# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_general _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '1-6.cif' _audit_creation_date 2011-07-19 _audit_creation_method 'SHELXL 97' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Ai-xia Zheng' _publ_contact_author_email aixiazheng8411@163.com _publ_contact_author_fax 86-512-65880089 _publ_contact_author_phone 86-512-65882865 _publ_contact_author_address ; College of Chemistry, Chemical Engineering and Materials Science Suzhou University, Suzhou 215123, Jiangsu, P. R. China ; _publ_requested_category FM _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_footnote _publ_author_address ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== # TEXT _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2001). CrystalStructure. Single Crystal Structure Analysis Software. Version 3.00. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W., CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; loop_ _publ_author_name 'Ai-xia Zheng' 'Hui-Fang Wang' 'Chun-Ning Lu' 'Zhi-Gang Ren' 'Hong-Xi Li' 'Jian-Ping Lang' #============================================================================== data_data_1^.^MeOH _database_code_depnum_ccdc_archive 'CCDC 835428' #TrackingRef '1-6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C19 H26 Cd N3 S3), 2(N O3), 2(C0.50 H2 O0.50) ' _chemical_formula_sum 'C39 H56 Cd2 N8 O7 S6' _chemical_formula_weight 1166.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.3605(15) _cell_length_b 10.169(2) _cell_length_c 18.260(4) _cell_angle_alpha 76.05(3) _cell_angle_beta 85.53(3) _cell_angle_gamma 81.31(3) _cell_volume 1310.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5467 _cell_measurement_theta_min 3.0752 _cell_measurement_theta_max 27.5748 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 1.101 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7336 _exptl_absorpt_correction_T_max 0.8099 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12513 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5913 _reflns_number_gt 4197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5913 _refine_ls_number_parameters 320 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1482 _refine_ls_wR_factor_gt 0.1348 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.25570(4) 1.01290(3) 0.46749(2) 0.03953(14) Uani 1 1 d . . . S1 S 0.47840(14) 0.81918(11) 0.54235(7) 0.0375(3) Uani 1 1 d . . . S2 S 0.00760(14) 1.16180(10) 0.52730(7) 0.0359(3) Uani 1 1 d . . . S3 S 0.2920(3) 1.0068(2) 0.19617(11) 0.0925(6) Uani 1 1 d . . . N1 N 0.2595(8) 0.7095(6) 0.8766(3) 0.0857(17) Uani 1 1 d D . . N2 N -0.2383(6) 1.7005(4) 0.3100(3) 0.0529(11) Uani 1 1 d . . . N3 N 0.2604(6) 1.0382(4) 0.3447(3) 0.0534(11) Uani 1 1 d . . . C1 C 0.4020(6) 0.7851(4) 0.6380(3) 0.0410(11) Uani 1 1 d . . . C2 C 0.2443(7) 0.8562(5) 0.6660(3) 0.0483(12) Uani 1 1 d . A . H2A H 0.1693 0.9224 0.6320 0.058 Uiso 1 1 calc R . . C3 C 0.1962(7) 0.8314(6) 0.7423(3) 0.0565(14) Uani 1 1 d . . . H3A H 0.0902 0.8809 0.7598 0.068 Uiso 1 1 calc R A . C4 C 0.3055(8) 0.7329(6) 0.7929(3) 0.0579(14) Uani 1 1 d . A . C5 C 0.4597(8) 0.6598(6) 0.7663(3) 0.0611(15) Uani 1 1 d . . . H5A H 0.5333 0.5926 0.8004 0.073 Uiso 1 1 calc R A . C6 C 0.5056(7) 0.6850(5) 0.6906(3) 0.0522(13) Uani 1 1 d . A . H6A H 0.6100 0.6333 0.6735 0.063 Uiso 1 1 calc R . . C7 C 0.078(2) 0.776(2) 0.8992(11) 0.129(7) Uani 0.442(10) 1 d PDU A 1 H7A H 0.0642 0.7556 0.9539 0.194 Uiso 0.442(10) 1 calc PR A 1 H7B H -0.0182 0.7419 0.8789 0.194 Uiso 0.442(10) 1 calc PR A 1 H7C H 0.0703 0.8742 0.8797 0.194 Uiso 0.442(10) 1 calc PR A 1 C8 C 0.419(2) 0.742(2) 0.9129(11) 0.122(7) Uani 0.442(10) 1 d PDU A 1 H8A H 0.3914 0.7298 0.9667 0.183 Uiso 0.442(10) 1 calc PR A 1 H8B H 0.4384 0.8355 0.8910 0.183 Uiso 0.442(10) 1 calc PR A 1 H8C H 0.5284 0.6805 0.9044 0.183 Uiso 0.442(10) 1 calc PR A 1 C9 C 0.261(3) 0.5550(11) 0.9078(9) 0.100(5) Uani 0.442(10) 1 d PDU A 1 H9A H 0.2314 0.5366 0.9617 0.151 Uiso 0.442(10) 1 calc PR A 1 H9B H 0.3817 0.5075 0.8985 0.151 Uiso 0.442(10) 1 calc PR A 1 H9C H 0.1699 0.5234 0.8828 0.151 Uiso 0.442(10) 1 calc PR A 1 C7' C 0.214(2) 0.8521(11) 0.8931(7) 0.096(5) Uani 0.558(10) 1 d PDU A 2 H7'1 H 0.2007 0.8434 0.9473 0.144 Uiso 0.558(10) 1 calc PR A 2 H7'2 H 0.1001 0.8978 0.8699 0.144 Uiso 0.558(10) 1 calc PR A 2 H7'3 H 0.3129 0.9054 0.8725 0.144 Uiso 0.558(10) 1 calc PR A 2 C8' C 0.413(2) 0.636(2) 0.9228(10) 0.140(7) Uani 0.558(10) 1 d PDU A 2 H8'1 H 0.3707 0.6144 0.9755 0.210 Uiso 0.558(10) 1 calc PR A 2 H8'2 H 0.5098 0.6934 0.9166 0.210 Uiso 0.558(10) 1 calc PR A 2 H8'3 H 0.4596 0.5525 0.9071 0.210 Uiso 0.558(10) 1 calc PR A 2 C9' C 0.085(2) 0.6488(19) 0.8882(8) 0.128(6) Uani 0.558(10) 1 d PDU A 2 H9'1 H 0.1103 0.5552 0.8826 0.193 Uiso 0.558(10) 1 calc PR A 2 H9'2 H -0.0009 0.7016 0.8511 0.193 Uiso 0.558(10) 1 calc PR A 2 H9'3 H 0.0333 0.6498 0.9385 0.193 Uiso 0.558(10) 1 calc PR A 2 C10 C -0.0581(6) 1.3181(4) 0.4625(3) 0.0366(10) Uani 1 1 d . . . C11 C -0.1828(7) 1.4176(4) 0.4878(3) 0.0426(11) Uani 1 1 d . . . H11A H -0.2270 1.3999 0.5385 0.051 Uiso 1 1 calc R . . C12 C -0.2425(7) 1.5420(5) 0.4394(3) 0.0442(11) Uani 1 1 d . . . H12A H -0.3267 1.6080 0.4569 0.053 Uiso 1 1 calc R . . C13 C -0.1766(7) 1.5672(4) 0.3655(3) 0.0451(12) Uani 1 1 d . . . C14 C -0.0513(7) 1.4723(5) 0.3397(3) 0.0501(12) Uani 1 1 d . . . H14A H -0.0053 1.4916 0.2893 0.060 Uiso 1 1 calc R . . C15 C 0.0072(7) 1.3479(5) 0.3880(3) 0.0454(12) Uani 1 1 d . . . H15A H 0.0922 1.2830 0.3699 0.054 Uiso 1 1 calc R . . C16 C -0.3719(8) 1.7954(5) 0.3458(4) 0.0592(15) Uani 1 1 d . . . H16A H -0.3148 1.8161 0.3870 0.089 Uiso 1 1 calc R . . H16B H -0.4803 1.7523 0.3650 0.089 Uiso 1 1 calc R . . H16C H -0.4070 1.8794 0.3084 0.089 Uiso 1 1 calc R . . C17 C -0.0743(9) 1.7740(6) 0.2784(4) 0.0683(17) Uani 1 1 d . . . H17A H -0.0142 1.7932 0.3193 0.102 Uiso 1 1 calc R . . H17B H -0.1158 1.8593 0.2431 0.102 Uiso 1 1 calc R . . H17C H 0.0119 1.7167 0.2525 0.102 Uiso 1 1 calc R . . C18 C -0.3301(11) 1.6710(7) 0.2458(4) 0.081(2) Uani 1 1 d . . . H18A H -0.4350 1.6239 0.2655 0.122 Uiso 1 1 calc R . . H18B H -0.2431 1.6138 0.2200 0.122 Uiso 1 1 calc R . . H18C H -0.3712 1.7563 0.2105 0.122 Uiso 1 1 calc R . . C19 C 0.2740(7) 1.0288(5) 0.2820(3) 0.0503(12) Uani 1 1 d . . . N4 N 0.8102(16) 0.3912(16) 0.8770(5) 0.171(6) Uani 1 1 d . . . O1 O 0.644(3) 0.3554(16) 0.8900(8) 0.325(11) Uani 1 1 d . . . O2 O 0.912(2) 0.2951(19) 0.9126(8) 0.358(12) Uani 1 1 d . . . O3 O 0.825(2) 0.4290(13) 0.8278(9) 0.255(8) Uani 1 1 d . . . O4 O 0.351(5) 1.134(3) 0.9668(11) 0.292(17) Uani 0.50 1 d P . . C21 C 0.180(4) 1.103(2) 0.9216(19) 0.182(12) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0314(2) 0.0394(2) 0.0430(2) -0.00439(14) -0.00165(14) 0.00143(14) S1 0.0296(5) 0.0337(5) 0.0446(7) -0.0017(5) -0.0018(5) -0.0019(4) S2 0.0310(5) 0.0312(5) 0.0435(7) -0.0066(4) -0.0007(5) -0.0017(4) S3 0.0934(13) 0.1306(17) 0.0486(10) -0.0322(10) -0.0077(9) 0.0211(12) N1 0.098(4) 0.100(4) 0.049(3) 0.000(3) 0.002(3) -0.011(4) N2 0.063(3) 0.040(2) 0.051(3) -0.0061(19) -0.015(2) 0.0071(19) N3 0.056(3) 0.052(2) 0.047(3) -0.003(2) 0.003(2) -0.008(2) C1 0.036(2) 0.034(2) 0.049(3) -0.001(2) -0.004(2) -0.0044(18) C2 0.049(3) 0.044(3) 0.045(3) -0.004(2) -0.005(2) 0.007(2) C3 0.051(3) 0.057(3) 0.054(4) -0.010(3) 0.004(3) 0.006(2) C4 0.063(3) 0.067(3) 0.040(3) -0.003(3) -0.005(3) -0.008(3) C5 0.057(3) 0.063(3) 0.049(3) 0.012(3) -0.013(3) 0.000(3) C6 0.043(3) 0.048(3) 0.054(3) 0.003(2) 0.000(2) 0.005(2) C7 0.148(13) 0.174(15) 0.048(9) -0.025(11) 0.027(10) 0.017(13) C8 0.160(15) 0.169(19) 0.043(10) -0.025(13) -0.035(10) -0.026(16) C9 0.139(13) 0.118(12) 0.034(8) 0.006(8) 0.012(8) -0.033(10) C7' 0.111(11) 0.138(12) 0.037(7) -0.028(7) 0.003(7) -0.002(9) C8' 0.172(13) 0.162(15) 0.054(8) 0.002(11) -0.023(9) 0.044(12) C9' 0.164(12) 0.147(13) 0.055(8) 0.009(9) 0.036(9) -0.034(11) C10 0.031(2) 0.031(2) 0.048(3) -0.0111(19) -0.0015(19) -0.0026(17) C11 0.047(3) 0.037(2) 0.043(3) -0.012(2) 0.002(2) -0.002(2) C12 0.045(3) 0.034(2) 0.052(3) -0.012(2) 0.001(2) 0.001(2) C13 0.046(3) 0.030(2) 0.054(3) -0.005(2) -0.007(2) 0.0052(19) C14 0.050(3) 0.041(3) 0.052(3) -0.003(2) 0.004(2) 0.002(2) C15 0.043(3) 0.037(2) 0.052(3) -0.011(2) 0.003(2) 0.005(2) C16 0.060(3) 0.039(3) 0.073(4) -0.010(3) -0.010(3) 0.011(2) C17 0.083(4) 0.043(3) 0.071(4) -0.003(3) 0.009(3) -0.007(3) C18 0.111(6) 0.061(4) 0.071(5) -0.013(3) -0.040(4) 0.006(4) C19 0.043(3) 0.051(3) 0.051(4) -0.005(2) -0.007(2) 0.003(2) N4 0.130(7) 0.252(14) 0.054(5) 0.027(6) 0.036(5) 0.098(9) O1 0.328(19) 0.305(17) 0.199(13) 0.100(12) 0.102(13) 0.091(15) O2 0.36(2) 0.44(2) 0.167(12) -0.011(12) -0.053(11) 0.219(19) O3 0.291(15) 0.186(10) 0.199(13) 0.015(10) 0.107(12) 0.090(10) O4 0.47(4) 0.37(4) 0.095(14) -0.066(18) -0.019(19) -0.23(3) C21 0.21(3) 0.104(16) 0.20(3) -0.020(17) 0.03(2) 0.031(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.193(5) . ? Cd1 S2 2.5439(15) . ? Cd1 S1 2.5517(15) . ? Cd1 S1 2.7542(13) 2_676 ? Cd1 S2 2.8019(13) 2_576 ? S1 C1 1.760(5) . ? S1 Cd1 2.7542(13) 2_676 ? S2 C10 1.764(4) . ? S2 Cd1 2.8019(13) 2_576 ? S3 C19 1.628(7) . ? N1 C8' 1.460(8) . ? N1 C7 1.477(9) . ? N1 C9' 1.483(9) . ? N1 C8 1.503(9) . ? N1 C4 1.508(8) . ? N1 C7' 1.535(8) . ? N1 C9 1.535(9) . ? N2 C16 1.497(7) . ? N2 C18 1.509(7) . ? N2 C13 1.514(6) . ? N2 C17 1.519(8) . ? N3 C19 1.167(7) . ? C1 C6 1.397(6) . ? C1 C2 1.401(7) . ? C2 C3 1.382(8) . ? C2 H2A 0.9400 . ? C3 C4 1.390(7) . ? C3 H3A 0.9400 . ? C4 C5 1.382(8) . ? C5 C6 1.369(8) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C7' H7'3 0.9700 . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C8' H8'3 0.9700 . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C9' H9'3 0.9700 . ? C10 C15 1.385(7) . ? C10 C11 1.400(6) . ? C11 C12 1.389(6) . ? C11 H11A 0.9400 . ? C12 C13 1.376(7) . ? C12 H12A 0.9400 . ? C13 C14 1.374(7) . ? C14 C15 1.385(6) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? N4 O3 0.893(12) . ? N4 O2 1.219(14) . ? N4 O1 1.32(2) . ? O1 O3 1.815(18) . ? O4 C21 1.66(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 S2 117.95(12) . . ? N3 Cd1 S1 117.63(12) . . ? S2 Cd1 S1 124.11(5) . . ? N3 Cd1 S1 92.68(12) . 2_676 ? S2 Cd1 S1 95.17(4) . 2_676 ? S1 Cd1 S1 87.77(4) . 2_676 ? N3 Cd1 S2 85.48(12) . 2_576 ? S2 Cd1 S2 86.88(4) . 2_576 ? S1 Cd1 S2 91.89(4) . 2_576 ? S1 Cd1 S2 177.73(4) 2_676 2_576 ? C1 S1 Cd1 108.81(15) . . ? C1 S1 Cd1 104.88(16) . 2_676 ? Cd1 S1 Cd1 92.23(4) . 2_676 ? C10 S2 Cd1 110.38(16) . . ? C10 S2 Cd1 109.10(14) . 2_576 ? Cd1 S2 Cd1 93.12(4) . 2_576 ? C8' N1 C7 129.8(12) . . ? C8' N1 C9' 117.4(10) . . ? C7 N1 C9' 54.3(10) . . ? C8' N1 C8 41.5(9) . . ? C7 N1 C8 114.0(11) . . ? C9' N1 C8 146.6(11) . . ? C8' N1 C4 113.3(9) . . ? C7 N1 C4 116.4(9) . . ? C9' N1 C4 105.2(7) . . ? C8 N1 C4 107.6(9) . . ? C8' N1 C7' 107.4(9) . . ? C7 N1 C7' 52.6(10) . . ? C9' N1 C7' 106.9(9) . . ? C8 N1 C7' 70.0(10) . . ? C4 N1 C7' 105.9(6) . . ? C8' N1 C9 62.9(9) . . ? C7 N1 C9 106.5(10) . . ? C9' N1 C9 59.4(9) . . ? C8 N1 C9 104.0(9) . . ? C4 N1 C9 107.5(7) . . ? C7' N1 C9 146.2(9) . . ? C16 N2 C18 108.3(5) . . ? C16 N2 C13 112.2(4) . . ? C18 N2 C13 109.3(4) . . ? C16 N2 C17 107.6(4) . . ? C18 N2 C17 108.9(5) . . ? C13 N2 C17 110.4(4) . . ? C19 N3 Cd1 168.7(4) . . ? C6 C1 C2 116.8(5) . . ? C6 C1 S1 119.2(4) . . ? C2 C1 S1 124.0(4) . . ? C3 C2 C1 121.8(4) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119.7(5) . . ? C5 C4 N1 120.2(5) . . ? C3 C4 N1 120.0(5) . . ? C6 C5 C4 120.2(5) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C1 122.0(5) . . ? C5 C6 H6A 119.0 . . ? C1 C6 H6A 119.0 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C7' H7'1 109.5 . . ? N1 C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? N1 C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? N1 C8' H8'1 109.5 . . ? N1 C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? N1 C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? N1 C9' H9'1 109.5 . . ? N1 C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? N1 C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C15 C10 C11 118.2(4) . . ? C15 C10 S2 123.6(3) . . ? C11 C10 S2 118.2(4) . . ? C12 C11 C10 121.1(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 119.0(4) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C14 C13 C12 120.9(4) . . ? C14 C13 N2 117.8(5) . . ? C12 C13 N2 121.3(4) . . ? C13 C14 C15 119.9(5) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C14 C15 C10 120.8(4) . . ? C14 C15 H15A 119.6 . . ? C10 C15 H15A 119.6 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 S3 176.9(5) . . ? O3 N4 O2 125.0(15) . . ? O3 N4 O1 109(2) . . ? O2 N4 O1 105.4(17) . . ? N4 O1 O3 27.8(7) . . ? N4 O3 O1 43.4(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C8' H8'1 O1 0.97 2.54 3.43(2) 152.6 2_667 C5 H5A O3 0.94 2.52 3.363(14) 150.1 . C8' H8'3 O1 0.97 2.32 3.26(2) 163.1 . C2 H2A S2 0.94 2.87 3.791(5) 166.7 . C14 H14A O3 0.94 2.45 3.370(14) 164.4 2_676 C17 H17C O3 0.97 2.45 3.407(14) 168.1 2_676 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.573 _refine_diff_density_min -1.045 _refine_diff_density_rms 0.117 #===END #============================================================================== data_data_2 _database_code_depnum_ccdc_archive 'CCDC 835429' #TrackingRef '1-6.