H513 H 0.0620 0.0726 0.3827 0.55(3) 1.0000 Uiso R . . . . . H514 H 0.0424 0.1554 0.3336 0.55(3) 1.0000 Uiso R . . . . . H611 H 0.4138 0.4570 0.4376 0.46(3) 1.0000 Uiso R . . . . . H612 H 0.4825 0.3911 0.3759 0.46(3) 1.0000 Uiso R . . . . . H613 H 0.5348 0.4902 0.3832 0.46(3) 1.0000 Uiso R . . . . . H614 H 0.5624 0.4217 0.4534 0.46(3) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0508(5) 0.0441(5) 0.0425(5) 0.0000 -0.0020(4) 0.0000 S1 0.0932(14) 0.0780(13) 0.0720(12) 0.0000 -0.0301(11) 0.0000 S2 0.1184(12) 0.0697(8) 0.0901(9) -0.0106(7) 0.0332(9) 0.0120(8) S3 0.1119(10) 0.0611(7) 0.0730(7) 0.0080(6) 0.0088(8) -0.0153(7) S4 0.0829(13) 0.0868(13) 0.0592(11) 0.0000 -0.0150(9) 0.0000 N1 0.060(3) 0.055(3) 0.052(3) 0.0000 -0.012(3) 0.0000 N2 0.068(2) 0.057(2) 0.058(2) -0.0082(19) 0.0042(18) 0.0081(19) N3 0.064(2) 0.049(2) 0.059(2) 0.0047(18) 0.0036(17) -0.0047(18) N4 0.070(3) 0.061(3) 0.049(3) 0.0000 -0.013(3) 0.0000 N5 0.089(3) 0.122(4) 0.104(3) 0.012(3) 0.000(3) 0.002(3) N6 0.085(4) 0.157(7) 0.308(10) 0.008(7) -0.001(5) -0.002(4) C1 0.059(4) 0.041(3) 0.068(4) 0.0000 0.006(3) 0.0000 C2 0.073(3) 0.075(3) 0.048(2) 0.006(2) 0.007(2) -0.007(3) C3 0.063(2) 0.061(3) 0.051(2) -0.012(2) -0.002(2) 0.004(2) C4 0.058(4) 0.049(4) 0.074(5) 0.0000 0.006(3) 0.0000 C5 0.155(7) 0.155(8) 0.155(7) -0.026(6) -0.009(6) -0.042(6) C6 0.100(7) 0.149(10) 0.111(8) 0.0000 0.000(7) 0.0000 O1 0.179(7) 0.157(6) 0.081(4) 0.0000 0.006(5) 0.0000 loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 . N2 3_555 1.997(4) yes Cr1 . N3 3_555 1.992(4) yes Cr1 . N1 . 2.005(5) yes Cr1 . N2 . 1.997(4) yes Cr1 . N3 . 1.992(4) yes Cr1 . N4 . 2.000(5) yes S1 . C1 . 1.655(7) yes S2 . C2 . 1.658(6) yes S3 . C3 . 1.652(5) yes S4 . C4 . 1.647(7) yes N1 . C1 . 1.127(7) yes N2 . C2 . 1.142(6) yes N3 . C3 . 1.139(5) yes N4 . C4 . 1.149(7) yes N5 . H511 . 0.905 no N5 . H512 . 0.909 no N5 . H513 . 0.907 no N5 . H514 . 0.901 no N6 . H611 . 0.950 no N6 . H612 . 0.950 no N6 . H613 . 0.950 no N6 . H614 . 0.950 no C5 . C6 . 1.526(10) yes C5 . H51 . 0.956 no C5 . H52 . 0.947 no C5 . H53 . 0.965 no C6 . O1 . 1.235(12) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 3_555 Cr1 . N3 3_555 89.04(15) yes N2 3_555 Cr1 . N1 . 89.92(15) yes N3 3_555 Cr1 . N1 . 89.39(15) yes N2 3_555 Cr1 . N2 . 90.8(2) yes N3 3_555 Cr1 . N2 . 179.29(15) yes N1 . Cr1 . N2 . 89.92(15) yes N2 3_555 Cr1 . N3 . 179.29(15) yes N3 3_555 Cr1 . N3 . 91.1(2) yes N1 . Cr1 . N3 . 89.39(15) yes N2 . Cr1 . N3 . 89.04(15) yes N2 3_555 Cr1 . N4 . 89.38(15) yes N3 3_555 Cr1 . N4 . 91.31(15) yes N1 . Cr1 . N4 . 179.0(2) yes N2 . Cr1 . N4 . 89.38(15) yes N3 . Cr1 . N4 . 91.31(15) yes Cr1 . N1 . C1 . 177.2(5) yes Cr1 . N2 . C2 . 170.1(4) yes Cr1 . N3 . C3 . 165.8(4) yes Cr1 . N4 . C4 . 168.1(5) yes H511 . N5 . H512 . 109.7 no H511 . N5 . H513 . 109.3 no H512 . N5 . H513 . 109.3 no H511 . N5 . H514 . 109.1 no H512 . N5 . H514 . 110.3 no H513 . N5 . H514 . 109.1 no H611 . N6 . H612 . 109.5 no H611 . N6 . H613 . 109.5 no H612 . N6 . H613 . 109.5 no H611 . N6 . H614 . 109.5 no H612 . N6 . H614 . 109.5 no H613 . N6 . H614 . 109.5 no S1 . C1 . N1 . 178.3(6) yes S2 . C2 . N2 . 179.5(4) yes S3 . C3 . N3 . 179.8(4) yes S4 . C4 . N4 . 180.0(6) yes C6 . C5 . H51 . 109.4 no C6 . C5 . H52 . 109.7 no H51 . C5 . H52 . 110.1 no C6 . C5 . H53 . 109.0 no H51 . C5 . H53 . 110.3 no H52 . C5 . H53 . 108.2 no C5 . C6 . C5 3_555 114.1(10) yes C5 . C6 . O1 . 122.8(5) yes C5 3_555 C6 . O1 . 122.8(5) yes _database_code_depnum_ccdc_archive 'CCDC 933715' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C18H36CrN9S6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C18 H36 Cr1 N9 S6' _chemical_formula_moiety 'C18 H36 Cr1 N9 S6' _chemical_compound_source ? _chemical_formula_weight 622.94 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _cell_length_a 24.8961(10) _cell_length_b 9.3234(4) _cell_length_c 28.4594(12) _cell_angle_alpha 90 _cell_angle_beta 100.021(2) _cell_angle_gamma 90 _cell_volume 6505.1(5) _cell_formula_units_Z 8 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 6378 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 46.96 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.17 _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 6.680 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.5309 _exptl_absorpt_correction_T_max 0.7493 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 18287 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_min 3.154 _diffrn_reflns_theta_max 47.198 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 47.198 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 2933 _reflns_limit_h_min -23 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 8 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _refine_diff_density_min -0.33 _refine_diff_density_max 0.53 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 2737 _refine_ls_number_restraints 0 _refine_ls_number_parameters 309 _oxford_refine_ls_R_factor_ref 0.0521 _refine_ls_wR_factor_ref 0.0557 _refine_ls_goodness_of_fit_ref 1.1121 _refine_ls_shift/su_max 0.0004146 _refine_ls_shift/su_mean 0.0000245 # The values computed from all data _oxford_reflns_number_all 2933 _refine_ls_R_factor_all 0.0562 _refine_ls_wR_factor_all 0.0634 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2737 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_gt 0.0557 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.416 0.522 0.298 0.116 0.369E-01 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cr1 Cr 0.5000 1.03381(12) 0.2500 0.0511 1.0000 Uani S T . . . . Cr2 Cr 0.7500 1.2500 0.5000 0.0490 1.0000 Uani S . . . . . S1 S 0.62060(7) 1.4047(2) 0.22060(6) 0.1017 1.0000 Uani . . . . . . S2 S 0.56602(8) 1.0559(2) 0.41636(5) 0.1183 1.0000 Uani . . . . . . S3 S 0.36749(7) 0.7916(2) 0.31252(7) 0.1085 1.0000 Uani . . . . . . S4 S 0.72687(8) 1.46318(17) 0.34535(5) 0.0972 1.0000 Uani . . . . . . S5 S 0.57135(7) 1.3930(2) 0.52037(8) 0.1182 1.0000 Uani . . . . . . S6 S 0.70241(7) 0.78404(15) 0.43886(5) 0.0824 1.0000 Uani . . . . . . N1 N 0.55309(18) 1.1857(5) 0.23903(14) 0.0660 1.0000 Uani . . . . . . N2 N 0.53091(16) 1.0344(5) 0.31947(17) 0.0638 1.0000 Uani . . . . . . N3 N 0.44670(18) 0.8856(5) 0.26279(15) 0.0677 1.0000 Uani . . . . . . N4 N 0.73721(16) 1.3386(4) 0.43506(15) 0.0602 1.0000 Uani . . . . . . N5 N 0.67480(19) 1.3043(4) 0.50836(14) 0.0647 1.0000 Uani . . . . . . N6 N 0.72380(17) 1.0614(5) 0.47283(14) 0.0616 1.0000 Uani . . . . . . N7 N 0.72553(15) 1.0092(4) 0.31698(13) 0.0530 1.0000 Uani . . . . . . N8 N 0.55042(16) 0.5536(4) 0.36191(14) 0.0612 1.0000 Uani . . . . . . N9 N 0.89235(16) 0.6332(4) 0.43388(13) 0.0624 1.0000 Uani . . . . . . C1 C 0.5819(2) 1.2737(6) 0.23128(16) 0.0579 1.0000 Uani . . . . . . C2 C 0.54449(19) 1.0416(5) 0.3597(2) 0.0612 1.0000 Uani . . . . . . C3 C 0.4143(2) 0.8457(5) 0.28350(18) 0.0590 1.0000 Uani . . . . . . C4 C 0.73307(19) 1.3917(5) 0.39862(19) 0.0548 1.0000 Uani . . . . . . C5 C 0.6323(3) 1.3422(6) 0.51357(17) 0.0645 1.0000 Uani . . . . . . C6 C 0.71488(19) 0.9473(6) 0.45935(16) 0.0553 1.0000 Uani . . . . . . C7 C 0.7320(3) 1.0795(6) 0.27130(19) 0.0890 1.0000 Uani . . . . . . C8 C 0.77085(19) 1.0546(5) 0.35520(18) 0.0657 1.0000 Uani . . . . . . C9 C 0.7269(2) 0.8514(6) 0.3114(2) 0.0864 1.0000 Uani . . . . . . C10 C 0.67243(19) 1.0534(6) 0.33032(19) 0.0775 1.0000 Uani . . . . . . C11 C 0.5619(7) 0.6345(14) 0.3236(5) 0.3450 1.0000 Uani . . . . . . C12 C 0.5070(6) 0.6045(17) 0.3827(5) 0.2928 1.0000 Uani . . . . . . C13 C 0.5395(8) 0.4190(14) 0.3475(6) 0.3519 1.0000 Uani . . . . . . C14 C 0.5961(4) 0.545(2) 0.3951(5) 0.3586 1.0000 Uani . . . . . . C15 C 0.8396(4) 0.7011(13) 0.4363(4) 0.2118 1.0000 Uani . . . . . . C16 C 0.9053(4) 0.6663(13) 0.3882(3) 0.1971 1.0000 Uani . . . . . . C17 C 0.9344(4) 0.6907(10) 0.4706(3) 0.1801 1.0000 Uani . . . . . . C18 C 0.8890(6) 0.4813(9) 0.4416(4) 0.2305 1.0000 Uani . . . . . . H71 H 0.7028 1.0503 0.2471 0.1049 1.0000 Uiso R . . . . . H72 H 0.7657 1.0515 0.2627 0.1049 1.0000 Uiso R . . . . . H73 H 0.7313 1.1808 0.2747 0.1049 1.0000 Uiso R . . . . . H81 H 0.7668 1.0101 0.3844 0.0806 1.0000 Uiso R . . . . . H82 H 0.8046 1.0266 0.3468 0.0806 1.0000 Uiso R . . . . . H83 H 0.7702 1.1559 0.3588 0.0806 1.0000 Uiso R . . . . . H91 H 0.7231 0.8069 0.3406 0.1012 1.0000 Uiso R . . . . . H92 H 0.7607 0.8241 0.3028 0.1012 1.0000 Uiso R . . . . . H93 H 0.6978 0.8221 0.2871 0.1012 1.0000 Uiso R . . . . . H101 H 0.6686 1.0094 0.3596 0.0913 1.0000 Uiso R . . . . . H102 H 0.6718 1.1547 0.3337 0.0913 1.0000 Uiso R . . . . . H103 H 0.6432 1.0245 0.3061 0.0913 1.0000 Uiso R . . . . . H111 H 0.5691 0.7313 0.3331 0.2835 1.0000 Uiso R . . . . . H112 H 0.5925 0.5961 0.3121 0.2835 1.0000 Uiso R . . . . . H113 H 0.5308 0.6306 0.2991 0.2835 1.0000 Uiso R . . . . . H121 H 0.5031 0.5445 0.4089 0.2944 1.0000 Uiso R . . . . . H122 H 0.5136 0.7002 0.3935 0.2944 1.0000 Uiso R . . . . . H123 H 0.4744 0.6013 0.3596 0.2944 1.0000 Uiso R . . . . . H131 H 0.5326 0.3591 0.3727 0.3327 1.0000 Uiso R . . . . . H132 H 0.5704 0.3843 0.3356 0.3327 1.0000 Uiso R . . . . . H133 H 0.5087 0.4187 0.3225 0.3327 1.0000 Uiso R . . . . . H141 H 0.6262 0.5128 0.3815 0.3724 1.0000 Uiso R . . . . . H142 H 0.6039 0.6379 0.4085 0.3724 1.0000 Uiso R . . . . . H143 H 0.5898 0.4805 0.4193 0.3724 1.0000 Uiso R . . . . . H151 H 0.8295 0.6810 0.4663 0.2413 1.0000 Uiso R . . . . . H152 H 0.8422 0.8020 0.4325 0.2413 1.0000 Uiso R . . . . . H153 H 0.8128 0.6635 0.4115 0.2413 1.0000 Uiso R . . . . . H161 H 0.9395 0.6245 0.3856 0.2237 1.0000 Uiso R . . . . . H162 H 0.9074 0.7674 0.3847 0.2237 1.0000 Uiso R . . . . . H163 H 0.8779 0.6290 0.3638 0.2237 1.0000 Uiso R . . . . . H171 H 0.9683 0.6464 0.4687 0.2025 1.0000 Uiso R . . . . . H172 H 0.9370 0.7910 0.4655 0.2025 1.0000 Uiso R . . . . . H173 H 0.9255 0.6742 0.5013 0.2025 1.0000 Uiso R . . . . . H181 H 0.9235 0.4392 0.4402 0.2396 1.0000 Uiso R . . . . . H182 H 0.8797 0.4635 0.4721 0.2396 1.0000 Uiso R . . . . . H183 H 0.8621 0.4406 0.4176 0.2396 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0467(7) 0.0556(7) 0.0541(7) 0.0000 0.0172(5) 0.0000 Cr2 0.0583(7) 0.0483(7) 0.0409(6) -0.0014(5) 0.0097(5) -0.0015(5) S1 0.0984(12) 0.1082(13) 0.1028(12) 0.0038(10) 0.0294(9) -0.0468(10) S2 0.1145(13) 0.178(2) 0.0575(10) -0.0024(11) 0.0015(9) 0.0407(13) S3 0.1035(12) 0.1182(14) 0.1173(13) 0.0008(11) 0.0568(11) -0.0330(11) S4 0.1658(16) 0.0750(10) 0.0560(9) 0.0181(7) 0.0335(9) 0.0289(10) S5 0.0972(12) 0.1006(13) 0.1745(19) 0.0021(12) 0.0725(13) 0.0216(10) S6 0.1076(12) 0.0576(9) 0.0780(10) -0.0115(7) 0.0053(8) -0.0086(8) N1 0.059(3) 0.070(3) 0.071(3) 0.005(2) 0.017(2) -0.006(2) N2 0.058(3) 0.075(3) 0.059(3) 0.002(2) 0.013(2) 0.002(2) N3 0.061(3) 0.071(3) 0.076(3) 0.000(2) 0.027(2) -0.009(2) N4 0.075(3) 0.060(3) 0.046(3) 0.004(2) 0.013(2) 0.000(2) N5 0.066(3) 0.066(3) 0.065(3) 0.000(2) 0.020(2) -0.003(2) N6 0.080(3) 0.052(3) 0.053(3) -0.004(2) 0.013(2) -0.008(2) N7 0.056(2) 0.050(3) 0.057(3) 0.0007(19) 0.019(2) 0.0028(19) N8 0.061(3) 0.057(3) 0.067(3) -0.001(2) 0.015(2) 0.000(2) N9 0.061(3) 0.069(3) 0.058(3) 0.007(2) 0.015(2) -0.004(2) C1 0.052(3) 0.070(4) 0.053(3) 0.001(3) 0.011(2) 0.000(3) C2 0.050(3) 0.067(4) 0.071(4) 0.005(3) 0.021(3) 0.013(3) C3 0.059(3) 0.049(3) 0.068(3) -0.004(3) 0.009(3) -0.002(3) C4 0.064(3) 0.048(3) 0.055(3) -0.008(3) 0.017(3) 0.003(2) C5 0.078(4) 0.058(3) 0.061(3) -0.001(3) 0.022(3) -0.004(3) C6 0.055(3) 0.066(4) 0.045(3) 0.011(3) 0.010(2) 0.000(3) C7 0.113(5) 0.095(4) 0.064(4) 0.019(3) 0.029(3) -0.003(4) C8 0.058(3) 0.071(3) 0.073(3) -0.003(3) 0.024(3) -0.001(3) C9 0.096(4) 0.071(4) 0.092(4) -0.016(3) 0.015(3) -0.007(3) C10 0.053(3) 0.096(4) 0.084(4) 0.006(3) 0.015(3) 0.002(3) C11 0.55(3) 0.261(16) 0.308(17) 0.207(15) 0.30(2) 0.219(19) C12 0.314(17) 0.35(2) 0.265(15) 0.065(14) 0.197(14) 0.174(16) C13 0.50(3) 0.186(13) 0.38(2) -0.152(15) 0.13(2) -0.186(17) C14 0.107(8) 0.75(4) 0.197(12) 0.022(19) -0.033(8) -0.076(15) C15 0.132(8) 0.265(14) 0.263(13) 0.006(11) 0.103(8) 0.049(9) C16 0.199(10) 0.297(14) 0.107(7) 0.075(8) 0.057(6) -0.013(10) C17 0.216(10) 0.135(7) 0.163(8) -0.029(7) -0.042(8) -0.010(7) C18 0.379(19) 0.087(7) 0.204(11) 0.022(7) -0.007(11) -0.060(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 . N1 5_655 1.999(5) yes Cr1 . N2 5_655 1.993(5) yes Cr1 . N3 5_655 1.992(5) yes Cr1 . N1 . 1.999(5) yes Cr1 . N2 . 1.993(5) yes Cr1 . N3 . 1.992(5) yes Cr2 . N4 4_676 1.999(4) yes Cr2 . N5 4_676 1.993(5) yes Cr2 . N6 4_676 1.985(5) yes Cr2 . N4 . 1.999(4) yes Cr2 . N5 . 1.993(5) yes Cr2 . N6 . 1.985(5) yes S1 . C1 . 1.616(6) yes S2 . C2 . 1.613(7) yes S3 . C3 . 1.622(6) yes S4 . C4 . 1.639(6) yes S5 . C5 . 1.632(6) yes S6 . C6 . 1.640(6) yes N1 . C1 . 1.136(6) yes N2 . C2 . 1.139(6) yes N3 . C3 . 1.141(6) yes N4 . C4 . 1.138(5) yes N5 . C5 . 1.150(6) yes N6 . C6 . 1.139(6) yes N7 . C7 . 1.489(6) yes N7 . C8 . 1.486(6) yes N7 . C9 . 1.481(6) yes N7 . C10 . 1.495(6) yes N8 . C11 . 1.396(9) yes N8 . C12 . 1.403(10) yes N8 . C13 . 1.333(11) yes N8 . C14 . 1.348(10) yes N9 . C15 . 1.471(9) yes N9 . C16 . 1.428(8) yes N9 . C17 . 1.447(8) yes N9 . C18 . 1.438(9) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C7 . H73 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . H151 . 0.950 no C15 . H152 . 0.950 no C15 . H153 . 0.950 no C16 . H161 . 0.950 no C16 . H162 . 0.950 no C16 . H163 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 5_655 Cr1 . N2 5_655 90.07(16) yes N1 5_655 Cr1 . N3 5_655 178.19(17) yes N2 5_655 Cr1 . N3 5_655 88.58(17) yes N1 5_655 Cr1 . N1 . 89.7(2) yes N2 5_655 Cr1 . N1 . 89.69(16) yes N3 5_655 Cr1 . N1 . 89.04(17) yes N1 5_655 Cr1 . N2 . 89.69(16) yes N2 5_655 Cr1 . N2 . 179.7(2) yes N3 5_655 Cr1 . N2 . 91.65(17) yes N1 . Cr1 . N2 . 90.07(16) yes N1 5_655 Cr1 . N3 . 89.04(17) yes N2 5_655 Cr1 . N3 . 91.65(17) yes N3 5_655 Cr1 . N3 . 92.2(2) yes N1 . Cr1 . N3 . 178.19(17) yes N2 . Cr1 . N3 . 88.58(17) yes N4 4_676 Cr2 . N5 4_676 90.20(16) yes N4 4_676 Cr2 . N6 4_676 91.00(15) yes N5 4_676 Cr2 . N6 4_676 91.14(17) yes N4 4_676 Cr2 . N4 . 179.994 yes N5 4_676 Cr2 . N4 . 89.80(16) yes N6 4_676 Cr2 . N4 . 89.00(15) yes N4 4_676 Cr2 . N5 . 89.80(16) yes N5 4_676 Cr2 . N5 . 179.994 yes N6 4_676 Cr2 . N5 . 88.86(17) yes N4 . Cr2 . N5 . 90.20(16) yes N4 4_676 Cr2 . N6 . 89.00(15) yes N5 4_676 Cr2 . N6 . 88.86(17) yes N6 4_676 Cr2 . N6 . 179.994 yes N4 . Cr2 . N6 . 91.00(15) yes N5 . Cr2 . N6 . 91.14(17) yes Cr1 . N1 . C1 . 177.4(4) yes Cr1 . N2 . C2 . 173.8(4) yes Cr1 . N3 . C3 . 150.9(4) yes Cr2 . N4 . C4 . 175.9(4) yes Cr2 . N5 . C5 . 176.8(4) yes Cr2 . N6 . C6 . 171.8(4) yes C7 . N7 . C8 . 109.3(4) yes C7 . N7 . C9 . 109.6(4) yes C8 . N7 . C9 . 109.5(4) yes C7 . N7 . C10 . 109.6(4) yes C8 . N7 . C10 . 109.2(4) yes C9 . N7 . C10 . 109.8(4) yes C11 . N8 . C12 . 115.1(8) yes C11 . N8 . C13 . 109.0(10) yes C12 . N8 . C13 . 108.5(10) yes C11 . N8 . C14 . 108.4(10) yes C12 . N8 . C14 . 110.1(9) yes C13 . N8 . C14 . 105.3(12) yes C15 . N9 . C16 . 107.1(7) yes C15 . N9 . C17 . 110.2(7) yes C16 . N9 . C17 . 109.2(7) yes C15 . N9 . C18 . 110.0(8) yes C16 . N9 . C18 . 112.4(8) yes C17 . N9 . C18 . 107.9(7) yes S1 . C1 . N1 . 177.1(5) yes S2 . C2 . N2 . 177.5(5) yes S3 . C3 . N3 . 178.9(5) yes S4 . C4 . N4 . 178.2(4) yes S5 . C5 . N5 . 178.8(5) yes S6 . C6 . N6 . 178.8(4) yes N7 . C7 . H71 . 108.8 no N7 . C7 . H72 . 109.7 no H71 . C7 . H72 . 109.5 no N7 . C7 . H73 . 109.9 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N7 . C8 . H81 . 109.5 no N7 . C8 . H82 . 109.2 no H81 . C8 . H82 . 109.5 no N7 . C8 . H83 . 109.6 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no N7 . C9 . H91 . 109.4 no N7 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.5 no N7 . C9 . H93 . 109.6 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N7 . C10 . H101 . 109.5 no N7 . C10 . H102 . 109.3 no H101 . C10 . H102 . 109.5 no N7 . C10 . H103 . 109.6 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N8 . C11 . H111 . 110.3 no N8 . C11 . H112 . 110.6 no H111 . C11 . H112 . 109.5 no N8 . C11 . H113 . 107.5 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no N8 . C12 . H121 . 108.8 no N8 . C12 . H122 . 110.5 no H121 . C12 . H122 . 109.5 no N8 . C12 . H123 . 109.1 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N8 . C13 . H131 . 112.0 no N8 . C13 . H132 . 107.2 no H131 . C13 . H132 . 109.5 no N8 . C13 . H133 . 109.1 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N8 . C14 . H141 . 111.2 no N8 . C14 . H142 . 108.6 no H141 . C14 . H142 . 109.5 no N8 . C14 . H143 . 108.6 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N9 . C15 . H151 . 109.5 no N9 . C15 . H152 . 109.9 no H151 . C15 . H152 . 109.5 no N9 . C15 . H153 . 108.9 no H151 . C15 . H153 . 109.5 no H152 . C15 . H153 . 109.5 no N9 . C16 . H161 . 109.1 no N9 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.5 no N9 . C16 . H163 . 109.8 no H161 . C16 . H163 . 109.5 no H162 . C16 . H163 . 109.5 no N9 . C17 . H171 . 109.6 no N9 . C17 . H172 . 108.3 no H171 . C17 . H172 . 109.5 no N9 . C17 . H173 . 110.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no N9 . C18 . H181 . 108.9 no N9 . C18 . H182 . 110.0 no H181 . C18 . H182 . 109.5 no N9 . C18 . H183 . 