# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Charles Young' _publ_contact_author_address ; School of Chemistry University of Melbourne Parkville Victoria 3010 AUSTRALIA ; _publ_contact_author_email CGYOUNG@UNIMELB.EDU.AU _publ_section_title ; Highly-Oxidised, Sulfur-Rich, Mixed-Valence Vanadium(IV/V) Complexes ; loop_ _publ_author_name 'C. Young' 'David J. Evans' 'Michelle K. Taylor' # Attachment 'Complexes_1a_1b.cif' data_c:complex_1a _database_code_depnum_ccdc_archive 'CCDC 614332' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C36H71N4S12V2,B0.40F1.60,CH2Cl2,0.6(BF4) _chemical_formula_sum 'C37 H74 B Cl2 F4 N4 S12 V2' _chemical_formula_weight 1219.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6884(8) _cell_length_b 16.6907(11) _cell_length_c 17.7774(11) _cell_angle_alpha 105.7420(10) _cell_angle_beta 95.2160(10) _cell_angle_gamma 107.4620(10) _cell_volume 3127.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 3098 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 26.11 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.356 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1274 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.840928 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS: Area-Detector Absorption Correction' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19387 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0865 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.50 _reflns_number_total 13518 _reflns_number_gt 8735 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1041P)^2^+3.3496P] 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 13518 _refine_ls_number_parameters 657 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.2086 _refine_ls_wR_factor_gt 0.1791 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.076 _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 V2 V 0.73285(8) 0.91260(6) 0.54444(5) 0.0224(2) Uani 1 1 d . . . V1 V 0.66069(7) 0.89377(6) 0.37634(5) 0.0218(2) Uani 1 1 d . . . Cl1 Cl 0.3181(3) 0.6259(3) 0.7784(2) 0.1352(14) Uani 1 1 d . . . Cl2 Cl 0.2059(4) 0.4660(3) 0.6474(3) 0.1672(18) Uani 1 1 d . . . S1 S 0.83083(11) 1.00328(9) 0.46990(7) 0.0254(3) Uani 1 1 d . . . S2 S 0.84910(12) 0.88350(10) 0.43848(7) 0.0273(3) Uani 1 1 d . . . S3 S 0.56969(12) 0.79274(9) 0.44712(8) 0.0268(3) Uani 1 1 d . . . S4 S 0.54127(11) 0.90887(9) 0.47898(7) 0.0232(3) Uani 1 1 d . . . S5 S 0.65670(12) 0.75430(9) 0.27916(8) 0.0270(3) Uani 1 1 d . . . S6 S 0.47241(11) 0.83337(9) 0.28033(7) 0.0268(3) Uani 1 1 d . . . S7 S 0.75640(12) 0.94955(9) 0.27614(7) 0.0253(3) Uani 1 1 d . . . S8 S 0.62175(12) 1.03318(9) 0.37550(8) 0.0254(3) Uani 1 1 d . . . S9 S 0.71786(11) 1.05583(9) 0.62056(7) 0.0249(3) Uani 1 1 d . . . S10 S 0.91417(11) 0.99517(9) 0.64859(7) 0.0255(3) Uani 1 1 d . . . S11 S 0.63184(12) 0.86874(10) 0.64811(8) 0.0281(3) Uani 1 1 d . . . S12 S 0.78985(14) 0.78980(10) 0.56898(8) 0.0333(3) Uani 1 1 d . . . F5 F 1.0375(8) 1.4159(5) 0.0982(5) 0.046(2) Uani 0.40 1 d PDU . . N1 N 0.4558(4) 0.6877(3) 0.1635(2) 0.0274(10) Uani 1 1 d . . . N2 N 0.7444(4) 1.1087(3) 0.2783(3) 0.0271(10) Uani 1 1 d . . . N3 N 