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H58 Cd2 N10 S2, 4(F6 P)' _chemical_formula_sum 'C58 H58 Cd2 F24 N10 P4 S2' _chemical_formula_weight 1763.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.798(2) _cell_length_b 12.628(3) _cell_length_c 13.622(3) _cell_angle_alpha 103.52(3) _cell_angle_beta 98.10(3) _cell_angle_gamma 106.14(3) _cell_volume 1692.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7917 _cell_measurement_theta_min 3.0672 _cell_measurement_theta_max 27.4816 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.731 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7152 _exptl_absorpt_correction_T_max 0.8408 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15462 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7574 _reflns_number_gt 6471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+1.3681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7574 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1324 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.12627(3) 0.65193(2) 0.06341(2) 0.03436(11) Uani 1 1 d . . . P1 P 0.78926(11) 0.88347(10) 0.30438(9) 0.0410(3) Uani 1 1 d . . . P2 P 0.50323(12) 0.72606(12) 0.63428(11) 0.0513(3) Uani 1 1 d . . . F1 F 0.6687(3) 0.8377(3) 0.2083(2) 0.0788(9) Uani 1 1 d . . . F2 F 0.8146(4) 0.7633(2) 0.2778(3) 0.0767(9) Uani 1 1 d . . . F3 F 0.8873(3) 0.9277(2) 0.2333(2) 0.0558(7) Uani 1 1 d . . . F4 F 0.9128(3) 0.9313(3) 0.4004(2) 0.0666(8) Uani 1 1 d . . . F5 F 0.7683(3) 1.0062(3) 0.3318(2) 0.0650(8) Uani 1 1 d . . . F6 F 0.6958(3) 0.8420(3) 0.3774(2) 0.0698(8) Uani 1 1 d . . . F7 F 0.5867(6) 0.8339(6) 0.7269(4) 0.178(3) Uani 1 1 d . . . F8 F 0.4086(5) 0.7953(5) 0.6208(4) 0.137(2) Uani 1 1 d . . . F9 F 0.4216(4) 0.6727(3) 0.7095(3) 0.0874(12) Uani 1 1 d . . . F10 F 0.4200(9) 0.6276(6) 0.5454(5) 0.255(5) Uani 1 1 d . . . F11 F 0.5845(3) 0.7773(3) 0.5580(2) 0.0686(8) Uani 1 1 d . . . F12 F 0.6082(7) 0.6728(8) 0.6612(6) 0.217(4) Uani 1 1 d . . . N1 N 0.2479(3) 0.7870(3) -0.0117(3) 0.0399(8) Uani 1 1 d . . . N2 N -0.0021(3) 0.7621(3) 0.0098(2) 0.0366(7) Uani 1 1 d . . . N3 N 0.2128(3) 0.7720(3) 0.2317(2) 0.0372(7) Uani 1 1 d . . . N4 N 0.3238(3) 0.6216(3) 0.1351(2) 0.0343(7) Uani 1 1 d . . . N9 N 0.0714(3) 0.3074(3) 0.4536(2) 0.0357(7) Uani 1 1 d . . . S1 S -0.07695(10) 0.51321(8) 0.11194(7) 0.0347(2) Uani 1 1 d . . . C1 C 0.3725(5) 0.7980(4) -0.0204(4) 0.0519(11) Uani 1 1 d . . . H1A H 0.4203 0.7631 0.0174 0.062 Uiso 1 1 calc R . . C2 C 0.4336(5) 0.8579(5) -0.0817(4) 0.0594(13) Uani 1 1 d . . . H2A H 0.5204 0.8616 -0.0876 0.071 Uiso 1 1 calc R . . C3 C 0.3660(5) 0.9122(4) -0.1344(4) 0.0580(13) Uani 1 1 d . . . H3A H 0.4056 0.9539 -0.1770 0.070 Uiso 1 1 calc R . . C4 C 0.2402(5) 0.9046(4) -0.1240(4) 0.0507(11) Uani 1 1 d . . . H4A H 0.1933 0.9432 -0.1579 0.061 Uiso 1 1 calc R . . C5 C 0.1817(4) 0.8400(3) -0.0634(3) 0.0378(9) Uani 1 1 d . . . C6 C 0.0437(4) 0.8258(3) -0.0518(3) 0.0364(8) Uani 1 1 d . . . C7 C -0.0366(5) 0.8760(4) -0.1011(3) 0.0450(10) Uani 1 1 d . . . H7A H -0.0041 0.9200 -0.1444 0.054 Uiso 1 1 calc R . . C8 C -0.1626(5) 0.8615(4) -0.0866(4) 0.0536(12) Uani 1 1 d . . . H8A H -0.2173 0.8943 -0.1206 0.064 Uiso 1 1 calc R . . C9 C -0.2081(5) 0.7980(4) -0.0214(4) 0.0558(12) Uani 1 1 d . . . H9A H -0.2936 0.7875 -0.0093 0.067 Uiso 1 1 calc R . . C10 C -0.1246(4) 0.7503(4) 0.0252(4) 0.0465(10) Uani 1 1 d . . . H10A H -0.1549 0.7075 0.0700 0.056 Uiso 1 1 calc R . . C11 C 0.1624(4) 0.8531(4) 0.2763(4) 0.0468(10) Uani 1 1 d . . . H11A H 0.0875 0.8605 0.2377 0.056 Uiso 1 1 calc R . . C12 C 0.2146(5) 0.9249(4) 0.3745(4) 0.0488(11) Uani 1 1 d . . . H12A H 0.1761 0.9798 0.4027 0.059 Uiso 1 1 calc R . . C13 C 0.3250(5) 0.9153(4) 0.4314(4) 0.0521(11) Uani 1 1 d . . . H13A H 0.3633 0.9639 0.4991 0.063 Uiso 1 1 calc R . . C14 C 0.3787(4) 0.8328(4) 0.3875(3) 0.0447(10) Uani 1 1 d . . . H14A H 0.4540 0.8249 0.4249 0.054 Uiso 1 1 calc R . . C15 C 0.3199(4) 0.7619(3) 0.2875(3) 0.0336(8) Uani 1 1 d . . . C16 C 0.3703(4) 0.6694(3) 0.2370(3) 0.0336(8) Uani 1 1 d . . . C17 C 0.4567(4) 0.6307(4) 0.2941(3) 0.0428(9) Uani 1 1 d . . . H17A H 0.4857 0.6629 0.3662 0.051 Uiso 1 1 calc R . . C18 C 0.4990(5) 0.5439(4) 0.2424(4) 0.0527(11) Uani 1 1 d . . . H18A H 0.5576 0.5167 0.2792 0.063 Uiso 1 1 calc R . . C19 C 0.4548(5) 0.4978(4) 0.1371(4) 0.0509(11) Uani 1 1 d . . . H19A H 0.4843 0.4400 0.1006 0.061 Uiso 1 1 calc R . . C20 C 0.3666(4) 0.5379(4) 0.0862(3) 0.0435(9) Uani 1 1 d . . . H20A H 0.3350 0.5055 0.0143 0.052 Uiso 1 1 calc R . . C21 C -0.0313(4) 0.4539(3) 0.2119(3) 0.0325(8) Uani 1 1 d . . . C22 C 0.0960(4) 0.4503(4) 0.2409(3) 0.0444(10) Uani 1 1 d . . . H22A H 0.1610 0.4798 0.2063 0.053 Uiso 1 1 calc R . . C23 C 0.1288(4) 0.4044(4) 0.3193(3) 0.0441(10) Uani 1 1 d . . . H23A H 0.2154 0.4031 0.3381 0.053 Uiso 1 1 calc R . . C24 C 0.0335(4) 0.3603(3) 0.3701(3) 0.0322(8) Uani 1 1 d . . . C25 C -0.0940(4) 0.3581(3) 0.3403(3) 0.0373(8) Uani 1 1 d . . . H25A H -0.1597 0.3244 0.3725 0.045 Uiso 1 1 calc R . . C26 C -0.1256(4) 0.4062(4) 0.2619(3) 0.0379(9) Uani 1 1 d . . . H26A H -0.2127 0.4062 0.2426 0.045 Uiso 1 1 calc R . . C27 C -0.0315(5) 0.2853(5) 0.5159(4) 0.0636(15) Uani 1 1 d . . . H27A H -0.0032 0.2514 0.5684 0.095 Uiso 1 1 calc R . . H27B H -0.1142 0.2328 0.4707 0.095 Uiso 1 1 calc R . . H27C H -0.0439 0.3573 0.5490 0.095 Uiso 1 1 calc R . . C28 C 0.2006(4) 0.3839(4) 0.5260(3) 0.0466(10) Uani 1 1 d . . . H28A H 0.2233 0.3481 0.5786 0.070 Uiso 1 1 calc R . . H28B H 0.1923 0.4577 0.5588 0.070 Uiso 1 1 calc R . . H28C H 0.2696 0.3951 0.4872 0.070 Uiso 1 1 calc R . . C29 C 0.0893(6) 0.1945(4) 0.4032(4) 0.0562(12) Uani 1 1 d . . . H29A H 0.1142 0.1598 0.4561 0.084 Uiso 1 1 calc R . . H29B H 0.1582 0.2079 0.3646 0.084 Uiso 1 1 calc R . . H29C H 0.0071 0.1431 0.3566 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03723(17) 0.03902(17) 0.03052(17) 0.01416(12) 0.00272(11) 0.01693(12) P1 0.0433(6) 0.0446(6) 0.0399(6) 0.0202(5) 0.0104(5) 0.0142(5) P2 0.0416(6) 0.0651(8) 0.0595(8) 0.0296(7) 0.0207(6) 0.0220(6) F1 0.0638(19) 0.095(2) 0.0572(19) 0.0245(18) -0.0107(15) 0.0040(18) F2 0.116(3) 0.0506(16) 0.081(2) 0.0312(16) 0.035(2) 0.0383(18) F3 0.0659(17) 0.0643(17) 0.0609(17) 0.0371(14) 0.0323(14) 0.0329(14) F4 0.0560(16) 0.079(2) 0.0569(18) 0.0329(16) -0.0029(14) 0.0063(15) F5 0.079(2) 0.0636(18) 0.072(2) 0.0281(16) 0.0317(17) 0.0391(16) F6 0.0608(18) 0.082(2) 0.0652(19) 0.0334(17) 0.0274(15) 0.0045(16) F7 0.141(5) 0.236(7) 0.070(3) 0.027(4) 0.018(3) -0.054(5) F8 0.145(4) 0.201(5) 0.174(5) 0.136(4) 0.095(4) 0.126(4) F9 0.094(2) 0.105(3) 0.122(3) 0.078(2) 0.077(2) 0.060(2) F10 0.301(9) 0.151(5) 0.138(5) -0.068(4) 0.128(6) -0.145(6) F11 0.0524(16) 0.102(2) 0.0608(19) 0.0435(18) 0.0196(14) 0.0199(16) F12 0.213(6) 0.360(10) 0.336(9) 0.306(9) 0.223(7) 0.241(7) N1 0.0450(19) 0.0437(19) 0.0374(19) 0.0164(16) 0.0107(15) 0.0194(16) N2 0.0426(18) 0.0360(17) 0.0323(17) 0.0112(14) 0.0045(14) 0.0154(15) N3 0.0394(17) 0.0411(18) 0.0318(17) 0.0116(14) 0.0028(14) 0.0157(15) N4 0.0333(16) 0.0395(17) 0.0346(18) 0.0149(14) 0.0057(14) 0.0161(14) N9 0.0402(17) 0.0386(17) 0.0319(17) 0.0178(14) 0.0067(14) 0.0122(14) S1 0.0399(5) 0.0397(5) 0.0283(5) 0.0141(4) 0.0050(4) 0.0163(4) C1 0.052(3) 0.057(3) 0.059(3) 0.028(2) 0.016(2) 0.025(2) C2 0.058(3) 0.069(3) 0.070(3) 0.036(3) 0.027(3) 0.030(3) C3 0.072(3) 0.061(3) 0.056(3) 0.032(3) 0.028(3) 0.025(3) C4 0.067(3) 0.049(2) 0.048(3) 0.024(2) 0.015(2) 0.027(2) C5 0.052(2) 0.0327(19) 0.027(2) 0.0066(16) 0.0028(17) 0.0170(18) C6 0.050(2) 0.0301(18) 0.0256(19) 0.0052(15) -0.0010(17) 0.0147(17) C7 0.056(3) 0.040(2) 0.042(2) 0.0165(19) -0.001(2) 0.022(2) C8 0.055(3) 0.048(3) 0.056(3) 0.016(2) -0.010(2) 0.024(2) C9 0.046(2) 0.061(3) 0.064(3) 0.021(3) 0.000(2) 0.025(2) C10 0.045(2) 0.047(2) 0.053(3) 0.019(2) 0.008(2) 0.020(2) C11 0.041(2) 0.055(3) 0.047(3) 0.014(2) 0.0054(19) 0.022(2) C12 0.048(2) 0.041(2) 0.054(3) 0.004(2) 0.016(2) 0.017(2) C13 0.048(3) 0.052(3) 0.041(3) -0.004(2) 0.003(2) 0.011(2) C14 0.038(2) 0.048(2) 0.039(2) 0.0055(19) -0.0020(18) 0.0115(19) C15 0.0329(18) 0.0346(19) 0.034(2) 0.0135(16) 0.0053(16) 0.0102(16) C16 0.0315(18) 0.0313(18) 0.037(2) 0.0126(16) 0.0038(16) 0.0079(15) C17 0.037(2) 0.045(2) 0.042(2) 0.0130(19) -0.0047(18) 0.0123(18) C18 0.044(2) 0.047(2) 0.065(3) 0.016(2) -0.006(2) 0.021(2) C19 0.046(2) 0.046(2) 0.061(3) 0.008(2) 0.003(2) 0.026(2) C20 0.041(2) 0.049(2) 0.042(2) 0.0096(19) 0.0076(18) 0.0201(19) C21 0.0342(18) 0.0368(19) 0.0283(19) 0.0103(16) 0.0053(15) 0.0140(16) C22 0.0320(19) 0.059(3) 0.052(3) 0.035(2) 0.0128(18) 0.0120(19) C23 0.0295(19) 0.059(3) 0.053(3) 0.032(2) 0.0081(18) 0.0160(19) C24 0.0342(18) 0.0330(18) 0.031(2) 0.0144(16) 0.0044(15) 0.0103(16) C25 0.0330(19) 0.048(2) 0.034(2) 0.0199(18) 0.0100(16) 0.0109(17) C26 0.0319(19) 0.052(2) 0.035(2) 0.0207(19) 0.0075(16) 0.0156(18) C27 0.055(3) 0.101(4) 0.057(3) 0.057(3) 0.021(2) 0.026(3) C28 0.050(2) 0.048(2) 0.036(2) 0.0107(19) -0.0036(19) 0.013(2) C29 0.081(4) 0.042(2) 0.047(3) 0.018(2) 0.004(2) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.326(3) . ? Cd1 N1 2.372(3) . ? Cd1 N2 2.378(3) . ? Cd1 N4 2.386(3) . ? Cd1 S1 2.6520(15) 2_565 ? Cd1 S1 2.6711(13) . ? Cd1 Cd1 3.860(2) 2_565 ? P1 F1 1.578(3) . ? P1 F2 1.584(3) . ? P1 F6 1.585(3) . ? P1 F5 1.595(3) . ? P1 F4 1.596(3) . ? P1 F3 1.607(3) . ? P2 F10 1.479(5) . ? P2 F12 1.515(4) . ? P2 F8 1.537(4) . ? P2 F7 1.566(6) . ? P2 F11 1.588(3) . ? P2 F9 1.590(3) . ? N1 C1 1.339(6) . ? N1 C5 1.342(5) . ? N2 C10 1.341(5) . ? N2 C6 1.344(5) . ? N3 C15 1.345(5) . ? N3 C11 1.352(5) . ? N4 C16 1.336(5) . ? N4 C20 1.342(5) . ? N9 C27 1.495(5) . ? N9 C28 1.507(5) . ? N9 C29 1.508(5) . ? N9 C24 1.512(4) . ? S1 C21 1.774(4) . ? S1 Cd1 2.6520(15) 2_565 ? C1 C2 1.371(6) . ? C1 H1A 0.9400 . ? C2 C3 1.372(7) . ? C2 H2A 0.9400 . ? C3 C4 1.365(7) . ? C3 H3A 0.9400 . ? C4 C5 1.387(6) . ? C4 H4A 0.9400 . ? C5 C6 1.486(6) . ? C6 C7 1.395(5) . ? C7 C8 1.370(7) . ? C7 H7A 0.9400 . ? C8 C9 1.382(7) . ? C8 H8A 0.9400 . ? C9 C10 1.378(6) . ? C9 H9A 0.9400 . ? C10 H10A 0.9400 . ? C11 C12 1.366(6) . ? C11 H11A 0.9400 . ? C12 C13 1.378(7) . ? C12 H12A 0.9400 . ? C13 C14 1.386(6) . ? C13 H13A 0.9400 . ? C14 C15 1.389(6) . ? C14 H14A 0.9400 . ? C15 C16 1.489(5) . ? C16 C17 1.393(5) . ? C17 C18 1.382(6) . ? C17 H17A 0.9400 . ? C18 C19 1.374(7) . ? C18 H18A 0.9400 . ? C19 C20 1.376(6) . ? C19 H19A 0.9400 . ? C20 H20A 0.9400 . ? C21 C26 1.382(5) . ? C21 C22 1.392(5) . ? C22 C23 1.378(6) . ? C22 H22A 0.9400 . ? C23 C24 1.382(5) . ? C23 H23A 0.9400 . ? C24 C25 1.370(5) . ? C25 C26 1.394(5) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C29 H29C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N1 93.86(12) . . ? N3 Cd1 N2 96.02(11) . . ? N1 Cd1 N2 69.16(11) . . ? N3 Cd1 N4 70.05(11) . . ? N1 Cd1 N4 90.78(11) . . ? N2 Cd1 N4 155.19(12) . . ? N3 Cd1 S1 163.61(8) . 2_565 ? N1 Cd1 S1 89.81(9) . 2_565 ? N2 Cd1 S1 100.21(9) . 2_565 ? N4 Cd1 S1 93.96(9) . 2_565 ? N3 Cd1 S1 94.46(9) . . ? N1 Cd1 S1 160.88(9) . . ? N2 Cd1 S1 92.85(9) . . ? N4 Cd1 S1 108.24(8) . . ? S1 Cd1 S1 87.04(5) 2_565 . ? N3 Cd1 Cd1 135.47(9) . 2_565 ? N1 Cd1 Cd1 130.65(9) . 2_565 ? N2 Cd1 Cd1 98.98(9) . 2_565 ? N4 Cd1 Cd1 105.31(8) . 2_565 ? S1 Cd1 Cd1 43.71(3) 2_565 2_565 ? S1 Cd1 Cd1 43.32(3) . 2_565 ? F1 P1 F2 90.9(2) . . ? F1 P1 F6 91.55(18) . . ? F2 P1 F6 90.18(18) . . ? F1 P1 F5 90.31(19) . . ? F2 P1 F5 178.3(2) . . ? F6 P1 F5 90.94(17) . . ? F1 P1 F4 178.90(18) . . ? F2 P1 F4 89.44(19) . . ? F6 P1 F4 89.50(17) . . ? F5 P1 F4 89.33(18) . . ? F1 P1 F3 90.05(17) . . ? F2 P1 F3 90.18(16) . . ? F6 P1 F3 178.35(19) . . ? F5 P1 F3 88.66(15) . . ? F4 P1 F3 88.90(16) . . ? F10 P2 F12 96.3(6) . . ? F10 P2 F8 92.2(5) . . ? F12 P2 F8 171.5(5) . . ? F10 P2 F7 177.1(6) . . ? F12 P2 F7 86.6(5) . . ? F8 P2 F7 85.0(4) . . ? F10 P2 F11 89.3(2) . . ? F12 P2 F11 89.0(2) . . ? F8 P2 F11 91.3(2) . . ? F7 P2 F11 90.4(2) . . ? F10 P2 F9 89.9(3) . . ? F12 P2 F9 90.5(2) . . ? F8 P2 F9 89.2(2) . . ? F7 P2 F9 90.4(2) . . ? F11 P2 F9 179.1(2) . . ? C1 N1 C5 118.1(4) . . ? C1 N1 Cd1 123.1(3) . . ? C5 N1 Cd1 117.8(3) . . ? C10 N2 C6 119.0(3) . . ? C10 N2 Cd1 123.0(3) . . ? C6 N2 Cd1 117.2(3) . . ? C15 N3 C11 117.9(3) . . ? C15 N3 Cd1 118.7(2) . . ? C11 N3 Cd1 123.4(3) . . ? C16 N4 C20 118.9(3) . . ? C16 N4 Cd1 115.9(2) . . ? C20 N4 Cd1 122.8(3) . . ? C27 N9 C28 108.6(4) . . ? C27 N9 C29 108.6(4) . . ? C28 N9 C29 107.7(3) . . ? C27 N9 C24 112.3(3) . . ? C28 N9 C24 110.9(3) . . ? C29 N9 C24 108.7(3) . . ? C21 S1 Cd1 105.59(13) . 2_565 ? C21 S1 Cd1 114.44(13) . . ? Cd1 S1 Cd1 92.96(5) 2_565 . ? N1 C1 C2 123.1(4) . . ? N1 C1 H1A 118.5 . . ? C2 C1 H1A 118.5 . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2A 120.6 . . ? C3 C2 H2A 120.6 . . ? C4 C3 C2 118.8(4) . . ? C4 C3 H3A 120.6 . . ? C2 C3 H3A 120.6 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.3(4) . . ? N2 C6 C7 120.3(4) . . ? N2 C6 C5 117.0(3) . . ? C7 C6 C5 122.6(4) . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 C8 118.2(5) . . ? C10 C9 H9A 120.9 . . ? C8 C9 H9A 120.9 . . ? N2 C10 C9 123.1(4) . . ? N2 C10 H10A 118.5 . . ? C9 C10 H10A 118.5 . . ? N3 C11 C12 123.3(4) . . ? N3 C11 H11A 118.3 . . ? C12 C11 H11A 118.3 . . ? C11 C12 C13 118.8(4) . . ? C11 C12 H12A 120.6 . . ? C13 C12 H12A 120.6 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 H13A 120.5 . . ? C14 C13 H13A 120.5 . . ? C13 C14 C15 119.3(4) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? N3 C15 C14 121.7(3) . . ? N3 C15 C16 116.4(3) . . ? C14 C15 C16 121.9(3) . . ? N4 C16 C17 121.6(3) . . ? N4 C16 C15 116.8(3) . . ? C17 C16 C15 121.5(4) . . ? C18 C17 C16 118.6(4) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 118.5(4) . . ? C18 C19 H19A 120.8 . . ? C20 C19 H19A 120.8 . . ? N4 C20 C19 122.6(4) . . ? N4 C20 H20A 118.7 . . ? C19 C20 H20A 118.7 . . ? C26 C21 C22 117.8(3) . . ? C26 C21 S1 119.5(3) . . ? C22 C21 S1 122.7(3) . . ? C23 C22 C21 121.4(4) . . ? C23 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C22 C23 C24 119.5(4) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 N9 121.1(3) . . ? C23 C24 N9 118.3(3) . . ? C24 C25 C26 119.4(3) . . ? C24 C25 H25A 120.3 . . ? C26 C25 H25A 120.3 . . ? C21 C26 C25 121.3(4) . . ? C21 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N9 C28 H28A 109.5 . . ? N9 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N9 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N9 C29 H29A 109.5 . . ? N9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C4 H4A F3 0.94 2.41 3.334(5) 168.9 2_675 C11 H11A F3 0.94 2.53 3.373(5) 149.2 1_455 C14 H14A F11 0.94 2.43 3.317(5) 157.6 . C22 H22A N4 0.94 2.60 3.507(5) 161.5 . C18 H18A F9 0.94 2.50 3.261(5) 138.1 2_666 C23 H23A F12 0.94 2.36 3.245(6) 157.3 2_666 C29 H29A F4 0.97 2.50 3.414(5) 157.0 2_666 C26 H26A F9 0.94 2.44 3.182(5) 135.3 2_566 C8 H8A F7 0.94 2.55 3.321(8) 139.5 1_454 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.124 _refine_diff_density_min -1.014 _refine_diff_density_rms 0.120 #===END #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 835430' #TrackingRef '1-6.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H58 Cd2 N10 S2, 4(F6 P)' _chemical_formula_sum 'C66 H58 Cd2 F24 N10 P4 S2' _chemical_formula_weight 1860.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.491(3) _cell_length_b 12.561(3) _cell_length_c 12.765(3) _cell_angle_alpha 105.68(3) _cell_angle_beta 98.99(3) _cell_angle_gamma 101.47(3) _cell_volume 1842.4(8) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7843 _cell_measurement_theta_min 3.3668 _cell_measurement_theta_max 27.5437 _exptl_crystal_description block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8516 _exptl_absorpt_correction_T_max 0.8516 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16613 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8273 _reflns_number_gt 5999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8273 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.39871(3) 0.50254(3) 0.60235(3) 0.04691(15) Uani 1 1 d . . . P1 P 0.0000 1.0000 0.0000 0.0776(8) Uani 1 2 d S . . P2 P 0.0000 0.5000 0.0000 0.0542(4) Uani 1 2 d S . . P3 P 0.5000 1.0000 0.0000 0.0492(4) Uani 1 2 d S . . P4 P 0.0000 1.0000 0.5000 0.0535(4) Uani 1 2 d S . . F1 F -0.0674(9) 1.012(2) 0.0784(10) 0.371(11) Uani 1 1 d . . . F2 F 0.0117(10) 1.1178(5) 0.0026(9) 0.287(8) Uani 1 1 d . . . F3 F 0.1043(5) 1.0432(4) 0.1004(5) 0.140(2) Uani 1 1 d . . . F4 F 0.0695(4) 0.6133(4) -0.0108(4) 0.0961(12) Uani 1 1 d . . . F5 F -0.0537(3) 0.5718(4) 0.0913(3) 0.0934(12) Uani 1 1 d . . . F6 F 0.0998(3) 0.5052(4) 0.0965(3) 0.0862(11) Uani 1 1 d . . . F7 F 0.3903(4) 1.0414(4) -0.0090(5) 0.1188(17) Uani 1 1 d . . . F8 F 0.5743(4) 1.1256(3) 0.0244(3) 0.0978(13) Uani 1 1 d . . . F9 F 0.5104(3) 1.0193(4) 0.1295(3) 0.0939(13) Uani 1 1 d . . . F10 F 0.0538(3) 1.1122(4) 0.5999(4) 0.1150(17) Uani 1 1 d . . . F11 F 0.0389(4) 1.0645(5) 0.4183(5) 0.126(2) Uani 1 1 d . . . F12 F 0.1148(3) 0.9615(3) 0.5119(3) 0.0702(9) Uani 1 1 d . . . S1 S 0.51231(9) 0.65279(10) 0.52446(11) 0.0482(3) Uani 1 1 d . . . N1 N 0.2759(3) 0.6212(3) 0.6419(3) 0.0475(9) Uani 1 1 d . . . N2 N 0.2302(3) 0.4279(3) 0.4627(4) 0.0477(9) Uani 1 1 d . . . N3 N 0.5290(3) 0.5869(3) 0.7783(3) 0.0471(9) Uani 1 1 d . . . N4 N 0.3769(3) 0.3800(3) 0.7121(4) 0.0502(9) Uani 1 1 d . . . N5 N 0.2345(3) 0.8744(3) 0.2574(3) 0.0446(9) Uani 1 1 d . . . C1 C 0.2967(4) 0.7150(5) 0.7306(5) 0.0609(13) Uani 1 1 d . . . H1A H 0.3558 0.7260 0.7910 0.073 Uiso 1 1 calc R . . C2 C 0.2354(4) 0.7963(5) 0.7376(5) 0.0643(14) Uani 1 1 d . . . H2A H 0.2520 0.8602 0.8018 0.077 Uiso 1 1 calc R . . C3 C 0.1512(4) 0.7822(5) 0.6501(5) 0.0610(14) Uani 1 1 d . . . H3A H 0.1090 0.8368 0.6531 0.073 Uiso 1 1 calc R . . C4 C 0.1267(4) 0.6848(4) 0.5539(5) 0.0500(11) Uani 1 1 d . . . C5 C 0.1919(3) 0.6071(4) 0.5547(4) 0.0447(10) Uani 1 1 d . . . C6 C 0.1682(3) 0.5055(4) 0.4596(4) 0.0443(10) Uani 1 1 d . . . C7 C 0.0802(4) 0.4874(5) 0.3682(4) 0.0494(11) Uani 1 1 d . . . C8 C 0.0173(4) 0.5720(5) 0.3716(5) 0.0612(15) Uani 1 1 d . . . H8A H -0.0414 0.5604 0.3106 0.073 Uiso 1 1 calc R . . C9 C 0.0395(4) 0.6665(5) 0.4584(5) 0.0578(13) Uani 1 1 d . . . H9A H -0.0019 0.7211 0.4571 0.069 Uiso 1 1 calc R . . C10 C 0.0578(4) 0.3862(6) 0.2791(5) 0.0642(15) Uani 1 1 d . . . H10A H 0.0007 0.3722 0.2159 0.077 Uiso 1 1 calc R . . C11 C 0.1187(5) 0.3079(6) 0.2838(5) 0.0692(16) Uani 1 1 d . . . H11A H 0.1027 0.2387 0.2255 0.083 Uiso 1 1 calc R . . C12 C 0.2055(4) 0.3329(5) 0.3772(5) 0.0630(14) Uani 1 1 d . . . H12A H 0.2484 0.2797 0.3795 0.076 Uiso 1 1 calc R . . C13 C 0.6016(4) 0.6899(4) 0.8144(5) 0.0553(12) Uani 1 1 d . . . H13A H 0.5899 0.7431 0.7771 0.066 Uiso 1 1 calc R . . C14 C 0.6925(4) 0.7226(5) 0.9029(5) 0.0635(14) Uani 1 1 d . . . H14A H 0.7416 0.7959 0.9251 0.076 Uiso 1 1 calc R . . C15 C 0.7094(4) 0.6454(5) 0.9576(5) 0.0620(14) Uani 1 1 d . . . H15A H 0.7721 0.6647 1.0168 0.074 Uiso 1 1 calc R . . C16 C 0.6343(4) 0.5389(5) 0.9261(4) 0.0509(11) Uani 1 1 d . . . C17 C 0.5430(4) 0.5118(4) 0.8357(4) 0.0436(10) Uani 1 1 d . . . C18 C 0.4635(4) 0.4030(4) 0.7992(4) 0.0451(10) Uani 1 1 d . . . C19 C 0.4761(4) 0.3228(5) 0.8571(4) 0.0528(12) Uani 1 1 d . . . C20 C 0.5710(5) 0.3537(5) 0.9494(4) 0.0602(14) Uani 1 1 d . . . H20A H 0.5806 0.3012 0.9881 0.072 Uiso 1 1 calc R . . C21 C 0.6454(5) 0.4549(5) 0.9814(4) 0.0569(13) Uani 1 1 d . . . H21A H 0.7065 0.4716 1.0416 0.068 Uiso 1 1 calc R . . C22 C 0.3981(5) 0.2191(5) 0.8207(5) 0.0689(15) Uani 1 1 d . . . H22A H 0.4056 0.1638 0.8564 0.083 Uiso 1 1 calc R . . C23 C 0.3089(6) 0.1957(6) 0.7319(6) 0.0762(17) Uani 1 1 d . . . H23A H 0.2537 0.1261 0.7083 0.091 Uiso 1 1 calc R . . C24 C 0.3028(5) 0.2790(5) 0.6780(5) 0.0685(15) Uani 1 1 d . . . H24A H 0.2443 0.2625 0.6154 0.082 Uiso 1 1 calc R . . C25 C 0.4226(4) 0.7125(4) 0.4489(4) 0.0452(10) Uani 1 1 d . . . C26 C 0.4258(5) 0.8298(4) 0.4939(5) 0.0630(14) Uani 1 1 d . . . H26A H 0.4702 0.8720 0.5653 0.076 Uiso 1 1 calc R . . C27 C 0.3642(5) 0.8828(5) 0.4337(5) 0.0647(15) Uani 1 1 d . . . H27A H 0.3672 0.9607 0.4637 0.078 Uiso 1 1 calc R . . C28 C 0.2979(3) 0.8192(4) 0.3283(4) 0.0441(10) Uani 1 1 d . . . C29 C 0.2860(3) 0.7042(4) 0.2891(4) 0.0400(9) Uani 1 1 d . . . H29A H 0.2362 0.6606 0.2208 0.048 Uiso 1 1 calc R . . C30 C 0.3476(3) 0.6517(4) 0.3500(4) 0.0394(9) Uani 1 1 d . . . H30A H 0.3376 0.5722 0.3227 0.047 Uiso 1 1 calc R . . C32 C 0.2666(5) 0.8546(6) 0.1479(5) 0.0726(18) Uani 1 1 d . . . H32A H 0.2539 0.7732 0.1121 0.109 Uiso 1 1 calc R . . H32B H 0.3453 0.8918 0.1592 0.109 Uiso 1 1 calc R . . H32C H 0.2217 0.8860 0.1009 0.109 Uiso 1 1 calc R . . C33 C 0.1113(4) 0.8235(5) 0.2391(5) 0.0534(12) Uani 1 1 d . . . H33A H 0.0946 0.7415 0.2042 0.080 Uiso 1 1 calc R . . H33B H 0.0701 0.8567 0.1910 0.080 Uiso 1 1 calc R . . H33C H 0.0894 0.8393 0.3102 0.080 Uiso 1 1 calc R . . C34 C 0.2560(5) 1.0026(4) 0.3121(5) 0.0652(15) Uani 1 1 d . . . H34A H 0.2135 1.0343 0.2635 0.098 Uiso 1 1 calc R . . H34B H 0.3352 1.0383 0.3251 0.098 Uiso 1 1 calc R . . H34C H 0.2330 1.0169 0.3828 0.098 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0454(2) 0.0469(2) 0.0478(2) 0.02076(17) -0.00340(15) 0.01258(15) P1 0.0848(15) 0.0419(10) 0.0807(16) 0.0190(10) -0.0436(13) 0.0075(10) P2 0.0537(10) 0.0507(10) 0.0443(10) 0.0081(8) -0.0054(8) 0.0041(8) P3 0.0631(10) 0.0369(8) 0.0482(10) 0.0194(8) 0.0090(8) 0.0081(8) P4 0.0561(10) 0.0518(10) 0.0598(12) 0.0186(9) 0.0143(9) 0.0268(9) F1 0.168(8) 0.66(3) 0.178(10) 0.022(14) 0.056(8) 0.004(12) F2 0.347(12) 0.069(3) 0.298(11) 0.055(5) -0.257(10) -0.017(5) F3 0.152(4) 0.067(3) 0.143(4) 0.027(3) -0.096(3) 0.007(3) F4 0.106(3) 0.077(2) 0.083(3) 0.033(2) -0.003(2) -0.019(2) F5 0.084(2) 0.100(3) 0.074(3) -0.004(2) 0.013(2) 0.020(2) F6 0.073(2) 0.100(3) 0.065(2) 0.022(2) -0.0231(17) 0.010(2) F7 0.101(3) 0.129(4) 0.168(5) 0.076(4) 0.046(3) 0.070(3) F8 0.143(4) 0.052(2) 0.079(3) 0.028(2) 0.012(2) -0.019(2) F9 0.109(3) 0.103(3) 0.054(2) 0.030(2) 0.013(2) -0.011(2) F10 0.073(2) 0.098(3) 0.131(4) -0.031(3) 0.005(2) 0.030(2) F11 0.128(3) 0.163(5) 0.187(5) 0.133(4) 0.105(4) 0.102(4) F12 0.0609(17) 0.085(2) 0.082(2) 0.0339(19) 0.0209(16) 0.0433(17) S1 0.0485(6) 0.0441(6) 0.0576(7) 0.0268(6) 0.0017(5) 0.0169(5) N1 0.046(2) 0.049(2) 0.045(2) 0.0154(19) -0.0007(17) 0.0129(17) N2 0.0382(18) 0.050(2) 0.051(2) 0.0161(19) 0.0009(17) 0.0090(17) N3 0.051(2) 0.049(2) 0.044(2) 0.0180(18) 0.0048(17) 0.0199(18) N4 0.051(2) 0.046(2) 0.051(2) 0.0215(19) 0.0001(18) 0.0077(18) N5 0.0443(19) 0.042(2) 0.048(2) 0.0227(18) -0.0024(16) 0.0107(16) C1 0.056(3) 0.061(3) 0.052(3) 0.010(3) -0.003(2) 0.009(3) C2 0.059(3) 0.052(3) 0.074(4) 0.008(3) 0.007(3) 0.017(3) C3 0.052(3) 0.048(3) 0.083(4) 0.019(3) 0.013(3) 0.015(2) C4 0.039(2) 0.057(3) 0.063(3) 0.034(3) 0.011(2) 0.013(2) C5 0.038(2) 0.050(3) 0.050(3) 0.024(2) 0.0058(19) 0.0102(19) C6 0.0328(19) 0.051(3) 0.048(3) 0.024(2) 0.0028(18) 0.0016(19) C7 0.036(2) 0.063(3) 0.049(3) 0.026(3) 0.0016(19) 0.006(2) C8 0.038(2) 0.083(4) 0.073(4) 0.052(4) 0.002(2) 0.009(3) C9 0.044(2) 0.062(3) 0.076(4) 0.036(3) 0.008(3) 0.016(2) C10 0.048(3) 0.090(4) 0.049(3) 0.028(3) 0.000(2) 0.005(3) C11 0.054(3) 0.078(4) 0.052(3) -0.002(3) 0.000(2) 0.005(3) C12 0.054(3) 0.062(3) 0.061(4) 0.006(3) 0.003(3) 0.015(3) C13 0.056(3) 0.048(3) 0.054(3) 0.015(2) 0.001(2) 0.007(2) C14 0.053(3) 0.066(3) 0.056(3) 0.009(3) -0.003(2) 0.005(3) C15 0.050(3) 0.079(4) 0.045(3) 0.006(3) -0.002(2) 0.017(3) C16 0.048(2) 0.067(3) 0.039(3) 0.013(2) 0.005(2) 0.026(2) C17 0.046(2) 0.049(3) 0.039(2) 0.013(2) 0.0075(19) 0.021(2) C18 0.050(2) 0.053(3) 0.039(2) 0.017(2) 0.011(2) 0.024(2) C19 0.065(3) 0.060(3) 0.048(3) 0.028(2) 0.016(2) 0.031(3) C20 0.073(3) 0.082(4) 0.049(3) 0.037(3) 0.018(3) 0.045(3) C21 0.061(3) 0.080(4) 0.042(3) 0.025(3) 0.009(2) 0.039(3) C22 0.085(4) 0.065(4) 0.074(4) 0.042(3) 0.023(3) 0.026(3) C23 0.080(4) 0.063(4) 0.086(5) 0.042(4) 0.004(3) 0.005(3) C24 0.065(3) 0.063(3) 0.071(4) 0.032(3) -0.003(3) 0.001(3) C25 0.044(2) 0.035(2) 0.057(3) 0.024(2) -0.001(2) 0.0082(18) C26 0.071(3) 0.037(2) 0.066(4) 0.012(2) -0.020(3) 0.011(2) C27 0.069(3) 0.043(3) 0.070(4) 0.017(3) -0.015(3) 0.015(2) C28 0.037(2) 0.041(2) 0.054(3) 0.024(2) -0.0055(19) 0.0081(18) C29 0.043(2) 0.037(2) 0.039(2) 0.0113(19) 0.0043(18) 0.0124(18) C30 0.044(2) 0.033(2) 0.042(2) 0.0128(19) 0.0070(18) 0.0105(18) C32 0.068(3) 0.106(5) 0.082(4) 0.063(4) 0.031(3) 0.049(3) C33 0.042(2) 0.056(3) 0.065(3) 0.020(3) 0.005(2) 0.021(2) C34 0.067(3) 0.044(3) 0.084(4) 0.033(3) -0.012(3) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N4 2.350(4) . ? Cd1 N1 2.361(4) . ? Cd1 N2 2.372(4) . ? Cd1 N3 2.388(4) . ? Cd1 S1 2.6371(14) . ? Cd1 S1 2.7165(16) 2_666 ? P1 F1 1.402(12) 2_575 ? P1 F1 1.402(12) . ? P1 F2 1.448(5) . ? P1 F2 1.448(5) 2_575 ? P1 F3 1.567(4) 2_575 ? P1 F3 1.567(4) . ? P2 F4 1.565(4) . ? P2 F4 1.565(4) 2_565 ? P2 F6 1.587(3) 2_565 ? P2 F6 1.587(3) . ? P2 F5 1.593(4) 2_565 ? P2 F5 1.593(4) . ? P3 F7 1.558(4) 2_675 ? P3 F7 1.558(4) . ? P3 F8 1.583(3) . ? P3 F8 1.583(3) 2_675 ? P3 F9 1.585(4) 2_675 ? P3 F9 1.585(4) . ? P4 F11 1.562(4) . ? P4 F11 1.562(4) 2_576 ? P4 F10 1.564(4) . ? P4 F10 1.564(4) 2_576 ? P4 F12 1.601(3) . ? P4 F12 1.601(3) 2_576 ? S1 C25 1.770(4) . ? S1 Cd1 2.7165(16) 2_666 ? N1 C1 1.343(7) . ? N1 C5 1.351(6) . ? N2 C12 1.325(7) . ? N2 C6 1.364(6) . ? N3 C13 1.338(7) . ? N3 C17 1.362(6) . ? N4 C24 1.328(7) . ? N4 C18 1.348(6) . ? N5 C32 1.485(7) . ? N5 C33 1.499(6) . ? N5 C28 1.504(5) . ? N5 C34 1.520(7) . ? C1 C2 1.386(8) . ? C1 H1A 0.9400 . ? C2 C3 1.356(8) . ? C2 H2A 0.9400 . ? C3 C4 1.421(8) . ? C3 H3A 0.9400 . ? C4 C5 1.392(6) . ? C4 C9 1.435(7) . ? C5 C6 1.446(7) . ? C6 C7 1.407(6) . ? C7 C10 1.402(8) . ? C7 C8 1.437(8) . ? C8 C9 1.332(9) . ? C8 H8A 0.9400 . ? C9 H9A 0.9400 . ? C10 C11 1.366(9) . ? C10 H10A 0.9400 . ? C11 C12 1.397(8) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 C14 1.377(8) . ? C13 H13A 0.9400 . ? C14 C15 1.369(8) . ? C14 H14A 0.9400 . ? C15 C16 1.387(8) . ? C15 H15A 0.9400 . ? C16 C17 1.404(7) . ? C16 C21 1.437(7) . ? C17 C18 1.428(7) . ? C18 C19 1.420(6) . ? C19 C22 1.374(8) . ? C19 C20 1.441(8) . ? C20 C21 1.333(8) . ? C20 H20A 0.9400 . ? C21 H21A 0.9400 . ? C22 C23 1.381(9) . ? C22 H22A 0.9400 . ? C23 C24 1.407(8) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 C30 1.371(7) . ? C25 C26 1.419(7) . ? C26 C27 1.386(7) . ? C26 H26A 0.9400 . ? C27 C28 1.394(7) . ? C27 H27A 0.9400 . ? C28 C29 1.364(6) . ? C29 C30 1.386(6) . ? C29 H29A 0.9400 . ? C30 H30A 0.9400 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N1 106.24(14) . . ? N4 Cd1 N2 102.21(14) . . ? N1 Cd1 N2 70.66(14) . . ? N4 Cd1 N3 70.19(14) . . ? N1 Cd1 N3 95.92(14) . . ? N2 Cd1 N3 162.59(14) . . ? N4 Cd1 S1 155.27(10) . . ? N1 Cd1 S1 89.26(10) . . ? N2 Cd1 S1 101.08(10) . . ? N3 Cd1 S1 89.47(10) . . ? N4 Cd1 S1 86.24(11) . 