109.6 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no _database_code_depnum_ccdc_archive 'CCDC 933716' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C22H48MnN10S6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C22 H48 Mn1 N10 S6' _chemical_formula_moiety 'C22 H48 Mn1 N10 S6' _chemical_compound_source ? _chemical_formula_weight 700.01 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 _cell_length_a 12.5278(6) _cell_length_b 12.4262(6) _cell_length_c 12.5900(6) _cell_angle_alpha 90 _cell_angle_beta 90.076(2) _cell_angle_gamma 90 _cell_volume 1959.92(16) _cell_formula_units_Z 2 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used 6378 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 46.96 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.17 _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 742 _exptl_absorpt_coefficient_mu 0.683 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.5309 _exptl_absorpt_correction_T_max 0.7493 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 4293 _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_theta_min 2.292 _diffrn_reflns_theta_max 28.349 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 25.205 _diffrn_measured_fraction_theta_full 0.968 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 4293 _reflns_limit_h_min -15 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _refine_diff_density_min -0.32 _refine_diff_density_max 0.54 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 1442 _refine_ls_number_restraints 6 _refine_ls_number_parameters 179 _oxford_refine_ls_R_factor_ref 0.0891 _refine_ls_wR_factor_ref 0.0879 _refine_ls_goodness_of_fit_ref 1.0799 _refine_ls_shift/su_max 0.0000637 _refine_ls_shift/su_mean 0.0000069 _refine_special_details ; Restraints DISTANCE 1.40000 , 0.02000 = N(5) TO C(8) DISTANCE 1.40000 , 0.02000 = C(9) TO N(5) DISTANCE 1.40000 , 0.02000 = C(4) TO N(4) DISTANCE 1.40000 , 0.02000 = C(5) TO N(4) DISTANCE 1.40000 , 0.02000 = C(10) TO N(5) DISTANCE 1.40000 , 0.02000 = C(11) TO N(5) ; # The values computed from all data _oxford_reflns_number_all 4293 _refine_ls_R_factor_all 0.1993 _refine_ls_wR_factor_all 0.1577 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1559 _refine_ls_R_factor_gt 0.0948 _refine_ls_wR_factor_gt 0.0910 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.820 0.929 0.727 0.363 0.229 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mn1 Mn 0.5000 0.5000 0.0000 0.0630 1.0000 Uani S . . . . . S1 S 0.5242(5) 0.5929(6) 0.3774(3) 0.2217 1.0000 Uani . . . . . . S2 S 0.1184(3) 0.5997(4) -0.0080(4) 0.1574 1.0000 Uani . . . . . . S3 S 0.4062(4) 0.1154(2) 0.0388(4) 0.1532 1.0000 Uani . . . . . . N1 N 0.5090(7) 0.5367(7) 0.1709(7) 0.0960 1.0000 Uani . . . . . . N2 N 0.3301(7) 0.5490(7) -0.0002(7) 0.0985 1.0000 Uani . . . . . . N3 N 0.4498(7) 0.3320(7) 0.0343(7) 0.0890 1.0000 Uani . . . . . . N4 N 0.1967(7) 0.3416(6) 0.2916(7) 0.0911 1.0000 Uani D . . . . . N5 N 0.6718(8) 0.2323(11) 0.3023(10) 0.1361 1.0000 Uani D . . . . . C1 C 0.5158(8) 0.5599(8) 0.2563(9) 0.0865 1.0000 Uani . . . . . . C2 C 0.2431(8) 0.5715(8) -0.0045(8) 0.0792 1.0000 Uani . . . . . . C3 C 0.4310(7) 0.2434(9) 0.0371(7) 0.0766 1.0000 Uani . . . . . . C4 C 0.2406(16) 0.2459(12) 0.2450(16) 0.2222 1.0000 Uani D . . . . . C5 C 0.2791(15) 0.4131(18) 0.317(3) 0.3432 1.0000 Uani D . . . . . C6 C 0.145(3) 0.4060(19) 0.222(2) 0.3688 1.0000 Uani . . . . . . C7 C 0.134(2) 0.3177(15) 0.376(2) 0.3279 1.0000 Uani . . . . . . C8 C 0.740(2) 0.312(2) 0.263(2) 0.3461 1.0000 Uani D . . . . . C9 C 0.581(3) 0.270(3) 0.351(4) 0.4990 1.0000 Uani D . . . . . C10 C 0.640(4) 0.164(4) 0.221(3) 0.6118 1.0000 Uani D . . . . . C11 C 0.724(2) 0.1701(19) 0.368(2) 0.3770 1.0000 Uani D . . . . . H43 H 0.1850 0.1965 0.2289 0.25(3) 1.0000 Uiso R . . . . . H42 H 0.2897 0.2133 0.2928 0.25(3) 1.0000 Uiso R . . . . . H41 H 0.2766 0.2652 0.1814 0.25(3) 1.0000 Uiso R . . . . . H53 H 0.2490 0.4755 0.3484 0.38(3) 1.0000 Uiso R . . . . . H52 H 0.3283 0.3810 0.3647 0.38(3) 1.0000 Uiso R . . . . . H51 H 0.3153 0.4328 0.2533 0.38(3) 1.0000 Uiso R . . . . . H83 H 0.8103 0.2840 0.2654 0.36(3) 1.0000 Uiso R . . . . . H82 H 0.7345 0.3731 0.3074 0.36(3) 1.0000 Uiso R . . . . . H81 H 0.7224 0.3312 0.1919 0.36(3) 1.0000 Uiso R . . . . . H63 H 0.1958 0.4209 0.1675 0.41(3) 1.0000 Uiso R . . . . . H62 H 0.1228 0.4716 0.2535 0.41(3) 1.0000 Uiso R . . . . . H61 H 0.0850 0.3707 0.1913 0.41(3) 1.0000 Uiso R . . . . . H73 H 0.1674 0.2726 0.4268 0.42(3) 1.0000 Uiso R . . . . . H72 H 0.1115 0.3826 0.4088 0.42(3) 1.0000 Uiso R . . . . . H71 H 0.0737 0.2817 0.3466 0.42(3) 1.0000 Uiso R . . . . . H113 H 0.6849 0.1118 0.3978 0.42(3) 1.0000 Uiso R . . . . . H112 H 0.7528 0.2130 0.4233 0.42(3) 1.0000 Uiso R . . . . . H111 H 0.7799 0.1428 0.3251 0.42(3) 1.0000 Uiso R . . . . . H91 H 0.5978 0.3160 0.4088 0.64(3) 1.0000 Uiso R . . . . . H92 H 0.5426 0.3091 0.2986 0.64(3) 1.0000 Uiso R . . . . . H93 H 0.5391 0.2114 0.3753 0.64(3) 1.0000 Uiso R . . . . . H101 H 0.7012 0.1346 0.1870 0.73(3) 1.0000 Uiso R . . . . . H102 H 0.6005 0.2055 0.1713 0.73(3) 1.0000 Uiso R . . . . . H103 H 0.5970 0.1079 0.2480 0.73(3) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0640(10) 0.0627(10) 0.0622(10) -0.0015(12) 0.0000(8) 0.0014(11) S1 0.253(6) 0.332(8) 0.080(2) -0.054(4) -0.006(3) 0.001(5) S2 0.0717(19) 0.221(4) 0.179(4) -0.012(3) -0.005(2) 0.031(2) S3 0.201(4) 0.0709(18) 0.188(4) 0.013(2) 0.059(3) -0.013(2) N1 0.108(6) 0.112(7) 0.069(5) -0.010(5) -0.004(5) -0.006(5) N2 0.073(6) 0.096(6) 0.126(7) -0.006(5) 0.009(6) -0.001(5) N3 0.103(6) 0.065(5) 0.099(6) 0.005(5) -0.004(5) -0.006(5) N4 0.103(6) 0.059(5) 0.112(6) 0.001(5) 0.050(5) 0.003(5) N5 0.087(6) 0.184(11) 0.137(9) 0.062(9) -0.005(7) 0.004(7) C1 0.107(8) 0.087(7) 0.066(7) 0.002(6) 0.016(6) -0.016(6) C2 0.068(6) 0.072(6) 0.097(7) 0.006(5) 0.007(6) -0.007(5) C3 0.075(6) 0.084(7) 0.070(6) 0.010(6) 0.021(5) 0.019(6) C4 0.24(2) 0.150(14) 0.28(2) -0.114(15) 0.069(17) 0.015(13) C5 0.165(19) 0.22(2) 0.65(6) -0.17(3) 0.12(3) -0.079(18) C6 0.63(7) 0.20(2) 0.28(3) 0.05(2) -0.21(4) 0.08(3) C7 0.39(3) 0.177(18) 0.42(4) 0.05(2) 0.34(3) 0.032(19) C8 0.36(4) 0.34(4) 0.34(4) 0.11(3) 0.15(3) -0.08(3) C9 0.33(4) 0.40(5) 0.77(9) 0.14(6) 0.37(6) 0.17(4) C10 0.65(10) 0.90(13) 0.29(4) -0.14(6) -0.13(5) -0.31(9) C11 0.42(5) 0.30(3) 0.41(4) 0.16(3) -0.28(4) 0.03(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1783(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . N2 2_665 2.214(9) yes Mn1 . N1 2_665 2.202(9) yes Mn1 . N3 2_665 2.223(8) yes Mn1 . N1 . 2.202(9) yes Mn1 . N2 . 2.214(9) yes Mn1 . N3 . 2.223(8) yes S1 . C1 . 1.582(12) yes S2 . C2 . 1.602(11) yes S3 . C3 . 1.621(11) yes N1 . C1 . 1.117(11) yes N2 . C2 . 1.126(11) yes N3 . C3 . 1.126(11) yes N4 . C4 . 1.436(12) yes N4 . C5 . 1.399(14) yes N4 . C6 . 1.356(19) yes N4 . C7 . 1.353(16) yes N5 . C8 . 1.393(15) yes N5 . C9 . 1.371(15) yes N5 . C10 . 1.384(17) yes N5 . C11 . 1.305(13) yes C4 . H43 . 0.950 no C4 . H42 . 0.950 no C4 . H41 . 0.950 no C5 . H53 . 0.950 no C5 . H52 . 0.950 no C5 . H51 . 0.950 no C6 . H63 . 0.950 no C6 . H62 . 0.950 no C6 . H61 . 0.950 no C7 . H73 . 0.950 no C7 . H72 . 0.950 no C7 . H71 . 0.950 no C8 . H83 . 0.950 no C8 . H82 . 0.950 no C8 . H81 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . H113 . 0.950 no C11 . H112 . 0.950 no C11 . H111 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 2_665 Mn1 . N1 2_665 89.6(3) yes N2 2_665 Mn1 . N3 2_665 89.2(3) yes N1 2_665 Mn1 . N3 2_665 91.1(3) yes N2 2_665 Mn1 . N1 . 90.4(3) yes N1 2_665 Mn1 . N1 . 179.995 yes N3 2_665 Mn1 . N1 . 88.9(3) yes N2 2_665 Mn1 . N2 . 179.995 yes N1 2_665 Mn1 . N2 . 90.4(3) yes N3 2_665 Mn1 . N2 . 90.8(3) yes N1 . Mn1 . N2 . 89.6(3) yes N2 2_665 Mn1 . N3 . 90.8(3) yes N1 2_665 Mn1 . N3 . 88.9(3) yes N3 2_665 Mn1 . N3 . 179.995 yes N1 . Mn1 . N3 . 91.1(3) yes N2 . Mn1 . N3 . 89.2(3) yes Mn1 . N1 . C1 . 176.7(9) yes Mn1 . N2 . C2 . 176.9(9) yes Mn1 . N3 . C3 . 169.5(9) yes C4 . N4 . C5 . 109.6(13) yes C4 . N4 . C6 . 113.9(16) yes C5 . N4 . C6 . 97.1(17) yes C4 . N4 . C7 . 111.2(13) yes C5 . N4 . C7 . 113.1(19) yes C6 . N4 . C7 . 111.2(20) yes C8 . N5 . C9 . 115(2) yes C8 . N5 . C10 . 110(2) yes C9 . N5 . C10 . 108(3) yes C8 . N5 . C11 . 110.0(19) yes C9 . N5 . C11 . 109(2) yes C10 . N5 . C11 . 104(3) yes S1 . C1 . N1 . 179.5(11) yes S2 . C2 . N2 . 178.0(10) yes S3 . C3 . N3 . 178.5(9) yes N4 . C4 . H43 . 109.9 no N4 . C4 . H42 . 109.9 no H43 . C4 . H42 . 109.5 no N4 . C4 . H41 . 108.6 no H43 . C4 . H41 . 109.5 no H42 . C4 . H41 . 109.5 no N4 . C5 . H53 . 108.6 no N4 . C5 . H52 . 110.7 no H53 . C5 . H52 . 109.5 no N4 . C5 . H51 . 109.1 no H53 . C5 . H51 . 109.5 no H52 . C5 . H51 . 109.5 no N4 . C6 . H63 . 105.1 no N4 . C6 . H62 . 111.8 no H63 . C6 . H62 . 109.5 no N4 . C6 . H61 . 111.4 no H63 . C6 . H61 . 109.5 no H62 . C6 . H61 . 109.5 no N4 . C7 . H73 . 113.8 no N4 . C7 . H72 . 109.2 no H73 . C7 . H72 . 109.5 no N4 . C7 . H71 . 105.3 no H73 . C7 . H71 . 109.5 no H72 . C7 . H71 . 109.5 no N5 . C8 . H83 . 107.6 no N5 . C8 . H82 . 108.5 no H83 . C8 . H82 . 109.5 no N5 . C8 . H81 . 112.3 no H83 . C8 . H81 . 109.5 no H82 . C8 . H81 . 109.5 no N5 . C9 . H91 . 111.6 no N5 . C9 . H92 . 106.7 no H91 . C9 . H92 . 109.5 no N5 . C9 . H93 . 110.1 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N5 . C10 . H101 . 110.1 no N5 . C10 . H102 . 107.9 no H101 . C10 . H102 . 109.5 no N5 . C10 . H103 . 110.4 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N5 . C11 . H113 . 116.5 no N5 . C11 . H112 . 108.8 no H113 . C11 . H112 . 109.5 no N5 . C11 . H111 . 102.8 no H113 . C11 . H111 . 109.5 no H112 . C11 . H111 . 109.5 no _database_code_depnum_ccdc_archive 'CCDC 933717' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C29H60Mn1N8S5 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C29 H60 Mn1 N8 S5' _chemical_formula_moiety 'C29 H60 Mn1 N8 S5' _chemical_compound_source ? _chemical_formula_weight 736.11 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.935(9) _cell_length_b 14.689(14) _cell_length_c 15.919(15) _cell_angle_alpha 80.442(16) _cell_angle_beta 72.682(17) _cell_angle_gamma 81.387(18) _cell_volume 2175(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6789 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 21.75 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.24 _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 790 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.6866 _exptl_absorpt_correction_T_max 0.7462 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 41407 _diffrn_reflns_av_R_equivalents 0.033 _diffrn_reflns_theta_min 1.826 _diffrn_reflns_theta_max 31.136 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 29.213 _diffrn_measured_fraction_theta_full 0.992529 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 12887 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -20 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 22 _refine_diff_density_min -0.34 _refine_diff_density_max 0.87 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 4755 _refine_ls_number_restraints 0 _refine_ls_number_parameters 422 _oxford_refine_ls_R_factor_ref 0.0653 _refine_ls_wR_factor_ref 0.0735 _refine_ls_goodness_of_fit_ref 1.0774 _refine_ls_shift/su_max 0.0002706 _refine_ls_shift/su_mean 0.0000126 # The values computed from all data _oxford_reflns_number_all 12887 _refine_ls_R_factor_all 0.1654 _refine_ls_wR_factor_all 0.2162 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5464 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_gt 0.0787 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.430 0.487 0.244 0.959E-01 0.332E-01 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Mn1 Mn 0.69645(7) 0.23393(4) 0.23955(4) 0.0675 1.0000 Uani . . . . . . S1 S 0.8316(3) 0.27502(15) 0.50716(12) 0.1460 1.0000 Uani . . . . . . S2 S 1.0644(3) 0.3471(2) -0.01773(12) 0.1738 1.0000 Uani . . . . . . S3 S 0.33738(16) 0.49232(10) 0.33608(9) 0.1049 1.0000 Uani . . . . . . S4 S 0.4787(2) 0.13923(15) 0.02439(12) 0.1293 1.0000 Uani . . . . . . S5 S 0.8366(2) -0.09412(9) 0.33389(10) 0.1154 1.0000 Uani . . . . . . N1 N 0.7743(5) 0.2531(3) 0.3516(3) 0.0961 1.0000 Uani . . . . . . N2 N 0.8623(5) 0.2880(3) 0.1346(3) 0.0944 1.0000 Uani . . . . . . N3 N 0.5281(5) 0.3408(3) 0.2804(3) 0.1039 1.0000 Uani . . . . . . N4 N 0.5949(4) 0.1982(3) 0.1438(2) 0.0813 1.0000 Uani . . . . . . N5 N 0.7268(5) 0.0861(3) 0.2835(3) 0.0900 1.0000 Uani . . . . . . N6 N 1.2564(4) 0.0509(3) 0.3398(2) 0.0884 1.0000 Uani . . . . . . N7 N 0.7774(4) 0.5968(3) 0.3311(2) 0.0817 1.0000 Uani . . . . . . N8 N 0.5000 0.5000 0.0000 0.0789 1.0000 Uani S . . . . . N9 N 0.0000 1.0000 0.0000 0.0709 1.0000 Uani S . . . . . C1 C 0.7979(5) 0.2618(3) 0.4160(3) 0.0825 1.0000 Uani . . . . . . C2 C 0.9446(6) 0.3136(3) 0.0715(3) 0.0834 1.0000 Uani . . . . . . C3 C 0.4485(5) 0.4031(3) 0.3039(3) 0.0768 1.0000 Uani . . . . . . C4 C 0.5474(5) 0.1744(3) 0.0940(3) 0.0801 1.0000 Uani . . . . . . C5 C 0.7708(5) 0.0111(3) 0.3044(3) 0.0717 1.0000 Uani . . . . . . C6 C 1.1150(6) 0.0811(5) 0.3215(5) 0.1299 1.0000 Uani . . . . . . C7 C 1.1189(8) 0.1443(7) 0.2331(5) 0.1715 1.0000 Uani . . . . . . C8 C 1.3275(7) 0.1383(5) 0.3439(5) 0.1328 1.0000 Uani . . . . . . C9 C 1.2391(11) 0.2018(6) 0.4109(5) 0.1839 1.0000 Uani . . . . . . C10 C 1.2299(7) -0.0102(4) 0.4307(4) 0.1126 1.0000 Uani . . . . . . C11 C 1.3632(9) -0.0488(6) 0.4592(5) 0.1504 1.0000 Uani . . . . . . C12 C 1.3597(6) -0.0001(5) 0.2680(4) 0.1217 1.0000 Uani . . . . . . C13 C 1.3085(10) -0.0898(6) 0.2570(5) 0.1628 1.0000 Uani . . . . . . C14 C 0.8111(9) 0.4961(4) 0.3157(5) 0.1489 1.0000 Uani . . . . . . C15 C 0.9446(11) 0.4717(6) 0.2454(6) 0.1871 1.0000 Uani . . . . . . C16 C 0.8996(8) 0.6272(6) 0.3579(5) 0.146(2) 1.0000 Uiso . . . . . . C17 C 0.9354(11) 0.5638(7) 0.4354(7) 0.199(4) 1.0000 Uiso . . . . . . C18 C 0.6448(8) 0.5994(6) 0.4140(5) 0.1437 1.0000 Uani . . . . . . C19 C 0.5831(11) 0.6828(10) 0.4471(7) 0.2533 1.0000 Uani . . . . . . C20 C 0.7491(11) 0.6655(6) 0.2555(5) 0.1768 1.0000 Uani . . . . . . C21 C 0.6307(10) 0.6646(9) 0.2247(6) 0.2263 1.0000 Uani . . . . . . C22 C 0.4778(12) 0.5680(7) 0.0782(6) 0.0958 0.508(10) Uani . . P . 1 . C23 C 0.3688(11) 0.5605(6) -0.0094(6) 0.0876 0.492(10) Uani . . P . 2 . C24 C 0.3314(9) 0.6294(5) 0.0778(5) 0.1714 1.0000 Uani . . . . . . C25 C 0.5285(11) 0.5695(6) -0.0878(6) 0.0884 0.513(11) Uani . . P . 1 . C26 C 0.6251(13) 0.5398(7) -0.0129(6) 0.0891 0.487(11) Uani . . P . 2 . C27 C 0.6691(7) 0.6093(4) -0.1103(4) 0.1191 1.0000 Uani . . . . . . C28 C 0.0528(11) 0.9063(6) -0.0161(6) 0.0916 0.517(10) Uani . . P . 1 . C29 C 0.0589(11) 0.9545(6) 0.0886(6) 0.0787 0.483(10) Uani . . P . 2 . C30 C 0.1093(7) 0.8528(4) 0.0779(6) 0.1493 1.0000 Uani . . . . . . C31 C -0.1252(9) 1.0168(6) 0.0799(5) 0.0767 0.485(10) Uani . . P . 2 . C32 C -0.1103(10) 0.9344(7) 0.0046(6) 0.0869 0.515(10) Uani . . P . 1 . C33 C -0.2379(6) 0.9405(5) 0.0911(4) 0.1264 1.0000 Uani . . . . . . H61 H 1.0548 0.1123 0.3689 0.203(5) 1.0000 Uiso R . . . . . H62 H 1.0754 0.0270 0.3189 0.203(5) 1.0000 Uiso R . . . . . H71 H 1.0271 0.1606 0.2249 0.234(5) 1.0000 Uiso R . . . . . H72 H 1.1578 0.1989 0.2352 0.234(5) 1.0000 Uiso R . . . . . H73 H 1.1785 0.1135 0.1851 0.234(5) 1.0000 Uiso R . . . . . H81 H 1.4131 0.1170 0.3594 0.210(5) 1.0000 Uiso R . . . . . H82 H 1.3484 0.1734 0.2867 0.210(5) 1.0000 Uiso R . . . . . H91 H 1.2879 0.2529 0.4102 0.250(5) 1.0000 Uiso R . . . . . H92 H 1.2181 0.1675 0.4685 0.250(5) 1.0000 Uiso R . . . . . H93 H 1.1534 0.2240 0.3958 0.250(5) 1.0000 Uiso R . . . . . H101 H 1.1701 0.0261 0.4745 0.184(5) 1.0000 Uiso R . . . . . H102 H 1.1831 -0.0610 0.4281 0.184(5) 1.0000 Uiso R . . . . . H111 H 1.3392 -0.0857 0.5155 0.217(5) 1.0000 Uiso R . . . . . H112 H 1.4107 0.0014 0.4627 0.217(5) 1.0000 Uiso R . . . . . H113 H 1.4236 -0.0857 0.4163 0.217(5) 1.0000 Uiso R . . . . . H121 H 1.4480 -0.0152 0.2815 0.202(5) 1.0000 Uiso R . . . . . H122 H 1.3724 0.0390 0.2130 0.202(5) 1.0000 Uiso R . . . . . H131 H 1.3753 -0.1203 0.2112 0.232(5) 1.0000 Uiso R . . . . . H132 H 1.2959 -0.1294 0.3117 0.232(5) 1.0000 Uiso R . . . . . H133 H 1.2204 -0.0752 0.2432 0.232(5) 1.0000 Uiso R . . . . . H141 H 0.8194 0.4603 0.3698 0.233(5) 1.0000 Uiso R . . . . . H142 H 0.7341 0.4788 0.3002 0.233(5) 1.0000 Uiso R . . . . . H153 H 0.9571 0.4073 0.2404 0.248(5) 1.0000 Uiso R . . . . . H152 H 1.0232 0.4878 0.2601 0.248(5) 1.0000 Uiso R . . . . . H151 H 0.9379 0.5063 0.1905 0.248(5) 1.0000 Uiso R . . . . . H161 H 0.8767 0.6894 0.3709 0.243(5) 1.0000 Uiso R . . . . . H162 H 0.9807 0.6238 0.3080 0.243(5) 1.0000 Uiso R . . . . . H171 H 1.0127 0.5809 0.4507 0.293(5) 1.0000 Uiso R . . . . . H172 H 0.8526 0.5676 0.4841 0.293(5) 1.0000 Uiso R . . . . . H173 H 0.9567 0.5019 0.4212 0.293(5) 1.0000 Uiso R . . . . . H201 H 0.7423 0.7258 0.2718 0.271(5) 1.0000 Uiso R . . . . . H202 H 0.8299 0.6572 0.2063 0.271(5) 1.0000 Uiso R . . . . . H191 H 0.5033 0.6754 0.4975 0.306(5) 1.0000 Uiso R . . . . . H192 H 0.6543 0.7073 0.4628 0.306(5) 1.0000 Uiso R . . . . . H193 H 0.5553 0.7243 0.4012 0.306(5) 1.0000 Uiso R . . . . . H181 H 0.6706 0.5588 0.4611 0.216(5) 1.0000 Uiso R . . . . . H182 H 0.5717 0.5758 0.3995 0.216(5) 1.0000 Uiso R . . . . . H211 H 0.6286 0.7117 0.1762 0.302(5) 1.0000 Uiso R . . . . . H212 H 0.5474 0.6741 0.2721 0.302(5) 1.0000 Uiso R . . . . . H213 H 0.6351 0.6055 0.2066 0.302(5) 1.0000 Uiso R . . . . . H251 H 0.4562 0.6202 -0.0810 0.165(5) 0.513(11) Uiso R . P . 1 . H252 H 0.5273 0.5390 -0.1357 0.165(5) 0.513(11) Uiso R . P . 1 . H261 H 0.6119 0.5763 0.0335 0.150(5) 0.487(11) Uiso R . P . 2 . H262 H 0.6998 0.4916 -0.0108 0.150(5) 0.487(11) Uiso R . P . 2 . H271 H 0.6836 0.6516 -0.1635 0.181(5) 1.0000 Uiso R . . . . . H272 H 0.6709 0.6402 -0.0629 0.181(5) 1.0000 Uiso R . . . . . H273 H 0.7421 0.5590 -0.1176 0.181(5) 1.0000 Uiso R . . . . . H241 H 0.2475 0.6705 0.0792 0.231(5) 1.0000 Uiso R . . . . . H242 H 0.4092 0.6643 0.0674 0.231(5) 1.0000 Uiso R . . . . . H243 H 0.3200 0.5907 0.1330 0.231(5) 1.0000 Uiso R . . . . . H231 H 0.3828 0.5973 -0.0657 0.161(5) 0.491(10) Uiso R . P . 2 . H232 H 0.2936 0.5236 -0.0002 0.161(5) 0.491(10) Uiso R . P . 2 . H221 H 0.5532 0.6059 0.0632 0.161(5) 0.509(10) Uiso R . P . 1 . H222 H 0.4729 0.5321 0.1342 0.161(5) 0.509(10) Uiso R . P . 1 . H301 H 0.1454 0.7899 0.0719 0.205(5) 1.0000 Uiso R . . . . . H302 H 0.1812 0.8855 0.0835 0.205(5) 1.0000 Uiso R . . . . . H303 H 0.0305 0.8554 0.1293 0.205(5) 1.0000 Uiso R . . . . . H281 H 0.1306 0.9051 -0.0681 0.150(5) 0.517(10) Uiso R . P . 1 . H282 H -0.0200 0.8750 -0.0224 0.150(5) 0.517(10) Uiso R . P . 1 . H291 H 0.1357 0.9857 0.0891 0.154(5) 0.483(10) Uiso R . P . 2 . H292 H -0.0154 0.9606 0.1418 0.154(5) 0.483(10) Uiso R . P . 2 . H311 H -0.1696 1.0780 0.0706 0.144(5) 0.485(10) Uiso R . P . 2 . H312 H -0.0936 1.0097 0.1316 0.144(5) 0.485(10) Uiso R . P . 2 . H321 H -0.1450 0.9506 -0.0460 0.147(5) 0.515(10) Uiso R . P . 1 . H322 H -0.0666 0.8723 0.0056 0.147(5) 0.515(10) Uiso R . P . 1 . H331 H -0.3052 0.8998 0.0935 0.187(5) 1.0000 Uiso R . . . . . H332 H -0.2819 1.0026 0.0902 0.187(5) 1.0000 Uiso R . . . . . H333 H -0.2034 0.9243 0.1418 0.187(5) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0748(4) 0.0646(4) 0.0605(3) -0.0107(3) -0.0172(3) 0.0001(3) S1 0.208(2) 0.1569(16) 0.1119(12) -0.0179(11) -0.0824(13) -0.0615(15) S2 0.194(2) 0.234(2) 0.0904(11) -0.0068(13) 0.0061(12) -0.123(2) S3 0.1027(10) 0.0984(9) 0.0976(9) -0.0266(7) -0.0116(7) 0.0209(7) S4 0.1244(13) 0.1741(16) 0.1153(11) -0.0466(11) -0.0476(10) -0.0361(11) S5 0.1670(15) 0.0619(7) 0.1020(10) 0.0027(6) -0.0273(9) -0.0003(8) N1 0.128(4) 0.084(3) 0.086(3) -0.015(2) -0.043(3) -0.009(2) N2 0.099(3) 0.109(3) 0.072(2) -0.001(2) -0.018(2) -0.024(2) N3 0.104(3) 0.108(3) 0.102(3) -0.045(3) -0.033(2) 0.026(3) N4 0.088(3) 0.083(2) 0.077(2) -0.0197(19) -0.030(2) 0.0039(19) N5 0.117(3) 0.069(2) 0.090(3) -0.010(2) -0.042(2) -0.002(2) N6 0.067(2) 0.120(3) 0.074(2) -0.006(2) -0.0105(18) -0.022(2) N7 0.092(3) 0.080(2) 0.074(2) -0.0087(18) -0.0154(19) -0.032(2) N8 0.079(4) 0.084(3) 0.069(3) 0.003(2) -0.029(3) 0.009(3) N9 0.070(3) 0.077(3) 0.070(3) -0.036(2) -0.012(2) -0.005(2) C1 0.102(3) 0.067(3) 0.084(3) -0.013(2) -0.030(3) -0.011(2) C2 0.105(4) 0.082(3) 0.067(3) -0.006(2) -0.027(3) -0.021(3) C3 0.079(3) 0.085(3) 0.069(2) -0.020(2) -0.022(2) -0.003(2) C4 0.070(3) 0.084(3) 0.084(3) -0.014(2) -0.018(2) -0.004(2) C5 0.091(3) 0.068(3) 0.059(2) -0.0103(19) -0.019(2) -0.018(2) C6 0.070(3) 0.176(6) 0.141(5) -0.035(5) -0.020(3) -0.007(4) C7 0.133(6) 0.230(9) 0.144(6) 0.001(6) -0.065(5) 0.030(6) C8 0.113(5) 0.148(6) 0.128(5) 0.017(4) -0.015(4) -0.063(4) C9 0.255(10) 0.139(6) 0.138(6) -0.042(5) 0.022(6) -0.094(7) C10 0.118(5) 0.128(5) 0.086(3) -0.012(3) -0.006(3) -0.047(4) C11 0.180(7) 0.172(7) 0.118(5) 0.019(5) -0.082(5) -0.033(6) C12 0.101(4) 0.161(6) 0.089(4) -0.025(4) -0.011(3) 0.009(4) C13 0.191(8) 0.173(7) 0.117(5) -0.064(5) -0.034(5) 0.033(6) C14 0.197(8) 0.087(4) 0.150(6) -0.024(4) -0.014(6) -0.038(4) C15 0.230(9) 0.129(6) 0.178(8) -0.081(6) 0.020(7) -0.034(6) C18 0.125(5) 0.188(7) 0.099(4) -0.006(4) -0.020(4) 0.006(5) C19 0.171(9) 0.371(18) 0.152(8) -0.061(10) 0.015(7) 0.083(10) C20 0.204(9) 0.178(8) 0.100(5) 0.026(5) -0.001(5) -0.007(7) C21 0.168(8) 0.365(16) 0.161(8) 0.092(9) -0.096(7) -0.113(9) C22 0.123(8) 0.087(7) 0.075(6) -0.016(5) -0.033(5) 0.010(6) C23 0.091(7) 0.076(6) 0.088(6) 0.002(5) -0.034(5) 0.021(5) C24 0.174(7) 0.109(5) 0.152(6) 0.010(4) 0.021(5) 0.061(5) C25 0.100(8) 0.088(6) 0.076(6) 0.005(4) -0.039(5) 0.009(5) C26 0.099(9) 0.093(7) 0.078(6) -0.008(5) -0.031(5) -0.010(6) C27 0.127(5) 0.119(5) 0.100(4) -0.010(3) -0.015(4) -0.020(4) C28 0.113(8) 0.062(5) 0.082(6) -0.017(4) -0.009(5) 0.018(5) C29 0.098(7) 0.080(6) 0.068(5) -0.018(4) -0.036(5) -0.001(5) C30 0.123(5) 0.097(4) 0.202(7) -0.016(4) -0.027(5) 0.027(4) C31 0.079(6) 0.088(7) 0.059(5) -0.028(4) -0.010(4) 0.005(5) C32 0.103(8) 0.093(7) 0.078(6) -0.022(5) -0.041(5) -0.003(5) C33 0.085(4) 0.193(7) 0.102(4) -0.005(4) -0.019(3) -0.047(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1705(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mn1 . N1 . 2.216(5) yes Mn1 . N2 . 2.110(5) yes Mn1 . N3 . 2.143(4) yes Mn1 . N4 . 2.226(4) yes Mn1 . N5 . 2.173(4) yes S1 . C1 . 1.629(5) yes S2 . C2 . 1.617(6) yes S3 . C3 . 1.628(5) yes S4 . C4 . 1.645(6) yes S5 . C5 . 1.636(5) yes N1 . C1 . 1.149(6) yes N2 . C2 . 1.137(6) yes N3 . C3 . 1.151(5) yes N4 . C4 . 1.158(5) yes N5 . C5 . 1.155(5) yes N6 . C6 . 1.507(7) yes N6 . C8 . 1.573(8) yes N6 . C10 . 