2_666 ? N1 Cd1 S1 157.19(10) . 2_666 ? N2 Cd1 S1 88.29(11) . 2_666 ? N3 Cd1 S1 106.37(10) . 2_666 ? S1 Cd1 S1 86.23(4) . 2_666 ? F1 P1 F1 180(2) 2_575 . ? F1 P1 F2 89.0(9) 2_575 . ? F1 P1 F2 91.0(9) . . ? F1 P1 F2 91.0(9) 2_575 2_575 ? F1 P1 F2 89.0(9) . 2_575 ? F2 P1 F2 180.0(9) . 2_575 ? F1 P1 F3 87.8(5) 2_575 2_575 ? F1 P1 F3 92.2(5) . 2_575 ? F2 P1 F3 92.1(3) . 2_575 ? F2 P1 F3 87.9(3) 2_575 2_575 ? F1 P1 F3 92.2(5) 2_575 . ? F1 P1 F3 87.8(5) . . ? F2 P1 F3 87.9(3) . . ? F2 P1 F3 92.1(3) 2_575 . ? F3 P1 F3 180.0(3) 2_575 . ? F4 P2 F4 180.0(3) . 2_565 ? F4 P2 F6 90.7(2) . 2_565 ? F4 P2 F6 89.3(2) 2_565 2_565 ? F4 P2 F6 89.3(2) . . ? F4 P2 F6 90.7(2) 2_565 . ? F6 P2 F6 180.0(3) 2_565 . ? F4 P2 F5 89.7(2) . 2_565 ? F4 P2 F5 90.3(2) 2_565 2_565 ? F6 P2 F5 89.5(2) 2_565 2_565 ? F6 P2 F5 90.5(2) . 2_565 ? F4 P2 F5 90.3(2) . . ? F4 P2 F5 89.7(2) 2_565 . ? F6 P2 F5 90.5(2) 2_565 . ? F6 P2 F5 89.5(2) . . ? F5 P2 F5 180.0(2) 2_565 . ? F7 P3 F7 180.000(1) 2_675 . ? F7 P3 F8 88.5(3) 2_675 . ? F7 P3 F8 91.5(3) . . ? F7 P3 F8 91.5(3) 2_675 2_675 ? F7 P3 F8 88.5(3) . 2_675 ? F8 P3 F8 180.0(3) . 2_675 ? F7 P3 F9 91.3(3) 2_675 2_675 ? F7 P3 F9 88.7(3) . 2_675 ? F8 P3 F9 89.1(2) . 2_675 ? F8 P3 F9 90.9(2) 2_675 2_675 ? F7 P3 F9 88.7(3) 2_675 . ? F7 P3 F9 91.3(3) . . ? F8 P3 F9 90.9(2) . . ? F8 P3 F9 89.1(2) 2_675 . ? F9 P3 F9 180.0(3) 2_675 . ? F11 P4 F11 180.0(3) . 2_576 ? F11 P4 F10 89.4(3) . . ? F11 P4 F10 90.6(3) 2_576 . ? F11 P4 F10 90.6(3) . 2_576 ? F11 P4 F10 89.4(3) 2_576 2_576 ? F10 P4 F10 180.0(3) . 2_576 ? F11 P4 F12 89.66(19) . . ? F11 P4 F12 90.34(19) 2_576 . ? F10 P4 F12 91.3(2) . . ? F10 P4 F12 88.7(2) 2_576 . ? F11 P4 F12 90.34(19) . 2_576 ? F11 P4 F12 89.66(19) 2_576 2_576 ? F10 P4 F12 88.7(2) . 2_576 ? F10 P4 F12 91.3(2) 2_576 2_576 ? F12 P4 F12 180.000(1) . 2_576 ? C25 S1 Cd1 111.69(15) . . ? C25 S1 Cd1 115.15(18) . 2_666 ? Cd1 S1 Cd1 93.77(4) . 2_666 ? C1 N1 C5 117.8(4) . . ? C1 N1 Cd1 125.6(3) . . ? C5 N1 Cd1 114.6(3) . . ? C12 N2 C6 118.6(4) . . ? C12 N2 Cd1 126.3(3) . . ? C6 N2 Cd1 113.3(3) . . ? C13 N3 C17 118.0(4) . . ? C13 N3 Cd1 126.9(3) . . ? C17 N3 Cd1 113.8(3) . . ? C24 N4 C18 119.3(4) . . ? C24 N4 Cd1 123.6(4) . . ? C18 N4 Cd1 114.8(3) . . ? C32 N5 C33 109.3(4) . . ? C32 N5 C28 110.0(4) . . ? C33 N5 C28 109.1(3) . . ? C32 N5 C34 108.4(4) . . ? C33 N5 C34 107.4(4) . . ? C28 N5 C34 112.5(4) . . ? N1 C1 C2 123.4(5) . . ? N1 C1 H1A 118.3 . . ? C2 C1 H1A 118.3 . . ? C3 C2 C1 118.8(6) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3A 120.1 . . ? C4 C3 H3A 120.1 . . ? C5 C4 C3 117.4(5) . . ? C5 C4 C9 120.5(5) . . ? C3 C4 C9 122.2(5) . . ? N1 C5 C4 122.7(5) . . ? N1 C5 C6 118.1(4) . . ? C4 C5 C6 119.2(4) . . ? N2 C6 C7 121.8(5) . . ? N2 C6 C5 118.7(4) . . ? C7 C6 C5 119.4(4) . . ? C10 C7 C6 117.7(5) . . ? C10 C7 C8 123.6(5) . . ? C6 C7 C8 118.7(5) . . ? C9 C8 C7 122.2(5) . . ? C9 C8 H8A 118.9 . . ? C7 C8 H8A 118.9 . . ? C8 C9 C4 120.0(5) . . ? C8 C9 H9A 120.0 . . ? C4 C9 H9A 120.0 . . ? C11 C10 C7 120.2(5) . . ? C11 C10 H10A 119.9 . . ? C7 C10 H10A 119.9 . . ? C10 C11 C12 118.5(6) . . ? C10 C11 H11A 120.7 . . ? C12 C11 H11A 120.7 . . ? N2 C12 C11 123.2(5) . . ? N2 C12 H12A 118.4 . . ? C11 C12 H12A 118.4 . . ? N3 C13 C14 123.9(5) . . ? N3 C13 H13A 118.1 . . ? C14 C13 H13A 118.1 . . ? C15 C14 C13 118.1(5) . . ? C15 C14 H14A 120.9 . . ? C13 C14 H14A 120.9 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C15 C16 C17 118.5(5) . . ? C15 C16 C21 123.2(5) . . ? C17 C16 C21 118.3(5) . . ? N3 C17 C16 121.2(5) . . ? N3 C17 C18 118.0(4) . . ? C16 C17 C18 120.8(4) . . ? N4 C18 C19 121.6(5) . . ? N4 C18 C17 119.1(4) . . ? C19 C18 C17 119.3(4) . . ? C22 C19 C18 118.1(5) . . ? C22 C19 C20 123.6(5) . . ? C18 C19 C20 118.3(5) . . ? C21 C20 C19 121.8(5) . . ? C21 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? C20 C21 C16 121.5(5) . . ? C20 C21 H21A 119.2 . . ? C16 C21 H21A 119.2 . . ? C19 C22 C23 120.4(5) . . ? C19 C22 H22A 119.8 . . ? C23 C22 H22A 119.8 . . ? C22 C23 C24 118.2(6) . . ? C22 C23 H23A 120.9 . . ? C24 C23 H23A 120.9 . . ? N4 C24 C23 122.4(6) . . ? N4 C24 H24A 118.8 . . ? C23 C24 H24A 118.8 . . ? C30 C25 C26 117.3(4) . . ? C30 C25 S1 124.1(3) . . ? C26 C25 S1 118.6(4) . . ? C27 C26 C25 120.8(5) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 119.2(5) . . ? C26 C27 H27A 120.4 . . ? C28 C27 H27A 120.4 . . ? C29 C28 C27 120.3(4) . . ? C29 C28 N5 118.6(4) . . ? C27 C28 N5 121.1(4) . . ? C28 C29 C30 119.9(4) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C25 C30 C29 121.9(4) . . ? C25 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? N5 C32 H32A 109.5 . . ? N5 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N5 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C33 H33A 109.5 . . ? N5 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N5 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N5 C34 H34A 109.5 . . ? N5 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N5 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C1 H1A F8 0.94 2.47 3.185(7) 132.4 2_676 C11 H11A F3 0.94 2.55 3.462(8) 164.4 1_545 C29 H29A F6 0.94 2.32 3.207(6) 156.7 . C32 H32B F9 0.97 2.49 3.404(7) 156.1 . C33 H33A F5 0.97 2.45 3.282(7) 144.1 . C33 H33C F12 0.97 2.55 3.434(7) 151.7 . C34 H34A F3 0.97 2.35 3.269(6) 158.6 . C34 H34C F12 0.97 2.52 3.410(8) 152.5 . C33 H33A F5 0.97 2.45 3.282(7) 144.1 . C20 H20A F8 0.94 2.36 3.263(6) 160.5 1_546 C33 H33C F10 0.97 2.36 3.197(7) 143.7 2_576 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.754 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.166 #===END #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 835431' #TrackingRef '1-6.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Cd N4 S2, 2(F6 P)' _chemical_formula_sum 'C32 H38 Cd F12 N4 P2 S2' _chemical_formula_weight 945.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.425(2) _cell_length_b 10.945(2) _cell_length_c 17.471(4) _cell_angle_alpha 73.48(3) _cell_angle_beta 77.38(3) _cell_angle_gamma 87.53(3) _cell_volume 1864.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 7913 _cell_measurement_theta_min 3.0443 _cell_measurement_theta_max 27.4971 _exptl_crystal_description flake _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6689 _exptl_absorpt_correction_T_max 0.7212 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17891 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8370 _reflns_number_gt 6529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8370 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.68774(3) 0.73053(3) 0.511929(18) 0.04483(13) Uani 1 1 d . . . P1 P 0.26444(12) 0.87314(13) 0.14124(8) 0.0530(3) Uani 1 1 d . . . P2 P 0.88823(14) 0.62782(12) 0.85543(8) 0.0554(3) Uani 1 1 d . . . F1 F 0.1562(5) 0.7683(6) 0.1824(4) 0.164(3) Uani 1 1 d . . . F2 F 0.1641(6) 0.9741(6) 0.1495(5) 0.174(3) Uani 1 1 d . . . F3 F 0.3114(5) 0.8692(7) 0.2204(3) 0.157(2) Uani 1 1 d . . . F4 F 0.3606(5) 0.7598(5) 0.1318(4) 0.1318(19) Uani 1 1 d . . . F5 F 0.2221(5) 0.8746(5) 0.0584(3) 0.1146(15) Uani 1 1 d . . . F6 F 0.3767(6) 0.9640(7) 0.0932(5) 0.204(4) Uani 1 1 d . . . F7 F 0.9434(6) 0.5951(8) 0.9348(3) 0.170(3) Uani 1 1 d . . . F8 F 0.9189(7) 0.7678(5) 0.8479(5) 0.179(3) Uani 1 1 d . . . F9 F 0.8307(6) 0.6666(7) 0.7791(3) 0.169(3) Uani 1 1 d . . . F10 F 0.8618(6) 0.4856(4) 0.8675(4) 0.148(2) Uani 1 1 d . . . F11 F 0.7461(4) 0.6319(5) 0.9133(3) 0.1154(15) Uani 1 1 d . . . F12 F 1.0268(4) 0.6190(5) 0.8029(3) 0.1173(16) Uani 1 1 d . . . S1 S 0.61380(11) 0.92450(11) 0.41899(7) 0.0490(3) Uani 1 1 d . . . S2 S 0.54965(11) 0.54372(12) 0.59584(7) 0.0527(3) Uani 1 1 d . . . N1 N 0.7895(3) 0.7606(3) 0.1082(2) 0.0431(8) Uani 1 1 d . . . N2 N 0.3558(4) 0.7398(4) 0.8910(2) 0.0530(10) Uani 1 1 d . . . N3 N 0.8852(3) 0.6656(3) 0.4491(2) 0.0412(8) Uani 1 1 d . . . N4 N 0.8462(3) 0.8040(3) 0.5630(2) 0.0401(7) Uani 1 1 d . . . C1 C 0.6678(4) 0.8818(4) 0.3265(2) 0.0400(9) Uani 1 1 d . . . C2 C 0.5767(4) 0.8440(4) 0.2898(3) 0.0465(10) Uani 1 1 d . A . H2A H 0.4866 0.8436 0.3137 0.056 Uiso 1 1 calc R . . C3 C 0.6157(4) 0.8068(4) 0.2189(3) 0.0474(10) Uani 1 1 d . . . H3A H 0.5524 0.7807 0.1956 0.057 Uiso 1 1 calc R A . C4 C 0.7470(4) 0.8079(4) 0.1826(2) 0.0372(8) Uani 1 1 d . A . C5 C 0.8387(4) 0.8455(5) 0.2173(3) 0.0488(10) Uani 1 1 d . . . H5A H 0.9286 0.8460 0.1929 0.059 Uiso 1 1 calc R A . C6 C 0.7992(4) 0.8827(4) 0.2882(3) 0.0488(10) Uani 1 1 d . A . H6A H 0.8632 0.9093 0.3109 0.059 Uiso 1 1 calc R . . C7 C 0.6846(11) 0.7537(12) 0.0658(9) 0.057(3) Uani 0.615(15) 1 d P A 1 H7A H 0.6622 0.8392 0.0377 0.086 Uiso 0.615(15) 1 calc PR A 1 H7B H 0.6077 0.7114 0.1053 0.086 Uiso 0.615(15) 1 calc PR A 1 H7C H 0.7143 0.7060 0.0264 0.086 Uiso 0.615(15) 1 calc PR A 1 C8 C 0.8451(14) 0.6336(10) 0.1324(7) 0.068(3) Uani 0.615(15) 1 d P A 1 H8A H 0.9377 0.6420 0.1316 0.102 Uiso 0.615(15) 1 calc PR A 1 H8B H 0.8353 0.5867 0.0944 0.102 Uiso 0.615(15) 1 calc PR A 1 H8C H 0.7991 0.5881 0.1871 0.102 Uiso 0.615(15) 1 calc PR A 1 C9 C 0.8946(16) 0.8540(14) 0.0473(8) 0.068(4) Uani 0.615(15) 1 d P A 1 H9A H 0.8684 0.9407 0.0457 0.102 Uiso 0.615(15) 1 calc PR A 1 H9B H 0.9042 0.8423 -0.0067 0.102 Uiso 0.615(15) 1 calc PR A 1 H9C H 0.9778 0.8382 0.0643 0.102 Uiso 0.615(15) 1 calc PR A 1 C16 C 0.3045(19) 0.6439(9) 0.9658(6) 0.095(6) Uani 0.615(15) 1 d P A 1 H16D H 0.3678 0.5766 0.9749 0.143 Uiso 0.615(15) 1 calc PR A 1 H16E H 0.2230 0.6086 0.9621 0.143 Uiso 0.615(15) 1 calc PR A 1 H16F H 0.2879 0.6816 1.0109 0.143 Uiso 0.615(15) 1 calc PR A 1 C17 C 0.2355(10) 0.8326(11) 0.8793(6) 0.066(3) Uani 0.615(15) 1 d P A 1 H17D H 0.2097 0.8661 0.9261 0.099 Uiso 0.615(15) 1 calc PR A 1 H17E H 0.1620 0.7859 0.8746 0.099 Uiso 0.615(15) 1 calc PR A 1 H17F H 0.2616 0.9026 0.8301 0.099 Uiso 0.615(15) 1 calc PR A 1 C18 C 0.459(2) 0.830(3) 0.8946(12) 0.081(5) Uani 0.615(15) 1 d P A 1 H18D H 0.4802 0.8959 0.8431 0.121 Uiso 0.615(15) 1 calc PR A 1 H18E H 0.5376 0.7825 0.9046 0.121 Uiso 0.615(15) 1 calc PR A 1 H18F H 0.4256 0.8679 0.9386 0.121 Uiso 0.615(15) 1 calc PR A 1 C7' C 0.695(4) 0.812(3) 0.0525(17) 0.119(13) Uani 0.385(15) 1 d P A 2 H7'A H 0.7011 0.9047 0.0347 0.178 Uiso 0.385(15) 1 calc PR A 2 H7'B H 0.6056 0.7858 0.0820 0.178 Uiso 0.385(15) 1 calc PR A 2 H7'C H 0.7166 0.7797 0.0052 0.178 Uiso 0.385(15) 1 calc PR A 2 C8' C 0.764(4) 0.609(2) 0.1375(17) 0.129(13) Uani 0.385(15) 1 d P A 2 H8'A H 0.8196 0.5696 0.1752 0.193 Uiso 0.385(15) 1 calc PR A 2 H8'B H 0.7845 0.5760 0.0905 0.193 Uiso 0.385(15) 1 calc PR A 2 H8'C H 0.6725 0.5905 0.1646 0.193 Uiso 0.385(15) 1 calc PR A 2 C9' C 0.927(3) 0.790(3) 0.063(2) 0.128(16) Uani 0.385(15) 1 d P A 2 H9'A H 0.9416 0.8821 0.0445 0.192 Uiso 0.385(15) 1 calc PR A 2 H9'B H 0.9449 0.7561 0.0167 0.192 Uiso 0.385(15) 1 calc PR A 2 H9'C H 0.9861 0.7525 0.0994 0.192 Uiso 0.385(15) 1 calc PR A 2 C16' C 0.415(2) 0.6524(17) 0.9705(9) 0.069(5) Uani 0.385(15) 1 d P A 2 H16A H 0.5099 0.6623 0.9581 0.103 Uiso 0.385(15) 1 calc PR A 2 H16B H 0.3916 0.5633 0.9812 0.103 Uiso 0.385(15) 1 calc PR A 2 H16C H 0.3778 0.6806 1.0184 0.103 Uiso 0.385(15) 1 calc PR A 2 C17' C 0.2155(14) 0.732(2) 0.9211(12) 0.078(7) Uani 0.385(15) 1 d P A 2 H17A H 0.1931 0.7652 0.9681 0.117 Uiso 0.385(15) 1 calc PR A 2 H17B H 0.1860 0.6436 0.9370 0.117 Uiso 0.385(15) 1 calc PR A 2 H17C H 0.1728 0.7815 0.8785 0.117 Uiso 0.385(15) 1 calc PR A 2 C18' C 0.419(4) 0.857(4) 0.8718(19) 0.104(14) Uani 0.385(15) 1 d P A 2 H18A H 0.4095 0.8846 0.9209 0.156 Uiso 0.385(15) 1 calc PR A 2 H18B H 0.3802 0.9197 0.8320 0.156 Uiso 0.385(15) 1 calc PR A 2 H18C H 0.5117 0.8499 0.8490 0.156 Uiso 0.385(15) 1 calc PR A 2 C10 C 0.4899(4) 0.5970(4) 0.6835(3) 0.0437(9) Uani 1 1 d . . . C11 C 0.3902(5) 0.6848(4) 0.6852(3) 0.0512(10) Uani 1 1 d . A . H11A H 0.3524 0.7145 0.6393 0.061 Uiso 1 1 calc R . . C12 C 0.3447(5) 0.7301(5) 0.7521(3) 0.0555(12) Uani 1 1 d . . . H12A H 0.2776 0.7904 0.7514 0.067 Uiso 1 1 calc R A . C13 C 0.3986(4) 0.6858(4) 0.8200(3) 0.0449(10) Uani 1 1 d . A . C14 C 0.4969(5) 0.5975(5) 0.8208(3) 0.0556(11) Uani 1 1 d . . . H14A H 0.5341 0.5679 0.8670 0.067 Uiso 1 1 calc R A . C15 C 0.5410(5) 0.5523(5) 0.7526(3) 0.0551(11) Uani 1 1 d . A . H15A H 0.6065 0.4904 0.7538 0.066 Uiso 1 1 calc R . . C19 C 0.7821(5) 0.5442(5) 0.3823(3) 0.0562(12) Uani 1 1 d . . . H19A H 0.7046 0.5720 0.4146 0.084 Uiso 1 1 calc R . . H19B H 0.7833 0.4518 0.3978 0.084 Uiso 1 1 calc R . . H19C H 0.7803 0.5762 0.3247 0.084 Uiso 1 1 calc R . . C20 C 0.9024(5) 0.5946(4) 0.3972(3) 0.0500(11) Uani 1 1 d . . . C21 C 1.0286(5) 0.5673(5) 0.3577(3) 0.0577(12) Uani 1 1 d . . . H21A H 1.0387 0.5172 0.3212 0.069 Uiso 1 1 calc R . . C22 C 1.1357(5) 0.6144(5) 0.3733(3) 0.0644(14) Uani 1 1 d . . . H22A H 1.2203 0.5969 0.3471 0.077 Uiso 1 1 calc R . . C23 C 1.1213(4) 0.6887(4) 0.4277(3) 0.0515(11) Uani 1 1 d . . . C24 C 0.9916(4) 0.7115(4) 0.4666(3) 0.0421(9) Uani 1 1 d . . . C25 C 0.9716(4) 0.7839(4) 0.5249(2) 0.0407(9) Uani 1 1 d . . . C26 C 1.0829(4) 0.8334(4) 0.5417(3) 0.0491(11) Uani 1 1 d . . . C27 C 1.2110(4) 0.8102(5) 0.5001(3) 0.0608(14) Uani 1 1 d . . . H27A H 1.2845 0.8448 0.5102 0.073 Uiso 1 1 calc R . . C28 C 1.2293(4) 0.7412(5) 0.4476(3) 0.0614(14) Uani 1 1 d . . . H28A H 1.3156 0.7262 0.4226 0.074 Uiso 1 1 calc R . . C29 C 1.0585(5) 0.9031(4) 0.5993(3) 0.0561(12) Uani 1 1 d . . . H29A H 1.1295 0.9378 0.6119 0.067 Uiso 1 1 calc R . . C30 C 0.9338(5) 0.9213(4) 0.6371(3) 0.0543(11) Uani 1 1 d . . . H30A H 0.9182 0.9673 0.6761 0.065 Uiso 1 1 calc R . . C31 C 0.8279(4) 0.8699(4) 0.6169(3) 0.0449(9) Uani 1 1 d . . . C32 C 0.6893(5) 0.8889(5) 0.6567(3) 0.0550(11) Uani 1 1 d . . . H32A H 0.6297 0.8477 0.6358 0.082 Uiso 1 1 calc R . . H32B H 0.6718 0.9794 0.6447 0.082 Uiso 1 1 calc R . . H32C H 0.6764 0.8521 0.7153 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.03414(18) 0.0644(2) 0.03575(19) -0.01403(15) -0.00624(12) -0.00420(14) P1 0.0442(6) 0.0707(8) 0.0471(7) -0.0180(6) -0.0145(5) 0.0007(6) P2 0.0618(8) 0.0589(7) 0.0494(7) -0.0159(6) -0.0203(6) 0.0080(6) F1 0.085(3) 0.164(5) 0.182(6) 0.051(4) -0.025(3) -0.037(3) F2 0.164(5) 0.191(5) 0.261(8) -0.173(6) -0.119(5) 0.108(4) F3 0.123(4) 0.298(8) 0.099(4) -0.112(5) -0.066(3) 0.069(4) F4 0.102(3) 0.147(4) 0.197(6) -0.096(4) -0.086(4) 0.059(3) F5 0.120(3) 0.162(4) 0.092(3) -0.054(3) -0.068(3) 0.028(3) F6 0.147(5) 0.219(7) 0.197(7) 0.060(5) -0.068(5) -0.120(5) F7 0.128(4) 0.304(8) 0.083(3) -0.038(4) -0.058(3) 0.007(5) F8 0.200(6) 0.079(3) 0.273(9) -0.090(4) -0.024(6) -0.002(3) F9 0.124(4) 0.264(7) 0.088(3) 0.032(4) -0.062(3) -0.027(4) F10 0.183(5) 0.085(3) 0.153(5) -0.050(3) 0.043(4) -0.042(3) F11 0.077(3) 0.151(4) 0.126(4) -0.066(3) -0.007(2) 0.018(2) F12 0.083(3) 0.129(3) 0.125(4) -0.041(3) 0.016(2) -0.002(2) S1 0.0458(6) 0.0651(7) 0.0432(6) -0.0239(5) -0.0147(5) 0.0111(5) S2 0.0480(6) 0.0642(7) 0.0481(6) -0.0250(5) -0.0001(5) -0.0119(5) N1 0.0375(17) 0.054(2) 0.0407(19) -0.0171(16) -0.0101(15) 0.0038(15) N2 0.053(2) 0.056(2) 0.047(2) -0.0186(18) 0.0028(18) -0.0119(17) N3 0.0416(18) 0.0449(18) 0.0322(17) -0.0044(14) -0.0059(14) -0.0014(14) N4 0.0374(17) 0.0452(18) 0.0353(17) -0.0034(14) -0.0130(14) -0.0030(14) C1 0.0352(19) 0.048(2) 0.037(2) -0.0099(17) -0.0087(16) -0.0014(16) C2 0.0308(19) 0.069(3) 0.041(2) -0.019(2) -0.0049(17) -0.0042(18) C3 0.035(2) 0.066(3) 0.049(3) -0.024(2) -0.0133(18) -0.0051(19) C4 0.0309(18) 0.045(2) 0.037(2) -0.0136(17) -0.0080(16) 0.0040(15) C5 0.0293(19) 0.070(3) 0.050(3) -0.024(2) -0.0055(18) -0.0016(18) C6 0.034(2) 0.068(3) 0.051(3) -0.025(2) -0.0117(18) -0.0063(19) C7 0.046(4) 0.084(8) 0.063(8) -0.047(7) -0.023(4) 0.008(5) C8 0.100(8) 0.044(5) 0.059(5) -0.023(4) -0.011(6) 0.038(5) C9 0.060(7) 0.104(10) 0.036(4) -0.025(6) 0.009(4) -0.009(6) C16 0.166(16) 0.057(5) 0.040(5) -0.004(4) 0.013(7) -0.001(7) C17 0.066(6) 0.070(7) 0.066(6) -0.029(5) -0.012(5) 0.018(5) C18 0.073(8) 0.127(13) 0.064(11) -0.060(10) -0.008(7) -0.034(7) C7' 0.20(3) 0.13(2) 0.049(11) -0.038(15) -0.069(15) 0.09(2) C8' 0.19(3) 0.082(13) 0.114(18) -0.077(13) 0.04(2) -0.033(17) C9' 0.071(17) 0.18(3) 0.15(3) -0.13(3) 0.056(17) -0.050(18) C16' 0.090(13) 0.079(10) 0.036(7) -0.013(6) -0.017(8) 0.020(9) C17' 0.051(8) 0.102(16) 0.086(13) -0.053(13) 0.009(8) 0.018(8) C18' 0.16(4) 0.11(2) 0.056(16) -0.063(16) 0.007(15) -0.06(2) C10 0.037(2) 0.050(2) 0.042(2) -0.0137(18) -0.0026(17) -0.0072(17) C11 0.055(3) 0.057(3) 0.045(2) -0.013(2) -0.022(2) 0.008(2) C12 0.055(3) 0.057(3) 0.060(3) -0.024(2) -0.016(2) 0.013(2) C13 0.044(2) 0.048(2) 0.042(2) -0.0169(18) -0.0019(18) -0.0060(18) C14 0.059(3) 0.068(3) 0.041(2) -0.015(2) -0.018(2) 0.010(2) C15 0.050(3) 0.068(3) 0.050(3) -0.023(2) -0.012(2) 0.012(2) C19 0.062(3) 0.056(3) 0.051(3) -0.017(2) -0.009(2) -0.008(2) C20 0.060(3) 0.046(2) 0.035(2) -0.0028(18) -0.005(2) 0.003(2) C21 0.066(3) 0.057(3) 0.042(2) -0.011(2) -0.003(2) 0.015(2) C22 0.048(3) 0.083(4) 0.048(3) -0.006(3) -0.001(2) 0.011(2) C23 0.039(2) 0.060(3) 0.043(2) -0.001(2) -0.0020(19) 0.002(2) C24 0.035(2) 0.046(2) 0.036(2) 0.0035(17) -0.0079(16) -0.0021(17) C25 0.038(2) 0.042(2) 0.034(2) 0.0075(16) -0.0139(16) -0.0061(16) C26 0.043(2) 0.048(2) 0.048(3) 0.007(2) -0.0199(19) -0.0107(18) C27 0.036(2) 0.067(3) 0.065(3) 0.009(3) -0.014(2) -0.014(2) C28 0.032(2) 0.075(3) 0.059(3) 0.006(3) -0.005(2) -0.003(2) C29 0.059(3) 0.054(3) 0.056(3) -0.002(2) -0.028(2) -0.015(2) C30 0.066(3) 0.052(2) 0.048(3) -0.009(2) -0.022(2) -0.007(2) C31 0.053(2) 0.046(2) 0.034(2) -0.0051(17) -0.0141(18) -0.0049(19) C32 0.056(3) 0.061(3) 0.051(3) -0.023(2) -0.006(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N3 2.297(3) . ? Cd1 N4 2.311(3) . ? Cd1 S2 2.4555(15) . ? Cd1 S1 2.4866(15) . ? P1 F6 1.502(5) . ? P1 F2 1.504(5) . ? P1 F1 1.547(5) . ? P1 F3 1.554(5) . ? P1 F4 1.584(4) . ? P1 F5 1.599(4) . ? P2 F9 1.525(5) . ? P2 F10 1.539(4) . ? P2 F8 1.541(5) . ? P2 F12 1.548(4) . ? P2 F7 1.559(5) . ? P2 F11 1.608(4) . ? S1 C1 1.776(4) . ? S2 C10 1.770(4) . ? N1 C7 1.463(12) . ? N1 C8 1.467(10) . ? N1 C9' 1.48(3) . ? N1 C4 1.507(5) . ? N1 C7' 1.52(3) . ? N1 C9 1.532(16) . ? N1 C8' 1.60(2) . ? N2 C18' 1.39(3) . ? N2 C16 1.435(10) . ? N2 C17' 1.439(14) . ? N2 C13 1.496(6) . ? N2 C18 1.51(2) . ? N2 C17 1.591(10) . ? N2 C16' 1.671(16) . ? N3 C20 1.332(6) . ? N3 C24 1.365(5) . ? N4 C31 1.319(5) . ? N4 C25 1.370(5) . ? C1 C6 1.387(6) . ? C1 C2 1.391(6) . ? C2 C3 1.384(6) . ? C2 H2A 0.9400 . ? C3 C4 1.376(5) . ? C3 H3A 0.9400 . ? C4 C5 1.371(6) . ? C5 C6 1.385(6) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C16 H16D 0.9700 . ? C16 H16E 0.9700 . ? C16 H16F 0.9700 . ? C17 H17D 0.9700 . ? C17 H17E 0.9700 . ? C17 H17F 0.9700 . ? C18 H18D 0.9700 . ? C18 H18E 0.9700 . ? C18 H18F 0.9700 . ? C7' H7'A 0.9700 . ? C7' H7'B 0.9700 . ? C7' H7'C 0.9700 . ? C8' H8'A 0.9700 . ? C8' H8'B 0.9700 . ? C8' H8'C 0.9700 . ? C9' H9'A 0.9700 . ? C9' H9'B 0.9700 . ? C9' H9'C 0.9700 . ? C16' H16A 0.9700 . ? C16' H16B 0.9700 . ? C16' H16C 0.9700 . ? C17' H17A 0.9700 . ? C17' H17B 0.9700 . ? C17' H17C 0.9700 . ? C18' H18A 0.9700 . ? C18' H18B 0.9700 . ? C18' H18C 0.9700 . ? C10 C15 1.378(7) . ? C10 C11 1.386(6) . ? C11 C12 1.380(7) . ? C11 H11A 0.9400 . ? C12 C13 1.378(7) . ? C12 H12A 0.9400 . ? C13 C14 1.377(7) . ? C14 C15 1.398(7) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C19 C20 1.493(7) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C20 C21 1.408(7) . ? C21 C22 1.359(8) . ? C21 H21A 0.9400 . ? C22 C23 1.397(8) . ? C22 H22A 0.9400 . ? C23 C24 1.420(6) . ? C23 C28 1.435(7) . ? C24 C25 1.436(6) . ? C25 C26 1.422(6) . ? C26 C29 1.402(7) . ? C26 C27 1.424(7) . ? C27 C28 1.325(8) . ? C27 H27A 0.9400 . ? C28 H28A 0.9400 . ? C29 C30 1.357(7) . ? C29 H29A 0.9400 . ? C30 C31 1.412(6) . ? C30 H30A 0.9400 . ? C31 C32 1.494(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cd1 N4 74.23(13) . . ? N3 Cd1 S2 109.79(9) . . ? N4 Cd1 S2 120.10(9) . . ? N3 Cd1 S1 110.28(9) . . ? N4 Cd1 S1 104.71(9) . . ? S2 Cd1 S1 125.93(5) . . ? F6 P1 F2 95.8(5) . . ? F6 P1 F1 172.0(5) . . ? F2 P1 F1 90.2(4) . . ? F6 P1 F3 88.7(4) . . ? F2 P1 F3 95.0(3) . . ? F1 P1 F3 96.1(4) . . ? F6 P1 F4 88.0(4) . . ? F2 P1 F4 175.2(3) . . ? F1 P1 F4 85.7(3) . . ? F3 P1 F4 88.0(3) . . ? F6 P1 F5 90.2(3) . . ? F2 P1 F5 87.3(3) . . ? F1 P1 F5 84.8(3) . . ? F3 P1 F5 177.5(3) . . ? F4 P1 F5 89.8(3) . . ? F9 P2 F10 91.8(4) . . ? F9 P2 F8 91.8(4) . . ? F10 P2 F8 176.4(4) . . ? F9 P2 F12 90.7(3) . . ? F10 P2 F12 90.3(3) . . ? F8 P2 F12 89.3(3) . . ? F9 P2 F7 176.7(5) . . ? F10 P2 F7 90.8(4) . . ? F8 P2 F7 85.6(4) . . ? F12 P2 F7 91.3(3) . . ? F9 P2 F11 91.5(3) . . ? F10 P2 F11 88.2(3) . . ? F8 P2 F11 92.0(3) . . ? F12 P2 F11 177.4(3) . . ? F7 P2 F11 86.5(3) . . ? C1 S1 Cd1 97.52(15) . . ? C10 S2 Cd1 98.48(14) . . ? C7 N1 C8 108.7(7) . . ? C7 N1 C9' 121.6(16) . . ? C8 N1 C9' 80.6(15) . . ? C7 N1 C4 114.5(6) . . ? C8 N1 C4 108.9(5) . . ? C9' N1 C4 115.9(12) . . ? C7 N1 C7' 24.0(13) . . ? C8 N1 C7' 131.0(12) . . ? C9' N1 C7' 111(2) . . ? C4 N1 C7' 107.5(12) . . ? C7 N1 C9 107.0(8) . . ? C8 N1 C9 110.0(7) . . ? C9' N1 C9 29.5(15) . . ? C4 N1 C9 107.6(6) . . ? C7' N1 C9 88.6(15) . . ? C7 N1 C8' 80.9(14) . . ? C8 N1 C8' 32.7(12) . . ? C9' N1 C8' 109.9(16) . . ? C4 N1 C8' 107.1(9) . . ? C7' N1 C8' 104.8(17) . . ? C9 N1 C8' 136.6(11) . . ? C18' N2 C16 134.4(13) . . ? C18' N2 C17' 118(2) . . ? C16 N2 C17' 62.3(10) . . ? C18' N2 C13 108.3(14) . . ? C16 N2 C13 112.5(5) . . ? C17' N2 C13 112.6(7) . . ? C18' N2 C18 25(2) . . ? C16 N2 C18 115.9(11) . . ? C17' N2 C18 131.5(12) . . ? C13 N2 C18 111.6(9) . . ? C18' N2 C17 79.6(19) . . ? C16 N2 C17 103.3(8) . . ? C17' N2 C17 43.6(8) . . ? C13 N2 C17 111.2(5) . . ? C18 N2 C17 101.4(11) . . ? C18' N2 C16' 103.1(16) . . ? C16 N2 C16' 43.9(8) . . ? C17' N2 C16' 104.0(11) . . ? C13 N2 C16' 109.7(6) . . ? C18 N2 C16' 78.6(11) . . ? C17 N2 C16' 135.7(7) . . ? C20 N3 C24 119.9(4) . . ? C20 N3 Cd1 126.5(3) . . ? C24 N3 Cd1 113.6(3) . . ? C31 N4 C25 119.5(4) . . ? C31 N4 Cd1 127.4(3) . . ? C25 N4 Cd1 112.7(3) . . ? C6 C1 C2 117.1(4) . . ? C6 C1 S1 122.9(3) . . ? C2 C1 S1 120.0(3) . . ? C3 C2 C1 121.5(4) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 N1 120.4(3) . . ? C3 C4 N1 119.9(3) . . ? C4 C5 C6 120.1(4) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 119.9 . . ? C5 C6 C1 121.6(4) . . ? C5 C6 H6A 119.2 . . ? C1 C6 H6A 119.2 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C16 H16D 109.5 . . ? N2 C16 H16E 109.5 . . ? N2 C16 H16F 109.5 . . ? N2 C17 H17D 109.5 . . ? N2 C17 H17E 109.5 . . ? N2 C17 H17F 109.5 . . ? N2 C18 H18D 109.5 . . ? N2 C18 H18E 109.5 . . ? N2 C18 H18F 109.5 . . ? N1 C7' H7'A 109.5 . . ? N1 C7' H7'B 109.5 . . ? H7'A C7' H7'B 109.5 . . ? N1 C7' H7'C 109.5 . . ? H7'A C7' H7'C 109.5 . . ? H7'B C7' H7'C 109.5 . . ? N1 C8' H8'A 109.5 . . ? N1 C8' H8'B 109.5 . . ? H8'A C8' H8'B 109.5 . . ? N1 C8' H8'C 109.5 . . ? H8'A C8' H8'C 109.5 . . ? H8'B C8' H8'C 109.5 . . ? N1 C9' H9'A 109.5 . . ? N1 C9' H9'B 109.5 . . ? H9'A C9' H9'B 109.5 . . ? N1 C9' H9'C 109.5 . . ? H9'A C9' H9'C 109.5 . . ? H9'B C9' H9'C 109.5 . . ? N2 C16' H16A 109.5 . . ? N2 C16' H16B 109.5 . . ? H16A C16' H16B 109.5 . . ? N2 C16' H16C 109.5 . . ? H16A C16' H16C 109.5 . . ? H16B C16' H16C 109.5 . . ? N2 C17' H17A 109.5 . . ? N2 C17' H17B 109.5 . . ? H17A C17' H17B 109.5 . . ? N2 C17' H17C 109.5 . . ? H17A C17' H17C 109.5 . . ? H17B C17' H17C 109.5 . . ? N2 C18' H18A 109.5 . . ? N2 C18' H18B 109.5 . . ? H18A C18' H18B 109.5 . . ? N2 C18' H18C 109.5 . . ? H18A C18' H18C 109.5 . . ? H18B C18' H18C 109.5 . . ? C15 C10 C11 117.7(4) . . ? C15 C10 S2 121.0(3) . . ? C11 C10 S2 121.2(4) . . ? C12 C11 C10 122.1(5) . . ? C12 C11 H11A 118.9 . . ? C10 C11 H11A 118.9 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 N2 119.9(4) . . ? C12 C13 N2 119.7(4) . . ? C13 C14 C15 119.6(5) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C10 C15 C14 121.0(5) . . ? C10 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 121.9(5) . . ? N3 C20 C19 117.4(4) . . ? C21 C20 C19 120.8(4) . . ? C22 C21 C20 119.0(5) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? C21 C22 C23 120.8(5) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C22 C23 C24 117.8(4) . . ? C22 C23 C28 124.0(4) . . ? C24 C23 C28 118.2(5) . . ? N3 C24 C23 120.8(4) . . ? N3 C24 C25 119.3(4) . . ? C23 C24 C25 120.0(4) . . ? N4 C25 C26 121.4(4) . . ? N4 C25 C24 119.6(4) . . ? C26 C25 C24 119.0(4) . . ? C29 C26 C25 117.0(4) . . ? C29 C26 C27 123.9(4) . . ? C25 C26 C27 119.1(5) . . ? C28 C27 C26 121.7(5) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C23 122.0(4) . . ? C27 C28 H28A 119.0 . . ? C23 C28 H28A 119.0 . . ? C30 C29 C26 121.0(4) . . ? C30 C29 H29A 119.5 . . ? C26 C29 H29A 119.5 . . ? C29 C30 C31 118.9(5) . . ? C29 C30 H30A 120.5 . . ? C31 C30 H30A 120.5 . . ? N4 C31 C30 122.2(4) . . ? N4 C31 C32 117.3(4) . . ? C30 C31 C32 120.5(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3 H3A F4 0.94 2.54 3.462(6) 167.0 . C5 H5A F1 0.94 2.47 3.348(7) 155.0 1_655 C7 H7C F11 0.97 2.30 3.238(14) 163.7 1_554 C8 H8A F10 0.97 2.46 3.270(14) 140.4 2_766 C16 H16F F5 0.97 2.50 3.356(11) 147.3 1_556 C17 H17D F5 0.97 2.37 3.262(11) 152.5 1_556 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.277 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.093 #===END #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 835432' #TrackingRef '1-6.