1.544(7) yes N6 . C12 . 1.509(7) yes N7 . C14 . 1.510(7) yes N7 . C16 . 1.546(8) yes N7 . C18 . 1.564(8) yes N7 . C20 . 1.503(8) yes N8 . C25 2_665 1.566(8) yes N8 . C22 2_665 1.668(9) yes N8 . C22 . 1.668(9) yes N8 . C25 . 1.566(8) yes N9 . C32 2_575 1.543(10) yes N9 . C28 2_575 1.433(8) yes N9 . C28 . 1.433(8) yes N9 . C32 . 1.543(10) yes C6 . C7 . 1.546(10) yes C6 . H61 . 0.950 no C6 . H62 . 0.950 no C7 . H71 . 0.950 no C7 . H72 . 0.950 no C7 . H73 . 0.950 no C8 . C9 . 1.519(10) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.526(9) yes C10 . H101 . 0.950 no C10 . H102 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . C13 . 1.534(10) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.499(10) yes C14 . H141 . 0.950 no C14 . H142 . 0.950 no C15 . H153 . 0.950 no C15 . H152 . 0.950 no C15 . H151 . 0.950 no C16 . C17 . 1.516(11) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C17 . H171 . 0.950 no C17 . H172 . 0.950 no C17 . H173 . 0.950 no C18 . C19 . 1.397(13) yes C18 . H181 . 0.950 no C18 . H182 . 0.950 no C19 . H191 . 0.950 no C19 . H192 . 0.950 no C19 . H193 . 0.950 no C20 . C21 . 1.405(12) yes C20 . H201 . 0.950 no C20 . H202 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . C24 . 1.593(12) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no C23 . H262 2_665 1.048 no C23 . C26 2_665 1.455(14) yes C23 . C24 . 1.770(12) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . C27 . 1.516(12) yes C25 . H251 . 0.950 no C25 . H252 . 0.950 no C26 . H232 2_665 1.172 no C26 . C27 . 1.686(11) yes C26 . H261 . 0.950 no C26 . H262 . 0.950 no C27 . H271 . 0.950 no C27 . H272 . 0.950 no C27 . H273 . 0.950 no C28 . C30 . 1.775(12) yes C28 . C32 . 1.560(14) yes C28 . H281 . 0.950 no C28 . H282 . 0.950 no C28 . H322 . 1.286 no C29 . C30 . 1.524(10) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . C33 . 1.652(11) yes C31 . H311 . 0.950 no C31 . H312 . 0.950 no C32 . C33 . 1.575(11) yes C32 . H282 . 1.187 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C33 . H331 . 0.950 no C33 . H332 . 0.950 no C33 . H333 . 0.950 no H282 . H322 . 0.539 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Mn1 . N2 . 98.29(17) yes N1 . Mn1 . N3 . 87.85(17) yes N2 . Mn1 . N3 . 110.81(19) yes N1 . Mn1 . N4 . 170.27(15) yes N2 . Mn1 . N4 . 91.01(16) yes N3 . Mn1 . N4 . 91.51(16) yes N1 . Mn1 . N5 . 85.92(15) yes N2 . Mn1 . N5 . 116.00(18) yes N3 . Mn1 . N5 . 133.19(18) yes N4 . Mn1 . N5 . 87.45(17) yes Mn1 . N1 . C1 . 171.6(4) yes Mn1 . N2 . C2 . 171.9(4) yes Mn1 . N3 . C3 . 172.7(4) yes Mn1 . N4 . C4 . 175.7(4) yes Mn1 . N5 . C5 . 166.1(4) yes C6 . N6 . C8 . 110.0(5) yes C6 . N6 . C10 . 107.8(4) yes C8 . N6 . C10 . 109.0(4) yes C6 . N6 . C12 . 112.6(4) yes C8 . N6 . C12 . 106.3(5) yes C10 . N6 . C12 . 111.1(4) yes C14 . N7 . C16 . 109.3(5) yes C14 . N7 . C18 . 105.3(5) yes C16 . N7 . C18 . 106.6(5) yes C14 . N7 . C20 . 116.8(6) yes C16 . N7 . C20 . 108.2(6) yes C18 . N7 . C20 . 110.0(5) yes C25 2_665 N8 . C22 2_665 103.3(5) yes C25 2_665 N8 . C22 . 76.7(5) yes C22 2_665 N8 . C22 . 179.993 yes C25 2_665 N8 . C25 . 179.993 yes C22 2_665 N8 . C25 . 76.7(5) yes C22 . N8 . C25 . 103.3(5) yes C32 2_575 N9 . C28 2_575 63.1(6) yes C32 2_575 N9 . C28 . 116.9(6) yes C28 2_575 N9 . C28 . 179.992 yes C32 2_575 N9 . C32 . 179.993 yes C28 2_575 N9 . C32 . 116.9(6) yes C28 . N9 . C32 . 63.1(6) yes S1 . C1 . N1 . 179.6(4) yes S2 . C2 . N2 . 178.3(5) yes S3 . C3 . N3 . 179.2(5) yes S4 . C4 . N4 . 179.1(5) yes S5 . C5 . N5 . 178.7(4) yes N6 . C6 . C7 . 115.7(5) yes N6 . C6 . H61 . 108.6 no C7 . C6 . H61 . 108.8 no N6 . C6 . H62 . 107.9 no C7 . C6 . H62 . 106.2 no H61 . C6 . H62 . 109.5 no C6 . C7 . H71 . 112.0 no C6 . C7 . H72 . 106.9 no H71 . C7 . H72 . 109.5 no C6 . C7 . H73 . 109.4 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N6 . C8 . C9 . 115.3(5) yes N6 . C8 . H81 . 108.1 no C9 . C8 . H81 . 107.2 no N6 . C8 . H82 . 108.3 no C9 . C8 . H82 . 108.4 no H81 . C8 . H82 . 109.5 no C8 . C9 . H91 . 111.2 no C8 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.5 no C8 . C9 . H93 . 108.0 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N6 . C10 . C11 . 114.9(5) yes N6 . C10 . H101 . 108.3 no C11 . C10 . H101 . 108.0 no N6 . C10 . H102 . 108.0 no C11 . C10 . H102 . 108.1 no H101 . C10 . H102 . 109.5 no C10 . C11 . H111 . 110.5 no C10 . C11 . H112 . 109.0 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 108.9 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no N6 . C12 . C13 . 113.2(5) yes N6 . C12 . H121 . 109.2 no C13 . C12 . H121 . 108.7 no N6 . C12 . H122 . 108.8 no C13 . C12 . H122 . 107.4 no H121 . C12 . H122 . 109.5 no C12 . C13 . H131 . 111.4 no C12 . C13 . H132 . 107.9 no H131 . C13 . H132 . 109.5 no C12 . C13 . H133 . 109.1 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N7 . C14 . C15 . 116.7(6) yes N7 . C14 . H141 . 107.9 no C15 . C14 . H141 . 107.0 no N7 . C14 . H142 . 107.8 no C15 . C14 . H142 . 107.8 no H141 . C14 . H142 . 109.5 no C14 . C15 . H153 . 110.9 no C14 . C15 . H152 . 109.2 no H153 . C15 . H152 . 109.5 no C14 . C15 . H151 . 108.3 no H153 . C15 . H151 . 109.5 no H152 . C15 . H151 . 109.5 no N7 . C16 . C17 . 112.9(7) yes N7 . C16 . H161 . 109.7 no C17 . C16 . H161 . 110.5 no N7 . C16 . H162 . 106.4 no C17 . C16 . H162 . 107.7 no H161 . C16 . H162 . 109.5 no C16 . C17 . H171 . 113.2 no C16 . C17 . H172 . 106.2 no H171 . C17 . H172 . 109.5 no C16 . C17 . H173 . 108.9 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no N7 . C18 . C19 . 121.1(8) yes N7 . C18 . H181 . 106.8 no C19 . C18 . H181 . 106.9 no N7 . C18 . H182 . 106.9 no C19 . C18 . H182 . 105.3 no H181 . C18 . H182 . 109.5 no C18 . C19 . H191 . 113.2 no C18 . C19 . H192 . 106.8 no H191 . C19 . H192 . 109.5 no C18 . C19 . H193 . 108.4 no H191 . C19 . H193 . 109.5 no H192 . C19 . H193 . 109.5 no N7 . C20 . C21 . 121.8(8) yes N7 . C20 . H201 . 107.2 no C21 . C20 . H201 . 106.0 no N7 . C20 . H202 . 105.9 no C21 . C20 . H202 . 106.1 no H201 . C20 . H202 . 109.5 no C20 . C21 . H211 . 111.6 no C20 . C21 . H212 . 108.4 no H211 . C21 . H212 . 109.5 no C20 . C21 . H213 . 108.3 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no N8 . C22 . C24 . 103.3(7) yes N8 . C22 . H221 . 110.6 no C24 . C22 . H221 . 110.9 no N8 . C22 . H222 . 110.9 no C24 . C22 . H222 . 111.5 no H221 . C22 . H222 . 109.5 no H262 2_665 C23 . N8 . 96.9 no H262 2_665 C23 . C26 2_665 40.7 no N8 . C23 . C26 2_665 56.6(6) yes H262 2_665 C23 . C24 . 108.1 no N8 . C23 . C24 . 102.8(6) yes C26 2_665 C23 . C24 . 118.4(7) yes H262 2_665 C23 . H231 . 122.2 no N8 . C23 . H231 . 112.4 no C26 2_665 C23 . H231 . 129.6 no C24 . C23 . H231 . 111.9 no H262 2_665 C23 . H232 . 14.7 no N8 . C23 . H232 . 110.0 no C26 2_665 C23 . H232 . 53.5 no C24 . C23 . H232 . 110.0 no H231 . C23 . H232 . 109.5 no C22 . C24 . H241 . 174.6 no C22 . C24 . H242 . 65.7 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 71.0 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no N8 . C25 . C27 . 112.9(6) yes N8 . C25 . H251 . 108.8 no C27 . C25 . H251 . 107.2 no N8 . C25 . H252 . 109.7 no C27 . C25 . H252 . 108.7 no H251 . C25 . H252 . 109.5 no H232 2_665 C26 . C23 2_665 40.6 no H232 2_665 C26 . N8 . 103.8 no C23 2_665 C26 . N8 . 63.2(6) yes H232 2_665 C26 . C27 . 118.0 no C23 2_665 C26 . C27 . 132.5(8) yes N8 . C26 . C27 . 112.4(7) yes H232 2_665 C26 . H261 . 105.3 no C23 2_665 C26 . H261 . 118.1 no N8 . C26 . H261 . 108.5 no C27 . C26 . H261 . 108.1 no H232 2_665 C26 . H262 . 8.6 no C23 2_665 C26 . H262 . 46.0 no N8 . C26 . H262 . 108.8 no C27 . C26 . H262 . 109.4 no H261 . C26 . H262 . 109.5 no C25 . C27 . H271 . 111.4 no C25 . C27 . H272 . 109.3 no H271 . C27 . H272 . 109.5 no C25 . C27 . H273 . 107.8 no H271 . C27 . H273 . 109.5 no H272 . C27 . H273 . 109.5 no N9 . C28 . C30 . 105.9(6) yes N9 . C28 . C32 . 61.9(5) yes C30 . C28 . C32 . 113.9(7) yes N9 . C28 . H281 . 110.9 no C30 . C28 . H281 . 109.9 no C32 . C28 . H281 . 135.9 no N9 . C28 . H282 . 110.3 no C30 . C28 . H282 . 110.4 no C32 . C28 . H282 . 49.5 no H281 . C28 . H282 . 109.5 no N9 . C28 . H322 . 98.4 no C30 . C28 . H322 . 97.5 no C32 . C28 . H322 . 37.5 no H281 . C28 . H322 . 131.5 no H282 . C28 . H322 . 22.0 no N9 . C29 . C30 . 106.2(6) yes N9 . C29 . H291 . 109.9 no C30 . C29 . H291 . 109.9 no N9 . C29 . H292 . 110.0 no C30 . C29 . H292 . 111.3 no H291 . C29 . H292 . 109.5 no C28 . C30 . H301 . 110.5 no C28 . C30 . H302 . 109.2 no H301 . C30 . H302 . 109.5 no C28 . C30 . H303 . 108.7 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no N9 . C31 . C33 . 108.5(5) yes N9 . C31 . H311 . 109.1 no C33 . C31 . H311 . 110.0 no N9 . C31 . H312 . 109.8 no C33 . C31 . H312 . 109.9 no H311 . C31 . H312 . 109.5 no N9 . C32 . C28 . 55.0(5) yes N9 . C32 . C33 . 111.1(6) yes C28 . C32 . C33 . 135.6(7) yes N9 . C32 . H282 . 91.8 no C28 . C32 . H282 . 37.5 no C33 . C32 . H282 . 134.3 no N9 . C32 . H321 . 109.4 no C28 . C32 . H321 . 114.9 no C33 . C32 . H321 . 109.4 no H282 . C32 . H321 . 98.4 no N9 . C32 . H322 . 109.2 no C28 . C32 . H322 . 55.4 no C33 . C32 . H322 . 108.2 no H282 . C32 . H322 . 26.3 no H321 . C32 . H322 . 109.5 no C32 . C33 . H331 . 110.6 no C32 . C33 . H332 . 108.3 no H331 . C33 . H332 . 109.5 no C32 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C23 2_665 H262 . C26 . 93.3 no C26 2_665 H232 . C23 . 85.9 no C32 . H282 . C28 . 93.1 no C32 . H282 . H322 . 51.4 no C28 . H282 . H322 . 116.7 no H282 . H322 . C32 . 102.2 no H282 . H322 . C28 . 41.3 no C32 . H322 . C28 . 87.1 no _database_code_depnum_ccdc_archive 'CCDC 933718' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C54H108FeN9OS6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C54 H108 Fe1 N9 O0.42 S6' _chemical_formula_moiety 'C54 H108 Fe1 N9 O0.42 S6' _chemical_compound_source ? _chemical_formula_weight 1138.45 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P a -3 ' _symmetry_space_group_name_Hall '-P 2ac 2ab 3' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -y+1/2,-z,x+1/2 y+1/2,z,-x+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 x+1/2,-y+1/2,-z -x+1/2,y+1/2,z -z,-x,-y z,x,y x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -y,z+1/2,-x+1/2 y,-z+1/2,x+1/2 z+1/2,-x+1/2,-y -z+1/2,x+1/2,y -z,x+1/2,-y+1/2 z,-x+1/2,y+1/2 -y+1/2,z+1/2,x y+1/2,-z+1/2,-x -z+1/2,-x,y+1/2 z+1/2,x,-y+1/2 y,z,x -y,-z,-x _cell_length_a 24.1615(2) _cell_length_b 24.1615(2) _cell_length_c 24.1615(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14105.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2210 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 13.15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_max 0.1 _exptl_crystal_density_diffrn 1.072 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 4962.769 _exptl_absorpt_coefficient_mu 0.429 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.6288 _exptl_absorpt_correction_T_max 0.7438 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type 'Bruker Kappa Apex2' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 34166 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_theta_min 1.686 _diffrn_reflns_theta_max 19.753 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 19.753 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 2123 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 2 _reflns_limit_l_max 22 _refine_diff_density_min -0.17 _refine_diff_density_max 0.24 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 1643 _refine_ls_number_restraints 0 _refine_ls_number_parameters 216 _oxford_refine_ls_R_factor_ref 0.0292 _refine_ls_wR_factor_ref 0.0322 _refine_ls_goodness_of_fit_ref 1.0007 _refine_ls_shift/su_max 0.0005499 _refine_ls_shift/su_mean 0.0000312 # The values computed from all data _oxford_reflns_number_all 2123 _refine_ls_R_factor_all 0.0448 _refine_ls_wR_factor_all 0.0547 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1643 _refine_ls_R_factor_gt 0.0292 _refine_ls_wR_factor_gt 0.0322 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.248 0.217 0.133 0.391E-01 0.850E-02 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Fe1 Fe 0.313247(17) 0.313247(17) 0.313247(17) 0.0375 1.0000 Uani S T . . . . S1 S 0.16809(3) 0.18368(3) 0.35789(4) 0.0542 1.0000 Uani . . . . . . S2 S 0.43410(4) 0.44883(4) 0.23074(4) 0.0549 1.0000 Uani . . . . . . N1 N 0.25551(12) 0.25641(12) 0.33997(11) 0.0493 1.0000 Uani . . . . . . N2 N 0.36757(11) 0.36954(12) 0.28233(11) 0.0448 1.0000 Uani . . . . . . N3 N 0.26449(10) 0.23954(10) 0.53254(9) 0.0402 1.0000 Uani . . . . . . C1 C 0.21881(14) 0.22645(13) 0.34691(13) 0.0387 1.0000 Uani . . . . . . C2 C 0.39545(13) 0.40247(14) 0.26039(13) 0.0395 1.0000 Uani . . . . . . C3 C 0.24770(13) 0.19351(13) 0.49327(12) 0.0441 1.0000 Uani . . . . . . C4 C 0.20970(15) 0.14997(14) 0.51794(14) 0.0573 1.0000 Uani . . . . . . C5 C 0.21098(16) 0.09623(14) 0.48794(16) 0.0689 1.0000 Uani . . . . . . C6 C 0.17420(17) 0.05336(15) 0.51466(16) 0.0783 1.0000 Uani . . . . . . C7 C 0.29751(13) 0.21612(13) 0.58059(12) 0.0450 1.0000 Uani . . . . . . C8 C 0.35033(14) 0.18684(15) 0.56468(14) 0.0603 1.0000 Uani . . . . . . C9 C 0.37849(15) 0.15921(15) 0.61258(14) 0.0607 1.0000 Uani . . . . . . C10 C 0.43059(15) 0.12918(16) 0.59429(16) 0.0700 1.0000 Uani . . . . . . C11 C 0.29929(13) 0.28060(12) 0.49941(12) 0.0410 1.0000 Uani . . . . . . C12 C 0.31896(14) 0.33065(13) 0.53147(13) 0.0495 1.0000 Uani . . . . . . C13 C 0.36514(13) 0.36081(13) 0.50146(13) 0.0486 1.0000 Uani . . . . . . C14 C 0.38567(15) 0.41029(14) 0.53425(16) 0.0668 1.0000 Uani . . . . . . C15 C 0.21383(13) 0.26716(13) 0.55704(13) 0.0471 1.0000 Uani . . . . . . C16 C 0.17271(13) 0.29116(14) 0.51619(14) 0.0531 1.0000 Uani . . . . . . C17 C 0.12219(15) 0.31325(16) 0.54588(16) 0.0691 1.0000 Uani . . . . . . C18 C 0.08011(16) 0.33885(18) 0.50727(19) 0.0930 1.0000 Uani . . . . . . O1 O 0.2024(4) 0.2024(4) 0.2024(4) 0.1423 0.42(2) Uani S T P . . . H31 H 0.2803 0.1750 0.4812 0.0472(18) 1.0000 Uiso R . . . . . H32 H 0.2297 0.2098 0.4623 0.0190(18) 1.0000 Uiso R . . . . . H41 H 0.2204 0.1439 0.5553 0.1015(18) 1.0000 Uiso R . . . . . H42 H 0.1729 0.1638 0.5170 0.0880(18) 1.0000 Uiso R . . . . . H51 H 0.2480 0.0830 0.4879 0.1163(18) 1.0000 Uiso R . . . . . H52 H 0.1991 0.1020 0.4509 0.1443(18) 1.0000 Uiso R . . . . . H61 H 0.1761 0.0195 0.4948 0.0777(18) 1.0000 Uiso R . . . . . H62 H 0.1861 0.0475 0.5517 0.0724(18) 1.0000 Uiso R . . . . . H63 H 0.1371 0.0665 0.5147 0.0965(18) 1.0000 Uiso R . . . . . H71 H 0.3075 0.2458 0.6043 0.0488(18) 1.0000 Uiso R . . . . . H72 H 0.2747 0.1908 0.6002 0.0488(18) 1.0000 Uiso R . . . . . H81 H 0.3751 0.2126 0.5483 0.0681(18) 1.0000 Uiso R . . . . . H82 H 0.3411 0.1591 0.5384 0.0681(18) 1.0000 Uiso R . . . . . H91 H 0.3878 0.1869 0.6389 0.0664(18) 1.0000 Uiso R . . . . . H92 H 0.3538 0.1333 0.6289 0.0664(18) 1.0000 Uiso R . . . . . H101 H 0.4481 0.1124 0.6252 0.0758(18) 1.0000 Uiso R . . . . . H102 H 0.4551 0.1552 0.5779 0.0758(18) 1.0000 Uiso R . . . . . H103 H 0.4212 0.1016 0.5679 0.0758(18) 1.0000 Uiso R . . . . . H111 H 0.3310 0.2617 0.4859 0.0445(18) 1.0000 Uiso R . . . . . H112 H 0.2778 0.2934 0.4691 0.0445(18) 1.0000 Uiso R . . . . . H121 H 0.3323 0.3186 0.5664 0.0526(18) 1.0000 Uiso R . . . . . H122 H 0.2888 0.3554 0.5368 0.0526(18) 1.0000 Uiso R . . . . . H131 H 0.3950 0.3359 0.4958 0.0538(18) 1.0000 Uiso R . . . . . H132 H 0.3516 0.3732 0.4667 0.0538(18) 1.0000 Uiso R . . . . . H141 H 0.4145 0.4288 0.5149 0.0730(18) 1.0000 Uiso R . . . . . H142 H 0.3991 0.3978 0.5690 0.0730(18) 1.0000 Uiso R . . . . . H143 H 0.3557 0.4351 0.5399 0.0730(18) 1.0000 Uiso R . . . . . H151 H 0.2259 0.2965 0.5802 0.0499(18) 1.0000 Uiso R . . . . . H152 H 0.1946 0.2405 0.5786 0.0499(18) 1.0000 Uiso R . . . . . H161 H 0.1899 0.3206 0.4966 0.0576(18) 1.0000 Uiso R . . . . . H162 H 0.1621 0.2630 0.4909 0.0576(18) 1.0000 Uiso R . . . . . H171 H 0.1336 0.3403 0.5721 0.0764(18) 1.0000 Uiso R . . . . . H172 H 0.1050 0.2833 0.5646 0.0764(18) 1.0000 Uiso R . . . . . H181 H 0.0490 0.3519 0.5275 0.1012(18) 1.0000 Uiso R . . . . . H182 H 0.0971 0.3689 0.4885 0.1012(18) 1.0000 Uiso R . . . . . H183 H 0.0684 0.3119 0.4811 0.1012(18) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0375(2) 0.0375(2) 0.0375(2) -0.0022(2) -0.0022(2) -0.0022(2) S1 0.0377(5) 0.0457(6) 0.0791(7) 0.0147(5) -0.0095(5) -0.0071(4) S2 0.0545(6) 0.0506(6) 0.0597(6) 0.0057(5) 0.0131(5) -0.0068(5) N1 0.0441(18) 0.0486(18) 0.0553(18) -0.0009(15) -0.0024(15) -0.0084(16) N2 0.0407(17) 0.0470(18) 0.0466(18) -0.0036(15) 0.0018(14) -0.0012(15) N3 0.0482(17) 0.0424(16) 0.0299(15) -0.0031(14) 0.0017(14) -0.0069(14) C1 0.040(2) 0.038(2) 0.038(2) -0.0029(16) -0.0070(17) 0.0119(19) C2 0.038(2) 0.043(2) 0.037(2) -0.0102(18) -0.0039(18) 0.0086(18) C3 0.051(2) 0.047(2) 0.0340(19) -0.0063(17) -0.0016(17) -0.0062(18) C4 0.066(2) 0.054(2) 0.052(2) -0.012(2) 0.0090(19) -0.021(2) C5 0.086(3) 0.047(2) 0.074(3) 0.000(2) 0.024(2) -0.010(2) C6 0.111(3) 0.051(2) 0.073(3) -0.011(2) 0.029(3) -0.018(2) C7 0.061(2) 0.043(2) 0.0318(19) 0.0046(17) -0.0027(18) -0.0125(18) C8 0.060(3) 0.073(3) 0.048(2) 0.012(2) -0.001(2) -0.001(2) C9 0.069(3) 0.058(2) 0.055(2) 0.010(2) -0.007(2) -0.008(2) C10 0.072(3) 0.065(3) 0.072(3) 0.014(2) -0.014(2) -0.006(2) C11 0.046(2) 0.044(2) 0.0334(19) 0.0095(17) -0.0002(16) -0.0102(17) C12 0.064(2) 0.039(2) 0.046(2) 0.0089(18) -0.0071(18) -0.0026(19) C13 0.049(2) 0.045(2) 0.051(2) 0.0088(18) -0.0165(18) -0.0108(18) C14 0.073(3) 0.043(2) 0.084(3) 0.012(2) -0.014(2) -0.011(2) C15 0.057(2) 0.043(2) 0.042(2) -0.0038(17) 0.0025(19) -0.0113(18) C16 0.054(2) 0.052(2) 0.053(2) 0.0014(19) 0.002(2) -0.0053(19) C17 0.062(3) 0.068(3) 0.078(3) 0.005(2) 0.008(2) 0.000(2) C18 0.062(3) 0.099(3) 0.118(4) 0.021(3) 0.008(3) 0.013(3) O1 0.142(10) 0.142(10) 0.142(10) -0.016(6) -0.016(6) -0.016(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.05490(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N1 10_555 2.061(3) yes Fe1 . N1 23_555 2.061(3) yes Fe1 . N2 10_555 2.032(3) yes Fe1 . N2 23_555 2.032(3) yes Fe1 . N1 . 2.061(3) yes Fe1 . N2 . 2.032(3) yes S1 . C1 . 1.625(4) yes S2 . C2 . 1.625(4) yes N1 . C1 . 1.157(4) yes N2 . C2 . 1.170(4) yes N3 . C3 . 1.517(4) yes N3 . C7 . 1.518(4) yes N3 . C11 . 1.527(4) yes N3 . C15 . 1.515(4) yes C3 . C4 . 1.518(4) yes C3 . H31 . 0.950 no C3 . H32 . 0.950 no C4 . C5 . 1.488(4) yes C4 . H41 . 0.950 no C4 . H42 . 0.950 no C5 . C6 . 1.510(5) yes C5 . H51 . 0.950 no C5 . H52 . 0.950 no C6 . H61 . 0.950 no C6 . H62 . 0.950 no C6 . H63 . 0.950 no C7 . C8 . 1.509(4) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C8 . C9 . 1.499(4) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . C10 . 1.519(5) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.513(4) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . C13 . 1.517(4) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C13 . C14 . 1.518(4) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.516(4) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . C17 . 1.513(5) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C17 . C18 . 1.512(5) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 10_555 Fe1 . N1 23_555 88.27(11) yes N1 10_555 Fe1 . N2 10_555 176.41(11) yes N1 23_555 Fe1 . N2 10_555 90.32(10) yes N1 10_555 Fe1 . N2 23_555 88.39(10) yes N1 23_555 Fe1 . N2 23_555 176.41(11) yes N2 10_555 Fe1 . N2 23_555 92.94(10) yes N1 10_555 Fe1 . N1 . 88.27(11) yes N1 23_555 Fe1 . N1 . 88.27(11) yes N2 10_555 Fe1 . N1 . 88.39(10) yes N2 23_555 Fe1 . N1 . 90.32(10) yes N1 10_555 Fe1 . N2 . 90.32(10) yes N1 23_555 Fe1 . N2 . 88.39(10) yes N2 10_555 Fe1 . N2 . 92.94(10) yes N2 23_555 Fe1 . N2 . 92.94(10) yes N1 . Fe1 . N2 . 176.41(11) yes Fe1 . N1 . C1 . 168.8(3) yes Fe1 . N2 . C2 . 173.6(3) yes C3 . N3 . C7 . 110.2(2) yes C3 . N3 . C11 . 107.2(2) yes C7 . N3 . C11 . 110.7(2) yes C3 . N3 . C15 . 110.6(2) yes C7 . N3 . C15 . 106.9(2) yes C11 . N3 . C15 . 111.3(2) yes S1 . C1 . N1 . 178.6(3) yes S2 . C2 . N2 . 179.1(3) yes N3 . C3 . C4 . 115.1(2) yes N3 . C3 . H31 . 108.4 no C4 . C3 . H31 . 107.2 no N3 . C3 . H32 . 108.2 no C4 . C3 . H32 . 108.5 no H31 . C3 . H32 . 109.5 no C3 . C4 . C5 . 113.6(3) yes C3 . C4 . H41 . 108.3 no C5 . C4 . H41 . 108.9 no C3 . C4 . H42 . 108.3 no C5 . C4 . H42 . 108.3 no H41 . C4 . H42 . 109.5 no C4 . C5 . C6 . 112.2(3) yes C4 . C5 . H51 . 108.3 no C6 . C5 . H51 . 108.9 no C4 . C5 . H52 . 108.9 no C6 . C5 . H52 . 109.0 no H51 . C5 . H52 . 109.5 no C5 . C6 . H61 . 110.3 no C5 . C6 . H62 . 109.1 no H61 . C6 . H62 . 109.5 no C5 . C6 . H63 . 109.0 no H61 . C6 . H63 . 109.5 no H62 . C6 . H63 . 109.5 no N3 . C7 . C8 . 115.1(2) yes N3 . C7 . H71 . 108.3 no C8 . C7 . H71 . 107.0 no N3 . C7 . H72 . 108.5 no C8 . C7 . H72 . 108.3 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 113.3(3) yes C7 . C8 . H81 . 109.4 no C9 . C8 . H81 . 109.1 no C7 . C8 . H82 . 107.7 no C9 . C8 . H82 . 107.9 no H81 . C8 . H82 . 109.5 no C8 . C9 . C10 . 111.4(3) yes C8 . C9 . H91 . 108.1 no C10 . C9 . H91 . 109.6 no C8 . C9 . H92 . 109.2 no C10 . C9 . H92 . 109.1 no H91 . C9 . H92 . 109.5 no C9 . C10 . H101 . 110.1 no C9 . C10 . H102 . 108.9 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.4 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N3 . C11 . C12 . 115.1(2) yes N3 . C11 . H111 . 108.2 no C12 . C11 . H111 . 107.9 no N3 . C11 . H112 . 108.3 no C12 . C11 . H112 . 107.8 no H111 . C11 . H112 . 109.5 no C11 . C12 . C13 . 111.7(3) yes C11 . C12 . H121 . 108.5 no C13 . C12 . H121 . 108.7 no C11 . C12 . H122 . 109.3 no C13 . C12 . H122 . 109.0 no H121 . C12 . H122 . 109.5 no C12 . C13 . C14 . 111.7(3) yes C12 . C13 . H131 . 108.9 no C14 . C13 . H131 . 109.0 no C12 . C13 . H132 . 108.7 no C14 . C13 . H132 . 109.1 no H131 . C13 . H132 . 109.5 no C13 . C14 . H141 . 110.7 no C13 . C14 . H142 . 108.9 no H141 . C14 . H142 . 109.5 no C13 . C14 . H143 . 108.8 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N3 . C15 . C16 . 116.4(2) yes N3 . C15 . H151 . 108.2 no C16 . C15 . H151 . 107.4 no N3 . C15 . H152 . 108.2 no C16 . C15 . H152 . 107.1 no H151 . C15 . H152 . 109.5 no C15 . C16 . C17 . 110.8(3) yes C15 . C16 . H161 . 108.9 no C17 . C16 . H161 . 109.0 no C15 . C16 . H162 . 108.9 no C17 . C16 . H162 . 109.8 no H161 . C16 . H162 . 109.5 no C16 . C17 . C18 . 113.2(3) yes C16 . C17 . H171 . 108.8 no C18 . C17 . H171 . 109.0 no C16 . C17 . H172 . 108.0 no C18 . C17 . H172 . 108.2 no H171 . C17 . H172 . 109.5 no C17 . C18 . H181 . 110.6 no C17 . C18 . H182 . 108.5 no H181 . C18 . H182 . 109.5 no C17 . C18 . H183 . 109.3 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no _database_code_depnum_ccdc_archive 'CCDC 933719' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C54H108EuN9S6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C53.94 H107.82 Eu1 N9 S6' _chemical_formula_moiety 'C53.94 H107.82 Eu1 N9 S6' _chemical_compound_source ? _chemical_formula_weight 1226.95 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.41400(10) _cell_length_b 12.88360(10) _cell_length_c 22.7811(2) _cell_angle_alpha 90.9370(10) _cell_angle_beta 92.3400(10) _cell_angle_gamma 96.7250(10) _cell_volume 3614.63(5) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.54 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1306.898 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.6258 _exptl_absorpt_correction_T_max 0.7454 #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 55962 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_min 1.592 _diffrn_reflns_theta_max 26.432 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.111 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 14706 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -0.25 _refine_diff_density_max 0.53 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 9367 _refine_ls_number_restraints 4 _refine_ls_number_parameters 652 _oxford_refine_ls_R_factor_ref 0.0322 _refine_ls_wR_factor_ref 0.0348 _refine_ls_goodness_of_fit_ref 1.0300 _refine_ls_shift/su_max 0.0008683 _refine_ls_shift/su_mean 0.0000280 _refine_special_details ; Restraints DISTANCE 1.500000 , 0.020000 = C(45) TO C(46) DISTANCE 1.500000 , 0.020000 = C(21) TO C(22) DISTANCE 1.500000 , 0.020000 = C(45) TO C(55) DISTANCE 1.500000 , 0.020000 = C(21) TO C(56) ; # The values computed from all data _oxford_reflns_number_all 14706 _refine_ls_R_factor_all 0.0539 _refine_ls_wR_factor_all 0.0637 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10083 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_gt 0.0360 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.272 0.308 0.193 0.796E-01 0.293E-01 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Eu1 Eu 0.433201(14) 0.292152(13) 0.251729(7) 0.0649 1.0000 Uani . . . . . . S1 S 0.18364(9) 0.47442(11) 0.11262(6) 0.1250 1.0000 Uani . . . . . . S2 S 0.23657(10) 0.44075(9) 0.42268(4) 0.1001 1.0000 Uani . . . . . . S3 S 0.16742(12) -0.04236(9) 0.25467(6) 0.1221 1.0000 Uani . . . . . . S4 S 0.65090(9) 0.07199(8) 0.38739(5) 0.0926 1.0000 Uani . . . . . . S5 S 0.66683(9) 0.16320(10) 0.08975(4) 0.0976 1.0000 Uani . . . . . . S6 S 0.69457(11) 0.63023(11) 0.26113(7) 0.1366 1.0000 Uani . . . . . . N1 N 0.3125(3) 0.3747(3) 0.18909(14) 0.0892 1.0000 Uani . . . . . . N2 N 0.3412(3) 0.3539(2) 0.33341(14) 0.0930 1.0000 Uani . . . . . . N3 N 0.3062(3) 0.1383(3) 0.24565(14) 0.0952 1.0000 Uani . . . . . . N4 N 0.5403(3) 0.2001(2) 0.31771(14) 0.0941 1.0000 Uani . . . . . . N5 N 0.5333(3) 0.2299(2) 0.17291(14) 0.0858 1.0000 Uani . . . . . . N6 N 0.5635(3) 0.4431(3) 0.26133(14) 0.0910 1.0000 Uani . . . . . . N7 N -0.0414(2) 0.3219(2) 0.24538(13) 0.0785 1.0000 Uani . . . . . . N8 N 0.44003(19) 0.24247(16) 0.53649(10) 0.0568 1.0000 Uani . . . . . . N9 N 0.6157(2) 0.1502(2) 0.89264(10) 0.0687 1.0000 Uani . . . . . . C1 C 0.2592(3) 0.4165(3) 0.15712(16) 0.0769 1.0000 Uani . . . . 1 . C2 C 0.2971(3) 0.3906(3) 0.37052(15) 0.0716 1.0000 Uani . . . . . . C3 C 0.2479(3) 0.0630(3) 0.24980(15) 0.0797 1.0000 Uani . . . . . . C4 C 0.5866(3) 0.1461(2) 0.34622(14) 0.0685 1.0000 Uani . . . . . . C5 C 0.5890(3) 0.2027(3) 0.13781(14) 0.0683 1.0000 Uani . . . . . . C6 C 0.6187(3) 0.5213(3) 0.26132(16) 0.0802 1.0000 Uani . . . . . . C7 C 0.0242(3) 0.2603(3) 0.20572(17) 0.0834 1.0000 Uani . . . . . . C8 C -0.0354(3) 0.1595(3) 0.18030(19) 0.0975 1.0000 Uani . . . . . . C9 C 0.0298(4) 0.1182(4) 0.1324(2) 0.1124 1.0000 Uani . . . . . . C10 C -0.0270(5) 0.0205(5) 0.1033(3) 0.1689 1.0000 Uani . . . . . . C11 C -0.1405(3) 0.3539(3) 0.2117(2) 0.0933 1.0000 Uani . . . . . . C12 C -0.1163(4) 0.4108(5) 0.1551(3) 0.1428 1.0000 Uani . . . . . . C13 C -0.2083(4) 0.4502(4) 0.1264(3) 0.1299 1.0000 Uani . . . . . . C14 C -0.1861(5) 0.5017(7) 0.0700(4) 0.2140 1.0000 Uani . . . . . . C15 C 0.0335(3) 0.4195(3) 0.26600(18) 0.0836 1.0000 Uani . . . . . . C16 C -0.0132(3) 0.4902(3) 0.3090(2) 0.1045 1.0000 Uani . . . . . . C17 C 0.0553(4) 0.5953(4) 0.3156(3) 0.1220 1.0000 Uani . . . . . . C18 C 0.0466(5) 0.6624(4) 0.2616(3) 0.1594 1.0000 Uani . . . . . . C19 C -0.0808(3) 0.2584(3) 0.29696(19) 0.0933 1.0000 Uani . . . . . . C20 C 0.0061(4) 0.2197(4) 0.3355(2) 0.1121 1.0000 Uani . . . . . . C21 C -0.0422(6) 0.1655(7) 0.3877(4) 0.1779 1.0000 Uani D . . . . . C22 C -0.038(2) 0.225(2) 0.4424(9) 0.1473 0.259(17) Uani D . P . 1 . C23 C 0.4911(2) 0.3335(2) 0.50111(13) 0.0617 1.0000 Uani . . . . . . C24 C 0.6010(3) 0.3233(2) 0.47791(14) 0.0692 1.0000 Uani . . . . . . C25 C 0.6320(3) 0.4132(3) 0.43735(16) 0.0805 1.0000 Uani . . . . . . C26 C 0.7402(4) 0.4119(4) 0.4115(2) 0.1201 1.0000 Uani . . . . . . C27 C 0.4212(2) 0.1426(2) 0.49853(12) 0.0608 1.0000 Uani . . . . . . C28 C 0.3477(3) 0.1464(3) 0.44474(14) 0.0796 1.0000 Uani . . . . . . C29 C 0.3255(3) 0.0387(3) 0.41419(16) 0.0904 1.0000 Uani . . . . . . C30 C 0.2547(4) -0.0408(3) 0.4452(2) 0.1046 1.0000 Uani . . . . . . C31 C 0.3336(2) 0.2746(2) 0.55713(13) 0.0624 1.0000 Uani . . . . . . C32 C 0.2631(3) 0.1925(3) 0.58916(17) 0.0787 1.0000 Uani . . . . . . C33 C 0.1554(3) 0.2303(3) 0.60184(19) 0.0910 1.0000 Uani . . . . . . C34 C 0.0784(4) 0.1514(4) 0.6295(3) 0.1626 1.0000 Uani . . . . . . C35 C 0.5137(2) 0.2196(2) 0.58827(13) 0.0617 1.0000 Uani . . . . . . C36 C 0.5426(3) 0.3079(2) 0.63292(14) 0.0702 1.0000 Uani . . . . . . C37 C 0.6253(3) 0.2790(3) 0.67860(15) 0.0779 1.0000 Uani . . . . . . C38 C 0.6468(3) 0.3602(3) 0.72748(15) 0.0920 1.0000 Uani . . . . . . C39 C 0.5634(3) 0.1251(3) 0.83159(13) 0.0752 1.0000 Uani . . . . . . C40 C 0.4425(3) 0.0934(3) 0.82928(15) 0.0900 1.0000 Uani . . . . . . C41 C 0.3982(3) 0.0669(4) 0.76832(17) 0.1017 1.0000 Uani . . . . . . C42 C 0.2786(4) 0.0354(5) 0.7646(2) 0.1398 1.0000 Uani . . . . . . C43 C 0.6076(3) 0.0530(3) 0.92985(14) 0.0773 1.0000 Uani . . . . . . C44 C 0.6685(3) -0.0349(3) 0.90941(18) 0.0930 1.0000 Uani . . . . . . C45 C 0.6590(4) -0.1225(4) 0.9534(2) 0.1241 1.0000 Uani D . . . . . C46 C 0.7309(7) -0.1138(8) 1.0007(4) 0.1424 0.603(10) Uani D . P . 1 . C47 C 0.7328(3) 0.1936(3) 0.88400(14) 0.0738 1.0000 Uani . . . . . . C48 C 0.8019(3) 0.2158(3) 0.93961(17) 0.0957 1.0000 Uani . . . . . . C49 C 0.9168(3) 0.2556(4) 0.9270(2) 0.1115 1.0000 Uani . . . . . . C50 C 0.9912(5) 0.2677(6) 0.9799(3) 0.1820 1.0000 Uani . . . . . . C51 C 0.5565(3) 0.2291(3) 0.92485(14) 0.0773 1.0000 Uani . . . . . . C52 C 0.5509(3) 0.3333(3) 0.89566(16) 0.0850 1.0000 Uani . . . . . . C53 C 0.4857(4) 0.4010(4) 0.9305(2) 0.1140 1.0000 Uani . . . . . . C54 C 0.4862(4) 0.5095(4) 0.9075(2) 0.1228 1.0000 Uani . . . . . . C55 C 0.7151(9) -0.2061(8) 0.9523(6) 0.1075 0.397(10) Uani D . P . 2 . C56 C 0.0249(10) 0.1399(12) 0.4318(6) 0.2071 0.741(17) Uani D . P . 2 . H71 H 0.0843 0.2442 0.2339 0.1866(14) 1.0000 Uiso R . . . . . H72 H 0.0513 0.3014 0.1741 0.0844(14) 1.0000 Uiso R . . . . . H81 H -0.0495 0.1084 0.2099 0.1072(14) 1.0000 Uiso R . . . . . H82 H -0.1052 0.1752 0.1633 0.1928(14) 1.0000 Uiso R . . . . . H91 H 0.0414 0.1675 0.1007 0.1662(14) 1.0000 Uiso R . . . . . H92 H 0.0997 0.1028 0.1482 0.1383(14) 1.0000 Uiso R . . . . . H101 H 0.0171 -0.0022 0.0737 0.1973(14) 1.0000 Uiso R . . . . . H102 H -0.0385 -0.0324 0.1318 0.1973(14) 1.0000 Uiso R . . . . . H103 H -0.0948 0.0339 0.0861 0.1973(14) 1.0000 Uiso R . . . . . H111 H -0.1849 0.2903 0.1979 0.0685(14) 1.0000 Uiso R . . . . . H112 H -0.1749 0.3965 0.2392 0.1205(14) 1.0000 Uiso R . . . . . H121 H -0.0665 0.4732 0.1703 0.1538(14) 1.0000 Uiso R . . . . . H122 H -0.0847 0.3725 0.1237 0.2330(14) 1.0000 Uiso R . . . . . H131 H -0.2321 0.5001 0.1526 0.1586(14) 1.0000 Uiso R . . . . . H132 H -0.2646 0.3942 0.1195 0.1586(14) 1.0000 Uiso R . . . . . H141 H -0.2509 0.5250 0.0543 0.2504(14) 1.0000 Uiso R . . . . . H142 H -0.1324 0.5599 0.0767 0.2504(14) 1.0000 Uiso R . . . . . H143 H -0.1608 0.4542 0.0429 0.2504(14) 1.0000 Uiso R . . . . . H151 H 0.0976 0.3947 0.2848 0.0884(14) 1.0000 Uiso R . . . . . H152 H 0.0583 0.4595 0.2316 0.1040(14) 1.0000 Uiso R . . . . . H161 H -0.0219 0.4555 0.3449 0.1207(14) 1.0000 Uiso R . . . . . H162 H -0.0861 0.5024 0.2947 0.1009(14) 1.0000 Uiso R . . . . . H171 H 0.1308 0.5857 0.3201 0.1249(14) 1.0000 Uiso R . . . . . H172 H 0.0339 0.6303 0.3513 0.1359(14) 1.0000 Uiso R . . . . . H181 H 0.0909 0.7272 0.2678 0.1915(14) 1.0000 Uiso R . . . . . H182 H -0.0266 0.6748 0.2540 0.1915(14) 1.0000 Uiso R . . . . . H183 H 0.0710 0.6263 0.2289 0.1915(14) 1.0000 Uiso R . . . . . H191 H -0.1193 0.3006 0.3226 0.1322(14) 1.0000 Uiso R . . . . . H192 H -0.1317 0.1977 0.2796 0.0924(14) 1.0000 Uiso R . . . . . H201 H 0.0584 0.2788 0.3479 0.1218(14) 1.0000 Uiso R . . . . . H202 H 0.0418 0.1679 0.3128 0.1558(14) 1.0000 Uiso R . . . . . H211 H -0.1037 0.2079 0.3972 0.2435(14) 1.0000 Uiso R . . . . . H212 H -0.0715 0.1009 0.3766 0.2435(14) 1.0000 Uiso R . . . . . H231 H 0.5102 0.3934 0.5289 0.0415(14) 1.0000 Uiso R . . . . . H232 H 0.4448 0.3465 0.4675 0.0919(14) 1.0000 Uiso R . . . . . H241 H 0.5928 0.2599 0.4526 0.0781(14) 1.0000 Uiso R . . . . . H242 H 0.6541 0.3237 0.5098 0.0704(14) 1.0000 Uiso R . . . . . H251 H 0.5774 0.4100 0.4035 0.0930(14) 1.0000 Uiso R . . . . . H252 H 0.6379 0.4746 0.4623 0.0949(14) 1.0000 Uiso R . . . . . H261 H 0.7538 0.4648 0.3831 0.1267(14) 1.0000 Uiso R . . . . . H262 H 0.7913 0.4235 0.4451 0.0740(14) 1.0000 Uiso R . . . . . H263 H 0.7407 0.3421 0.3936 0.1739(14) 1.0000 Uiso R . . . . . H271 H 0.3920 0.0873 0.5244 0.0679(14) 1.0000 Uiso R . . . . . H272 H 0.4942 0.1309 0.4879 0.0568(14) 1.0000 Uiso R . . . . . H281 H 0.3800 0.1944 0.4151 0.1390(14) 1.0000 Uiso R . . . . . H282 H 0.2733 0.1606 0.4527 0.1013(14) 1.0000 Uiso R . . . . . H291 H 0.3945 0.0150 0.4017 0.1034(14) 1.0000 Uiso R . . . . . H292 H 0.2867 0.0601 0.3783 0.1179(14) 1.0000 Uiso R . . . . . H301 H 0.1827 -0.0198 0.4492 0.1041(14) 1.0000 Uiso R . . . . . H302 H 0.2499 -0.1063 0.4234 0.2248(14) 1.0000 Uiso R . . . . . H303 H 0.2878 -0.0495 0.4830 0.1707(14) 1.0000 Uiso R . . . . . H311 H 0.3532 0.3352 0.5855 0.0703(14) 1.0000 Uiso R . . . . . H312 H 0.2958 0.2933 0.5229 0.1028(14) 1.0000 Uiso R . . . . . H321 H 0.2995 0.1790 0.6260 0.1175(14) 1.0000 Uiso R . . . . . H322 H 0.2484 0.1310 0.5663 0.0948(14) 1.0000 Uiso R . . . . . H331 H 0.1635 0.2934 0.6243 0.1494(14) 1.0000 Uiso R . . . . . H332 H 0.1204 0.2431 0.5644 0.0890(14) 1.0000 Uiso R . . . . . H341 H 0.0128 0.1802 0.6361 0.2033(14) 1.0000 Uiso R . . . . . H342 H 0.1100 0.1332 0.6660 0.2033(14) 1.0000 Uiso R . . . . . H343 H 0.0634 0.0907 0.6049 0.2033(14) 1.0000 Uiso R . . . . . H351 H 0.4775 0.1586 0.6071 0.0818(14) 1.0000 Uiso R . . . . . H352 H 0.5831 0.2060 0.5727 0.0805(14) 1.0000 Uiso R . . . . . H361 H 0.4781 0.3252 0.6515 0.1013(14) 1.0000 Uiso R . . . . . H362 H 0.5665 0.3728 0.6139 0.1013(14) 1.0000 Uiso R . . . . . H371 H 0.5921 0.2126 0.6929 0.1393(14) 1.0000 Uiso R . . . . . H372 H 0.6955 0.2722 0.6607 0.0828(14) 1.0000 Uiso R . . . . . H381 H 0.6996 0.3356 0.7547 0.1336(14) 1.0000 Uiso R . . . . . H382 H 0.6747 0.4276 0.7128 0.1053(14) 1.0000 Uiso R . . . . . H383 H 0.5826 0.3668 0.7485 0.2072(14) 1.0000 Uiso R . . . . . H391 H 0.6016 0.0748 0.8143 0.0649(14) 1.0000 Uiso R . . . . . H392 H 0.5739 0.1887 0.8074 0.1263(14) 1.0000 Uiso R . . . . . H401 H 0.4267 0.0357 0.8550 0.1193(14) 1.0000 Uiso R . . . . . H402 H 0.4097 0.1520 0.8473 0.0998(14) 1.0000 Uiso R . . . . . H411 H 0.4300 0.0108 0.7547 0.1098(14) 1.0000 Uiso R . . . . . H412 H 0.4143 0.1230 0.7420 0.0958(14) 1.0000 Uiso R . . . . . H421 H 0.2574 -0.0183 0.7336 0.2238(14) 1.0000 Uiso R . . . . . H422 H 0.2445 0.0981 0.7580 0.2067(14) 1.0000 Uiso R . . . . . H423 H 0.2610 0.0057 0.8032 0.2710(14) 1.0000 Uiso R . . . . . H431 H 0.6357 0.0723 0.9710 0.1101(14) 1.0000 Uiso R . . . . . H432 H 0.5290 0.0264 0.9266 0.1284(14) 1.0000 Uiso R . . . . . H441 H 0.6429 -0.0575 0.8713 0.1058(14) 1.0000 Uiso R . . . . . H442 H 0.7444 -0.0056 0.9070 0.1006(14) 1.0000 Uiso R . . . . . H451 H 0.5970 -0.1129 0.9750 0.1576(14) 1.0000 Uiso R . . . . . H452 H 0.6450 -0.1851 0.9303 0.1576(14) 1.0000 Uiso R . . . . . H461 H 0.7184 -0.1732 1.0247 0.1717(14) 0.603(10) Uiso R . P . 1 . H462 H 0.7205 -0.0527 1.0227 0.1717(14) 0.603(10) Uiso R . P . 1 . H463 H 0.8031 -0.1079 0.9879 0.1717(14) 0.603(10) Uiso R . P . 1 . H471 H 0.7598 0.1375 0.8634 0.1033(14) 1.0000 Uiso R . . . . . H472 H 0.7341 0.2588 0.8591 0.1284(14) 1.0000 Uiso R . . . . . H481 H 0.8008 0.1454 0.9573 0.1804(14) 1.0000 Uiso R . . . . . H482 H 0.7749 0.2696 0.9650 0.0720(14) 1.0000 Uiso R . . . . . H491 H 0.9146 0.3224 0.9075 0.1379(14) 1.0000 Uiso R . . . . . H492 H 0.9426 0.2034 0.8995 0.1694(14) 1.0000 Uiso R . . . . . H501 H 1.0624 0.2931 0.9691 0.2223(14) 1.0000 Uiso R . . . . . H502 H 0.9656 0.3166 1.0061 0.2223(14) 1.0000 Uiso R . . . . . H503 H 0.9924 0.2026 0.9987 0.2223(14) 1.0000 Uiso R . . . . . H511 H 0.4847 0.2006 0.9334 0.1054(14) 1.0000 Uiso R . . . . . H512 H 0.5998 0.2444 0.9615 0.1209(14) 1.0000 Uiso R . . . . . H521 H 0.5092 0.3120 0.8591 0.1681(14) 1.0000 Uiso R . . . . . H522 H 0.6182 0.3689 0.8827 0.1422(14) 1.0000 Uiso R . . . . . H531 H 0.5127 0.4054 0.9719 0.1570(14) 1.0000 Uiso R . . . . . H532 H 0.4091 0.3688 0.9276 0.1565(14) 1.0000 Uiso R . . . . . H541 H 0.4437 0.5486 0.9313 0.1461(14) 1.0000 Uiso R . . . . . H542 H 0.5588 0.5426 0.9082 0.1461(14) 1.0000 Uiso R . . . . . H543 H 0.4569 0.5058 0.8682 0.1461(14) 1.0000 Uiso R . . . . . H551 H 0.6940 -0.2493 0.9842 0.1263(14) 0.397(10) Uiso R . P . 2 . H552 H 0.7906 -0.1831 0.9564 0.1263(14) 0.397(10) Uiso R . P . 2 . H553 H 0.7000 -0.2447 0.9164 0.1263(14) 0.397(10) Uiso R . P . 2 . H561 H -0.0169 0.1077 0.4620 0.2502(14) 0.741(17) Uiso R . P . 2 . H562 H 0.0671 0.2014 0.4471 0.2502(14) 0.741(17) Uiso R . P . 2 . H563 H 0.0716 0.0928 0.4175 0.2502(14) 0.741(17) Uiso R . P . 2 . H221 H -0.0691 0.1831 0.4730 0.1288(14) 0.259(17) Uiso R . P . 1 . H222 H 0.0349 0.2495 0.4531 0.1288(14) 0.259(17) Uiso R . P . 1 . H223 H -0.0784 0.2823 0.4364 0.1288(14) 0.259(17) Uiso R . P . 1 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Eu1 0.07601(11) 0.06106(10) 0.05836(9) 0.00612(6) -0.00121(7) 0.01134(7) S1 0.0794(7) 0.1452(10) 0.1498(11) 0.0738(9) -0.0181(7) 0.0091(7) S2 0.1189(8) 0.1109(8) 0.0760(6) -0.0092(5) 0.0063(6) 0.0376(7) S3 0.1420(11) 0.0903(7) 0.1230(9) 0.0035(7) 0.0121(8) -0.0342(7) S4 0.1069(7) 0.0868(6) 0.0905(6) 0.0190(5) -0.0046(5) 0.0386(5) S5 0.0877(7) 0.1270(9) 0.0759(6) -0.0157(6) 0.0157(5) 0.0010(6) S6 0.1129(9) 0.1078(9) 0.1785(13) -0.0456(9) 0.0366(9) -0.0353(7) N1 0.085(2) 0.097(2) 0.086(2) 0.0197(17) -0.0092(17) 0.0142(17) N2 0.122(3) 0.087(2) 0.075(2) 0.0060(17) 0.0174(19) 0.0278(19) N3 0.107(2) 0.084(2) 0.090(2) 0.0058(17) 0.0044(18) -0.0104(19) N4 0.118(3) 0.086(2) 0.082(2) 0.0129(17) -0.0148(18) 0.0326(19) N5 0.090(2) 0.091(2) 0.0765(19) -0.0026(16) 0.0108(17) 0.0083(17) N6 0.094(2) 0.080(2) 0.095(2) -0.0031(17) -0.0060(17) -0.0002(18) N7 0.0515(15) 0.0808(18) 0.102(2) -0.0027(16) 0.0088(14) 0.0011(13) N8 0.0691(15) 0.0460(12) 0.0572(13) 0.0058(10) 0.0062(11) 0.0128(11) N9 0.0703(16) 0.0823(17) 0.0504(13) 0.0043(12) 0.0051(12) -0.0043(14) C1 0.062(2) 0.083(2) 0.084(2) 0.0165(18) -0.0005(17) 0.0016(17) C2 0.084(2) 0.0648(19) 0.065(2) 0.0086(16) -0.0086(17) 0.0100(17) C3 0.092(3) 0.079(2) 0.067(2) 0.0022(17) 0.0059(18) 0.006(2) C4 0.081(2) 0.0613(18) 0.0645(18) 0.0003(15) 0.0026(16) 0.0122(16) C5 0.069(2) 0.073(2) 0.0590(18) 0.0015(15) -0.0034(16) -0.0052(16) C6 0.070(2) 0.085(3) 0.083(2) -0.0170(19) -0.0002(18) 0.007(2) C7 0.064(2) 0.087(2) 0.100(3) -0.005(2) 0.0176(18) 0.0101(18) C8 0.085(3) 0.093(3) 0.115(3) -0.015(2) 0.011(2) 0.012(2) C9 0.112(3) 0.126(4) 0.103(3) -0.016(3) 0.003(3) 0.036(3) C10 0.185(6) 0.151(5) 0.171(6) -0.068(5) 0.006(5) 0.033(5) C11 0.059(2) 0.096(3) 0.124(3) -0.012(2) -0.001(2) 0.0092(19) C12 0.078(3) 0.179(5) 0.171(5) 0.057(4) -0.010(3) 0.014(3) C13 0.099(3) 0.125(4) 0.167(5) 0.010(4) 0.000(3) 0.019(3) C14 0.129(5) 0.283(10) 0.234(8) 0.139(8) 0.014(5) 0.024(6) C15 0.060(2) 0.079(2) 0.111(3) 0.000(2) 0.0072(19) 0.0008(17) C16 0.088(3) 0.090(3) 0.134(4) -0.012(3) 0.014(3) 0.000(2) C17 0.107(3) 0.089(3) 0.166(5) -0.018(3) 0.010(3) -0.005(3) C18 0.150(5) 0.095(3) 0.230(7) 0.014(4) 0.004(5) 0.002(3) C19 0.077(2) 0.088(3) 0.112(3) -0.004(2) 0.018(2) -0.009(2) C20 0.110(3) 0.108(3) 0.113(3) 0.013(3) 0.005(3) -0.014(3) C21 0.166(6) 0.172(6) 0.186(7) 0.067(6) -0.002(6) -0.030(5) C22 0.131(19) 0.18(3) 0.13(2) 0.052(18) 0.005(15) 0.021(17) C23 0.077(2) 0.0468(15) 0.0625(17) 0.0065(13) 0.0082(15) 0.0081(14) C24 0.081(2) 0.0560(17) 0.0723(19) 0.0006(14) 0.0157(16) 0.0097(15) C25 0.096(3) 0.070(2) 0.075(2) 0.0037(16) 0.0235(19) -0.0014(18) C26 0.119(4) 0.113(3) 0.130(4) 0.010(3) 0.053(3) 0.002(3) C27 0.0698(19) 0.0519(15) 0.0622(17) 0.0026(13) 0.0085(14) 0.0108(14) C28 0.099(3) 0.071(2) 0.068(2) 0.0008(16) -0.0057(18) 0.0110(18) C29 0.102(3) 0.092(3) 0.075(2) -0.0115(19) -0.003(2) 0.006(2) C30 0.095(3) 0.094(3) 0.121(3) -0.004(2) -0.008(2) 0.000(2) C31 0.0650(18) 0.0577(17) 0.0674(18) 0.0035(14) 0.0086(14) 0.0173(14) C32 0.078(2) 0.068(2) 0.093(2) 0.0062(17) 0.0210(19) 0.0103(17) C33 0.075(2) 0.090(3) 0.109(3) -0.003(2) 0.019(2) 0.0065(19) C34 0.123(4) 0.117(4) 0.251(7) 0.007(4) 0.084(5) 0.000(3) C35 0.0676(19) 0.0550(16) 0.0643(17) 0.0117(13) 0.0046(14) 0.0126(14) C36 0.080(2) 0.0647(18) 0.0672(19) 0.0008(15) 0.0015(16) 0.0125(16) C37 0.081(2) 0.078(2) 0.073(2) 0.0075(17) -0.0040(17) 0.0050(18) C38 0.111(3) 0.094(3) 0.068(2) 0.0056(19) -0.007(2) 0.003(2) C39 0.084(2) 0.087(2) 0.0529(17) 0.0004(15) 0.0019(16) 0.0002(18) C40 0.092(3) 0.103(3) 0.069(2) 0.0028(19) -0.0026(19) -0.014(2) C41 0.106(3) 0.116(3) 0.077(2) -0.005(2) -0.014(2) -0.006(3) C42 0.108(4) 0.184(5) 0.113(4) 0.000(3) -0.031(3) -0.035(3) C43 0.079(2) 0.088(2) 0.0607(18) 0.0130(17) 0.0006(16) -0.0085(19) C44 0.093(3) 0.088(3) 0.095(3) 0.014(2) 0.002(2) -0.003(2) C45 0.109(3) 0.113(4) 0.145(4) 0.044(3) -0.016(3) -0.004(3) C46 0.122(7) 0.166(10) 0.136(8) 0.050(7) -0.008(6) 0.001(6) C47 0.070(2) 0.081(2) 0.0682(19) 0.0063(16) 0.0075(16) -0.0045(17) C48 0.082(3) 0.112(3) 0.087(3) 0.000(2) -0.004(2) -0.016(2) C49 0.084(3) 0.101(3) 0.145(4) 0.029(3) -0.020(3) 0.000(2) C50 0.122(4) 0.204(7) 0.204(7) 0.049(5) -0.067(4) -0.033(4) C51 0.075(2) 0.096(2) 0.0583(18) 0.0010(17) 0.0074(16) -0.0021(18) C52 0.086(2) 0.088(2) 0.080(2) 0.0015(19) 0.0148(19) 0.002(2) C53 0.134(4) 0.117(3) 0.099(3) 0.012(3) 0.030(3) 0.039(3) C54 0.118(4) 0.138(4) 0.117(4) 0.008(3) 0.019(3) 0.031(3) C55 0.112(9) 0.078(7) 0.135(10) 0.016(7) 0.013(7) 0.017(6) C56 0.163(10) 0.224(14) 0.224(12) 0.110(10) -0.037(9) -0.022(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.10395(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Eu1 . N1 . 