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H35 Cd N7 S2, 2(F6 P)' _chemical_formula_sum 'C29 H35 Cd F12 N7 P2 S2' _chemical_formula_weight 948.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.725(7) _cell_length_b 10.164(2) _cell_length_c 10.385(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.67(3) _cell_angle_gamma 90.00 _cell_volume 3630.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 4057 _cell_measurement_theta_min 3.0282 _cell_measurement_theta_max 27.4623 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7146 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10087 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4100 _reflns_number_gt 3498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+8.6587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4100 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1498 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.5000 0.30868(4) 0.7500 0.03389(17) Uani 1 2 d S . . S1 S 0.45224(4) 0.41654(16) 0.85254(12) 0.0526(4) Uani 1 1 d . . . N1 N 0.30791(11) 0.3765(4) 0.3845(4) 0.0366(8) Uani 1 1 d . . . N2 N 0.56381(12) 0.2699(5) 1.0720(4) 0.0497(11) Uani 1 1 d . . . H2A H 0.5659 0.3530 1.0927 0.060 Uiso 1 1 calc R . . N3 N 0.54016(12) 0.2220(4) 0.9582(4) 0.0414(9) Uani 1 1 d . . . N4 N 0.5000 0.0765(5) 0.7500 0.0413(13) Uani 1 2 d S . . P1 P 0.18193(5) 0.36714(14) 0.04207(14) 0.0532(4) Uani 1 1 d . . . F1 F 0.22080(13) 0.4446(5) 0.0981(6) 0.118(2) Uani 1 1 d . . . F2 F 0.19436(16) 0.2645(5) 0.1594(5) 0.1043(16) Uani 1 1 d . . . F3 F 0.1706(3) 0.4676(6) -0.0715(6) 0.185(4) Uani 1 1 d . . . F4 F 0.1419(3) 0.2937(6) -0.0048(11) 0.218(6) Uani 1 1 d . . . F5 F 0.1986(4) 0.2731(7) -0.0390(8) 0.257(7) Uani 1 1 d . . . F6 F 0.16323(19) 0.4563(6) 0.1250(8) 0.153(3) Uani 1 1 d . . . C1 C 0.41029(14) 0.4054(5) 0.7145(5) 0.0407(11) Uani 1 1 d . . . C2 C 0.40140(15) 0.5024(5) 0.6158(5) 0.0455(12) Uani 1 1 d . . . H2B H 0.4179 0.5754 0.6219 0.055 Uiso 1 1 calc R . . C3 C 0.36831(15) 0.4924(5) 0.5084(5) 0.0423(11) Uani 1 1 d . . . H3A H 0.3626 0.5584 0.4426 0.051 Uiso 1 1 calc R . . C4 C 0.34392(13) 0.3855(4) 0.4987(4) 0.0338(9) Uani 1 1 d . . . C5 C 0.35194(17) 0.2889(5) 0.5963(5) 0.0483(12) Uani 1 1 d . . . H5A H 0.3353 0.2163 0.5905 0.058 Uiso 1 1 calc R . . C6 C 0.38489(17) 0.3007(5) 0.7025(6) 0.0514(13) Uani 1 1 d . . . H6A H 0.3902 0.2352 0.7689 0.062 Uiso 1 1 calc R . . C7 C 0.27491(16) 0.4403(7) 0.4243(6) 0.0581(15) Uani 1 1 d . . . H7A H 0.2817 0.5306 0.4510 0.087 Uiso 1 1 calc R . . H7B H 0.2698 0.3925 0.4985 0.087 Uiso 1 1 calc R . . H7C H 0.2519 0.4392 0.3491 0.087 Uiso 1 1 calc R . . C8 C 0.2974(2) 0.2361(6) 0.3447(6) 0.0630(16) Uani 1 1 d . . . H8A H 0.2941 0.1877 0.4214 0.095 Uiso 1 1 calc R . . H8B H 0.3180 0.1961 0.3134 0.095 Uiso 1 1 calc R . . H8C H 0.2733 0.2341 0.2738 0.095 Uiso 1 1 calc R . . C9 C 0.31250(18) 0.4452(6) 0.2619(5) 0.0570(14) Uani 1 1 d . . . H9A H 0.3192 0.5367 0.2828 0.086 Uiso 1 1 calc R . . H9B H 0.2883 0.4404 0.1918 0.086 Uiso 1 1 calc R . . H9C H 0.3330 0.4031 0.2318 0.086 Uiso 1 1 calc R . . C10 C 0.58388(18) 0.1738(7) 1.1497(6) 0.0648(18) Uani 1 1 d . . . H10A H 0.6019 0.1843 1.2338 0.078 Uiso 1 1 calc R . . C11 C 0.57312(18) 0.0577(7) 1.0829(6) 0.0632(17) Uani 1 1 d . . . H11A H 0.5823 -0.0270 1.1110 0.076 Uiso 1 1 calc R . . C12 C 0.54544(15) 0.0921(5) 0.9635(5) 0.0458(12) Uani 1 1 d . . . C13 C 0.52255(16) 0.0101(5) 0.8545(5) 0.0477(13) Uani 1 1 d . . . C14 C 0.52290(19) -0.1269(6) 0.8570(7) 0.0629(17) Uani 1 1 d . . . H14A H 0.5386 -0.1724 0.9308 0.075 Uiso 1 1 calc R . . C15 C 0.5000 -0.1947(8) 0.7500 0.072(3) Uani 1 2 d S . . H15 H 0.5000 -0.2872 0.7500 0.087 Uiso 1 2 calc SR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0324(3) 0.0316(3) 0.0392(3) 0.000 0.01239(19) 0.000 S1 0.0423(7) 0.0738(10) 0.0403(6) -0.0115(6) 0.0089(5) 0.0190(6) N1 0.040(2) 0.033(2) 0.0393(19) 0.0020(16) 0.0145(17) 0.0013(17) N2 0.038(2) 0.067(3) 0.042(2) 0.013(2) 0.0065(18) -0.001(2) N3 0.037(2) 0.046(2) 0.044(2) 0.0106(18) 0.0158(17) 0.0070(18) N4 0.048(3) 0.034(3) 0.056(3) 0.000 0.037(3) 0.000 P1 0.0732(10) 0.0369(7) 0.0467(7) -0.0051(6) 0.0113(7) -0.0026(7) F1 0.056(2) 0.086(3) 0.203(6) 0.034(3) 0.018(3) -0.014(2) F2 0.117(4) 0.090(3) 0.096(3) 0.034(3) 0.010(3) -0.009(3) F3 0.308(10) 0.092(4) 0.097(4) 0.047(3) -0.046(5) -0.023(5) F4 0.177(7) 0.085(4) 0.283(10) 0.028(5) -0.124(8) -0.061(4) F5 0.57(2) 0.101(5) 0.178(7) -0.019(5) 0.236(11) 0.069(8) F6 0.147(5) 0.102(4) 0.263(8) -0.036(5) 0.145(6) 0.005(4) C1 0.038(2) 0.047(3) 0.041(2) -0.008(2) 0.016(2) 0.011(2) C2 0.049(3) 0.047(3) 0.042(2) 0.001(2) 0.015(2) -0.009(2) C3 0.046(3) 0.041(3) 0.040(2) 0.007(2) 0.012(2) -0.004(2) C4 0.035(2) 0.033(2) 0.036(2) -0.0001(18) 0.0138(18) 0.0036(18) C5 0.056(3) 0.033(3) 0.054(3) 0.009(2) 0.013(2) -0.007(2) C6 0.058(3) 0.037(3) 0.053(3) 0.010(2) 0.004(3) 0.009(2) C7 0.039(3) 0.086(4) 0.050(3) -0.010(3) 0.013(2) 0.010(3) C8 0.076(4) 0.038(3) 0.065(4) -0.004(3) 0.001(3) -0.012(3) C9 0.057(3) 0.070(4) 0.040(3) 0.009(3) 0.007(2) -0.009(3) C10 0.047(3) 0.092(5) 0.056(3) 0.028(3) 0.016(3) 0.021(3) C11 0.057(4) 0.076(4) 0.064(3) 0.032(3) 0.028(3) 0.030(3) C12 0.047(3) 0.044(3) 0.055(3) 0.019(2) 0.029(2) 0.018(2) C13 0.057(3) 0.036(3) 0.065(3) 0.013(2) 0.041(3) 0.010(2) C14 0.073(4) 0.042(3) 0.093(5) 0.013(3) 0.055(4) 0.015(3) C15 0.094(7) 0.031(4) 0.121(8) 0.000 0.080(7) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N4 2.360(6) . ? Cd1 N3 2.416(4) 2_656 ? Cd1 N3 2.416(4) . ? Cd1 S1 2.4957(14) 2_656 ? Cd1 S1 2.4957(14) . ? S1 C1 1.776(5) . ? N1 C7 1.498(6) . ? N1 C4 1.499(6) . ? N1 C9 1.499(6) . ? N1 C8 1.505(7) . ? N2 C10 1.344(7) . ? N2 N3 1.344(6) . ? N2 H2A 0.8700 . ? N3 C12 1.333(6) . ? N4 C13 1.346(6) . ? N4 C13 1.346(6) 2_656 ? P1 F5 1.499(6) . ? P1 F6 1.523(5) . ? P1 F3 1.530(5) . ? P1 F1 1.565(5) . ? P1 F4 1.569(7) . ? P1 F2 1.574(5) . ? C1 C6 1.382(8) . ? C1 C2 1.396(7) . ? C2 C3 1.393(7) . ? C2 H2B 0.9400 . ? C3 C4 1.379(7) . ? C3 H3A 0.9400 . ? C4 C5 1.384(7) . ? C5 C6 1.384(8) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.370(10) . ? C10 H10A 0.9400 . ? C11 C12 1.405(8) . ? C11 H11A 0.9400 . ? C12 C13 1.464(8) . ? C13 C14 1.392(7) . ? C14 C15 1.374(8) . ? C14 H14A 0.9400 . ? C15 C14 1.374(8) 2_656 ? C15 H15 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Cd1 N3 68.61(11) . 2_656 ? N4 Cd1 N3 68.61(10) . . ? N3 Cd1 N3 137.2(2) 2_656 . ? N4 Cd1 S1 116.06(4) . 2_656 ? N3 Cd1 S1 95.02(10) 2_656 2_656 ? N3 Cd1 S1 103.47(10) . 2_656 ? N4 Cd1 S1 116.06(4) . . ? N3 Cd1 S1 103.47(10) 2_656 . ? N3 Cd1 S1 95.02(10) . . ? S1 Cd1 S1 127.89(8) 2_656 . ? C1 S1 Cd1 98.77(15) . . ? C7 N1 C4 109.1(4) . . ? C7 N1 C9 107.9(4) . . ? C4 N1 C9 112.1(4) . . ? C7 N1 C8 109.2(5) . . ? C4 N1 C8 111.9(4) . . ? C9 N1 C8 106.6(4) . . ? C10 N2 N3 111.8(5) . . ? C10 N2 H2A 124.1 . . ? N3 N2 H2A 124.1 . . ? C12 N3 N2 105.9(4) . . ? C12 N3 Cd1 116.2(3) . . ? N2 N3 Cd1 137.3(3) . . ? C13 N4 C13 119.8(6) . 2_656 ? C13 N4 Cd1 120.1(3) . . ? C13 N4 Cd1 120.1(3) 2_656 . ? F5 P1 F6 176.5(6) . . ? F5 P1 F3 93.2(5) . . ? F6 P1 F3 88.5(4) . . ? F5 P1 F1 94.8(6) . . ? F6 P1 F1 88.3(3) . . ? F3 P1 F1 88.5(4) . . ? F5 P1 F4 89.4(6) . . ? F6 P1 F4 87.5(6) . . ? F3 P1 F4 92.8(4) . . ? F1 P1 F4 175.6(6) . . ? F5 P1 F2 86.6(4) . . ? F6 P1 F2 91.8(4) . . ? F3 P1 F2 179.0(4) . . ? F1 P1 F2 90.5(3) . . ? F4 P1 F2 88.2(4) . . ? C6 C1 C2 117.7(5) . . ? C6 C1 S1 120.8(4) . . ? C2 C1 S1 121.5(4) . . ? C3 C2 C1 120.8(5) . . ? C3 C2 H2B 119.6 . . ? C1 C2 H2B 119.6 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 120.2(4) . . ? C3 C4 N1 119.7(4) . . ? C5 C4 N1 120.0(4) . . ? C6 C5 C4 119.0(5) . . ? C6 C5 H5A 120.5 . . ? C4 C5 H5A 120.5 . . ? C1 C6 C5 122.3(5) . . ? C1 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 C11 106.9(6) . . ? N2 C10 H10A 126.6 . . ? C11 C10 H10A 126.6 . . ? C10 C11 C12 105.5(5) . . ? C10 C11 H11A 127.2 . . ? C12 C11 H11A 127.2 . . ? N3 C12 C11 109.9(5) . . ? N3 C12 C13 119.3(4) . . ? C11 C12 C13 130.8(5) . . ? N4 C13 C14 121.1(6) . . ? N4 C13 C12 115.2(4) . . ? C14 C13 C12 123.7(5) . . ? C15 C14 C13 119.1(7) . . ? C15 C14 H14A 120.5 . . ? C13 C14 H14A 120.5 . . ? C14 C15 C14 119.8(8) . 2_656 ? C14 C15 H15 120.1 . . ? C14 C15 H15 120.1 2_656 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A S1 0.87 2.53 3.368(5) 160.6 5_667 C3 H3A F4 0.94 2.49 3.084(7) 120.9 4 C9 H9A F2 0.97 2.47 3.372(8) 154.1 4 C5 H5A F3 0.94 2.54 3.356(8) 145.4 4_545 C8 H8A F1 0.97 2.52 3.124(8) 120.0 4_545 C9 H9B F1 0.97 2.34 3.258(7) 156.9 . _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.929 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.110 #===END #============================================================================== data_6^.^H~2~O _database_code_depnum_ccdc_archive 'CCDC 835433' #TrackingRef '1-6.cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C102 H138 Cd4 N18 S8, 8(F6 P), (H2 O)' _chemical_formula_sum 'C102 H140 Cd4 F48 N18 O P8 S8' _chemical_formula_weight 3500.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.331(3) _cell_length_b 16.928(3) _cell_length_c 18.448(4) _cell_angle_alpha 112.86(3) _cell_angle_beta 97.28(3) _cell_angle_gamma 97.77(3) _cell_volume 3727.1(13) _cell_formula_units_Z 1 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17075 _cell_measurement_theta_min 3.0539 _cell_measurement_theta_max 28.0389 _exptl_crystal_description clubbed _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1758 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6466 _exptl_absorpt_correction_T_max 0.8454 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28270 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12926 _reflns_number_gt 9042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1852P)^2^+2.1977P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12926 _refine_ls_number_parameters 852 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1279 _refine_ls_R_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.3121 _refine_ls_wR_factor_gt 0.2799 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.89391(4) 0.56292(4) 0.68280(4) 0.0456(2) Uani 1 1 d . . . Cd2 Cd 0.60163(5) 0.45085(4) 0.52371(4) 0.0541(3) Uani 1 1 d . . . S1 S 0.5869(2) 0.30742(17) 0.52901(18) 0.0649(7) Uani 1 1 d . . . S2 S 0.48556(18) 0.54376(16) 0.61014(14) 0.0544(6) Uani 1 1 d . . . S3 S 0.77956(15) 0.54933(14) 0.55380(14) 0.0473(5) Uani 1 1 d . . . S4 S 1.07735(16) 0.62622(16) 0.69540(14) 0.0536(6) Uani 1 1 d . . . N1 N 0.8236(8) 0.0803(7) 0.2956(7) 0.084(3) Uani 1 1 d . . . N2 N 0.2003(6) 0.3533(6) 0.7483(5) 0.063(2) Uani 1 1 d . . . N3 N 0.6784(6) 0.9066(5) 0.6194(6) 0.066(2) Uani 1 1 d . . . N4 N 0.8825(5) 0.4095(5) 0.6212(4) 0.0494(17) Uani 1 1 d . . . N5 N 0.8379(5) 0.3611(5) 0.6590(4) 0.0470(16) Uani 1 1 d . . . N6 N 0.8110(5) 0.4897(5) 0.7515(4) 0.0508(17) Uani 1 1 d . . . N7 N 0.7997(7) 0.6263(5) 0.8410(5) 0.068(2) Uani 1 1 d . . . N8 N 0.8411(6) 0.6617(5) 0.7929(5) 0.0577(19) Uani 1 1 d . . . N9 N 1.3123(7) 0.7590(6) 1.0406(5) 0.065(2) Uani 1 1 d . . . P1 P 0.0000 0.0000 0.5000 0.0853(13) Uani 1 2 d S . . P2 P 1.0000 0.5000 1.0000 0.0893(14) Uani 1 2 d S . . P3 P -0.0143(4) 0.1251(4) 0.8383(3) 0.1348(19) Uani 1 1 d . . . P4 P 0.47465(18) 0.14406(15) 0.68737(16) 0.0541(6) Uani 1 1 d . . . P5 P 0.5000 0.5000 1.0000 0.0700(11) Uani 1 2 d S . . F1 F 0.0471(12) 0.0875(7) 0.4954(9) 0.191(6) Uani 1 1 d . . . F2 F 0.0090(9) 0.0550(8) 0.5949(6) 0.163(4) Uani 1 1 d . . . F3 F 0.1088(8) -0.0236(8) 0.5133(6) 0.157(4) Uani 1 1 d . . . F4 F 1.0364(8) 0.4750(11) 1.0708(8) 0.186(6) Uani 1 1 d . . . F5 F 1.0249(9) 0.5987(7) 1.0560(8) 0.176(5) Uani 1 1 d . . . F6 F 0.8867(6) 0.4930(6) 1.0194(6) 0.130(3) Uani 1 1 d . . . F7 F -0.0243(15) 0.1771(16) 0.9267(9) 0.280(11) Uani 1 1 d . . . F8 F 0.0754(15) 0.1004(16) 0.8737(10) 0.327(15) Uani 1 1 d . . . F9 F -0.0132(11) 0.0790(14) 0.7505(8) 0.274(11) Uani 1 1 d . . . F10 F -0.1170(12) 0.1455(11) 0.8122(8) 0.211(6) Uani 1 1 d . . . F11 F -0.065(2) 0.0431(15) 0.8431(16) 0.361(17) Uani 1 1 d . . . F12 F 0.0377(19) 0.2116(17) 0.8300(12) 0.339(15) Uani 1 1 d . . . F13 F 0.4716(6) 0.0598(5) 0.6072(4) 0.095(2) Uani 1 1 d . . . F14 F 0.4538(5) 0.0818(4) 0.7305(4) 0.0815(18) Uani 1 1 d . . . F15 F 0.4814(7) 0.2301(4) 0.7683(4) 0.102(2) Uani 1 1 d . . . F16 F 0.4946(5) 0.2054(5) 0.6419(4) 0.091(2) Uani 1 1 d . . . F17 F 0.3535(5) 0.1347(5) 0.6593(5) 0.090(2) Uani 1 1 d . . . F18 F 0.5976(5) 0.1505(5) 0.7119(5) 0.090(2) Uani 1 1 d . . . F19 F 0.6163(5) 0.4939(6) 0.9972(4) 0.105(2) Uani 1 1 d . . . F20 F 0.4873(8) 0.5244(11) 0.9271(7) 0.194(6) Uani 1 1 d . . . F21 F 0.4669(9) 0.4025(6) 0.9398(10) 0.209(7) Uani 1 1 d . . . C1 C 0.6578(7) 0.2449(6) 0.4603(6) 0.056(2) Uani 1 1 d . . . C2 C 0.6627(7) 0.1592(7) 0.4528(8) 0.077(3) Uani 1 1 d . . . H2A H 0.6296 0.1378 0.4855 0.092 Uiso 1 1 calc R . . C3 C 0.7139(7) 0.1059(7) 0.3999(7) 0.068(3) Uani 1 1 d . . . H3A H 0.7131 0.0484 0.3951 0.082 Uiso 1 1 calc R . . C4 C 0.7653(8) 0.1367(7) 0.3548(7) 0.068(3) Uani 1 1 d . . . C5 C 0.7637(9) 0.2219(7) 0.3610(7) 0.073(3) Uani 1 1 d . . . H5A H 0.7977 0.2425 0.3282 0.088 Uiso 1 1 calc R . . C6 C 0.7133(8) 0.2752(7) 0.4140(7) 0.068(3) Uani 1 1 d . . . H6A H 0.7162 0.3330 0.4193 0.081 Uiso 1 1 calc R . . C7 C 0.9378(11) 0.1135(11) 0.3222(13) 0.132(7) Uani 1 1 d . . . H7A H 0.9728 0.0764 0.2833 0.198 Uiso 1 1 calc R . . H7B H 0.9600 0.1127 0.3740 0.198 Uiso 1 1 calc R . . H7C H 0.9546 0.1730 0.3266 0.198 Uiso 1 1 calc R . . C8 C 0.8066(12) -0.0107(9) 0.2888(11) 0.112(5) Uani 1 1 d . . . H8A H 0.8452 -0.0443 0.2507 0.168 Uiso 1 1 calc R . . H8B H 0.7336 -0.0368 0.2703 0.168 Uiso 1 1 calc R . . H8C H 0.8298 -0.0106 0.3408 0.168 Uiso 1 1 calc R . . C9 C 0.790(2) 0.0782(17) 0.2150(13) 0.192(12) Uani 1 1 d . . . H9A H 0.8280 0.0424 0.1778 0.288 Uiso 1 1 calc R . . H9B H 0.8037 0.1372 0.2179 0.288 Uiso 1 1 calc R . . H9C H 0.7168 0.0536 0.1966 0.288 Uiso 1 1 calc R . . C10 C 0.3993(6) 0.4832(6) 0.6448(6) 0.055(2) Uani 1 1 d . . . C11 C 0.3064(8) 0.5082(6) 0.6616(6) 0.059(2) Uani 1 1 d . . . H11A H 0.2867 0.5534 0.6490 0.071 Uiso 1 1 calc R . . C12 C 0.2419(7) 0.4676(6) 0.6966(6) 0.058(2) Uani 1 1 d . . . H12A H 0.1805 0.4865 0.7087 0.069 Uiso 1 1 calc R . . C13 C 0.2691(7) 0.3992(7) 0.7134(6) 0.058(2) Uani 1 1 d . . . C14 C 0.3624(8) 0.3732(7) 0.6955(6) 0.065(3) Uani 1 1 d . . . H14A H 0.3810 0.3265 0.7058 0.078 Uiso 1 1 calc R . . C15 C 0.4255(8) 0.4146(7) 0.6637(7) 0.068(3) Uani 1 1 d . . . H15A H 0.4883 0.3972 0.6539 0.081 Uiso 1 1 calc R . . C16 C 0.2612(11) 0.3472(14) 0.8192(10) 0.140(7) Uani 1 1 d . . . H16A H 0.2911 0.4057 0.8598 0.210 Uiso 1 1 calc R . . H16B H 0.3158 0.3159 0.8027 0.210 Uiso 1 1 calc R . . H16C H 0.2161 0.3162 0.8411 0.210 Uiso 1 1 calc R . . C17 C 0.1559(11) 0.2590(8) 0.6888(8) 0.093(4) Uani 1 1 d . . . H17A H 0.1153 0.2584 0.6410 0.140 Uiso 1 1 calc R . . H17B H 0.1124 0.2299 0.7132 0.140 Uiso 1 1 calc R . . H17C H 0.2119 0.2286 0.6744 0.140 Uiso 1 1 calc R . . C18 C 0.1083(10) 0.3923(10) 0.7694(10) 0.108(5) Uani 1 1 d . . . H18A H 0.1309 0.4528 0.8078 0.163 Uiso 1 1 calc R . . H18B H 0.0681 0.3596 0.7928 0.163 Uiso 1 1 calc R . . H18C H 0.0660 0.3896 0.7214 0.163 Uiso 1 1 calc R . . C19 C 0.7485(6) 0.6539(5) 0.5731(5) 0.0429(18) Uani 1 1 d . . . C20 C 0.7026(8) 0.6944(7) 0.6365(6) 0.062(3) Uani 1 1 d . . . H20A H 0.6849 0.6654 0.6688 0.075 Uiso 1 1 calc R . . C21 C 0.6814(9) 0.7787(7) 0.6543(7) 0.069(3) Uani 1 1 d . . . H21A H 0.6527 0.8068 0.6993 0.083 Uiso 1 1 calc R . . C22 C 0.7035(7) 0.8189(6) 0.6045(6) 0.058(2) Uani 1 1 d . . . C23 C 0.7498(9) 0.7792(7) 0.5408(8) 0.078(3) Uani 1 1 d . . . H23A H 0.7678 0.8080 0.5084 0.093 Uiso 1 1 calc R . . C24 C 0.7702(9) 0.6945(6) 0.5246(7) 0.069(3) Uani 1 1 d . . . H24A H 0.7990 0.6661 0.4799 0.083 Uiso 1 1 calc R . . C25 C 0.6352(12) 0.9113(9) 0.5426(8) 0.101(5) Uani 1 1 d . . . H25A H 0.6851 0.9005 0.5077 0.152 Uiso 1 1 calc R . . H25B H 0.6202 0.9690 0.5540 0.152 Uiso 1 1 calc R . . H25C H 0.5721 0.8675 0.5163 0.152 Uiso 1 1 calc R . . C26 C 0.5978(14) 0.9261(10) 0.6713(11) 0.120(6) Uani 1 1 d . . . H26A H 0.5345 0.8829 0.6442 0.180 Uiso 1 1 calc R . . H26B H 0.5846 0.9839 0.6807 0.180 Uiso 1 1 calc R . . H26C H 0.6228 0.9241 0.7221 0.180 Uiso 1 1 calc R . . C27 C 0.7725(12) 0.9769(8) 0.6660(11) 0.120(6) Uani 1 1 d . . . H27A H 0.8270 0.9688 0.6352 0.180 Uiso 1 1 calc R . . H27B H 0.7956 0.9736 0.7166 0.180 Uiso 1 1 calc R . . H27C H 0.7556 1.0338 0.6763 0.180 Uiso 1 1 calc R . . C28 C 0.9804(8) 0.3873(7) 0.5135(6) 0.061(2) Uani 1 1 d . . . H28A H 0.9774 0.4484 0.5279 0.091 Uiso 1 1 calc R . . H28B H 0.9459 0.3529 0.4581 0.091 Uiso 1 1 calc R . . H28C H 1.0520 0.3814 0.5198 0.091 Uiso 1 1 calc R . . C29 C 0.9277(6) 0.3553(5) 0.5670(5) 0.0443(18) Uani 1 1 d . . . C30 C 0.9127(7) 0.2728(6) 0.5694(6) 0.056(2) Uani 1 1 d . . . H30A H 0.9377 0.2243 0.5374 0.067 Uiso 1 1 calc R . . C31 C 0.8559(7) 0.2752(6) 0.6257(6) 0.058(2) Uani 1 1 d . . . C32 C 0.8239(10) 0.2076(7) 0.6560(8) 0.084(4) Uani 1 1 d . . . H32A H 0.8436 0.1534 0.6241 0.125 Uiso 1 1 calc R . . H32B H 0.7496 0.1975 0.6519 0.125 Uiso 1 1 calc R . . H32C H 0.8576 0.2279 0.7116 0.125 Uiso 1 1 calc R . . C33 C 0.7856(6) 0.4025(6) 0.7180(6) 0.048(2) Uani 1 1 d . . . C34 C 0.7061(7) 0.3576(6) 0.7400(6) 0.057(2) Uani 1 1 d . . . H34A H 0.6862 0.2962 0.7156 0.069 Uiso 1 1 calc R . . C35 C 0.6589(8) 0.4084(7) 0.7994(7) 0.065(3) Uani 1 1 d . . . H35A H 0.6063 0.3805 0.8159 0.078 Uiso 1 1 calc R . . C36 C 0.6862(8) 0.4979(7) 0.8348(7) 0.069(3) Uani 1 1 d . . . H36A H 0.6541 0.5318 0.8753 0.082 Uiso 1 1 calc R . . C37 C 0.7614(7) 0.5346(6) 0.8087(6) 0.060(2) Uani 1 1 d . . . C38 C 0.7792(15) 0.6764(11) 0.9906(9) 0.121(5) Uani 1 1 d . . . H38A H 0.7499 0.6153 0.9756 0.182 Uiso 1 1 calc R . . H38B H 0.7291 0.7117 1.0109 0.182 Uiso 1 1 calc R . . H38C H 0.8408 0.6947 1.0319 0.182 Uiso 1 1 calc R . . C39 C 0.8076(10) 0.6886(8) 0.9155(8) 0.084(3) Uani 1 1 d . . . C40 C 0.8522(11) 0.7679(8) 0.9151(7) 0.096(4) Uani 1 1 d . . . H40A H 0.8664 0.8236 0.9579 0.116 Uiso 1 1 calc R . . C41 C 0.8709(9) 0.7473(7) 0.8389(7) 0.072(3) Uani 1 1 d . . . C42 C 0.9220(11) 0.8077(8) 0.8062(9) 0.099(4) Uani 1 1 d . . . H42A H 0.9246 0.7746 0.7504 0.148 Uiso 1 1 calc R . . H42B H 0.9916 0.8344 0.8369 0.148 Uiso 1 1 calc R . . H42C H 0.8827 0.8529 0.8102 0.148 Uiso 1 1 calc R . . C43 C 1.1378(6) 0.6633(6) 0.7965(6) 0.051(2) Uani 1 1 d . . . C44 C 1.2420(7) 0.7115(7) 0.8215(7) 0.069(3) Uani 1 1 d . A . H44A H 1.2746 0.7244 0.7840 0.083 Uiso 1 1 calc R . . C45 C 1.2952(7) 0.7393(7) 0.8979(6) 0.064(3) Uani 1 1 d . . . H45A H 1.3645 0.7686 0.9115 0.077 Uiso 1 1 calc R A . C46 C 1.2496(7) 0.7254(6) 0.9549(6) 0.057(2) Uani 1 1 d . A . C47 C 1.1484(8) 0.6840(8) 0.9359(7) 0.076(3) Uani 1 1 d . . . H47A H 1.1156 0.6766 0.9756 0.091 Uiso 1 1 calc R A . C48 C 1.0943(7) 0.6529(8) 0.8573(7) 0.074(3) Uani 1 1 d . A . H48A H 1.0251 0.6236 0.8451 0.089 Uiso 1 1 calc R . . C49 C 1.402(2) 0.721(3) 1.0357(18) 0.098(10) Uiso 0.52(4) 1 d P A 1 H49A H 1.4448 0.7417 1.0053 0.146 Uiso 0.52(4) 1 calc PR A 1 H49B H 1.3815 0.6577 1.0092 0.146 Uiso 0.52(4) 1 calc PR A 1 H49C H 1.4412 0.7377 1.0893 0.146 Uiso 0.52(4) 1 calc PR A 1 C50 C 1.341(3) 0.8526(18) 1.0778(18) 0.094(9) Uiso 0.52(4) 1 d P A 1 H50A H 1.3898 0.8721 1.0502 0.141 Uiso 0.52(4) 1 calc PR A 1 H50B H 1.3735 0.8715 1.1336 0.141 Uiso 0.52(4) 1 calc PR A 1 H50C H 1.2804 0.8775 1.0748 0.141 Uiso 0.52(4) 1 calc PR A 1 C51 C 1.235(2) 0.7293(18) 1.0925(14) 0.076(8) Uiso 0.52(4) 1 d P A 1 H51A H 1.2258 0.6666 1.0767 0.115 Uiso 0.52(4) 1 calc PR A 1 H51B H 1.1680 0.7439 1.0819 0.115 Uiso 0.52(4) 1 calc PR A 1 H51C H 1.2643 0.7598 1.1493 0.115 Uiso 0.52(4) 1 calc PR A 1 C49' C 1.427(2) 0.768(3) 1.0464(19) 0.092(10) Uiso 0.48(4) 1 d P A 2 H49D H 1.4477 0.7879 1.0067 0.137 Uiso 0.48(4) 1 calc PR A 2 H49E H 1.4457 0.7118 1.0365 0.137 Uiso 0.48(4) 1 calc PR A 2 H49F H 1.4622 0.8103 1.0996 0.137 Uiso 0.48(4) 1 calc PR A 2 C50' C 1.295(3) 0.8580(17) 1.0881(17) 0.079(8) Uiso 0.48(4) 1 d P A 2 H50D H 1.3368 0.8975 1.0717 0.119 Uiso 0.48(4) 1 calc PR A 2 H50E H 1.3162 0.8759 1.1454 0.119 Uiso 0.48(4) 1 calc PR A 2 H50F H 1.2231 0.8598 1.0755 0.119 Uiso 0.48(4) 1 calc PR A 2 C51' C 1.277(2) 0.7087(17) 1.0874(14) 0.065(7) Uiso 0.48(4) 1 d P A 2 H51D H 1.3245 0.6704 1.0894 0.098 Uiso 0.48(4) 1 calc PR A 2 H51E H 1.2085 0.6740 1.0616 0.098 Uiso 0.48(4) 1 calc PR A 2 H51F H 1.2764 0.7493 1.1415 0.098 Uiso 0.48(4) 1 calc PR A 2 P6 P 0.525(2) 0.930(2) 0.9015(18) 0.259(10) Uiso 0.50 1 d PD . . F27 F 0.548(4) 0.879(3) 0.957(3) 0.293(19) Uiso 0.50 1 d PD . . F26 F 0.628(3) 0.913(2) 0.863(2) 0.237(14) Uiso 0.50 1 d PD . . F25 F 0.492(4) 0.841(3) 0.822(3) 0.36(3) Uiso 0.50 1 d PD . . F24 F 0.567(4) 1.012(3) 0.985(3) 0.34(3) Uiso 0.50 1 d PD . . F23 F 0.483(3) 0.965(3) 0.839(2) 0.261(16) Uiso 0.50 1 d PD . . F22 F 0.422(3) 0.934(3) 0.938(3) 0.30(2) Uiso 0.50 1 d PD . . O1 O -0.143(4) 0.019(4) 1.006(3) 0.30(2) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0365(4) 0.0520(4) 0.0619(4) 0.0362(3) 0.0149(3) 0.0095(3) Cd2 0.0412(4) 0.0558(5) 0.0792(5) 0.0425(4) 0.0094(3) 0.0113(3) S1 0.0589(14) 0.0599(15) 0.0971(19) 0.0501(14) 0.0259(13) 0.0159(11) S2 0.0486(12) 0.0617(14) 0.0637(14) 0.0353(12) 0.0119(10) 0.0158(10) S3 0.0367(10) 0.0533(12) 0.0652(13) 0.0368(11) 0.0103(9) 0.0140(9) S4 0.0369(11) 0.0723(15) 0.0659(14) 0.0451(12) 0.0115(9) 0.0050(10) N1 0.089(7) 0.083(7) 0.103(8) 0.055(6) 0.032(6) 0.023(5) N2 0.053(5) 0.078(6) 0.074(5) 0.043(5) 0.022(4) 0.019(4) N3 0.060(5) 0.052(5) 0.087(6) 0.030(4) 0.009(4) 0.018(4) N4 0.044(4) 0.054(4) 0.070(5) 0.047(4) 0.015(3) 0.007(3) N5 0.038(4) 0.051(4) 0.064(4) 0.033(4) 0.018(3) 0.008(3) N6 0.051(4) 0.056(5) 0.055(4) 0.032(4) 0.026(3) 0.002(3) N7 0.085(6) 0.064(5) 0.061(5) 0.024(4) 0.039(4) 0.019(4) N8 0.060(5) 0.056(5) 0.067(5) 0.035(4) 0.022(4) 0.008(4) N9 0.063(5) 0.068(5) 0.069(5) 0.034(4) 0.011(4) 0.015(4) P1 0.097(3) 0.074(3) 0.106(4) 0.052(3) 0.027(3) 0.036(2) P2 0.070(3) 0.099(4) 0.121(4) 0.067(3) 0.033(3) 0.009(2) P3 0.114(4) 0.156(5) 0.103(3) 0.017(3) 0.023(3) 0.031(3) P4 0.0462(12) 0.0498(13) 0.0755(16) 0.0365(12) 0.0124(11) 0.0065(10) P5 0.049(2) 0.088(3) 0.066(2) 0.022(2) 0.0250(17) 0.0082(19) F1 0.248(15) 0.109(8) 0.256(15) 0.103(9) 0.103(12) 0.033(8) F2 0.187(11) 0.210(11) 0.101(6) 0.056(7) 0.030(7) 0.097(9) F3 0.136(8) 0.216(12) 0.143(8) 0.069(8) 0.042(7) 0.109(8) F4 0.101(7) 0.312(17) 0.229(13) 0.208(14) 0.027(8) 0.020(9) F5 0.159(10) 0.114(8) 0.226(13) 0.033(8) 0.102(9) -0.012(7) F6 0.092(6) 0.146(8) 0.184(9) 0.089(7) 0.071(6) 0.022(5) F7 0.239(18) 0.38(3) 0.152(12) 0.020(15) 0.020(12) 0.154(19) F8 0.234(18) 0.41(3) 0.185(14) -0.067(16) -0.038(13) 0.22(2) F9 0.145(11) 0.41(3) 0.145(10) -0.036(13) 0.046(9) 0.096(14) F10 0.182(13) 0.260(16) 0.180(12) 0.058(11) 0.026(10) 0.121(12) F11 0.42(3) 0.27(2) 0.36(3) 0.22(2) -0.15(3) -0.14(2) F12 0.33(3) 0.37(3) 0.24(2) 0.15(2) -0.004(17) -0.18(2) F13 0.123(6) 0.086(5) 0.091(5) 0.046(4) 0.018(4) 0.040(4) F14 0.071(4) 0.096(5) 0.107(5) 0.076(4) 0.014(3) 0.012(3) F15 0.132(6) 0.065(4) 0.093(5) 0.013(4) 0.018(4) 0.032(4) F16 0.089(5) 0.094(5) 0.119(5) 0.079(4) 0.017(4) 0.005(4) F17 0.055(3) 0.097(5) 0.134(6) 0.068(5) 0.007(4) 0.016(3) F18 0.052(3) 0.097(5) 0.144(6) 0.075(5) 0.014(4) 0.010(3) F19 0.060(4) 0.159(7) 0.101(5) 0.049(5) 0.035(4) 0.031(4) F20 0.094(6) 0.41(2) 0.193(11) 0.224(14) 0.070(7) 0.082(9) F21 0.130(8) 0.096(7) 0.293(16) -0.001(8) -0.074(9) 0.035(6) C1 0.041(5) 0.052(5) 0.085(7) 0.040(5) 0.011(4) 0.006(4) C2 0.036(5) 0.074(7) 0.153(11) 0.081(8) 0.021(6) 0.014(5) C3 0.046(5) 0.066(6) 0.122(9) 0.068(6) 0.015(5) 0.013(5) C4 0.055(6) 0.067(6) 0.097(8) 0.047(6) 0.021(5) 0.011(5) C5 0.080(7) 0.076(7) 0.081(7) 0.051(6) 0.021(6) 0.007(6) C6 0.074(7) 0.056(6) 0.089(7) 0.041(6) 0.029(6) 0.019(5) C7 0.072(9) 0.108(11) 0.25(2) 0.095(13) 0.074(11) 0.015(8) C8 0.114(11) 0.076(8) 0.177(15) 0.066(10) 0.075(11) 0.032(8) C9 0.28(3) 0.24(3) 0.142(17) 0.108(18) 0.11(2) 0.18(3) C10 0.039(4) 0.066(6) 0.071(6) 0.038(5) 0.009(4) 0.014(4) C11 0.064(6) 0.055(5) 0.063(6) 0.026(5) 0.011(5) 0.026(5) C12 0.047(5) 0.065(6) 0.069(6) 0.030(5) 0.022(4) 0.021(4) C13 0.055(5) 0.069(6) 0.058(5) 0.031(5) 0.016(4) 0.021(5) C14 0.066(6) 0.076(7) 0.080(7) 0.052(6) 0.029(5) 0.032(5) C15 0.059(6) 0.088(7) 0.085(7) 0.054(6) 0.027(5) 0.041(5) C16 0.073(9) 0.27(2) 0.151(14) 0.166(16) 0.018(9) 0.018(11) C17 0.103(10) 0.079(9) 0.104(10) 0.041(8) 0.037(8) 0.014(7) C18 0.073(8) 0.122(12) 0.154(14) 0.066(11) 0.058(9) 0.032(8) C19 0.034(4) 0.043(4) 0.063(5) 0.032(4) 0.008(4) 0.012(3) C20 0.064(6) 0.089(7) 0.059(5) 0.046(5) 0.024(5) 0.035(5) C21 0.084(7) 0.056(6) 0.079(7) 0.032(5) 0.029(6) 0.028(5) C22 0.054(5) 0.053(5) 0.077(6) 0.035(5) 0.006(5) 0.018(4) C23 0.097(8) 0.059(6) 0.110(9) 0.060(7) 0.038(7) 0.027(6) C24 0.088(7) 0.048(5) 0.097(8) 0.044(6) 0.036(6) 0.031(5) C25 0.147(13) 0.101(9) 0.109(10) 0.078(8) 0.037(9) 0.073(9) C26 0.139(14) 0.106(11) 0.176(16) 0.094(12) 0.071(13) 0.073(11) C27 0.120(12) 0.051(7) 0.177(16) 0.050(9) -0.020(11) 0.014(7) C28 0.062(6) 0.064(6) 0.069(6) 0.039(5) 0.022(5) 0.008(5) C29 0.036(4) 0.049(5) 0.056(5) 0.026(4) 0.014(4) 0.015(4) C30 0.045(5) 0.054(5) 0.080(6) 0.037(5) 0.017(4) 0.018(4) C31 0.058(5) 0.046(5) 0.087(7) 0.041(5) 0.023(5) 0.016(4) C32 0.091(8) 0.061(7) 0.131(10) 0.062(7) 0.048(8) 0.026(6) C33 0.035(4) 0.052(5) 0.079(6) 0.047(5) 0.018(4) 0.012(4) C34 0.058(5) 0.058(6) 0.067(6) 0.034(5) 0.024(5) 0.010(4) C35 0.059(6) 0.071(7) 0.087(7) 0.050(6) 0.038(5) 0.010(5) C36 0.070(7) 0.070(7) 0.079(7) 0.034(6) 0.045(6) 0.016(5) C37 0.062(6) 0.057(6) 0.070(6) 0.036(5) 0.025(5) 0.002(4) C38 0.173(17) 0.113(12) 0.089(10) 0.049(9) 0.053(10) 0.017(11) C39 0.089(8) 0.074(8) 0.099(9) 0.046(7) 0.030(7) 0.004(6) C40 