2.379(3) yes Eu1 . N2 . 2.395(3) yes Eu1 . N3 . 2.382(3) yes Eu1 . N4 . 2.387(3) yes Eu1 . N5 . 2.405(3) yes Eu1 . N6 . 2.381(3) yes S1 . C1 . 1.605(4) yes S2 . C2 . 1.598(4) yes S3 . C3 . 1.596(4) yes S4 . C4 . 1.605(3) yes S5 . C5 . 1.605(4) yes S6 . C6 . 1.596(4) yes N1 . C1 . 1.147(4) yes N2 . C2 . 1.151(4) yes N3 . C3 . 1.148(4) yes N4 . C4 . 1.146(4) yes N5 . C5 . 1.154(4) yes N6 . C6 . 1.151(4) yes N7 . C7 . 1.515(4) yes N7 . C11 . 1.525(5) yes N7 . C15 . 1.529(4) yes N7 . C19 . 1.507(5) yes N8 . C23 . 1.525(3) yes N8 . C27 . 1.528(4) yes N8 . C31 . 1.520(4) yes N8 . C35 . 1.517(4) yes N9 . C39 . 1.524(4) yes N9 . C43 . 1.520(4) yes N9 . C47 . 1.517(4) yes N9 . C51 . 1.518(4) yes C7 . C8 . 1.512(5) yes C7 . H71 . 1.006 no C7 . H72 . 0.950 no C8 . C9 . 1.511(6) yes C8 . H81 . 0.957 no C8 . H82 . 0.978 no C9 . C10 . 1.498(7) yes C9 . H91 . 0.974 no C9 . H92 . 0.969 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.516(6) yes C11 . H111 . 0.972 no C11 . H112 . 0.971 no C12 . C13 . 1.441(6) yes C12 . H121 . 1.002 no C12 . H122 . 0.983 no C13 . C14 . 1.476(8) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.506(5) yes C15 . H151 . 0.978 no C15 . H152 . 0.985 no C16 . C17 . 1.514(6) yes C16 . H161 . 0.941 no C16 . H162 . 0.980 no C17 . C18 . 1.523(7) yes C17 . H171 . 0.961 no C17 . H172 . 0.984 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . C20 . 1.499(6) yes C19 . H191 . 0.969 no C19 . H192 . 1.011 no C20 . C21 . 1.499(7) yes C20 . H201 . 0.971 no C20 . H202 . 0.993 no C21 . C22 . 1.447(17) yes C21 . H211 . 1.019 no C21 . H212 . 0.896 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.501(4) yes C23 . H231 . 0.990 no C23 . H232 . 0.968 no C24 . C25 . 1.517(4) yes C24 . H241 . 0.985 no C24 . H242 . 0.961 no C25 . C26 . 1.490(5) yes C25 . H251 . 1.002 no C25 . H252 . 0.961 no C26 . H261 . 0.954 no C26 . H262 . 0.972 no C26 . H263 . 0.982 no C27 . C28 . 1.503(4) yes C27 . H271 . 0.978 no C27 . H272 . 0.976 no C28 . C29 . 1.533(5) yes C28 . H281 . 0.989 no C28 . H282 . 0.985 no C29 . C30 . 1.478(5) yes C29 . H291 . 0.992 no C29 . H292 . 0.992 no C30 . H301 . 0.971 no C30 . H302 . 0.967 no C30 . H303 . 0.953 no C31 . C32 . 1.509(4) yes C31 . H311 . 1.006 no C31 . H312 . 0.944 no C32 . C33 . 1.512(5) yes C32 . H321 . 0.966 no C32 . H322 . 0.937 no C33 . C34 . 1.479(6) yes C33 . H331 . 0.946 no C33 . H332 . 0.966 no C34 . H341 . 0.950 no C34 . H342 . 0.950 no C34 . H343 . 0.950 no C35 . C36 . 1.514(4) yes C35 . H351 . 0.974 no C35 . H352 . 0.979 no C36 . C37 . 1.513(4) yes C36 . H361 . 0.967 no C36 . H362 . 0.968 no C37 . C38 . 1.509(5) yes C37 . H371 . 0.973 no C37 . H372 . 0.989 no C38 . H381 . 0.968 no C38 . H382 . 0.967 no C38 . H383 . 0.958 no C39 . C40 . 1.507(5) yes C39 . H391 . 0.938 no C39 . H392 . 0.994 no C40 . C41 . 1.492(5) yes C40 . H401 . 0.961 no C40 . H402 . 0.990 no C41 . C42 . 1.491(6) yes C41 . H411 . 0.918 no C41 . H412 . 0.954 no C42 . H421 . 0.986 no C42 . H422 . 0.966 no C42 . H423 . 0.988 no C43 . C44 . 1.510(5) yes C43 . H431 . 1.004 no C43 . H432 . 0.996 no C44 . C45 . 1.519(5) yes C44 . H441 . 0.942 no C44 . H442 . 0.977 no C45 . C46 . 1.366(9) yes C45 . H451 . 0.950 no C45 . H452 . 0.950 no C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . C48 . 1.505(5) yes C47 . H471 . 0.956 no C47 . H472 . 1.019 no C48 . C49 . 1.499(5) yes C48 . H481 . 0.997 no C48 . H482 . 0.992 no C49 . C50 . 1.484(7) yes C49 . H491 . 0.977 no C49 . H492 . 0.999 no C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H503 . 0.950 no C51 . C52 . 1.515(5) yes C51 . H511 . 0.952 no C51 . H512 . 0.979 no C52 . C53 . 1.497(5) yes C52 . H521 . 0.980 no C52 . H522 . 0.965 no C53 . C54 . 1.500(6) yes C53 . H531 . 0.986 no C53 . H532 . 0.991 no C54 . H541 . 0.950 no C54 . H542 . 0.950 no C54 . H543 . 0.950 no C55 . H452 . 1.051 no C55 . H551 . 0.950 no C55 . H552 . 0.950 no C55 . H553 . 0.950 no C56 . H561 . 0.950 no C56 . H562 . 0.950 no C56 . H563 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Eu1 . N2 . 87.82(11) yes N1 . Eu1 . N3 . 88.41(11) yes N2 . Eu1 . N3 . 89.75(12) yes N1 . Eu1 . N4 . 174.87(11) yes N2 . Eu1 . N4 . 89.62(11) yes N3 . Eu1 . N4 . 87.14(12) yes N1 . Eu1 . N5 . 94.75(11) yes N2 . Eu1 . N5 . 177.17(11) yes N3 . Eu1 . N5 . 91.50(11) yes N4 . Eu1 . N5 . 87.91(11) yes N1 . Eu1 . N6 . 93.84(11) yes N2 . Eu1 . N6 . 89.60(12) yes N3 . Eu1 . N6 . 177.63(11) yes N4 . Eu1 . N6 . 90.58(11) yes N5 . Eu1 . N6 . 89.05(11) yes Eu1 . N1 . C1 . 176.2(3) yes Eu1 . N2 . C2 . 174.8(3) yes Eu1 . N3 . C3 . 171.8(3) yes Eu1 . N4 . C4 . 172.5(3) yes Eu1 . N5 . C5 . 174.4(3) yes Eu1 . N6 . C6 . 172.0(3) yes C7 . N7 . C11 . 110.6(3) yes C7 . N7 . C15 . 106.4(2) yes C11 . N7 . C15 . 109.6(3) yes C7 . N7 . C19 . 111.4(3) yes C11 . N7 . C19 . 107.9(3) yes C15 . N7 . C19 . 110.9(3) yes C23 . N8 . C27 . 110.6(2) yes C23 . N8 . C31 . 106.0(2) yes C27 . N8 . C31 . 111.3(2) yes C23 . N8 . C35 . 111.4(2) yes C27 . N8 . C35 . 106.6(2) yes C31 . N8 . C35 . 111.0(2) yes C39 . N9 . C43 . 110.6(2) yes C39 . N9 . C47 . 106.7(2) yes C43 . N9 . C47 . 111.8(3) yes C39 . N9 . C51 . 110.7(3) yes C43 . N9 . C51 . 106.2(2) yes C47 . N9 . C51 . 110.9(2) yes S1 . C1 . N1 . 179.5(3) yes S2 . C2 . N2 . 179.3(3) yes S3 . C3 . N3 . 179.2(4) yes S4 . C4 . N4 . 178.8(3) yes S5 . C5 . N5 . 179.0(3) yes S6 . C6 . N6 . 179.6(4) yes N7 . C7 . C8 . 115.1(3) yes N7 . C7 . H71 . 101.1 no C8 . C7 . H71 . 109.5 no N7 . C7 . H72 . 111.2 no C8 . C7 . H72 . 108.1 no H71 . C7 . H72 . 111.8 no C7 . C8 . C9 . 109.4(3) yes C7 . C8 . H81 . 111.8 no C9 . C8 . H81 . 110.7 no C7 . C8 . H82 . 107.7 no C9 . C8 . H82 . 109.2 no H81 . C8 . H82 . 108.0 no C8 . C9 . C10 . 112.3(4) yes C8 . C9 . H91 . 112.0 no C10 . C9 . H91 . 104.9 no C8 . C9 . H92 . 110.5 no C10 . C9 . H92 . 108.0 no H91 . C9 . H92 . 108.8 no C9 . C10 . H101 . 109.1 no C9 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.9 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N7 . C11 . C12 . 115.0(3) yes N7 . C11 . H111 . 107.5 no C12 . C11 . H111 . 102.8 no N7 . C11 . H112 . 105.3 no C12 . C11 . H112 . 111.6 no H111 . C11 . H112 . 114.9 no C11 . C12 . C13 . 114.9(4) yes C11 . C12 . H121 . 101.0 no C13 . C12 . H121 . 106.7 no C11 . C12 . H122 . 117.5 no C13 . C12 . H122 . 103.9 no H121 . C12 . H122 . 112.6 no C12 . C13 . C14 . 115.0(5) yes C12 . C13 . H131 . 106.9 no C14 . C13 . H131 . 108.1 no C12 . C13 . H132 . 109.0 no C14 . C13 . H132 . 108.3 no H131 . C13 . H132 . 109.5 no C13 . C14 . H141 . 109.1 no C13 . C14 . H142 . 108.9 no H141 . C14 . H142 . 109.5 no C13 . C14 . H143 . 110.4 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N7 . C15 . C16 . 115.8(3) yes N7 . C15 . H151 . 106.3 no C16 . C15 . H151 . 108.3 no N7 . C15 . H152 . 109.5 no C16 . C15 . H152 . 109.8 no H151 . C15 . H152 . 106.8 no C15 . C16 . C17 . 111.5(4) yes C15 . C16 . H161 . 108.7 no C17 . C16 . H161 . 113.0 no C15 . C16 . H162 . 109.1 no C17 . C16 . H162 . 107.9 no H161 . C16 . H162 . 106.4 no C16 . C17 . C18 . 112.8(5) yes C16 . C17 . H171 . 110.0 no C18 . C17 . H171 . 105.3 no C16 . C17 . H172 . 107.9 no C18 . C17 . H172 . 112.1 no H171 . C17 . H172 . 108.8 no C17 . C18 . H181 . 109.6 no C17 . C18 . H182 . 110.3 no H181 . C18 . H182 . 109.5 no C17 . C18 . H183 . 108.6 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no N7 . C19 . C20 . 115.6(3) yes N7 . C19 . H191 . 109.7 no C20 . C19 . H191 . 105.2 no N7 . C19 . H192 . 105.6 no C20 . C19 . H192 . 110.4 no H191 . C19 . H192 . 110.3 no C19 . C20 . C21 . 110.5(5) yes C19 . C20 . H201 . 108.7 no C21 . C20 . H201 . 110.8 no C19 . C20 . H202 . 108.8 no C21 . C20 . H202 . 107.7 no H201 . C20 . H202 . 110.4 no C20 . C21 . C22 . 117.6(12) yes C20 . C21 . H211 . 103.0 no C22 . C21 . H211 . 59.7 no C20 . C21 . H212 . 108.9 no C22 . C21 . H212 . 133.4 no H211 . C21 . H212 . 108.1 no C21 . C22 . H221 . 111.3 no C21 . C22 . H222 . 109.2 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 107.9 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no N8 . C23 . C24 . 116.6(2) yes N8 . C23 . H231 . 107.2 no C24 . C23 . H231 . 99.8 no N8 . C23 . H232 . 111.2 no C24 . C23 . H232 . 106.2 no H231 . C23 . H232 . 115.6 no C23 . C24 . C25 . 109.2(3) yes C23 . C24 . H241 . 106.6 no C25 . C24 . H241 . 105.4 no C23 . C24 . H242 . 110.2 no C25 . C24 . H242 . 110.1 no H241 . C24 . H242 . 115.0 no C24 . C25 . C26 . 114.3(3) yes C24 . C25 . H251 . 109.1 no C26 . C25 . H251 . 106.6 no C24 . C25 . H252 . 104.7 no C26 . C25 . H252 . 106.0 no H251 . C25 . H252 . 116.5 no C25 . C26 . H261 . 112.1 no C25 . C26 . H262 . 104.2 no H261 . C26 . H262 . 111.1 no C25 . C26 . H263 . 106.7 no H261 . C26 . H263 . 110.8 no H262 . C26 . H263 . 111.7 no N8 . C27 . C28 . 115.9(2) yes N8 . C27 . H271 . 106.0 no C28 . C27 . H271 . 110.3 no N8 . C27 . H272 . 103.5 no C28 . C27 . H272 . 111.0 no H271 . C27 . H272 . 109.8 no C27 . C28 . C29 . 110.9(3) yes C27 . C28 . H281 . 112.3 no C29 . C28 . H281 . 106.0 no C27 . C28 . H282 . 114.6 no C29 . C28 . H282 . 101.1 no H281 . C28 . H282 . 111.1 no C28 . C29 . C30 . 115.7(3) yes C28 . C29 . H291 . 110.3 no C30 . C29 . H291 . 114.4 no C28 . C29 . H292 . 97.9 no C30 . C29 . H292 . 109.9 no H291 . C29 . H292 . 107.1 no C29 . C30 . H301 . 111.3 no C29 . C30 . H302 . 108.7 no H301 . C30 . H302 . 110.0 no C29 . C30 . H303 . 108.0 no H301 . C30 . H303 . 110.1 no H302 . C30 . H303 . 108.7 no N8 . C31 . C32 . 115.9(2) yes N8 . C31 . H311 . 106.5 no C32 . C31 . H311 . 106.9 no N8 . C31 . H312 . 105.5 no C32 . C31 . H312 . 109.6 no H311 . C31 . H312 . 112.6 no C31 . C32 . C33 . 110.5(3) yes C31 . C32 . H321 . 108.9 no C33 . C32 . H321 . 108.5 no C31 . C32 . H322 . 110.7 no C33 . C32 . H322 . 107.5 no H321 . C32 . H322 . 110.6 no C32 . C33 . C34 . 113.9(4) yes C32 . C33 . H331 . 112.6 no C34 . C33 . H331 . 110.0 no C32 . C33 . H332 . 107.1 no C34 . C33 . H332 . 104.7 no H331 . C33 . H332 . 108.1 no C33 . C34 . H341 . 109.3 no C33 . C34 . H342 . 108.6 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 110.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no N8 . C35 . C36 . 116.1(2) yes N8 . C35 . H351 . 106.4 no C36 . C35 . H351 . 110.3 no N8 . C35 . H352 . 107.3 no C36 . C35 . H352 . 104.9 no H351 . C35 . H352 . 111.9 no C35 . C36 . C37 . 110.7(3) yes C35 . C36 . H361 . 110.3 no C37 . C36 . H361 . 110.5 no C35 . C36 . H362 . 111.2 no C37 . C36 . H362 . 112.3 no H361 . C36 . H362 . 101.5 no C36 . C37 . C38 . 112.1(3) yes C36 . C37 . H371 . 103.3 no C38 . C37 . H371 . 111.6 no C36 . C37 . H372 . 110.7 no C38 . C37 . H372 . 107.4 no H371 . C37 . H372 . 111.8 no C37 . C38 . H381 . 106.9 no C37 . C38 . H382 . 111.5 no H381 . C38 . H382 . 110.0 no C37 . C38 . H383 . 111.4 no H381 . C38 . H383 . 107.5 no H382 . C38 . H383 . 109.4 no N9 . C39 . C40 . 115.7(3) yes N9 . C39 . H391 . 107.0 no C40 . C39 . H391 . 112.6 no N9 . C39 . H392 . 109.0 no C40 . C39 . H392 . 105.0 no H391 . C39 . H392 . 107.1 no C39 . C40 . C41 . 112.3(3) yes C39 . C40 . H401 . 108.7 no C41 . C40 . H401 . 111.3 no C39 . C40 . H402 . 106.4 no C41 . C40 . H402 . 112.5 no H401 . C40 . H402 . 105.2 no C40 . C41 . C42 . 113.6(4) yes C40 . C41 . H411 . 108.2 no C42 . C41 . H411 . 106.7 no C40 . C41 . H412 . 112.3 no C42 . C41 . H412 . 108.1 no H411 . C41 . H412 . 107.7 no C41 . C42 . H421 . 111.9 no C41 . C42 . H422 . 107.2 no H421 . C42 . H422 . 111.9 no C41 . C42 . H423 . 105.2 no H421 . C42 . H423 . 109.1 no H422 . C42 . H423 . 111.3 no N9 . C43 . C44 . 116.5(3) yes N9 . C43 . H431 . 109.5 no C44 . C43 . H431 . 106.6 no N9 . C43 . H432 . 103.4 no C44 . C43 . H432 . 106.8 no H431 . C43 . H432 . 114.2 no C43 . C44 . C45 . 110.0(4) yes C43 . C44 . H441 . 109.7 no C45 . C44 . H441 . 112.7 no C43 . C44 . H442 . 106.6 no C45 . C44 . H442 . 110.0 no H441 . C44 . H442 . 107.6 no C44 . C45 . C46 . 117.4(5) yes C44 . C45 . H451 . 105.6 no C46 . C45 . H451 . 95.8 no C44 . C45 . H452 . 105.2 no C46 . C45 . H452 . 121.8 no H451 . C45 . H452 . 109.5 no C45 . C46 . H461 . 110.2 no C45 . C46 . H462 . 108.2 no H461 . C46 . H462 . 109.5 no C45 . C46 . H463 . 110.0 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no N9 . C47 . C48 . 115.3(3) yes N9 . C47 . H471 . 102.3 no C48 . C47 . H471 . 107.6 no N9 . C47 . H472 . 109.0 no C48 . C47 . H472 . 110.8 no H471 . C47 . H472 . 111.5 no C47 . C48 . C49 . 111.7(3) yes C47 . C48 . H481 . 102.9 no C49 . C48 . H481 . 108.8 no C47 . C48 . H482 . 112.2 no C49 . C48 . H482 . 106.6 no H481 . C48 . H482 . 114.8 no C48 . C49 . C50 . 113.8(4) yes C48 . C49 . H491 . 106.8 no C50 . C49 . H491 . 110.8 no C48 . C49 . H492 . 106.6 no C50 . C49 . H492 . 108.6 no H491 . C49 . H492 . 110.1 no C49 . C50 . H501 . 109.8 no C49 . C50 . H502 . 108.2 no H501 . C50 . H502 . 109.5 no C49 . C50 . H503 . 110.3 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no N9 . C51 . C52 . 116.5(3) yes N9 . C51 . H511 . 111.6 no C52 . C51 . H511 . 108.4 no N9 . C51 . H512 . 104.2 no C52 . C51 . H512 . 106.0 no H511 . C51 . H512 . 109.7 no C51 . C52 . C53 . 110.8(3) yes C51 . C52 . H521 . 101.6 no C53 . C52 . H521 . 107.9 no C51 . C52 . H522 . 116.8 no C53 . C52 . H522 . 114.2 no H521 . C52 . H522 . 104.1 no C52 . C53 . C54 . 113.6(4) yes C52 . C53 . H531 . 110.0 no C54 . C53 . H531 . 109.1 no C52 . C53 . H532 . 107.6 no C54 . C53 . H532 . 106.3 no H531 . C53 . H532 . 110.2 no C53 . C54 . H541 . 109.9 no C53 . C54 . H542 . 109.2 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 109.4 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no C45 . C55 . H452 . 44.5 no C45 . C55 . H551 . 108.3 no H452 . C55 . H551 . 108.9 no C45 . C55 . H552 . 109.4 no H452 . C55 . H552 . 139.4 no H551 . C55 . H552 . 109.5 no C45 . C55 . H553 . 110.6 no H452 . C55 . H553 . 68.9 no H551 . C55 . H553 . 109.5 no H552 . C55 . H553 . 109.5 no C21 . C56 . H561 . 109.3 no C21 . C56 . H562 . 109.3 no H561 . C56 . H562 . 109.5 no C21 . C56 . H563 . 109.7 no H561 . C56 . H563 . 109.5 no H562 . C56 . H563 . 109.5 no C55 . H452 . C45 . 84.6 no _database_code_depnum_ccdc_archive 'CCDC 933720' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C54H108GdN9S6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C54 H108 Gd1 N9 S6' _chemical_formula_moiety 'C54 H108 Gd1 N9 S6' _chemical_compound_source ? _chemical_formula_weight 1233.16 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.2313(8) _cell_length_b 12.7903(8) _cell_length_c 22.5105(14) _cell_angle_alpha 90.806(4) _cell_angle_beta 91.127(4) _cell_angle_gamma 96.777(4) _cell_volume 3495.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9951 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.54 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.23 _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1310 _exptl_absorpt_coefficient_mu 1.165 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6305 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 50214 _diffrn_reflns_av_R_equivalents 0.077 _diffrn_reflns_theta_min 1.604 _diffrn_reflns_theta_max 26.916 _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.032 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 14635 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _refine_diff_density_min -1.14 _refine_diff_density_max 1.12 _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 10563 _refine_ls_number_restraints 0 _refine_ls_number_parameters 632 _oxford_refine_ls_R_factor_ref 0.0520 _refine_ls_wR_factor_ref 0.0504 _refine_ls_goodness_of_fit_ref 0.9786 _refine_ls_shift/su_max 0.0014223 _refine_ls_shift/su_mean 0.0000206 # The values computed from all data _oxford_reflns_number_all 14635 _refine_ls_R_factor_all 0.0832 _refine_ls_wR_factor_all 0.0768 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10563 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_gt 0.0504 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.696 0.824 0.679 0.317 0.175 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Gd1 Gd 0.94397(2) 0.300491(18) 0.251952(10) 0.0281 1.0000 Uani . . . . . . S1 S 1.15582(12) 0.06954(10) 0.38729(6) 0.0441 1.0000 Uani . . . . . . S2 S 0.66393(14) -0.03371(11) 0.25572(7) 0.0514 1.0000 Uani . . . . . . S3 S 0.73560(13) 0.45032(12) 0.42537(6) 0.0478 1.0000 Uani . . . . . . S4 S 0.69433(13) 0.47887(15) 0.10802(8) 0.0651 1.0000 Uani . . . . . . S5 S 1.20702(14) 0.64510(13) 0.25653(8) 0.0619 1.0000 Uani . . . . . . S6 S 1.18101(12) 0.16659(12) 0.08595(6) 0.0445 1.0000 Uani . . . . . . N1 N 1.0488(4) 0.2055(3) 0.31857(19) 0.0451 1.0000 Uani . . . . . . N2 N 0.8118(4) 0.1466(3) 0.24797(19) 0.0430 1.0000 Uani . . . . . . N3 N 0.8498(4) 0.3640(3) 0.33505(19) 0.0416 1.0000 Uani . . . . . . N4 N 0.8240(4) 0.3817(4) 0.18851(19) 0.0411 1.0000 Uani . . . . . . N5 N 1.0759(4) 0.4524(3) 0.25988(19) 0.0422 1.0000 Uani . . . . . . N6 N 1.0447(4) 0.2352(3) 0.17200(19) 0.0419 1.0000 Uani . . . . . . N7 N 1.0630(3) -0.2411(3) 0.46477(15) 0.0274 1.0000 Uani . . . . . . N8 N 0.4688(3) 0.3266(3) 0.24538(17) 0.0321 1.0000 Uani . . . . . . N9 N 0.8924(3) 0.8568(3) 0.10939(16) 0.0304 1.0000 Uani . . . . . . C1 C 1.0943(4) 0.1481(3) 0.3469(2) 0.0339 1.0000 Uani . . . . . . C2 C 0.7503(4) 0.0716(4) 0.25137(19) 0.0332 1.0000 Uani . . . . . . C3 C 0.8019(4) 0.4003(4) 0.3729(2) 0.0334 1.0000 Uani . . . . . . C4 C 0.7703(4) 0.4233(4) 0.1547(2) 0.0412 1.0000 Uani . . . . . . C5 C 1.1312(4) 0.5331(4) 0.2584(2) 0.0365 1.0000 Uani . . . . . . C6 C 1.1010(4) 0.2068(4) 0.1359(2) 0.0314 1.0000 Uani . . . . . . C7 C 1.1726(4) -0.2728(3) 0.4437(2) 0.0297 1.0000 Uani . . . . . . C8 C 1.2461(4) -0.1884(4) 0.4122(2) 0.0344 1.0000 Uani . . . . . . C9 C 1.3550(4) -0.2295(4) 0.3974(2) 0.0347 1.0000 Uani . . . . . . C10 C 1.4360(5) -0.1473(5) 0.3689(3) 0.0570 1.0000 Uani . . . . . . C11 C 1.0799(4) -0.1413(3) 0.50308(18) 0.0286 1.0000 Uani . . . . . . C12 C 1.1530(5) -0.1455(4) 0.5574(2) 0.0374 1.0000 Uani . . . . . . C13 C 1.1743(5) -0.0377(4) 0.5894(2) 0.0427 1.0000 Uani . . . . . . C14 C 1.2429(5) 0.0468(4) 0.5548(2) 0.0454 1.0000 Uani . . . . . . C15 C 1.0097(4) -0.3333(3) 0.49990(18) 0.0276 1.0000 Uani . . . . . . C16 C 0.8983(4) -0.3250(3) 0.5249(2) 0.0321 1.0000 Uani . . . . . . C17 C 0.8667(4) -0.4183(4) 0.5650(2) 0.0348 1.0000 Uani . . . . . . C18 C 0.7561(5) -0.4155(5) 0.5937(3) 0.0598 1.0000 Uani . . . . . . C19 C 0.9899(4) -0.2182(3) 0.41213(18) 0.0277 1.0000 Uani . . . . . . C20 C 0.9640(4) -0.3059(3) 0.36667(19) 0.0313 1.0000 Uani . . . . . . C21 C 0.8785(4) -0.2763(4) 0.3211(2) 0.0318 1.0000 Uani . . . . . . C22 C 0.8596(4) -0.3571(4) 0.2708(2) 0.0379 1.0000 Uani . . . . . . C23 C 0.5356(4) 0.2640(4) 0.2052(2) 0.0331 1.0000 Uani . . . . . . C24 C 0.4760(4) 0.1615(4) 0.1801(2) 0.0378 1.0000 Uani . . . . . . C25 C 0.5427(5) 0.1206(4) 0.1301(2) 0.0432 1.0000 Uani . . . . . . C26 C 0.4844(6) 0.0200(5) 0.1014(3) 0.0613 1.0000 Uani . . . . . . C27 C 0.3686(4) 0.3579(4) 0.2105(2) 0.0414 1.0000 Uani . . . . . . C28 C 0.3948(5) 0.4061(6) 0.1497(3) 0.0696 1.0000 Uani . . . . . . C29 C 0.3022(5) 0.4556(5) 0.1225(3) 0.0550 1.0000 Uani . . . . . . C30 C 0.3238(7) 0.4898(7) 0.0603(4) 0.0916 1.0000 Uani . . . . . . C31 C 0.5438(4) 0.4243(3) 0.2653(2) 0.0337 1.0000 Uani . . . . . . C32 C 0.4945(4) 0.4962(4) 0.3096(2) 0.0393 1.0000 Uani . . . . . . C33 C 0.5649(5) 0.6034(4) 0.3142(2) 0.0426 1.0000 Uani . . . . . . C34 C 0.5583(5) 0.6693(4) 0.2594(3) 0.0571 1.0000 Uani . . . . . . C35 C 0.4266(4) 0.2623(4) 0.2974(2) 0.0394 1.0000 Uani . . . . . . C36 C 0.5128(5) 0.2246(4) 0.3370(2) 0.0492 1.0000 Uani . . . . . . C37 C 0.4567(7) 0.1714(6) 0.3915(3) 0.0797 1.0000 Uani . . . . . . C38 C 0.5332(8) 0.1413(8) 0.4340(5) 0.1088 1.0000 Uani . . . . . . C39 C 0.9530(4) 0.7793(4) 0.07451(19) 0.0346 1.0000 Uani . . . . . . C40 C 0.9607(4) 0.6746(4) 0.1029(2) 0.0395 1.0000 Uani . . . . . . C41 C 1.0319(5) 0.6088(4) 0.0669(3) 0.0498 1.0000 Uani . . . . . . C42 C 1.0290(5) 0.4979(5) 0.0882(3) 0.0543 1.0000 Uani . . . . . . C43 C 0.7726(4) 0.8114(4) 0.11952(19) 0.0317 1.0000 Uani . . . . . . C44 C 0.7001(4) 0.7954(4) 0.0642(2) 0.0406 1.0000 Uani . . . . . . C45 C 0.5841(4) 0.7510(4) 0.0799(3) 0.0451 1.0000 Uani . . . . . . C46 C 0.5055(5) 0.7459(5) 0.0272(3) 0.0610 1.0000 Uani . . . . . . C47 C 0.9463(4) 0.8786(4) 0.17067(18) 0.0322 1.0000 Uani . . . . . . C48 C 1.0687(4) 0.9102(4) 0.1715(2) 0.0390 1.0000 Uani . . . . . . C49 C 1.1133(4) 0.9388(4) 0.2342(2) 0.0437 1.0000 Uani . . . . . . C50 C 1.2360(5) 0.9709(6) 0.2350(3) 0.0631 1.0000 Uani . . . . . . C51 C 0.8993(4) 0.9570(4) 0.07364(19) 0.0332 1.0000 Uani . . . . . . C52 C 0.8389(5) 1.0441(4) 0.0986(2) 0.0408 1.0000 Uani . . . . . . C53 C 0.8411(5) 1.1379(4) 0.0566(2) 0.0445 1.0000 Uani . . . . . . C54 C 0.7714(5) 1.1154(5) 0.0011(3) 0.0525 1.0000 Uani . . . . . . H71 H 1.2125 -0.2910 0.4779 0.0350(15) 1.0000 Uiso R . . . . . H72 H 1.1586 -0.3325 0.4179 0.0350(15) 1.0000 Uiso R . . . . . H81 H 1.2093 -0.1705 0.3769 0.0374(15) 1.0000 Uiso R . . . . . H82 H 1.2615 -0.1276 0.4370 0.0374(15) 1.0000 Uiso R . . . . . H91 H 1.3388 -0.2865 0.3699 0.0412(15) 1.0000 Uiso R . . . . . H92 H 1.3867 -0.2540 0.4327 0.0412(15) 1.0000 Uiso R . . . . . H101 H 1.4531 -0.0901 0.3962 0.0700(15) 1.0000 Uiso R . . . . . H102 H 1.4052 -0.1226 0.3334 0.0700(15) 1.0000 Uiso R . . . . . H103 H 1.5012 -0.1775 0.3600 0.0700(15) 1.0000 Uiso R . . . . . H111 H 1.0102 -0.1272 0.5170 0.0340(15) 1.0000 Uiso R . . . . . H112 H 1.1099 -0.0849 0.4791 0.0340(15) 1.0000 Uiso R . . . . . H121 H 1.1211 -0.1972 0.5838 0.0404(15) 1.0000 Uiso R . . . . . H122 H 1.2218 -0.1641 0.5446 0.0404(15) 1.0000 Uiso R . . . . . H131 H 1.2113 -0.0460 0.6263 0.0491(15) 1.0000 Uiso R . . . . . H132 H 1.1046 -0.0148 0.5966 0.0491(15) 1.0000 Uiso R . . . . . H141 H 1.2516 0.1112 0.5768 0.0486(15) 1.0000 Uiso R . . . . . H142 H 1.3132 0.0251 0.5477 0.0486(15) 1.0000 Uiso R . . . . . H143 H 1.2065 0.0563 0.5180 0.0486(15) 1.0000 Uiso R . . . . . H151 H 1.0583 -0.3428 0.5323 0.0310(15) 1.0000 Uiso R . . . . . H152 H 1.0030 -0.3939 0.4746 0.0310(15) 1.0000 Uiso R . . . . . H161 H 0.9006 -0.2615 0.5475 0.0332(15) 1.0000 Uiso R . . . . . H162 H 0.8455 -0.3248 0.4934 0.0332(15) 1.0000 Uiso R . . . . . H171 H 0.8645 -0.4810 0.5416 0.0376(15) 1.0000 Uiso R . . . . . H172 H 0.9213 -0.4184 0.5956 0.0376(15) 1.0000 Uiso R . . . . . H181 H 0.7576 -0.3533 0.6174 0.0841(15) 1.0000 Uiso R . . . . . H182 H 0.7007 -0.4159 0.5634 0.0841(15) 1.0000 Uiso R . . . . . H183 H 0.7404 -0.4754 0.6178 0.0841(15) 1.0000 Uiso R . . . . . H191 H 1.0262 -0.1590 0.3924 0.0303(15) 1.0000 Uiso R . . . . . H192 H 0.9217 -0.2012 0.4267 0.0303(15) 1.0000 Uiso R . . . . . H201 H 1.0297 -0.3172 0.3469 0.0369(15) 1.0000 Uiso R . . . . . H202 H 0.9358 -0.3685 0.3862 0.0369(15) 1.0000 Uiso R . . . . . H211 H 0.8108 -0.2721 0.3405 0.0349(15) 1.0000 Uiso R . . . . . H212 H 0.9038 -0.2097 0.3050 0.0349(15) 1.0000 Uiso R . . . . . H221 H 0.8341 -0.4237 0.2867 0.0408(15) 1.0000 Uiso R . . . . . H222 H 0.8064 -0.3372 0.2432 0.0408(15) 1.0000 Uiso R . . . . . H223 H 0.9271 -0.3613 0.2513 0.0408(15) 1.0000 Uiso R . . . . . H231 H 0.5995 0.2486 0.2265 0.0377(15) 1.0000 Uiso R . . . . . H232 H 0.5568 0.3070 0.1724 0.0377(15) 1.0000 Uiso R . . . . . H241 H 0.4050 0.1724 0.1653 0.0437(15) 1.0000 Uiso R . . . . . H242 H 0.4688 0.1110 0.2107 0.0437(15) 1.0000 Uiso R . . . . . H251 H 0.5515 0.1724 0.1002 0.0471(15) 1.0000 Uiso R . . . . . H252 H 0.6130 0.1085 0.1454 0.0471(15) 1.0000 Uiso R . . . . . H261 H 0.5272 -0.0034 0.0702 0.0719(15) 1.0000 Uiso R . . . . . H262 H 0.4756 -0.0320 0.1311 0.0719(15) 1.0000 Uiso R . . . . . H263 H 0.4141 0.0319 0.0860 0.0719(15) 1.0000 Uiso R . . . . . H271 H 0.3347 0.4067 0.2340 0.0458(15) 1.0000 Uiso R . . . . . H272 H 0.3187 0.2958 0.2040 0.0458(15) 1.0000 Uiso R . . . . . H281 H 0.4564 0.4584 0.1548 0.0932(15) 1.0000 Uiso R . . . . . H282 H 0.4129 0.3527 0.1231 0.0932(15) 1.0000 Uiso R . . . . . H291 H 0.2913 0.5158 0.1458 0.0636(15) 1.0000 Uiso R . . . . . H292 H 0.2376 0.4065 0.1228 0.0636(15) 1.0000 Uiso R . . . . . H301 H 0.2626 0.5211 0.0451 0.1094(15) 1.0000 Uiso R . . . . . H302 H 0.3880 0.5393 0.0595 0.1094(15) 1.0000 Uiso R . . . . . H303 H 0.3343 0.4300 0.0365 0.1094(15) 1.0000 Uiso R . . . . . H311 H 0.5634 0.4643 0.2310 0.0383(15) 1.0000 Uiso R . . . . . H312 H 0.6081 0.4024 0.2832 0.0383(15) 1.0000 Uiso R . . . . . H321 H 0.4222 0.5061 0.2964 0.0448(15) 1.0000 Uiso R . . . . . H322 H 0.4913 0.4642 0.3475 0.0448(15) 1.0000 Uiso R . . . . . H331 H 0.5394 0.6419 0.3465 0.0482(15) 1.0000 Uiso R . . . . . H332 H 0.6389 0.5913 0.3220 0.0482(15) 1.0000 Uiso R . . . . . H341 H 0.6040 0.7341 0.2657 0.0710(15) 1.0000 Uiso R . . . . . H342 H 0.5844 0.6323 0.2267 0.0710(15) 1.0000 Uiso R . . . . . H343 H 0.4849 0.6829 0.2511 0.0710(15) 1.0000 Uiso R . . . . . H351 H 0.3847 0.3044 0.3209 0.0426(15) 1.0000 Uiso R . . . . . H352 H 0.3803 0.2026 0.2822 0.0426(15) 1.0000 Uiso R . . . . . H361 H 0.5641 0.2821 0.3504 0.0575(15) 1.0000 Uiso R . . . . . H362 H 0.5504 0.1752 0.3161 0.0575(15) 1.0000 Uiso R . . . . . H371 H 0.4138 0.2189 0.4104 0.0941(15) 1.0000 Uiso R . . . . . H372 H 0.4103 0.1100 0.3787 0.0941(15) 1.0000 Uiso R . . . . . H381 H 0.5014 0.1082 0.4681 0.1298(15) 1.0000 Uiso R . . . . . H382 H 0.5758 0.0946 0.4142 0.1298(15) 1.0000 Uiso R . . . . . H383 H 0.5792 0.2035 0.4458 0.1298(15) 1.0000 Uiso R . . . . . H391 H 0.9177 0.7671 0.0367 0.0391(15) 1.0000 Uiso R . . . . . H392 H 1.0264 0.8110 0.0696 0.0391(15) 1.0000 Uiso R . . . . . H401 H 0.9928 0.6849 0.1417 0.0422(15) 1.0000 Uiso R . . . . . H402 H 0.8884 0.6389 0.1056 0.0422(15) 1.0000 Uiso R . . . . . H411 H 1.0036 0.6055 0.0272 0.0561(15) 1.0000 Uiso R . . . . . H412 H 1.1056 0.6422 0.0675 0.0561(15) 1.0000 Uiso R . . . . . H421 H 1.0577 0.5002 0.1277 0.0645(15) 1.0000 Uiso R . . . . . H422 H 0.9557 0.4635 0.0874 0.0645(15) 1.0000 Uiso R . . . . . H423 H 1.0733 0.4602 0.0634 0.0645(15) 1.0000 Uiso R . . . . . H431 H 0.7403 0.8584 0.1451 0.0347(15) 1.0000 Uiso R . . . . . H432 H 0.7724 0.7451 0.1380 0.0347(15) 1.0000 Uiso R . . . . . H441 H 0.6990 0.8609 0.0450 0.0483(15) 1.0000 Uiso R . . . . . H442 H 0.7300 0.7473 0.0383 0.0483(15) 1.0000 Uiso R . . . . . H451 H 0.5845 0.6819 0.0948 0.0502(15) 1.0000 Uiso R . . . . . H452 H 0.5580 0.7949 0.1096 0.0502(15) 1.0000 Uiso R . . . . . H461 H 0.4330 0.7184 0.0376 0.0726(15) 1.0000 Uiso R . . . . . H462 H 0.5049 0.8149 0.0122 0.0726(15) 1.0000 Uiso R . . . . . H463 H 0.5314 0.7019 -0.0025 0.0726(15) 1.0000 Uiso R . . . . . H471 H 0.9329 0.8157 0.1927 0.0363(15) 1.0000 Uiso R . . . . . H472 H 0.9126 0.9330 0.1897 0.0363(15) 1.0000 Uiso R . . . . . H481 H 1.1040 0.8538 0.1558 0.0444(15) 1.0000 Uiso R . . . . . H482 H 1.0836 0.9701 0.1472 0.0444(15) 1.0000 Uiso R . . . . . H491 H 1.0986 0.8788 0.2585 0.0508(15) 1.0000 Uiso R . . . . . H492 H 1.0779 0.9950 0.2498 0.0508(15) 1.0000 Uiso R . . . . . H501 H 1.2718 0.9148 0.2195 0.0727(15) 1.0000 Uiso R . . . . . H502 H 1.2510 1.0310 0.2109 0.0727(15) 1.0000 Uiso R . . . . . H503 H 1.2623 0.9875 0.2744 0.0727(15) 1.0000 Uiso R . . . . . H511 H 0.9747 0.9842 0.0707 0.0371(15) 1.0000 Uiso R . . . . . H512 H 0.8694 0.9388 0.0351 0.0371(15) 1.0000 Uiso R . . . . . H521 H 0.8716 1.0671 0.1359 0.0476(15) 1.0000 Uiso R . . . . . H522 H 0.7641 1.0170 0.1039 0.0476(15) 1.0000 Uiso R . . . . . H531 H 0.8160 1.1958 0.0770 0.0488(15) 1.0000 Uiso R . . . . . H532 H 0.9154 1.1562 0.0455 0.0488(15) 1.0000 Uiso R . . . . . H541 H 0.6967 1.0976 0.0117 0.0616(15) 1.0000 Uiso R . . . . . H542 H 0.7961 1.0579 -0.0198 0.0616(15) 1.0000 Uiso R . . . . . H543 H 0.7771 1.1755 -0.0235 0.0616(15) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.03193(12) 0.02621(11) 0.02629(11) 0.00170(7) -0.00022(8) 0.00415(8) S1 0.0570(9) 0.0398(7) 0.0390(7) 0.0067(5) -0.0028(6) 0.0195(6) S2 0.0610(10) 0.0401(7) 0.0480(8) 0.0016(6) 0.0009(7) -0.0149(6) S3 0.0572(9) 0.0558(8) 0.0343(6) -0.0056(6) 0.0012(6) 0.0231(7) S4 0.0361(8) 0.0840(12) 0.0748(11) 0.0457(9) -0.0100(7) 0.0022(8) S5 0.0521(9) 0.0487(8) 0.0796(11) -0.0208(8) 0.0181(8) -0.0161(7) S6 0.0389(7) 0.0579(8) 0.0358(6) -0.0083(6) 0.0061(5) 0.0022(6) N1 0.059(3) 0.038(2) 0.040(2) 0.0049(19) -0.005(2) 0.014(2) N2 0.052(3) 0.036(2) 0.039(2) 0.0023(18) 0.006(2) -0.008(2) N3 0.048(3) 0.038(2) 0.041(2) 0.0038(19) 0.008(2) 0.011(2) N4 0.035(2) 0.051(3) 0.039(2) 0.0144(19) -0.0074(18) 0.0077(19) N5 0.047(3) 0.033(2) 0.044(2) -0.0034(18) -0.006(2) 0.000(2) N6 0.045(3) 0.042(2) 0.040(2) -0.0044(19) 0.007(2) 0.006(2) N7 0.033(2) 0.0252(17) 0.0258(17) 0.0022(14) 0.0025(15) 0.0099(15) N8 0.022(2) 0.032(2) 0.042(2) -0.0064(16) 0.0031(16) -0.0005(15) N9 0.030(2) 0.035(2) 0.0244(17) -0.0022(15) 0.0020(15) -0.0024(16) C1 0.046(3) 0.024(2) 0.033(2) 0.0012(18) 0.001(2) 0.005(2) C2 0.039(3) 0.035(2) 0.026(2) -0.0009(18) 0.0010(19) 0.005(2) C3 0.038(3) 0.034(2) 0.029(2) 0.0031(18) -0.008(2) 0.008(2) C4 0.037(3) 0.041(3) 0.043(3) 0.005(2) 0.003(2) -0.006(2) C5 0.032(3) 0.039(3) 0.040(3) -0.005(2) 0.004(2) 0.011(2) C6 0.029(2) 0.034(2) 0.029(2) -0.0016(18) -0.0043(19) -0.0008(19) C7 0.031(2) 0.027(2) 0.033(2) -0.0012(17) 0.0030(18) 0.0082(18) C8 0.031(3) 0.030(2) 0.043(3) 0.0052(19) 0.009(2) 0.0043(19) C9 0.032(3) 0.035(2) 0.038(2) 0.0010(19) 0.0061(19) 0.0038(19) C10 0.042(3) 0.044(3) 0.086(4) 0.007(3) 0.028(3) 0.003(3) C11 0.040(3) 0.0217(19) 0.025(2) 0.0016(16) 0.0014(18) 0.0084(18) C12 0.049(3) 0.034(2) 0.029(2) 0.0016(18) -0.005(2) 0.006(2) C13 0.049(3) 0.046(3) 0.032(2) -0.003(2) -0.005(2) 0.003(2) C14 0.050(3) 0.040(3) 0.045(3) -0.003(2) -0.006(2) 0.002(2) C15 0.034(2) 0.024(2) 0.026(2) 0.0049(16) 0.0031(17) 0.0075(17) C16 0.032(3) 0.024(2) 0.040(2) -0.0040(18) 0.0052(19) 0.0034(18) C17 0.033(3) 0.037(2) 0.036(2) 0.0030(19) 0.0066(19) 0.006(2) C18 0.055(4) 0.054(3) 0.073(4) 0.006(3) 0.034(3) 0.008(3) C19 0.031(2) 0.026(2) 0.027(2) 0.0051(16) -0.0011(17) 0.0079(18) C20 0.036(3) 0.029(2) 0.029(2) -0.0012(17) -0.0040(18) 0.0044(19) C21 0.032(2) 0.031(2) 0.033(2) 0.0027(18) -0.0033(18) 0.0044(19) C22 0.039(3) 0.043(3) 0.031(2) 0.001(2) -0.002(2) 0.005(2) C23 0.021(2) 0.040(2) 0.039(2) -0.0061(19) 0.0016(18) 0.0071(19) C24 0.035(3) 0.036(3) 0.042(3) -0.011(2) 0.003(2) 0.005(2) C25 0.041(3) 0.047(3) 0.043(3) -0.007(2) -0.004(2) 0.010(2) C26 0.065(4) 0.055(4) 0.063(4) -0.025(3) 0.006(3) 0.006(3) C27 0.021(2) 0.047(3) 0.056(3) -0.007(2) -0.003(2) 0.007(2) C28 0.035(3) 0.087(5) 0.087(5) 0.025(4) -0.006(3) 0.005(3) C29 0.042(3) 0.054(3) 0.069(4) 0.000(3) 0.000(3) 0.008(3) C30 0.083(6) 0.102(6) 0.090(6) 0.044(5) 0.008(5) 0.008(5) C31 0.027(2) 0.029(2) 0.045(3) 0.0007(19) 0.0005(19) 0.0007(18) C32 0.032(3) 0.038(3) 0.048(3) -0.008(2) 0.006(2) 0.001(2) C33 0.040(3) 0.031(2) 0.055(3) -0.010(2) 0.000(2) 0.000(2) C34 0.056(4) 0.036(3) 0.080(4) 0.008(3) -0.002(3) 0.005(3) C35 0.032(3) 0.039(3) 0.044(3) -0.010(2) 0.012(2) -0.007(2) C36 0.059(4) 0.043(3) 0.041(3) -0.001(2) 0.002(2) -0.015(3) C37 0.098(6) 0.068(4) 0.066(4) 0.024(4) 0.004(4) -0.024(4) C38 0.103(7) 0.109(7) 0.110(7) 0.039(6) -0.016(6) -0.007(6) C39 0.030(2) 0.047(3) 0.025(2) -0.0064(19) 0.0066(18) -0.001(2) C40 0.039(3) 0.045(3) 0.034(2) -0.002(2) 0.003(2) 0.003(2) C41 0.055(4) 0.052(3) 0.044(3) 0.001(2) 0.010(3) 0.012(3) C42 0.055(4) 0.062(4) 0.047(3) 0.002(3) 0.006(3) 0.012(3) C43 0.022(2) 0.044(3) 0.028(2) 0.0020(18) 0.0060(17) -0.0025(19) C44 0.034(3) 0.048(3) 0.038(3) -0.002(2) -0.005(2) -0.002(2) C45 0.034(3) 0.042(3) 0.059(3) 0.009(2) -0.002(2) 0.005(2) C46 0.043(3) 0.054(4) 0.085(5) 0.004(3) -0.020(3) 0.003(3) C47 0.034(3) 0.038(2) 0.023(2) -0.0006(17) 0.0006(18) 0.000(2) C48 0.038(3) 0.046(3) 0.031(2) -0.002(2) -0.001(2) -0.006(2) C49 0.041(3) 0.051(3) 0.036(3) -0.009(2) -0.010(2) -0.004(2) C50 0.053(4) 0.086(5) 0.043(3) 0.001(3) -0.012(3) -0.018(3) C51 0.028(2) 0.044(3) 0.027(2) 0.0022(19) 0.0013(17) 0.001(2) C52 0.047(3) 0.040(3) 0.034(2) -0.001(2) 0.002(2) -0.001(2) C53 0.038(3) 0.045(3) 0.048(3) 0.003(2) 0.000(2) -0.005(2) C54 0.045(3) 0.061(4) 0.053(3) 0.005(3) -0.001(3) 0.007(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Gd1 . N1 . 2.390(4) yes Gd1 . N2 . 2.395(4) yes Gd1 . N3 . 2.398(4) yes Gd1 . N4 . 2.365(4) yes Gd1 . N5 . 2.376(4) yes Gd1 . N6 . 2.396(4) yes S1 . C1 . 1.606(5) yes S2 . C2 . 1.617(5) yes S3 . C3 . 1.613(5) yes S4 . C4 . 1.616(6) yes S5 . C5 . 1.614(5) yes S6 . C6 . 1.622(5) yes N1 . C1 . 1.163(6) yes N2 . C2 . 1.151(6) yes N3 . C3 . 1.164(6) yes N4 . C4 . 1.169(7) yes N5 . C5 . 1.167(6) yes N6 . C6 . 1.158(6) yes N7 . C7 . 1.529(6) yes N7 . C11 . 1.521(5) yes N7 . C15 . 1.519(5) yes N7 . C19 . 1.522(5) yes N8 . C23 . 1.513(6) yes N8 . C27 . 1.539(6) yes N8 . C31 . 1.517(6) yes N8 . C35 . 1.504(6) yes N9 . C39 . 1.524(6) yes N9 . C43 . 1.534(6) yes N9 . C47 . 1.525(5) yes N9 . C51 . 1.518(6) yes C7 . C8 . 1.515(6) yes C7 . H71 . 0.950 no C7 . H72 . 0.950 no C8 . C9 . 1.529(7) yes C8 . H81 . 0.950 no C8 . H82 . 0.950 no C9 . C10 . 1.516(7) yes C9 . H91 . 0.950 no C9 . H92 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.507(6) yes C11 . H111 . 0.950 no C11 . H112 . 0.950 no C12 . C13 . 1.538(7) yes C12 . H121 . 0.950 no C12 . H122 . 0.950 no C13 . C14 . 1.521(7) yes C13 . H131 . 0.950 no C13 . H132 . 0.950 no C14 . H141 . 0.950 no C14 . H142 . 0.950 no C14 . H143 . 0.950 no C15 . C16 . 1.499(6) yes C15 . H151 . 0.950 no C15 . H152 . 0.950 no C16 . C17 . 1.524(6) yes C16 . H161 . 0.950 no C16 . H162 . 0.950 no C17 . C18 . 1.515(7) yes C17 . H171 . 0.950 no C17 . H172 . 0.950 no C18 . H181 . 0.950 no C18 . H182 . 0.950 no C18 . H183 . 0.950 no C19 . C20 . 1.510(6) yes C19 . H191 . 0.950 no C19 . H192 . 0.950 no C20 . C21 . 1.534(6) yes C20 . H201 . 0.950 no C20 . H202 . 0.950 no C21 . C22 . 1.517(6) yes C21 . H211 . 0.950 no C21 . H212 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.520(6) yes C23 . H231 . 0.950 no C23 . H232 . 0.950 no C24 . C25 . 1.525(7) yes C24 . H241 . 0.950 no C24 . H242 . 0.950 no C25 . C26 . 1.524(7) yes C25 . H251 . 0.950 no C25 . H252 . 0.950 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . C28 . 1.533(9) yes C27 . H271 . 0.950 no C27 . H272 . 0.950 no C28 . C29 . 1.486(9) yes C28 . H281 . 0.950 no C28 . H282 . 0.950 no C29 . C30 . 1.493(10) yes C29 . H291 . 0.950 no C29 . H292 . 0.950 no C30 . H301 . 0.950 no C30 . H302 . 0.950 no C30 . H303 . 0.950 no C31 . C32 . 1.528(6) yes C31 . H311 . 0.950 no C31 . H312 . 0.950 no C32 . C33 . 1.531(7) yes C32 . H321 . 0.950 no C32 . H322 . 0.950 no C33 . C34 . 1.511(8) yes C33 . H331 . 0.950 no C33 . H332 . 0.950 no C34 . H341 . 0.950 no C34 . H342 . 0.950 no C34 . H343 . 0.950 no C35 . C36 . 1.495(8) yes C35 . H351 . 0.950 no C35 . H352 . 0.950 no C36 . C37 . 1.543(8) yes C36 . H361 . 0.950 no C36 . H362 . 0.950 no C37 . C38 . 1.415(12) yes C37 . H371 . 0.950 no C37 . H372 . 0.950 no C38 . H381 . 0.950 no C38 . H382 . 0.950 no C38 . H383 . 0.950 no C39 . C40 . 1.504(7) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . C41 . 1.520(7) yes C40 . H401 . 0.950 no C40 . H402 . 0.950 no C41 . C42 . 1.500(8) yes C41 . H411 . 0.950 no C41 . H412 . 0.950 no C42 . H421 . 0.950 no C42 . H422 . 0.950 no C42 . H423 . 0.950 no C43 . C44 . 1.512(6) yes C43 . H431 . 0.950 no C43 . H432 . 0.950 no C44 . C45 . 1.516(7) yes C44 . H441 . 0.950 no C44 . H442 . 0.950 no C45 . C46 . 1.509(8) yes C45 . H451 . 0.950 no C45 . H452 . 0.950 no C46 . H461 . 0.950 no C46 . H462 . 0.950 no C46 . H463 . 0.950 no C47 . C48 . 1.504(7) yes C47 . H471 . 0.950 no C47 . H472 . 0.950 no C48 . C49 . 1.527(6) yes C48 . H481 . 0.950 no C48 . H482 . 0.950 no C49 . C50 . 1.508(8) yes C49 . H491 . 0.950 no C49 . H492 . 0.950 no C50 . H501 . 0.950 no C50 . H502 . 0.950 no C50 . H503 . 0.950 no C51 . C52 . 1.516(7) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C52 . C53 . 1.537(7) yes C52 . H521 . 0.950 no C52 . H522 . 0.950 no C53 . C54 . 1.503(8) yes C53 . H531 . 0.950 no C53 . H532 . 0.950 no C54 . H541 . 0.950 no C54 . H542 . 0.950 no C54 . H543 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Gd1 . N2 . 86.61(16) yes N1 . Gd1 . N3 . 89.46(16) yes N2 . Gd1 . N3 . 89.06(15) yes N1 . Gd1 . N4 . 173.96(16) yes N2 . Gd1 . N4 . 87.70(16) yes N3 . Gd1 . N4 . 88.42(15) yes N1 . Gd1 . N5 . 91.77(16) yes N2 . Gd1 . N5 . 177.81(16) yes N3 . Gd1 . N5 . 89.46(15) yes N4 . Gd1 . N5 . 93.87(15) yes N1 . Gd1 . N6 . 88.06(15) yes N2 . Gd1 . N6 . 91.67(15) yes N3 . Gd1 . N6 . 177.37(17) yes N4 . Gd1 . N6 . 94.13(16) yes N5 . Gd1 . N6 . 89.74(15) yes Gd1 . N1 . C1 . 171.3(4) yes Gd1 . N2 . C2 . 173.9(4) yes Gd1 . N3 . C3 . 175.3(4) yes Gd1 . N4 . C4 . 175.6(4) yes Gd1 . N5 . C5 . 170.7(4) yes Gd1 . N6 . C6 . 174.5(4) yes C7 . N7 . C11 . 111.4(3) yes C7 . N7 . C15 . 106.1(3) yes C11 . N7 . C15 . 110.9(3) yes C7 . N7 . C19 . 110.8(3) yes C11 . N7 . C19 . 106.8(3) yes C15 . N7 . C19 . 111.0(3) yes C23 . N8 . C27 . 109.5(4) yes C23 . N8 . C31 . 106.7(3) yes C27 . N8 . C31 . 110.1(4) yes C23 . N8 . C35 . 111.0(4) yes C27 . N8 . C35 . 107.8(4) yes C31 . N8 . C35 . 111.7(4) yes C39 . N9 . C43 . 111.1(3) yes C39 . N9 . C47 . 110.3(4) yes C43 . N9 . C47 . 106.7(3) yes C39 . N9 . C51 . 106.6(3) yes C43 . N9 . C51 . 111.6(4) yes C47 . N9 . C51 . 110.6(3) yes S1 . C1 . N1 . 178.7(5) yes S2 . C2 . N2 . 179.7(4) yes S3 . C3 . N3 . 179.9(4) yes S4 . C4 . N4 . 178.9(5) yes S5 . C5 . N5 . 179.7(5) yes S6 . C6 . N6 . 179.2(5) yes N7 . C7 . C8 . 115.7(3) yes N7 . C7 . H71 . 107.3 no C8 . C7 . H71 . 106.9 no N7 . C7 . H72 . 109.0 no C8 . C7 . H72 . 108.4 no H71 . C7 . H72 . 109.5 no C7 . C8 . C9 . 109.5(4) yes C7 . C8 . H81 . 108.7 no C9 . C8 . H81 . 110.4 no C7 . C8 . H82 . 110.2 no C9 . C8 . H82 . 108.4 no H81 . C8 . H82 . 109.5 no C8 . C9 . C10 . 112.8(4) yes C8 . C9 . H91 . 107.4 no C10 . C9 . H91 . 107.9 no C8 . C9 . H92 . 109.2 no C10 . C9 . H92 . 110.0 no H91 . C9 . H92 . 109.5 no C9 . C10 . H101 . 108.6 no C9 . C10 . H102 . 110.6 no H101 . C10 . H102 . 109.5 no C9 . C10 . H103 . 109.2 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N7 . C11 . C12 . 115.8(3) yes N7 . C11 . H111 . 108.3 no C12 . C11 . H111 . 106.2 no N7 . C11 . H112 . 108.4 no C12 . C11 . H112 . 108.6 no H111 . C11 . H112 . 109.5 no C11 . C12 . C13 . 111.6(4) yes C11 . C12 . H121 . 110.0 no C13 . C12 . H121 . 110.3 no C11 . C12 . H122 . 107.5 no C13 . C12 . H122 . 107.9 no H121 . C12 . H122 . 109.5 no C12 . C13 . C14 . 114.6(4) yes C12 . C13 . H131 . 108.9 no C14 . C13 . H131 . 108.1 no C12 . C13 . H132 . 107.2 no C14 . C13 . H132 . 108.5 no H131 . C13 . H132 . 109.5 no C13 . C14 . H141 . 110.0 no C13 . C14 . H142 . 109.4 no H141 . C14 . H142 . 109.5 no C13 . C14 . H143 . 109.0 no H141 . C14 . H143 . 109.5 no H142 . C14 . H143 . 109.5 no N7 . C15 . C16 . 117.8(3) yes N7 . C15 . H151 . 106.9 no C16 . C15 . H151 . 107.5 no N7 . C15 . H152 . 107.7 no C16 . C15 . H152 . 107.3 no H151 . C15 . H152 . 109.5 no C15 . C16 . C17 . 109.3(4) yes C15 . C16 . H161 . 109.3 no C17 . C16 . H161 . 109.1 no C15 . C16 . H162 . 109.7 no C17 . C16 . H162 . 109.8 no H161 . C16 . H162 . 109.5 no C16 . C17 . C18 . 113.3(4) yes C16 . C17 . H171 . 108.1 no C18 . C17 . H171 . 108.8 no C16 . C17 . H172 . 108.8 no C18 . C17 . H172 . 108.4 no H171 . C17 . H172 . 109.5 no C17 . C18 . H181 . 109.6 no C17 . C18 . H182 . 109.1 no H181 . C18 . H182 . 109.5 no C17 . C18 . H183 . 109.7 no H181 . C18 . H183 . 109.5 no H182 . C18 . H183 . 109.5 no N7 . C19 . C20 . 116.3(3) yes N7 . C19 . H191 . 107.4 no C20 . C19 . H191 . 107.8 no N7 . C19 . H192 . 108.5 no C20 . C19 . H192 . 107.2 no H191 . C19 . H192 . 109.5 no C19 . C20 . C21 . 110.0(4) yes C19 . C20 . H201 . 109.0 no C21 . C20 . H201 . 109.4 no C19 . C20 . H202 . 109.3 no C21 . C20 . H202 . 109.6 no H201 . C20 . H202 . 109.5 no C20 . C21 . C22 . 111.6(4) yes C20 . C21 . H211 . 108.9 no C22 . C21 . H211 . 108.9 no C20 . C21 . H212 . 109.0 no C22 . C21 . H212 . 108.9 no H211 . C21 . H212 . 109.5 no C21 . C22 . H221 . 109.1 no C21 . C22 . H222 . 110.2 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.1 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no N8 . C23 . C24 . 115.7(4) yes N8 . C23 . H231 . 108.9 no C24 . C23 . H231 . 108.4 no N8 . C23 . H232 . 107.3 no C24 . C23 . H232 . 106.9 no H231 . C23 . H232 . 109.5 no C23 . C24 . C25 . 109.6(4) yes C23 . C24 . H241 . 110.1 no C25 . C24 . H241 . 109.7 no C23 . C24 . H242 . 108.9 no C25 . C24 . H242 . 109.0 no H241 . C24 . H242 . 109.5 no C24 . C25 . C26 . 111.9(5) yes C24 . C25 . H251 . 108.4 no C26 . C25 . H251 . 107.6 no C24 . C25 . H252 . 109.2 no C26 . C25 . H252 . 110.2 no H251 . C25 . H252 . 109.5 no C25 . C26 . H261 . 110.3 no C25 . C26 . H262 . 107.8 no H261 . C26 . H262 . 109.5 no C25 . C26 . H263 . 110.4 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no N8 . C27 . C28 . 114.8(4) yes N8 . C27 . H271 . 108.4 no C28 . C27 . H271 . 108.9 no N8 . C27 . H272 . 107.4 no C28 . C27 . H272 . 107.7 no H271 . C27 . H272 . 109.5 no C27 . C28 . C29 . 113.6(5) yes C27 . C28 . H281 . 107.9 no C29 . C28 . H281 . 108.6 no C27 . C28 . H282 . 109.1 no C29 . C28 . H282 . 108.1 no H281 . C28 . H282 . 109.5 no C28 . C29 . C30 . 112.8(6) yes C28 . C29 . H291 . 108.3 no C30 . C29 . H291 . 108.3 no C28 . C29 . H292 . 108.8 no C30 . C29 . H292 . 109.1 no H291 . C29 . H292 . 109.5 no C29 . C30 . H301 . 109.5 no C29 . C30 . H302 . 109.9 no H301 . C30 . H302 . 109.5 no C29 . C30 . H303 . 109.0 no H301 . C30 . H303 . 109.5 no H302 . C30 . H303 . 109.5 no N8 . C31 . C32 . 115.4(4) yes N8 . C31 . H311 . 108.0 no C32 . C31 . H311 . 107.9 no N8 . C31 . H312 . 108.0 no C32 . C31 . H312 . 108.0 no H311 . C31 . H312 . 109.5 no C31 . C32 . C33 . 110.3(4) yes C31 . C32 . H321 . 109.1 no C33 . C32 . H321 . 109.1 no C31 . C32 . H322 . 109.2 no C33 . C32 . H322 . 109.7 no H321 . C32 . H322 . 109.5 no C32 . C33 . C34 . 113.7(5) yes C32 . C33 . H331 . 108.3 no C34 . C33 . H331 . 107.2 no C32 . C33 . H332 . 107.9 no C34 . C33 . H332 . 110.1 no H331 . C33 . H332 . 109.5 no C33 . C34 . H341 . 108.6 no C33 . C34 . H342 . 108.4 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 111.4 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no N8 . C35 . C36 . 115.6(4) yes N8 . C35 . H351 . 107.9 no C36 . C35 . H351 . 107.5 no N8 . C35 . H352 . 107.8 no C36 . C35 . H352 . 108.4 no H351 . C35 . H352 . 109.5 no C35 . C36 . C37 . 108.9(5) yes C35 . C36 . H361 . 110.5 no C37 . C36 . H361 . 108.8 no C35 . C36 . H362 . 109.7 no C37 . C36 . H362 . 109.4 no H361 . C36 . H362 . 109.5 no C36 . C37 . C38 . 112.7(7) yes C36 . C37 . H371 . 109.4 no C38 . C37 . H371 . 107.8 no C36 . C37 . H372 . 109.3 no C38 . C37 . H372 . 108.1 no H371 . C37 . H372 . 109.5 no C37 . C38 . H381 . 114.9 no C37 . C38 . H382 . 106.6 no H381 . C38 . H382 . 109.5 no C37 . C38 . H383 . 106.8 no H381 . C38 . H383 . 109.5 no H382 . C38 . H383 . 109.5 no N9 . C39 . C40 . 116.1(4) yes N9 . C39 . H391 . 108.5 no C40 . C39 . H391 . 108.4 no N9 . C39 . H392 . 107.6 no C40 . C39 . H392 . 106.7 no H391 . C39 . H392 . 109.5 no C39 . C40 . C41 . 111.0(4) yes C39 . C40 . H401 . 110.0 no C41 . C40 . H401 . 108.0 no C39 . C40 . H402 . 108.3 no C41 . C40 . H402 . 110.0 no H401 . C40 . H402 . 109.5 no C40 . C41 . C42 . 113.2(5) yes C40 . C41 . H411 . 107.2 no C42 . C41 . H411 . 107.5 no C40 . C41 . H412 . 109.3 no C42 . C41 . H412 . 110.1 no H411 . C41 . H412 . 109.5 no C41 . C42 . H421 . 108.2 no C41 . C42 . H422 . 110.9 no H421 . C42 . H422 . 109.5 no C41 . C42 . H423 . 109.4 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no N9 . C43 . C44 . 115.5(4) yes N9 . C43 . H431 . 108.4 no C44 . C43 . H431 . 107.2 no N9 . C43 . H432 . 108.5 no C44 . C43 . H432 . 107.8 no H431 . C43 . H432 . 109.5 no C43 . C44 . C45 . 110.5(4) yes C43 . C44 . H441 . 109.1 no C45 . C44 . H441 . 109.9 no C43 . C44 . H442 . 108.6 no C45 . C44 . H442 . 109.3 no H441 . C44 . H442 . 109.5 no C44 . C45 . C46 . 112.3(5) yes C44 . C45 . H451 . 109.6 no C46 . C45 . H451 . 108.4 no C44 . C45 . H452 . 109.0 no C46 . C45 . H452 . 108.1 no H451 . C45 . H452 . 109.5 no C45 . C46 . H461 . 111.6 no C45 . C46 . H462 . 108.5 no H461 . C46 . H462 . 109.5 no C45 . C46 . H463 . 108.3 no H461 . C46 . H463 . 109.5 no H462 . C46 . H463 . 109.5 no N9 . C47 . C48 . 115.7(4) yes N9 . C47 . H471 . 107.3 no C48 . C47 . H471 . 107.5 no N9 . C47 . H472 . 108.6 no C48 . C47 . H472 . 108.2 no H471 . C47 . H472 . 109.5 no C47 . C48 . C49 . 111.7(4) yes C47 . C48 . H481 . 109.1 no C49 . C48 . H481 . 109.7 no C47 . C48 . H482 . 108.3 no C49 . C48 . H482 . 108.5 no H481 . C48 . H482 . 109.5 no C48 . C49 . C50 . 111.8(5) yes C48 . C49 . H491 . 108.6 no C50 . C49 . H491 . 108.2 no C48 . C49 . H492 . 109.7 no C50 . C49 . H492 . 109.0 no H491 . C49 . H492 . 109.5 no C49 . C50 . H501 . 109.3 no C49 . C50 . H502 . 108.5 no H501 . C50 . H502 . 109.5 no C49 . C50 . H503 . 110.5 no H501 . C50 . H503 . 109.5 no H502 . C50 . H503 . 109.5 no N9 . C51 . C52 . 115.9(4) yes N9 . C51 . H511 . 108.4 no C52 . C51 . H511 . 107.5 no N9 . C51 . H512 . 107.6 no C52 . C51 . H512 . 107.9 no H511 . C51 . H512 . 109.5 no C51 . C52 . C53 . 112.1(4) yes C51 . C52 . H521 . 109.1 no C53 . C52 . H521 . 109.7 no C51 . C52 . H522 . 108.6 no C53 . C52 . H522 . 107.9 no H521 . C52 . H522 . 109.5 no C52 . C53 . C54 . 113.9(4) yes C52 . C53 . H531 . 109.3 no C54 . C53 . H531 . 108.2 no C52 . C53 . H532 . 107.4 no C54 . C53 . H532 . 108.6 no H531 . C53 . H532 . 109.5 no C53 . C54 . H541 . 109.3 no C53 . C54 . H542 . 108.9 no H541 . C54 . H542 . 109.5 no C53 . C54 . H543 . 110.2 no H541 . C54 . H543 . 109.5 no H542 . C54 . H543 . 109.5 no _database_code_depnum_ccdc_archive 'CCDC 933721' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_C54H108DyN9S6 #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_sum 'C54 H108 Dy1 N9 S6' _chemical_formula_moiety 'C54 H108 Dy1 N9 S6' _chemical_compound_source ? _chemical_formula_weight 1238.41 #============================================================= # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.4126(3) _cell_length_b 12.8565(3) _cell_length_c 22.7613(5) _cell_angle_alpha 90.8850(10) _cell_angle_beta 92.3090(10) _cell_angle_gamma 96.6870(10) _cell_volume 3603.93(14) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 23.43 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.21 _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1314 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' #============================================================================= # 7. EXPERIMENTAL DATA _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 62821 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_theta_min 1.595 _diffrn_reflns_theta_max 24.990 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.990 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 #========================================================================== # 8. REFINEMENT DATA _reflns_number_total 12651 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 27 _refine_diff_density_min -0.57 _refine_diff_density_max 0.62 _oxford_reflns_threshold_expression_ref I>2.5\s(I) _refine_ls_number_reflns 8457 _refine_ls_number_restraints 6 _refine_ls_number_parameters 632 _oxford_refine_ls_R_factor_ref 0.0340 _refine_ls_wR_factor_ref 0.0319 _refine_ls_goodness_of_fit_ref 1.1303 _refine_ls_shift/su_max 0.0006754 _refine_ls_shift/su_mean 0.0000168 _refine_special_details ; Restraints DISTANCE 1.500000 , 0.020000 = C(25) TO C(26) DISTANCE 1.500000 , 0.020000 = C(41) TO C(42) DISTANCE 1.500000 , 0.020000 = C(13) TO C(14) DISTANCE 1.500000 , 0.020000 = C(10) TO C(9) DISTANCE 1.500000 , 0.020000 = C(22) TO C(21) DISTANCE 1.500000 , 0.020000 = C(32) TO C(33) ; # The values computed from all data _oxford_reflns_number_all 12651 _refine_ls_R_factor_all 0.0577 _refine_ls_wR_factor_all 0.0489 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8746 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_gt 0.0324 _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.368 0.454 0.354 0.176 0.810E-01 ; #========================================================== # 9. General computing _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' #=================================================================== # 10. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Dy1 Dy -0.067551(17) 0.290622(16) 0.251811(9) 0.0656 1.0000 Uani . . . . . . S1 S 0.15040(11) 0.07300(10) 0.38632(6) 0.0945 1.0000 Uani . . . . . . S2 S -0.33111(14) -0.04201(11) 0.25472(7) 0.1223 1.0000 Uani . . . . . . S3 S -0.26123(12) 0.43976(11) 0.42183(5) 0.1008 1.0000 Uani . . . . . . S4 S -0.31423(11) 0.47221(13) 0.11342(8) 0.1261 1.0000 Uani . . . . . . S5 S 0.19357(13) 0.62576(13) 0.26196(8) 0.1353 1.0000 Uani . . . . . . S6 S 0.16511(11) 0.16432(11) 0.09070(5) 0.0991 1.0000 Uani . . . . . . N1 N 0.0379(3) 0.2002(3) 0.31645(16) 0.0923 1.0000 Uani . . . . . . N2 N -0.1924(3) 0.1393(3) 0.24607(17) 0.0940 1.0000 Uani . . . . . . N3 N -0.1581(3) 0.3514(3) 0.33191(17) 0.0914 1.0000 Uani . . . . . . N4 N -0.1849(3) 0.3722(3) 0.18986(17) 0.0880 1.0000 Uani . . . . . . N5 N 0.0603(3) 0.4395(3) 0.26101(17) 0.0911 1.0000 Uani . . . . . . N6 N 0.0308(3) 0.2299(3) 0.17402(17) 0.0853 1.0000 Uani . . . . . . N7 N -0.0600(2) 0.2420(2) 0.53661(12) 0.0595 1.0000 Uani . . . . . . N8 N 0.4588(3) 0.3217(3) 0.24588(16) 0.0793 1.0000 Uani . . . . . . N9 N 0.8847(3) 0.8489(3) 0.10714(13) 0.0693 1.0000 Uani . . . . . . C1 C 0.0848(3) 0.1461(3) 0.34520(18) 0.0705 1.0000 Uani . . . . . . C2 C -0.2501(4) 0.0634(4) 0.24973(18) 0.0797 1.0000 Uani . . . . . . C3 C -0.2008(4) 0.3890(3) 0.36927(19) 0.0713 1.0000 Uani . . . . . . C4 C -0.2380(3) 0.4141(3) 0.1578(2) 0.0777 1.0000 Uani . . . . . . C5 C 0.1158(4) 0.5174(4) 0.2614(2) 0.0824 1.0000 Uani . . . . . . C6 C 0.0868(4) 0.2035(3) 0.13897(18) 0.0715 1.0000 Uani . . . . . . C7 C -0.0780(3) 0.1423(3) 0.49895(16) 0.0646 1.0000 Uani . . . . . . C8 C -0.1525(4) 0.1457(3) 0.44482(17) 0.0806 1.0000 Uani . . . . . . C9 C -0.1745(4) 0.0386(4) 0.4143(2) 0.0923 1.0000 Uani D . . . . . C10 C -0.2458(4) -0.0412(4) 0.4461(2) 0.1082 1.0000 Uani D . . . . . C11 C -0.1662(3) 0.2740(3) 0.55764(16) 0.0648 1.0000 Uani . . . . . . C12 C -0.2369(3) 0.1924(3) 0.5899(2) 0.0802 1.0000 Uani . . . . . . C13 C -0.3449(4) 0.2303(4) 0.6020(2) 0.0927 1.0000 Uani D . . . . . C14 C -0.4216(5) 0.1512(5) 0.6303(4) 0.1712 1.0000 Uani D . . . . . C15 C 0.0139(3) 0.2198(3) 0.58858(15) 0.0617 1.0000 Uani . . . . . . C16 C 0.0428(3) 0.3078(3) 0.63306(17) 0.0710 1.0000 Uani . . . . . . C17 C 0.1254(4) 0.2798(3) 0.67887(18) 0.0785 1.0000 Uani . . . . . . C18 C 0.1481(4) 0.3607(4) 0.72785(18) 0.0922 1.0000 Uani . . . . . . C19 C -0.0085(3) 0.3335(3) 0.50167(16) 0.0631 1.0000 Uani . . . . . . C20 C 0.1012(3) 0.3233(3) 0.47818(18) 0.0725 1.0000 Uani . . . . . . C21 C 0.1326(4) 0.4132(3) 0.43732(19) 0.0816 1.0000 Uani D . . . . . C22 C 0.2413(4) 0.4118(4) 0.4120(3) 0.1239 1.0000 Uani D . . . . . C23 C 0.4197(4) 0.2576(4) 0.2974(2) 0.0944 1.0000 Uani . . . . . . C24 C 0.5068(5) 0.2195(4) 0.3361(2) 0.1144 1.0000 Uani . . . . . . C25 C 0.4572(7) 0.1660(7) 0.3886(4) 0.1897 1.0000 Uani D . . . . . C26 C 0.5145(9) 0.1526(11) 0.4335(5) 0.3366 1.0000 Uani D . . . . . C27 C 0.5344(3) 0.4187(3) 0.2667(2) 0.0856 1.0000 Uani . . . . . . C28 C 0.4873(4) 0.4897(4) 0.3096(2) 0.1026 1.0000 Uani . . . . . . C29 C 0.5559(5) 0.5955(4) 0.3158(3) 0.1252 1.0000 Uani . . . . . . C30 C 0.5476(6) 0.6625(5) 0.2617(4) 0.1635 1.0000 Uani . . . . . . C31 C 0.3599(3) 0.3531(4) 0.2117(2) 0.0935 1.0000 Uani . . . . . . C32 C 0.3847(4) 0.4121(6) 0.1561(3) 0.1486 1.0000 Uani D . . . . . C33 C 0.2934(5) 0.4507(5) 0.1259(3) 0.1328 1.0000 Uani D . . . . . C34 C 0.3162(6) 0.5019(8) 0.0696(4) 0.2208 1.0000 Uani . . . . . . C35 C 0.5236(3) 0.2598(3) 0.2060(2) 0.0851 1.0000 Uani . . . . . . C36 C 0.4651(4) 0.1585(4) 0.1806(2) 0.0981 1.0000 Uani . . . . . . C37 C 0.5297(4) 0.1168(4) 0.1322(2) 0.1125 1.0000 Uani . . . . . . C38 C 0.4734(6) 0.0197(5) 0.1033(3) 0.1694 1.0000 Uani . . . . . . C39 C 0.8919(4) 0.9465(3) 0.06975(17) 0.0803 1.0000 Uani . . . . . . C40 C 0.8318(4) 1.0339(4) 0.0907(2) 0.0945 1.0000 Uani . . . . . . C41 C 0.8404(5) 1.1234(5) 0.0480(3) 0.1337 1.0000 Uani D . . . . . C42 C 0.7746(7) 1.1483(11) 0.0173(6) 0.4419 1.0000 Uani D . . . . . C43 C 0.7674(3) 0.8053(3) 0.11533(17) 0.0757 1.0000 Uani . . . . . . C44 C 0.6988(4) 0.7833(4) 0.0599(2) 0.0971 1.0000 Uani . . . . . . C45 C 0.5834(4) 0.7428(4) 0.0730(3) 0.1133 1.0000 Uani . . . . . . C46 C 0.5095(5) 0.7316(6) 0.0198(3) 0.1869 1.0000 Uani . . . . . . C47 C 0.9441(3) 0.7699(3) 0.07482(17) 0.0784 1.0000 Uani . . . . . . C48 C 0.9498(4) 0.6663(3) 0.1040(2) 0.0864 1.0000 Uani . . . . . . C49 C 1.0159(5) 0.5981(4) 0.0695(2) 0.1154 1.0000 Uani . . . . . . C50 C 1.0156(5) 0.4893(5) 0.0924(3) 0.1218 1.0000 Uani . . . . . . C51 C 0.9364(3) 0.8741(3) 0.16822(16) 0.0766 1.0000 Uani . . . . . . C52 C 1.0577(4) 0.9058(4) 0.17073(19) 0.0917 1.0000 Uani . . . . . . C53 C 1.1019(4) 0.9323(4) 0.2319(2) 0.1035 1.0000 Uani . . . . . . C54 C 1.2218(5) 0.9635(5) 0.2354(3) 0.1415 1.0000 Uani . . . . . . H71 H -0.0071 0.1273 0.4862 0.0725(16) 1.0000 Uiso R . . . . . H72 H -0.1073 0.0879 0.5246 0.0721(16) 1.0000 Uiso R . . . . . H81 H -0.2217 0.1670 0.4565 0.0905(16) 1.0000 Uiso R . . . . . H82 H -0.1178 0.1951 0.4179 0.0905(16) 1.0000 Uiso R . . . . . H91 H -0.2116 0.0464 0.3769 0.1054(16) 1.0000 Uiso R . . . . . H92 H -0.1049 0.0134 0.4086 0.1057(16) 1.0000 Uiso R . . . . . H101 H -0.3105 -0.0097 0.4554 0.1492(16) 1.0000 Uiso R . . . . . H102 H -0.2648 -0.1015 0.4203 0.1493(16) 1.0000 Uiso R . . . . . H103 H -0.2072 -0.0598 0.4815 0.1496(16) 1.0000 Uiso R . . . . . H111 H -0.1473 0.3349 0.5840 0.0716(16) 1.0000 Uiso R . . . . . H112 H -0.2082 0.2920 0.5224 0.0712(16) 1.0000 Uiso R . . . . . H121 H -0.2501 0.1301 0.5653 0.0896(16) 1.0000 Uiso R . . . . . H122 H -0.1999 0.1776 0.6269 0.0896(16) 1.0000 Uiso R . . . . . H131 H -0.3822 0.2467 0.5632 0.1053(16) 1.0000 Uiso R . . . . . H132 H -0.3305 0.2920 0.6274 0.1053(16) 1.0000 Uiso R . . . . . H141 H -0.4332 0.0883 0.6052 0.2385(16) 1.0000 Uiso R . . . . . H142 H -0.4903 0.1785 0.6365 0.2383(16) 1.0000 Uiso R . . . . . H143 H -0.3881 0.1352 0.6678 0.2384(16) 1.0000 Uiso R . . . . . H151 H 0.0814 0.2007 0.5728 0.0686(16) 1.0000 Uiso R . . . . . H152 H -0.0236 0.1602 0.6088 0.0683(16) 1.0000 Uiso R . . . . . H161 H -0.0228 0.3213 0.6522 0.0796(16) 1.0000 Uiso R . . . . . H162 H 0.0724 0.3699 0.6128 0.0798(16) 1.0000 Uiso R . . . . . H171 H 0.0977 0.2126 0.6956 0.0886(16) 1.0000 Uiso R . . . . . H172 H 0.1926 0.2721 0.6597 0.0886(16) 1.0000 Uiso R . . . . . H181 H 0.1702 0.4271 0.7108 0.1251(16) 1.0000 Uiso R . . . . . H182 H 0.2039 0.3404 0.7548 0.1254(16) 1.0000 Uiso R . . . . . H183 H 0.0807 0.3624 0.7476 0.1254(16) 1.0000 Uiso R . . . . . H191 H -0.0022 0.3957 0.5276 0.0703(16) 1.0000 Uiso R . . . . . H192 H -0.0588 0.3400 0.4686 0.0706(16) 1.0000 Uiso R . . . . . H201 H 0.1544 0.3259 0.5106 0.0813(16) 1.0000 Uiso R . . . . . H202 H 0.0987 0.2582 0.4572 0.0814(16) 1.0000 Uiso R . . . . . H211 H 0.0790 0.4099 0.4048 0.0919(16) 1.0000 Uiso R . . . . . H212 H 0.1332 0.4783 0.4597 0.0915(16) 1.0000 Uiso R . . . . . H221 H 0.2553 0.4700 0.3870 0.1484(16) 1.0000 Uiso R . . . . . H222 H 0.2954 0.4160 0.4429 0.1484(16) 1.0000 Uiso R . . . . . H223 H 0.2427 0.3487 0.3899 0.1484(16) 1.0000 Uiso R . . . . . H231 H 0.3814 0.3027 0.3220 0.1066(16) 1.0000 Uiso R . . . . . H232 H 0.3723 0.1971 0.2824 0.1064(16) 1.0000 Uiso R . . . . . H241 H 0.5593 0.2772 0.3492 0.1305(16) 1.0000 Uiso R . . . . . H242 H 0.5421 0.1689 0.3141 0.1305(16) 1.0000 Uiso R . . . . . H251 H 0.3996 0.2112 0.4018 0.2203(16) 1.0000 Uiso R . . . . . H252 H 0.4149 0.1020 0.3757 0.2203(16) 1.0000 Uiso R . . . . . H261 H 0.4709 0.1175 0.4622 0.3981(16) 1.0000 Uiso R . . . . . H262 H 0.5458 0.2189 0.4488 0.3981(16) 1.0000 Uiso R . . . . . H263 H 0.5704 0.1117 0.4237 0.3981(16) 1.0000 Uiso R . . . . . H271 H 0.5544 0.4580 0.2321 0.0955(16) 1.0000 Uiso R . . . . . H272 H 0.5979 0.3938 0.2859 0.0953(16) 1.0000 Uiso R . . . . . H281 H 0.4850 0.4555 0.3477 0.1167(16) 1.0000 Uiso R . . . . . H282 H 0.4142 0.5005 0.2949 0.1164(16) 1.0000 Uiso R . . . . . H291 H 0.5374 0.6338 0.3518 0.1434(16) 1.0000 Uiso R . . . . . H292 H 0.6309 0.5804 0.3214 0.1435(16) 1.0000 Uiso R . . . . . H301 H 0.4715 0.6688 0.2520 0.2194(16) 1.0000 Uiso R . . . . . H302 H 0.5781 0.6305 0.2278 0.2192(16) 1.0000 Uiso R . . . . . H303 H 0.5858 0.7325 0.2695 0.2194(16) 1.0000 Uiso R . . . . . H311 H 0.3124 0.2894 0.2014 0.1065(16) 1.0000 Uiso R . . . . . H312 H 0.3252 0.3977 0.2382 0.1068(16) 1.0000 Uiso R . . . . . H321 H 0.4118 0.3653 0.1282 0.1666(16) 1.0000 Uiso R . . . . . H322 H 0.4377 0.4718 0.1653 0.1666(16) 1.0000 Uiso R . . . . . H331 H 0.2365 0.3931 0.1193 0.1539(16) 1.0000 Uiso R . . . . . H332 H 0.2710 0.5043 0.1519 0.1539(16) 1.0000 Uiso R . . . . . H341 H 0.3428 0.5741 0.0786 0.2864(16) 1.0000 Uiso R . . . . . H342 H 0.2499 0.4965 0.0455 0.2863(16) 1.0000 Uiso R . . . . . H343 H 0.3708 0.4661 0.0516 0.2864(16) 1.0000 Uiso R . . . . . H351 H 0.5869 0.2428 0.2293 0.0965(16) 1.0000 Uiso R . . . . . H352 H 0.5463 0.3040 0.1732 0.0964(16) 1.0000 Uiso R . . . . . H361 H 0.4570 0.1073 0.2118 0.1098(16) 1.0000 Uiso R . . . . . H362 H 0.3944 0.1715 0.1646 0.1096(16) 1.0000 Uiso R . . . . . H371 H 0.6000 0.1028 0.1486 0.1295(16) 1.0000 Uiso R . . . . . H372 H 0.5386 0.1701 0.1029 0.1297(16) 1.0000 Uiso R . . . . . H381 H 0.4046 0.0353 0.0874 0.2330(16) 1.0000 Uiso R . . . . . H382 H 0.5156 -0.0036 0.0725 0.2332(16) 1.0000 Uiso R . . . . . H383 H 0.4634 -0.0330 0.1325 0.2333(16) 1.0000 Uiso R . . . . . H391 H 0.8640 0.9256 0.0308 0.0886(16) 1.0000 Uiso R . . . . . H392 H 0.9677 0.9728 0.0689 0.0883(16) 1.0000 Uiso R . . . . . H401 H 0.8634 1.0596 0.1285 0.1089(16) 1.0000 Uiso R . . . . . H402 H 0.7561 1.0083 0.0937 0.1083(16) 1.0000 Uiso R . . . . . H411 H 0.8715 1.1860 0.0701 0.1560(16) 1.0000 Uiso R . . . . . H412 H 0.8975 1.1067 0.0221 0.1560(16) 1.0000 Uiso R . . . . . H421 H 0.7938 1.2109 -0.0034 0.5266(16) 1.0000 Uiso R . . . . . H422 H 0.7051 1.1501 0.0331 0.5266(16) 1.0000 Uiso R . . . . . H423 H 0.7726 1.0897 -0.0088 0.5266(16) 1.0000 Uiso R . . . . . H431 H 0.7359 0.8564 0.1391 0.0866(16) 1.0000 Uiso R . . . . . H432 H 0.7687 0.7408 0.1367 0.0864(16) 1.0000 Uiso R . . . . . H441 H 0.6982 0.8470 0.0379 0.1116(16) 1.0000 Uiso R . . . . . H442 H 0.7283 0.7291 0.0372 0.1115(16) 1.0000 Uiso R . . . . . H451 H 0.5837 0.6759 0.0916 0.1265(16) 1.0000 Uiso R . . . . . H452 H 0.5560 0.7924 0.1003 0.1266(16) 1.0000 Uiso R . . . . . H461 H 0.5363 0.6799 -0.0057 0.2473(16) 1.0000 Uiso R . . . . . H462 H 0.4361 0.7088 0.0305 0.2474(16) 1.0000 Uiso R . . . . . H463 H 0.5133 0.7992 0.0009 0.2473(16) 1.0000 Uiso R . . . . . H471 H 1.0182 0.8028 0.0690 0.0846(16) 1.0000 Uiso R . . . . . H472 H 0.9063 0.7555 0.0363 0.0845(16) 1.0000 Uiso R . . . . . H481 H 0.9835 0.6785 0.1434 0.0975(16) 1.0000 Uiso R . . . . . H482 H 0.8763 0.6307 0.1062 0.0979(16) 1.0000 Uiso R . . . . . H491 H 1.0908 0.6317 0.0710 0.1329(16) 1.0000 Uiso R . . . . . H492 H 0.9858 0.5939 0.0299 0.1326(16) 1.0000 Uiso R . . . . . H501 H 1.0358 0.4960 0.1340 0.1694(16) 1.0000 Uiso R . . . . . H502 H 1.0680 0.4531 0.0712 0.1693(16) 1.0000 Uiso R . . . . . H503 H 0.9420 0.4537 0.0862 0.1696(16) 1.0000 Uiso R . . . . . H511 H 0.9207 0.8108 0.1911 0.0862(16) 1.0000 Uiso R . . . . . H512 H 0.9016 0.9313 0.1850 0.0868(16) 1.0000 Uiso R . . . . . H521 H 1.0947 0.8480 0.1567 0.1050(16) 1.0000 Uiso R . . . . . H522 H 1.0740 0.9664 0.1464 0.1045(16) 1.0000 Uiso R . . . . . H531 H 1.0644 0.9897 0.2463 0.1188(16) 1.0000 Uiso R . . . . . H532 H 1.0862 0.8702 0.2559 0.1186(16) 1.0000 Uiso R . . . . . H541 H 1.2476 0.9729 0.2757 0.1972(16) 1.0000 Uiso R . . . . . H542 H 1.2551 0.9084 0.2163 0.1972(16) 1.0000 Uiso R . . . . . H543 H 1.2369 1.0279 0.2146 0.1973(16) 1.0000 Uiso R . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.07677(13) 0.06190(11) 0.05866(11) 0.00572(7) -0.00118(8) 0.01160(8) S1 0.1086(9) 0.0881(8) 0.0928(8) 0.0186(6) -0.0052(7) 0.0383(7) S2 0.1420(13) 0.0913(9) 0.1235(12) 0.0042(8) 0.0119(10) -0.0314(9) S3 0.1190(10) 0.1118(10) 0.0770(8) -0.0085(7) 0.0064(7) 0.0374(8) S4 0.0818(9) 0.1447(13) 0.1507(13) 0.0736(11) -0.0195(8) 0.0080(8) S5 0.1116(11) 0.1087(11) 0.1760(16) -0.0442(11) 0.0367(11) -0.0319(9) S6 0.0897(9) 0.1256(11) 0.0798(8) -0.0162(7) 0.0169(7) 0.0005(8) N1 0.115(3) 0.083(3) 0.082(3) 0.011(2) -0.012(2) 0.029(2) N2 0.108(3) 0.080(3) 0.089(3) 0.005(2) 0.005(2) -0.010(2) N3 0.118(3) 0.086(3) 0.075(3) 0.002(2) 0.015(2) 0.025(2) N4 0.083(3) 0.093(3) 0.088(3) 0.023(2) -0.006(2) 0.015(2) N5 0.091(3) 0.080(3) 0.100(3) -0.001(2) -0.006(2) 0.001(2) N6 0.092(3) 0.088(3) 0.076(2) -0.001(2) 0.011(2) 0.008(2) N7 0.0706(19) 0.0495(16) 0.0602(17) 0.0061(13) 0.0041(15) 0.0129(14) N8 0.055(2) 0.078(2) 0.104(3) -0.006(2) 0.0119(19) 0.0036(17) N9 0.072(2) 0.082(2) 0.0515(17) 0.0037(16) 0.0033(15) -0.0052(17) C1 0.084(3) 0.063(2) 0.065(2) -0.001(2) 0.001(2) 0.014(2) C2 0.092(3) 0.078(3) 0.070(3) 0.004(2) 0.003(2) 0.012(3) C3 0.085(3) 0.063(2) 0.065(3) 0.007(2) -0.007(2) 0.011(2) C4 0.066(3) 0.080(3) 0.086(3) 0.015(2) 0.004(2) 0.001(2) C5 0.079(3) 0.085(3) 0.082(3) -0.016(2) 0.000(2) 0.009(3) C6 0.075(3) 0.073(3) 0.062(3) 0.002(2) -0.006(2) -0.006(2) C7 0.077(3) 0.051(2) 0.066(2) 0.0017(17) 0.0089(19) 0.0091(18) C8 0.098(3) 0.074(3) 0.069(3) 0.003(2) -0.004(2) 0.012(2) C9 0.107(4) 0.091(3) 0.077(3) -0.013(2) -0.006(3) 0.010(3) C10 0.111(4) 0.089(3) 0.120(4) -0.008(3) -0.009(3) 0.001(3) C11 0.069(2) 0.061(2) 0.067(2) 0.0047(18) 0.0086(19) 0.0170(19) C12 0.076(3) 0.071(3) 0.097(3) 0.008(2) 0.021(2) 0.013(2) C13 0.081(3) 0.086(3) 0.111(4) -0.008(3) 0.023(3) 0.004(2) C14 0.123(5) 0.125(5) 0.270(9) 0.015(6) 0.082(6) 0.008(4) C15 0.071(2) 0.054(2) 0.062(2) 0.0091(17) 0.0068(18) 0.0139(18) C16 0.077(3) 0.069(2) 0.068(2) 0.003(2) 0.004(2) 0.012(2) C17 0.083(3) 0.078(3) 0.073(3) 0.006(2) -0.001(2) 0.005(2) C18 0.105(4) 0.100(3) 0.069(3) 0.006(2) -0.004(2) 0.002(3) C19 0.081(3) 0.050(2) 0.059(2) 0.0088(16) 0.0108(19) 0.0091(18) C20 0.085(3) 0.056(2) 0.077(3) -0.0009(19) 0.019(2) 0.008(2) C21 0.099(3) 0.067(3) 0.079(3) 0.004(2) 0.020(2) 0.003(2) C22 0.124(5) 0.109(4) 0.141(5) 0.008(4) 0.066(4) 0.003(3) C23 0.081(3) 0.084(3) 0.115(4) -0.005(3) 0.021(3) -0.006(3) C24 0.111(4) 0.110(4) 0.116(4) 0.015(3) 0.002(3) -0.011(3) C25 0.157(7) 0.201(8) 0.198(9) 0.089(7) -0.025(6) -0.038(6) C26 0.272(14) 0.45(2) 0.232(12) 0.173(13) -0.087(10) -0.181(14) C27 0.063(3) 0.082(3) 0.111(4) 0.004(3) 0.007(2) 0.003(2) C28 0.091(3) 0.086(3) 0.129(4) -0.014(3) 0.011(3) 0.001(3) C29 0.119(5) 0.085(4) 0.168(6) -0.015(4) 0.005(4) -0.002(3) C30 0.153(6) 0.100(4) 0.235(9) 0.013(5) 0.000(6) 0.006(4) C31 0.062(3) 0.100(3) 0.119(4) -0.012(3) -0.002(3) 0.013(2) C32 0.079(4) 0.178(6) 0.189(7) 0.065(6) -0.010(4) 0.015(4) C33 0.102(4) 0.120(5) 0.176(6) -0.001(4) -0.006(4) 0.016(4) C34 0.148(7) 0.290(11) 0.230(9) 0.147(9) 0.018(6) 0.026(7) C35 0.062(3) 0.092(3) 0.102(3) -0.003(3) 0.012(2) 0.012(2) C36 0.081(3) 0.099(3) 0.115(4) -0.017(3) 0.003(3) 0.014(3) C37 0.116(4) 0.118(4) 0.108(4) -0.018(3) 0.005(3) 0.035(3) C38 0.178(7) 0.154(6) 0.177(7) -0.070(5) 0.004(5) 0.036(5) C39 0.084(3) 0.091(3) 0.062(2) 0.013(2) 0.003(2) -0.011(2) C40 0.095(3) 0.088(3) 0.098(3) 0.011(3) 0.001(3) -0.005(3) C41 0.099(4) 0.139(5) 0.157(6) 0.064(4) -0.027(4) -0.008(4) C42 0.104(6) 0.67(3) 0.58(2) 0.54(2) 0.068(10) 0.086(10) C43 0.074(3) 0.082(3) 0.070(3) 0.008(2) 0.010(2) -0.003(2) C44 0.084(3) 0.105(4) 0.095(3) 0.009(3) -0.005(3) -0.012(3) C45 0.083(3) 0.102(4) 0.152(5) 0.029(3) -0.020(3) 0.001(3) C46 0.121(5) 0.208(8) 0.215(8) 0.056(6) -0.071(5) -0.036(5) C47 0.073(3) 0.099(3) 0.060(2) -0.003(2) 0.007(2) 0.000(2) C48 0.087(3) 0.090(3) 0.080(3) 0.000(2) 0.010(2) 0.002(3) C49 0.137(5) 0.119(4) 0.098(4) 0.012(3) 0.023(3) 0.038(4) C50 0.124(5) 0.129(5) 0.118(4) 0.004(4) 0.016(4) 0.033(4) C51 0.088(3) 0.088(3) 0.050(2) 0.0004(19) -0.001(2) -0.001(2) C52 0.092(3) 0.102(3) 0.074(3) 0.003(2) -0.005(2) -0.016(3) C53 0.107(4) 0.117(4) 0.080(3) -0.004(3) -0.018(3) -0.005(3) C54 0.110(4) 0.191(6) 0.109(4) -0.001(4) -0.025(3) -0.034(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.10509(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Dy1 . N1 . 2.341(4) yes Dy1 . N2 . 2.340(4) yes Dy1 . N3 . 2.350(4) yes Dy1 . N4 . 2.333(4) yes Dy1 . N5 . 2.340(4) yes Dy1 . N6 . 2.364(4) yes S1 . C1 . 1.602(4) yes S2 . C2 . 1.599(5) yes S3 . C3 . 1.607(5) yes S4 . C4 . 1.607(5) yes S5 . C5 . 1.599(5) yes S6 . C6 . 1.609(5) yes N1 . C1 . 1.152(5) yes N2 . C2 . 1.147(5) yes N3 . C3 . 1.150(5) yes N4 . C4 . 1.146(5) yes N5 . C5 . 1.148(5) yes N6 . C6 . 1.152(5) yes N7 . C7 . 1.520(4) yes N7 . C11 . 1.519(4) yes N7 . C15 . 1.519(4) yes N7 . C19 . 1.523(4) yes N8 . C23 . 1.507(6) yes N8 . C27 . 1.527(5) yes N8 . C31 . 1.524(5) yes N8 . C35 . 1.513(5) yes N9 . C39 . 1.523(5) yes N9 . C43 . 1.517(5) yes N9 . C47 . 1.520(5) yes N9 . C51 . 1.522(4) yes C7 . C8 . 1.515(5) yes C7 . H71 . 0.976 no C7 . H72 . 0.967 no C8 . C9 . 1.524(6) yes C8 . H81 . 0.977 no C8 . H82 . 0.966 no C9 . C10 . 1.491(6) yes C9 . H91 . 0.962 no C9 . H92 . 0.970 no C10 . H101 . 0.970 no C10 . H102 . 0.967 no C10 . H103 . 0.968 no C11 . C12 . 1.507(5) yes C11 . H111 . 0.979 no C11 . H112 . 0.985 no C12 . C13 . 1.512(5) yes C12 . H121 . 0.965 no C12 . H122 . 0.976 no C13 . C14 . 1.483(6) yes C13 . H131 . 1.016 no C13 . H132 . 0.970 no C14 . H141 . 0.976 no C14 . H142 . 0.974 no C14 . H143 . 0.969 no C15 . C16 . 1.508(5) yes C15 . H151 . 0.981 no C15 . H152 . 0.980 no C16 . C17 . 1.510(5) yes C16 . H161 . 0.970 no C16 . H162 . 0.971 no C17 . C18 . 1.508(6) yes C17 . H171 . 0.981 no C17 . H172 . 0.972 no C18 . H181 . 0.959 no C18 . H182 . 0.967 no C18 . H183 . 0.968 no C19 . C20 . 1.501(5) yes C19 . H191 . 0.981 no C19 . H192 . 0.969 no C20 . C21 . 1.520(5) yes C20 . H201 . 0.968 no C20 . H202 . 0.955 no C21 . C22 . 1.491(6) yes C21 . H211 . 0.973 no C21 . H212 . 0.972 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.499(7) yes C23 . H231 . 0.977 no C23 . H232 . 0.968 no C24 . C25 . 1.505(8) yes C24 . H241 . 0.963 no C24 . H242 . 0.969 no C25 . C26 . 1.247(9) yes C25 . H251 . 1.024 no C25 . H252 . 0.959 no C26 . H261 . 0.950 no C26 . H262 . 0.950 no C26 . H263 . 0.950 no C27 . C28 . 1.507(6) yes C27 . H271 . 0.968 no C27 . H272 . 0.975 no C28 . C29 . 1.520(6) yes C28 . H281 . 0.980 no C28 . H282 . 0.979 no C29 . C30 . 1.520(8) yes C29 . H291 . 0.998 no C29 . H292 . 0.977 no C30 . H301 . 0.975 no C30 . H302 . 0.980 no C30 . H303 . 0.977 no C31 . C32 . 1.510(7) yes C31 . H311 . 0.972 no C31 . H312 . 0.972 no C32 . C33 . 1.443(7) yes C32 . H321 . 0.965 no C32 . H322 . 0.966 no C33 . C34 . 1.474(8) yes C33 . H331 . 0.967 no C33 . H332 . 0.973 no C34 . H341 . 0.964 no C34 . H342 . 0.965 no C34 . H343 . 0.963 no C35 . C36 . 1.510(6) yes C35 . H351 . 0.977 no C35 . H352 . 0.976 no C36 . C37 . 1.517(6) yes C36 . H361 . 0.975 no C36 . H362 . 0.971 no C37 . C38 . 1.489(7) yes C37 . H371 . 0.972 no C37 . H372 . 0.963 no C38 . H381 . 0.958 no C38 . H382 . 0.957 no C38 . H383 . 0.958 no C39 . C40 . 1.502(6) yes C39 . H391 . 0.961 no C39 . H392 . 0.964 no C40 . C41 . 1.516(6) yes C40 . H401 . 0.967 no C40 . H402 . 0.964 no C41 . C42 . 1.131(8) yes C41 . H411 . 0.974 no C41 . H412 . 0.980 no C42 . H421 . 0.950 no C42 . H422 . 0.950 no C42 . H423 . 0.950 no C43 . C44 . 1.498(5) yes C43 . H431 . 0.971 no C43 . H432 . 0.969 no C44 . C45 . 1.508(6) yes C44 . H441 . 0.968 no C44 . H442 . 0.976 no C45 . C46 . 1.485(7) yes C45 . H451 . 0.965 no C45 . H452 . 0.982 no C46 . H461 . 0.972 no C46 . H462 . 0.966 no C46 . H463 . 0.973 no C47 . C48 . 1.505(6) yes C47 . H471 . 0.981 no C47 . H472 . 0.983 no C48 . C49 . 1.501(6) yes C48 . H481 . 0.978 no C48 . H482 . 0.975 no C49 . C50 . 1.499(7) yes C49 . H491 . 0.978 no C49 . H492 . 0.961 no C50 . H501 . 0.970 no C50 . H502 . 0.980 no C50 . H503 . 0.977 no C51 . C52 . 1.512(6) yes C51 . H511 . 0.977 no C51 . H512 . 0.976 no C52 . C53 . 1.494(6) yes C52 . H521 . 0.974 no C52 . H522 . 0.968 no C53 . C54 . 1.494(7) yes C53 . H531 . 0.977 no C53 . H532 . 0.981 no C54 . H541 . 0.960 no C54 . H542 . 0.966 no C54 . H543 . 0.962 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Dy1 . N2 . 87.19(14) yes N1 . Dy1 . N3 . 89.83(14) yes N2 . Dy1 . N3 . 89.66(14) yes N1 . Dy1 . N4 . 175.39(14) yes N2 . Dy1 . N4 . 88.71(13) yes N3 . Dy1 . N4 . 88.05(13) yes N1 . Dy1 . N5 . 90.65(13) yes N2 . Dy1 . N5 . 177.72(14) yes N3 . Dy1 . N5 . 89.61(14) yes N4 . Dy1 . N5 . 93.43(13) yes N1 . Dy1 . N6 . 88.02(13) yes N2 . Dy1 . N6 . 91.69(13) yes N3 . Dy1 . N6 . 177.40(14) yes N4 . Dy1 . N6 . 94.20(13) yes N5 . Dy1 . N6 . 88.95(13) yes Dy1 . N1 . C1 . 172.7(4) yes Dy1 . N2 . C2 . 172.3(4) yes Dy1 . N3 . C3 . 174.6(3) yes Dy1 . N4 . C4 . 176.5(4) yes Dy1 . N5 . C5 . 172.7(4) yes Dy1 . N6 . C6 . 174.0(4) yes C7 . N7 . C11 . 111.8(3) yes C7 . N7 . C15 . 106.6(2) yes C11 . N7 . C15 . 110.5(3) yes C7 . N7 . C19 . 110.9(3) yes C11 . N7 . C19 . 106.3(2) yes C15 . N7 . C19 . 110.8(3) yes C23 . N8 . C27 . 110.9(4) yes C23 . N8 . C31 . 108.2(3) yes C27 . N8 . C31 . 110.5(3) yes C23 . N8 . C35 . 111.1(3) yes C27 . N8 . C35 . 106.4(3) yes C31 . N8 . C35 . 109.7(3) yes C39 . N9 . C43 . 111.1(3) yes C39 . N9 . C47 . 106.3(3) yes C43 . N9 . C47 . 110.8(3) yes C39 . N9 . C51 . 110.8(3) yes C43 . N9 . C51 . 106.9(3) yes C47 . N9 . C51 . 111.0(3) yes S1 . C1 . N1 . 178.7(4) yes S2 . C2 . N2 . 179.7(5) yes S3 . C3 . N3 . 179.1(4) yes S4 . C4 . N4 . 179.0(4) yes S5 . C5 . N5 . 179.8(5) yes S6 . C6 . N6 . 178.8(4) yes N7 . C7 . C8 . 115.9(3) yes N7 . C7 . H71 . 107.5 no C8 . C7 . H71 . 108.2 no N7 . C7 . H72 . 105.8 no C8 . C7 . H72 . 109.8 no H71 . C7 . H72 . 109.6 no C7 . C8 . C9 . 111.3(3) yes C7 . C8 . H81 . 109.1 no C9 . C8 . H81 . 108.4 no C7 . C8 . H82 . 108.3 no C9 . C8 . H82 . 109.0 no H81 . C8 . H82 . 110.7 no C8 . C9 . C10 . 115.0(4) yes C8 . C9 . H91 . 108.6 no C10 . C9 . H91 . 105.6 no C8 . C9 . H92 . 107.5 no C10 . C9 . H92 . 109.6 no H91 . C9 . H92 . 110.4 no C9 . C10 . H101 . 107.2 no C9 . C10 . H102 . 108.4 no H101 . C10 . H102 . 110.0 no C9 . C10 . H103 . 108.9 no H101 . C10 . H103 . 111.1 no H102 . C10 . H103 . 111.1 no N7 . C11 . C12 . 116.3(3) yes N7 . C11 . H111 . 106.6 no C12 . C11 . H111 . 108.3 no N7 . C11 . H112 . 106.7 no C12 . C11 . H112 . 107.4 no H111 . C11 . H112 . 111.6 no C11 . C12 . C13 . 110.6(3) yes C11 . C12 . H121 . 108.3 no C13 . C12 . H121 . 108.4 no C11 . C12 . H122 . 109.3 no C13 . C12 . H122 . 109.7 no H121 . C12 . H122 . 110.6 no C12 . C13 . C14 . 113.6(4) yes C12 . C13 . H131 . 109.2 no C14 . C13 . H131 . 105.8 no C12 . C13 . H132 . 107.5 no C14 . C13 . H132 . 109.3 no H131 . C13 . H132 . 111.5 no C13 . C14 . H141 . 108.8 no C13 . C14 . H142 . 110.7 no H141 . C14 . H142 . 110.3 no C13 . C14 . H143 . 107.3 no H141 . C14 . H143 . 109.8 no H142 . C14 . H143 . 109.9 no N7 . C15 . C16 . 116.5(3) yes N7 . C15 . H151 . 107.3 no C16 . C15 . H151 . 108.1 no N7 . C15 . H152 . 106.5 no C16 . C15 . H152 . 108.1 no H151 . C15 . H152 . 110.2 no C15 . C16 . C17 . 111.3(3) yes C15 . C16 . H161 . 108.4 no C17 . C16 . H161 . 109.2 no C15 . C16 . H162 . 108.9 no C17 . C16 . H162 . 109.3 no H161 . C16 . H162 . 109.8 no C16 . C17 . C18 . 113.2(4) yes C16 . C17 . H171 . 108.0 no C18 . C17 . H171 . 109.0 no C16 . C17 . H172 . 108.5 no C18 . C17 . H172 . 108.9 no H171 . C17 . H172 . 109.1 no C17 . C18 . H181 . 108.3 no C17 . C18 . H182 . 109.6 no H181 . C18 . H182 . 111.3 no C17 . C18 . H183 . 106.4 no H181 . C18 . H183 . 110.6 no H182 . C18 . H183 . 110.5 no N7 . C19 . C20 . 116.8(3) yes N7 . C19 . H191 . 107.0 no C20 . C19 . H191 . 108.3 no N7 . C19 . H192 . 105.3 no C20 . C19 . H192 . 108.2 no H191 . C19 . H192 . 111.1 no C19 . C20 . C21 . 109.7(3) yes C19 . C20 . H201 . 109.3 no C21 . C20 . H201 . 109.1 no C19 . C20 . H202 . 109.2 no C21 . C20 . H202 . 109.8 no H201 . C20 . H202 . 109.8 no C20 . C21 . C22 . 114.3(4) yes C20 . C21 . H211 . 108.6 no C22 . C21 . H211 . 107.6 no C20 . C21 . H212 . 107.8 no C22 . C21 . H212 . 108.1 no H211 . C21 . H212 . 110.4 no C21 . C22 . H221 . 109.5 no C21 . C22 . H222 . 109.3 no H221 . C22 . H222 . 109.5 no C21 . C22 . H223 . 109.6 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no N8 . C23 . C24 . 115.5(4) yes N8 . C23 . H231 . 106.9 no C24 . C23 . H231 . 106.5 no N8 . C23 . H232 . 108.3 no C24 . C23 . H232 . 108.0 no H231 . C23 . H232 . 111.7 no C23 . C24 . C25 . 109.7(5) yes C23 . C24 . H241 . 110.4 no C25 . C24 . H241 . 109.6 no C23 . C24 . H242 . 108.8 no C25 . C24 . H242 . 108.3 no H241 . C24 . H242 . 109.9 no C24 . C25 . C26 . 120.4(8) yes C24 . C25 . H251 . 105.8 no C26 . C25 . H251 . 106.0 no C24 . C25 . H252 . 109.0 no C26 . C25 . H252 . 111.1 no H251 . C25 . H252 . 102.9 no C25 . C26 . H261 . 109.7 no C25 . C26 . H262 . 109.0 no H261 . C26 . H262 . 109.5 no C25 . C26 . H263 . 109.7 no H261 . C26 . H263 . 109.5 no H262 . C26 . H263 . 109.5 no N8 . C27 . C28 . 115.3(3) yes N8 . C27 . H271 . 107.2 no C28 . C27 . H271 . 108.7 no N8 . C27 . H272 . 106.8 no C28 . C27 . H272 . 107.9 no H271 . C27 . H272 . 110.8 no C27 . C28 . C29 . 111.3(4) yes C27 . C28 . H281 . 107.8 no C29 . C28 . H281 . 109.5 no C27 . C28 . H282 . 108.5 no C29 . C28 . H282 . 108.8 no H281 . C28 . H282 . 111.0 no C28 . C29 . C30 . 113.1(5) yes C28 . C29 . H291 . 110.5 no C30 . C29 . H291 . 110.9 no C28 . C29 . H292 . 105.9 no C30 . C29 . H292 . 108.7 no H291 . C29 . H292 . 107.4 no C29 . C30 . H301 . 109.5 no C29 . C30 . H302 . 110.9 no H301 . C30 . H302 . 108.0 no C29 . C30 . H303 . 110.2 no H301 . C30 . H303 . 108.7 no H302 . C30 . H303 . 109.5 no N8 . C31 . C32 . 115.0(4) yes N8 . C31 . H311 . 107.6 no C32 . C31 . H311 . 108.4 no N8 . C31 . H312 . 106.3 no C32 . C31 . H312 . 108.6 no H311 . C31 . H312 . 111.1 no C31 . C32 . C33 . 115.8(5) yes C31 . C32 . H321 . 108.5 no C33 . C32 . H321 . 105.2 no C31 . C32 . H322 . 109.1 no C33 . C32 . H322 . 107.2 no H321 . C32 . H322 . 111.0 no C32 . C33 . C34 . 115.7(6) yes C32 . C33 . H331 . 108.6 no C34 . C33 . H331 . 108.9 no C32 . C33 . H332 . 105.7 no C34 . C33 . H332 . 106.2 no H331 . C33 . H332 . 111.7 no C33 . C34 . H341 . 107.0 no C33 . C34 . H342 . 108.7 no H341 . C34 . H342 . 111.1 no C33 . C34 . H343 . 106.8 no H341 . C34 . H343 . 111.2 no H342 . C34 . H343 . 111.7 no N8 . C35 . C36 . 115.9(3) yes N8 . C35 . H351 . 107.1 no C36 . C35 . H351 . 107.7 no N8 . C35 . H352 . 108.1 no C36 . C35 . H352 . 107.7 no H351 . C35 . H352 . 110.4 no C35 . C36 . C37 . 110.1(4) yes C35 . C36 . H361 . 108.9 no C37 . C36 . H361 . 109.3 no C35 . C36 . H362 . 108.8 no C37 . C36 . H362 . 109.4 no H361 . C36 . H362 . 110.3 no C36 . C37 . C38 . 112.6(5) yes C36 . C37 . H371 . 109.1 no C38 . C37 . H371 . 109.3 no C36 . C37 . H372 . 107.2 no C38 . C37 . H372 . 108.1 no H371 . C37 . H372 . 110.4 no C37 . C38 . H381 . 108.0 no C37 . C38 . H382 . 110.4 no H381 . C38 . H382 . 109.8 no C37 . C38 . H383 . 108.1 no H381 . C38 . H383 . 110.5 no H382 . C38 . H383 . 110.0 no N9 . C39 . C40 . 116.3(3) yes N9 . C39 . H391 . 107.8 no C40 . C39 . H391 . 108.1 no N9 . C39 . H392 . 106.7 no C40 . C39 . H392 . 107.9 no H391 . C39 . H392 . 110.1 no C39 . C40 . C41 . 110.9(4) yes C39 . C40 . H401 . 108.8 no C41 . C40 . H401 . 108.7 no C39 . C40 . H402 . 109.3 no C41 . C40 . H402 . 108.3 no H401 . C40 . H402 . 110.9 no C40 . C41 . C42 . 127.9(7) yes C40 . C41 . H411 . 107.1 no C42 . C41 . H411 . 106.5 no C40 . C41 . H412 . 103.5 no C42 . C41 . H412 . 104.8 no H411 . C41 . H412 . 105.1 no C41 . C42 . H421 . 115.4 no C41 . C42 . H422 . 116.6 no H421 . C42 . H422 . 109.5 no C41 . C42 . H423 . 95.2 no H421 . C42 . H423 . 109.5 no H422 . C42 . H423 . 109.5 no N9 . C43 . C44 . 115.6(3) yes N9 . C43 . H431 . 106.8 no C44 . C43 . H431 . 108.8 no N9 . C43 . H432 . 106.9 no C44 . C43 . H432 . 108.8 no H431 . C43 . H432 . 109.7 no C43 . C44 . C45 . 111.4(4) yes C43 . C44 . H441 . 109.5 no C45 . C44 . H441 . 108.7 no C43 . C44 . H442 . 108.6 no C45 . C44 . H442 . 107.6 no H441 . C44 . H442 . 111.1 no C44 . C45 . C46 . 113.2(5) yes C44 . C45 . H451 . 108.3 no C46 . C45 . H451 . 109.6 no C44 . C45 . H452 . 108.4 no C46 . C45 . H452 . 108.0 no H451 . C45 . H452 . 109.2 no C45 . C46 . H461 . 106.4 no C45 . C46 . H462 . 110.2 no H461 . C46 . H462 . 110.9 no C45 . C46 . H463 . 108.0 no H461 . C46 . H463 . 110.6 no H462 . C46 . H463 . 110.6 no N9 . C47 . C48 . 116.4(3) yes N9 . C47 . H471 . 107.6 no C48 . C47 . H471 . 108.9 no N9 . C47 . H472 . 107.3 no C48 . C47 . H472 . 107.4 no H471 . C47 . H472 . 109.1 no C47 . C48 . C49 . 111.0(4) yes C47 . C48 . H481 . 109.1 no C49 . C48 . H481 . 108.9 no C47 . C48 . H482 . 108.7 no C49 . C48 . H482 . 108.8 no H481 . C48 . H482 . 110.4 no C48 . C49 . C50 . 114.2(4) yes C48 . C49 . H491 . 107.6 no C50 . C49 . H491 . 108.3 no C48 . C49 . H492 . 107.0 no C50 . C49 . H492 . 108.9 no H491 . C49 . H492 . 110.9 no C49 . C50 . H501 . 107.1 no C49 . C50 . H502 . 109.3 no H501 . C50 . H502 . 110.8 no C49 . C50 . H503 . 107.5 no H501 . C50 . H503 . 110.8 no H502 . C50 . H503 . 111.2 no N9 . C51 . C52 . 115.7(3) yes N9 . C51 . H511 . 106.1 no C52 . C51 . H511 . 108.9 no N9 . C51 . H512 . 107.6 no C52 . C51 . H512 . 108.3 no H511 . C51 . H512 . 110.2 no C51 . C52 . C53 . 112.5(4) yes C51 . C52 . H521 . 109.8 no C53 . C52 . H521 . 106.6 no C51 . C52 . H522 . 109.1 no C53 . C52 . H522 . 108.7 no H521 . C52 . H522 . 110.1 no C52 . C53 . C54 . 113.4(4) yes C52 . C53 . H531 . 106.9 no C54 . C53 . H531 . 110.0 no C52 . C53 . H532 . 108.1 no C54 . C53 . H532 . 108.0 no H531 . C53 . H532 . 110.5 no C53 . C54 . H541 . 110.4 no C53 . C54 . H542 . 107.2 no H541 . C54 . H542 . 110.8 no C53 . C54 . H543 . 108.2 no H541 . C54 . H543 . 110.2 no H542 . C54 . H543 . 110.0 no _database_code_depnum_ccdc_archive 'CCDC 933722'