0.129(11) 0.070(8) 0.070(7) 0.003(6) 0.053(7) 0.002(7) C41 0.080(7) 0.061(7) 0.075(7) 0.028(6) 0.030(6) 0.003(5) C42 0.117(11) 0.057(7) 0.114(10) 0.027(7) 0.048(8) -0.007(7) C43 0.030(4) 0.058(5) 0.078(6) 0.038(5) 0.018(4) 0.012(4) C44 0.041(5) 0.095(8) 0.091(8) 0.062(7) 0.011(5) 0.002(5) C45 0.046(5) 0.082(7) 0.069(6) 0.043(6) 0.006(4) -0.005(5) C46 0.049(5) 0.055(5) 0.064(6) 0.026(5) 0.000(4) 0.010(4) C47 0.060(6) 0.119(10) 0.076(7) 0.063(7) 0.027(5) 0.019(6) C48 0.042(5) 0.114(9) 0.089(7) 0.075(7) -0.001(5) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 N8 2.336(8) . ? Cd1 N6 2.360(6) . ? Cd1 N4 2.370(7) . ? Cd1 S4 2.477(2) . ? Cd1 S3 2.569(2) . ? Cd2 S1 2.450(2) . ? Cd2 S3 2.568(2) . ? Cd2 S2 2.597(3) . ? Cd2 S2 2.633(2) 2_666 ? S1 C1 1.775(10) . ? S2 C10 1.778(9) . ? S2 Cd2 2.633(2) 2_666 ? S3 C19 1.783(7) . ? S4 C43 1.760(10) . ? N1 C8 1.479(15) . ? N1 C9 1.48(2) . ? N1 C7 1.496(17) . ? N1 C4 1.521(15) . ? N2 C13 1.484(12) . ? N2 C18 1.493(14) . ? N2 C16 1.497(15) . ? N2 C17 1.525(15) . ? N3 C22 1.495(11) . ? N3 C25 1.497(14) . ? N3 C27 1.502(16) . ? N3 C26 1.512(17) . ? N4 C29 1.339(10) . ? N4 N5 1.388(8) . ? N5 C33 1.377(11) . ? N5 C31 1.410(11) . ? N6 C33 1.334(11) . ? N6 C37 1.348(11) . ? N7 C39 1.349(15) . ? N7 N8 1.378(10) . ? N7 C37 1.419(12) . ? N8 C41 1.335(13) . ? N9 C49 1.43(3) . ? N9 C50 1.43(3) . ? N9 C51' 1.50(2) . ? N9 C49' 1.50(3) . ? N9 C46 1.537(12) . ? N9 C50' 1.62(3) . ? N9 C51 1.65(3) . ? P1 F1 1.568(10) . ? P1 F1 1.568(10) 2_556 ? P1 F3 1.570(9) 2_556 ? P1 F3 1.570(9) . ? P1 F2 1.611(10) . ? P1 F2 1.611(10) 2_556 ? P2 F5 1.547(11) . ? P2 F5 1.547(11) 2_767 ? P2 F4 1.564(10) . ? P2 F4 1.564(10) 2_767 ? P2 F6 1.595(7) 2_767 ? P2 F6 1.595(7) . ? P3 F8 1.477(16) . ? P3 F11 1.500(18) . ? P3 F9 1.502(13) . ? P3 F10 1.522(13) . ? P3 F7 1.557(16) . ? P3 F12 1.60(2) . ? P4 F14 1.565(6) . ? P4 F16 1.585(6) . ? P4 F13 1.597(8) . ? P4 F17 1.599(6) . ? P4 F15 1.613(7) . ? P4 F18 1.621(6) . ? P5 F20 1.549(9) 2_667 ? P5 F20 1.549(9) . ? P5 F21 1.551(10) 2_667 ? P5 F21 1.551(10) . ? P5 F19 1.574(6) . ? P5 F19 1.574(6) 2_667 ? C1 C6 1.392(13) . ? C1 C2 1.416(12) . ? C2 C3 1.372(16) . ? C2 H2A 0.9400 . ? C3 C4 1.350(13) . ? C3 H3A 0.9400 . ? C4 C5 1.405(14) . ? C5 C6 1.366(15) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.396(12) . ? C10 C15 1.408(12) . ? C11 C12 1.398(13) . ? C11 H11A 0.9400 . ? C12 C13 1.391(12) . ? C12 H12A 0.9400 . ? C13 C14 1.410(13) . ? C14 C15 1.352(14) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C24 1.357(12) . ? C19 C20 1.374(12) . ? C20 C21 1.411(13) . ? C20 H20A 0.9400 . ? C21 C22 1.376(13) . ? C21 H21A 0.9400 . ? C22 C23 1.377(15) . ? C23 C24 1.419(13) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C29 1.500(11) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 H28C 0.9700 . ? C29 C30 1.402(11) . ? C30 C31 1.351(13) . ? C30 H30A 0.9400 . ? C31 C32 1.494(12) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C33 C34 1.413(11) . ? C34 C35 1.389(13) . ? C34 H34A 0.9400 . ? C35 C36 1.369(15) . ? C35 H35A 0.9400 . ? C36 C37 1.346(12) . ? C36 H36A 0.9400 . ? C38 C39 1.563(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C38 H38C 0.9700 . ? C39 C40 1.395(16) . ? C40 C41 1.376(15) . ? C40 H40A 0.9400 . ? C41 C42 1.506(15) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C42 H42C 0.9700 . ? C43 C48 1.384(13) . ? C43 C44 1.431(12) . ? C44 C45 1.363(14) . ? C44 H44A 0.9400 . ? C45 C46 1.358(13) . ? C45 H45A 0.9400 . ? C46 C47 1.366(14) . ? C47 C48 1.391(15) . ? C47 H47A 0.9400 . ? C48 H48A 0.9400 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C49 H49C 0.9700 . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C50 H50C 0.9700 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 H51C 0.9700 . ? C49' H49D 0.9700 . ? C49' H49E 0.9700 . ? C49' H49F 0.9700 . ? C50' H50D 0.9700 . ? C50' H50E 0.9700 . ? C50' H50F 0.9700 . ? C51' H51D 0.9700 . ? C51' H51E 0.9700 . ? C51' H51F 0.9700 . ? P6 F23 1.573(18) . ? P6 F24 1.59(2) . ? P6 F27 1.594(19) . ? P6 F25 1.60(2) . ? P6 F22 1.612(19) . ? P6 F26 1.630(19) . ? F24 F22 1.33(5) 2_677 ? F22 F24 1.33(5) 2_677 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Cd1 N6 69.1(2) . . ? N8 Cd1 N4 136.7(2) . . ? N6 Cd1 N4 67.6(2) . . ? N8 Cd1 S4 105.2(2) . . ? N6 Cd1 S4 132.39(19) . . ? N4 Cd1 S4 104.55(17) . . ? N8 Cd1 S3 108.6(2) . . ? N6 Cd1 S3 113.92(19) . . ? N4 Cd1 S3 87.85(17) . . ? S4 Cd1 S3 112.51(8) . . ? S1 Cd2 S3 120.47(8) . . ? S1 Cd2 S2 111.41(8) . . ? S3 Cd2 S2 108.00(8) . . ? S1 Cd2 S2 117.64(10) . 2_666 ? S3 Cd2 S2 101.43(8) . 2_666 ? S2 Cd2 S2 94.42(8) . 2_666 ? C1 S1 Cd2 108.0(3) . . ? C10 S2 Cd2 113.2(3) . . ? C10 S2 Cd2 112.0(3) . 2_666 ? Cd2 S2 Cd2 85.58(8) . 2_666 ? C19 S3 Cd2 102.7(3) . . ? C19 S3 Cd1 107.0(3) . . ? Cd2 S3 Cd1 112.18(8) . . ? C43 S4 Cd1 107.6(3) . . ? C8 N1 C9 108.4(14) . . ? C8 N1 C7 105.2(10) . . ? C9 N1 C7 109.6(15) . . ? C8 N1 C4 112.1(9) . . ? C9 N1 C4 110.1(10) . . ? C7 N1 C4 111.4(11) . . ? C13 N2 C18 114.4(8) . . ? C13 N2 C16 109.9(8) . . ? C18 N2 C16 111.0(11) . . ? C13 N2 C17 110.8(8) . . ? C18 N2 C17 104.9(10) . . ? C16 N2 C17 105.4(11) . . ? C22 N3 C25 111.2(8) . . ? C22 N3 C27 109.7(8) . . ? C25 N3 C27 112.2(10) . . ? C22 N3 C26 111.7(8) . . ? C25 N3 C26 106.5(10) . . ? C27 N3 C26 105.4(12) . . ? C29 N4 N5 105.9(6) . . ? C29 N4 Cd1 135.8(5) . . ? N5 N4 Cd1 116.5(5) . . ? C33 N5 N4 117.4(6) . . ? C33 N5 C31 132.8(7) . . ? N4 N5 C31 109.8(7) . . ? C33 N6 C37 118.8(7) . . ? C33 N6 Cd1 119.3(5) . . ? C37 N6 Cd1 118.5(6) . . ? C39 N7 N8 110.6(8) . . ? C39 N7 C37 130.6(8) . . ? N8 N7 C37 118.7(7) . . ? C41 N8 N7 105.2(8) . . ? C41 N8 Cd1 134.7(6) . . ? N7 N8 Cd1 115.3(6) . . ? C49 N9 C50 110.3(19) . . ? C49 N9 C51' 88.5(16) . . ? C50 N9 C51' 120.7(16) . . ? C49 N9 C49' 29.8(14) . . ? C50 N9 C49' 81.2(18) . . ? C51' N9 C49' 109.3(16) . . ? C49 N9 C46 107.4(14) . . ? C50 N9 C46 112.0(13) . . ? C51' N9 C46 114.6(11) . . ? C49' N9 C46 114.6(13) . . ? C49 N9 C50' 132.7(19) . . ? C50 N9 C50' 24.4(15) . . ? C51' N9 C50' 106.2(14) . . ? C49' N9 C50' 104.8(18) . . ? C46 N9 C50' 106.4(11) . . ? C49 N9 C51 113.7(16) . . ? C50 N9 C51 107.4(16) . . ? C51' N9 C51 25.3(10) . . ? C49' N9 C51 131.5(16) . . ? C46 N9 C51 106.1(11) . . ? C50' N9 C51 87.1(14) . . ? F1 P1 F1 180.000(1) . 2_556 ? F1 P1 F3 87.3(7) . 2_556 ? F1 P1 F3 92.7(7) 2_556 2_556 ? F1 P1 F3 92.7(7) . . ? F1 P1 F3 87.3(7) 2_556 . ? F3 P1 F3 180.0(8) 2_556 . ? F1 P1 F2 88.0(7) . . ? F1 P1 F2 92.0(7) 2_556 . ? F3 P1 F2 88.0(5) 2_556 . ? F3 P1 F2 92.0(5) . . ? F1 P1 F2 92.0(7) . 2_556 ? F1 P1 F2 88.0(7) 2_556 2_556 ? F3 P1 F2 92.0(5) 2_556 2_556 ? F3 P1 F2 88.0(5) . 2_556 ? F2 P1 F2 180.000(2) . 2_556 ? F5 P2 F5 180.0(5) . 2_767 ? F5 P2 F4 92.0(8) . . ? F5 P2 F4 88.0(8) 2_767 . ? F5 P2 F4 88.0(8) . 2_767 ? F5 P2 F4 92.0(8) 2_767 2_767 ? F4 P2 F4 180.000(4) . 2_767 ? F5 P2 F6 90.3(5) . 2_767 ? F5 P2 F6 89.7(5) 2_767 2_767 ? F4 P2 F6 91.2(5) . 2_767 ? F4 P2 F6 88.8(5) 2_767 2_767 ? F5 P2 F6 89.7(5) . . ? F5 P2 F6 90.3(5) 2_767 . ? F4 P2 F6 88.8(5) . . ? F4 P2 F6 91.2(5) 2_767 . ? F6 P2 F6 180.00(16) 2_767 . ? F8 P3 F11 79.1(15) . . ? F8 P3 F9 100.6(9) . . ? F11 P3 F9 93.1(15) . . ? F8 P3 F10 169.3(14) . . ? F11 P3 F10 92.8(13) . . ? F9 P3 F10 86.6(8) . . ? F8 P3 F7 85.2(9) . . ? F11 P3 F7 88.5(15) . . ? F9 P3 F7 174.2(10) . . ? F10 P3 F7 87.8(8) . . ? F8 P3 F12 102.5(15) . . ? F11 P3 F12 177.9(12) . . ? F9 P3 F12 85.2(12) . . ? F10 P3 F12 85.8(13) . . ? F7 P3 F12 93.0(13) . . ? F14 P4 F16 178.8(4) . . ? F14 P4 F13 88.5(4) . . ? F16 P4 F13 90.4(4) . . ? F14 P4 F17 91.2(3) . . ? F16 P4 F17 88.2(4) . . ? F13 P4 F17 88.6(4) . . ? F14 P4 F15 92.3(4) . . ? F16 P4 F15 88.8(4) . . ? F13 P4 F15 178.2(5) . . ? F17 P4 F15 93.0(4) . . ? F14 P4 F18 89.3(3) . . ? F16 P4 F18 91.2(4) . . ? F13 P4 F18 89.0(4) . . ? F17 P4 F18 177.5(4) . . ? F15 P4 F18 89.5(4) . . ? F20 P5 F20 180.000(5) 2_667 . ? F20 P5 F21 87.8(9) 2_667 2_667 ? F20 P5 F21 92.2(9) . 2_667 ? F20 P5 F21 92.2(9) 2_667 . ? F20 P5 F21 87.8(9) . . ? F21 P5 F21 180.0(5) 2_667 . ? F20 P5 F19 87.5(4) 2_667 . ? F20 P5 F19 92.5(4) . . ? F21 P5 F19 90.5(6) 2_667 . ? F21 P5 F19 89.5(5) . . ? F20 P5 F19 92.5(4) 2_667 2_667 ? F20 P5 F19 87.5(4) . 2_667 ? F21 P5 F19 89.5(5) 2_667 2_667 ? F21 P5 F19 90.5(6) . 2_667 ? F19 P5 F19 180.000(3) . 2_667 ? C6 C1 C2 116.2(9) . . ? C6 C1 S1 124.6(7) . . ? C2 C1 S1 119.1(8) . . ? C3 C2 C1 122.8(9) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C4 C3 C2 119.4(9) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.7(10) . . ? C3 C4 N1 121.3(9) . . ? C5 C4 N1 119.0(9) . . ? C6 C5 C4 120.9(9) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C1 120.8(9) . . ? C5 C6 H6A 119.6 . . ? C1 C6 H6A 119.6 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.5(8) . . ? C11 C10 S2 120.1(7) . . ? C15 C10 S2 122.1(7) . . ? C10 C11 C12 121.5(8) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C13 C12 C11 119.7(8) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C12 C13 C14 118.8(9) . . ? C12 C13 N2 120.6(8) . . ? C14 C13 N2 120.7(8) . . ? C15 C14 C13 121.0(9) . . ? C15 C14 H14A 119.5 . . ? C13 C14 H14A 119.5 . . ? C14 C15 C10 121.5(9) . . ? C14 C15 H15A 119.2 . . ? C10 C15 H15A 119.2 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 119.2(8) . . ? C24 C19 S3 119.9(7) . . ? C20 C19 S3 120.9(6) . . ? C19 C20 C21 121.4(9) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C22 C21 C20 118.7(9) . . ? C22 C21 H21A 120.7 . . ? C20 C21 H21A 120.7 . . ? C21 C22 C23 120.5(8) . . ? C21 C22 N3 120.3(9) . . ? C23 C22 N3 119.2(8) . . ? C22 C23 C24 119.3(9) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C19 C24 C23 120.8(10) . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 C30 110.2(7) . . ? N4 C29 C28 119.2(7) . . ? C30 C29 C28 130.5(8) . . ? C31 C30 C29 108.2(8) . . ? C31 C30 H30A 125.9 . . ? C29 C30 H30A 125.9 . . ? C30 C31 N5 105.8(7) . . ? C30 C31 C32 130.3(8) . . ? N5 C31 C32 123.6(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N6 C33 N5 115.6(7) . . ? N6 C33 C34 120.9(8) . . ? N5 C33 C34 123.4(8) . . ? C35 C34 C33 116.8(9) . . ? C35 C34 H34A 121.6 . . ? C33 C34 H34A 121.6 . . ? C36 C35 C34 122.3(8) . . ? C36 C35 H35A 118.9 . . ? C34 C35 H35A 118.9 . . ? C37 C36 C35 116.5(9) . . ? C37 C36 H36A 121.8 . . ? C35 C36 H36A 121.8 . . ? C36 C37 N6 124.7(9) . . ? C36 C37 N7 123.0(9) . . ? N6 C37 N7 112.3(7) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 107.0(10) . . ? N7 C39 C38 127.8(11) . . ? C40 C39 C38 125.1(12) . . ? C41 C40 C39 105.4(10) . . ? C41 C40 H40A 127.3 . . ? C39 C40 H40A 127.3 . . ? N8 C41 C40 111.7(9) . . ? N8 C41 C42 120.2(9) . . ? C40 C41 C42 128.0(11) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 114.6(9) . . ? C48 C43 S4 126.8(7) . . ? C44 C43 S4 118.5(7) . . ? C45 C44 C43 121.9(9) . . ? C45 C44 H44A 119.0 . . ? C43 C44 H44A 119.0 . . ? C46 C45 C44 121.0(9) . . ? C46 C45 H45A 119.5 . . ? C44 C45 H45A 119.5 . . ? C45 C46 C47 119.8(9) . . ? C45 C46 N9 119.1(8) . . ? C47 C46 N9 121.0(9) . . ? C46 C47 C48 119.6(9) . . ? C46 C47 H47A 120.2 . . ? C48 C47 H47A 120.2 . . ? C43 C48 C47 122.9(9) . . ? C43 C48 H48A 118.6 . . ? C47 C48 H48A 118.6 . . ? N9 C49 H49A 109.5 . . ? N9 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N9 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N9 C50 H50A 109.5 . . ? N9 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N9 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N9 C51 H51A 109.5 . . ? N9 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N9 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N9 C49' H49D 109.5 . . ? N9 C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? N9 C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? N9 C50' H50D 109.5 . . ? N9 C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? N9 C50' H50F 109.5 . . ? H50D C50' H50F 109.5 . . ? H50E C50' H50F 109.5 . . ? N9 C51' H51D 109.5 . . ? N9 C51' H51E 109.5 . . ? H51D C51' H51E 109.5 . . ? N9 C51' H51F 109.5 . . ? H51D C51' H51F 109.5 . . ? H51E C51' H51F 109.5 . . ? F23 P6 F24 107(3) . . ? F23 P6 F27 169(3) . . ? F24 P6 F27 81(3) . . ? F23 P6 F25 79(3) . . ? F24 P6 F25 173(4) . . ? F27 P6 F25 92(3) . . ? F23 P6 F22 93(3) . . ? F24 P6 F22 80(3) . . ? F27 P6 F22 81(3) . . ? F25 P6 F22 102(4) . . ? F23 P6 F26 91(2) . . ? F24 P6 F26 104(3) . . ? F27 P6 F26 94(3) . . ? F25 P6 F26 73(3) . . ? F22 P6 F26 173(3) . . ? F22 F24 P6 161(5) 2_677 . ? F24 F22 P6 116(5) 2_677 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C5 H5A S4 0.94 2.80 3.653(10) 151.5 2_766 C8 H8A F8 0.97 2.55 3.47(2) 159.9 2_656 C8 H8A F9 0.97 2.39 3.188(18) 139.0 2_656 C8 H8B F14 0.97 2.51 3.443(16) 161.7 2_656 C8 H8C F3 0.97 2.52 3.48(2) 168.0 2_656 C15 H15A S1 0.94 2.82 3.606(10) 142.2 . C27 H27B F11 0.97 2.54 3.36(3) 142.7 1_665 C36 H36A F20 0.94 2.54 3.316(13) 140.6 . C49 H49C F15 0.97 2.51 3.47(3) 171.5 2_767 C51 H51B F10 0.97 2.37 2.96(4) 118.3 2_667 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.996 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.155 #===END