0.9226(4) 1.1621(3) 0.7266(2) 0.0234(9) Uani 1 1 d . . . N4 N 0.6881(5) 0.7374(3) 0.6845(3) 0.0379(12) Uani 1 1 d . . . C1 C 0.5185(5) 0.7480(4) 0.2314(3) 0.0248(11) Uani 1 1 d . . . C2 C 0.4941(5) 0.6116(4) 0.1261(3) 0.0307(13) Uani 1 1 d . . . H2A H 0.4731 0.5961 0.0675 0.037 Uiso 1 1 calc R . . H2B H 0.5839 0.6293 0.1410 0.037 Uiso 1 1 calc R . . C3 C 0.4372(11) 0.5334(5) 0.1492(6) 0.091(4) Uani 1 1 d D . . C4 C 0.4631(13) 0.4536(6) 0.0948(7) 0.119(5) Uani 1 1 d . . . H4A H 0.5471 0.4574 0.1122 0.179 Uiso 1 1 calc R . . H4B H 0.4523 0.4543 0.0397 0.179 Uiso 1 1 calc R . . H4C H 0.4062 0.3985 0.0981 0.179 Uiso 1 1 calc R . . C6 C 0.3455(5) 0.6928(4) 0.1229(3) 0.0306(12) Uani 1 1 d . . . H6A H 0.3088 0.7261 0.1628 0.037 Uiso 1 1 calc R . . H6B H 0.2860 0.6322 0.0986 0.037 Uiso 1 1 calc R . . C7 C 0.3666(7) 0.7373(7) 0.0580(6) 0.072(3) Uani 1 1 d . . . H7 H 0.3721 0.6900 0.0114 0.086 Uiso 1 1 calc R . . C8 C 0.2498(8) 0.7527(8) 0.0317(7) 0.100(4) Uani 1 1 d . . . H8A H 0.2437 0.8045 0.0712 0.150 Uiso 1 1 calc R . . H8B H 0.1793 0.7006 0.0270 0.150 Uiso 1 1 calc R . . H8C H 0.2510 0.7631 -0.0199 0.150 Uiso 1 1 calc R . . C9 C 0.4728(9) 0.8083(11) 0.0687(8) 0.139(6) Uani 1 1 d . . . H9A H 0.4764 0.8244 0.0197 0.208 Uiso 1 1 calc R . . H9B H 0.5440 0.7917 0.0815 0.208 Uiso 1 1 calc R . . H9C H 0.4729 0.8589 0.1124 0.208 Uiso 1 1 calc R . . C10 C 0.7134(4) 1.0411(4) 0.3053(3) 0.0238(11) Uani 1 1 d . . . C11 C 0.8166(5) 1.1080(4) 0.2136(3) 0.0330(13) Uani 1 1 d . . . H11A H 0.8790 1.0808 0.2226 0.040 Uiso 1 1 calc R . . H11B H 0.8598 1.1698 0.2160 0.040 Uiso 1 1 calc R . . C12 C 0.7397(7) 1.0583(6) 0.1321(4) 0.055(2) Uani 1 1 d . . . H12 H 0.7048 0.9951 0.1304 0.066 Uiso 1 1 calc R . . C13 C 0.8226(7) 1.0599(6) 0.0699(4) 0.062(2) Uani 1 1 d . . . H13A H 0.7743 1.0224 0.0173 0.094 Uiso 1 1 calc R . . H13B H 0.8877 1.0376 0.0836 0.094 Uiso 1 1 calc R . . H13C H 0.8589 1.1207 0.0692 0.094 Uiso 1 1 calc R . . C14 C 0.6367(9) 1.0852(8) 0.1123(5) 0.087(3) Uani 1 1 d . . . H14A H 0.5813 1.0767 0.1499 0.131 Uiso 1 1 calc R . . H14B H 0.5931 1.0492 0.0582 0.131 Uiso 1 1 calc R . . H14C H 0.6662 1.1477 0.1155 0.131 Uiso 1 1 calc R . . C15 C 0.7092(5) 1.1866(4) 0.3119(3) 0.0327(13) Uani 1 1 d . . . H15A H 0.6232 1.1665 0.3189 0.039 Uiso 1 1 calc R . . H15B H 0.7141 1.2206 0.2738 0.039 Uiso 1 1 calc R . . C16 C 0.7892(6) 1.2473(4) 0.3916(4) 0.0421(15) Uani 1 1 d . . . H16 H 0.7911 1.2102 0.4271 0.050 Uiso 1 1 calc R . . C17 C 0.9204(7) 1.2911(5) 0.3839(5) 0.059(2) Uani 1 1 d . . . H17A H 0.9555 1.2455 0.3615 0.088 Uiso 1 1 calc R . . H17B H 0.9686 1.3287 0.4365 0.088 Uiso 1 1 calc R . . H17C H 0.9213 1.3273 0.3487 0.088 Uiso 1 1 calc R . . C18 C 0.7333(8) 1.3154(5) 0.4301(5) 0.064(2) Uani 1 1 d . . . H18A H 0.7852 1.3539 0.4815 0.096 Uiso 1 1 calc R . . H18B H 0.6518 1.2854 0.4384 0.096 Uiso 1 1 calc R . . H18C H 0.7269 1.3512 0.3954 0.096 Uiso 1 1 calc R . . C19 C 0.8618(4) 1.0825(4) 0.6736(3) 0.0242(11) Uani 1 1 d . . . C20 C 0.8745(5) 1.2345(4) 0.7379(3) 0.0307(13) Uani 1 1 d . . . H20A H 0.8908 1.2671 0.7955 0.037 Uiso 1 1 calc R . . H20B H 0.7848 1.2096 0.7197 0.037 Uiso 1 1 calc R . . C21 C 0.9279(6) 1.2993(4) 0.6943(4) 0.0387(14) Uani 1 1 d . . . H21 H 1.0172 1.3283 0.7168 0.046 Uiso 1 1 calc R . . C22 C 0.9125(7) 1.2564(5) 0.6050(4) 0.0533(18) Uani 1 1 d . . . H22A H 0.9519 1.2113 0.5952 0.080 Uiso 1 1 calc R . . H22B H 0.9503 1.3016 0.5808 0.080 Uiso 1 1 calc R . . H22C H 0.8253 1.2287 0.5816 0.080 Uiso 1 1 calc R . . C23 C 0.8673(7) 1.3716(5) 0.7110(5) 0.0559(19) Uani 1 1 d . . . H23A H 0.7801 1.3448 0.6876 0.084 Uiso 1 1 calc R . . H23B H 0.9062 1.4172 0.6875 0.084 Uiso 1 1 calc R . . H23C H 0.8774 1.3984 0.7686 0.084 Uiso 1 1 calc R . . C24 C 1.0414(5) 1.1799(4) 0.7756(3) 0.0275(12) Uani 1 1 d . . . H24A H 1.0985 1.2373 0.7757 0.033 Uiso 1 1 calc R . . H24B H 1.0754 1.1334 0.7513 0.033 Uiso 1 1 calc R . . C25 C 1.0335(5) 1.1825(4) 0.8614(3) 0.0337(13) Uani 1 1 d . . . H25 H 0.9988 1.2295 0.8852 0.040 Uiso 1 1 calc R . . C26 C 1.1623(6) 1.2086(5) 0.9082(3) 0.0489(18) Uani 1 1 d . . . H26A H 1.1582 1.2101 0.9634 0.073 Uiso 1 1 calc R . . H26B H 1.2114 1.2672 0.9073 0.073 Uiso 1 1 calc R . . H26C H 1.1999 1.1652 0.8840 0.073 Uiso 1 1 calc R . . C27 C 0.9513(7) 1.0963(5) 0.8661(4) 0.0556(19) Uani 1 1 d . . . H27A H 0.8702 1.0812 0.8345 0.083 Uiso 1 1 calc R . . H27B H 0.9446 1.1017 0.9216 0.083 Uiso 1 1 calc R . . H27C H 0.9854 1.0497 0.8450 0.083 Uiso 1 1 calc R . . C28 C 0.7002(5) 0.7892(4) 0.6404(3) 0.0297(12) Uani 1 1 d . . . C29 C 0.6219(6) 0.7473(4) 0.7511(4) 0.0413(15) Uani 1 1 d . . . H29A H 0.5712 0.6876 0.7503 0.050 Uiso 1 1 calc R . . H29B H 0.5659 0.7795 0.7423 0.050 Uiso 1 1 calc R . . C30 C 0.7003(8) 0.7946(10) 0.8316(5) 0.111(5) Uani 1 1 d . . . H30 H 0.7328 0.7485 0.8411 0.133 Uiso 1 1 calc R . . C31 C 0.8061(10) 0.8640(8) 0.8423(5) 0.120(5) Uani 1 1 d . . . H31A H 0.7861 0.9136 0.8321 0.180 Uiso 1 1 calc R . . H31B H 0.8573 0.8454 0.8054 0.180 Uiso 1 1 calc R . . H31C H 0.8502 0.8827 0.8972 0.180 Uiso 1 1 calc R . . C32 C 0.6242(8) 0.8045(8) 0.8942(5) 0.086(3) Uani 1 1 d . . . H32A H 0.6765 0.8262 0.9469 0.129 Uiso 1 1 calc R . . H32B H 0.5627 0.7470 0.8876 0.129 Uiso 1 1 calc R . . H32C H 0.5834 0.8467 0.8893 0.129 Uiso 1 1 calc R . . C33 C 0.7437(7) 0.6670(4) 0.6715(4) 0.0446(16) Uani 1 1 d . . . H33A H 0.7530 0.6515 0.7211 0.054 Uiso 1 1 calc R . . H33B H 0.8261 0.6901 0.6597 0.054 Uiso 1 1 calc R . . C34 C 0.6691(8) 0.5844(5) 0.6043(5) 0.057(2) Uani 1 1 d . . . H34 H 0.6685 0.6002 0.5539 0.069 Uiso 1 1 calc R . . C35 C 0.7325(10) 0.5175(6) 0.5973(6) 0.088(3) Uani 1 1 d . . . H35A H 0.8123 0.5402 0.5830 0.131 Uiso 1 1 calc R . . H35B H 0.6828 0.4622 0.5560 0.131 Uiso 1 1 calc R . . H35C H 0.7439 0.5063 0.6483 0.131 Uiso 1 1 calc R . . C36 C 0.5321(9) 0.5446(7) 0.6127(7) 0.098(3) Uani 1 1 d . . . H36A H 0.5297 0.5266 0.6608 0.147 Uiso 1 1 calc R . . H36B H 0.4888 0.4931 0.5660 0.147 Uiso 1 1 calc R . . H36C H 0.4928 0.5895 0.6166 0.147 Uiso 1 1 calc R . . C37 C 0.1944(10) 0.5281(8) 0.7393(7) 0.102(4) Uani 1 1 d . . . H37A H 0.1895 0.4928 0.7763 0.122 Uiso 1 1 calc R . . H37B H 0.1182 0.5423 0.7344 0.122 Uiso 1 1 calc R . . B2 B 1.0442(11) 1.3564(8) 0.1385(7) 0.039(4) Uani 0.40 1 d PDU . . F6A F 1.1788(9) 1.3747(8) 0.1647(7) 0.017(3) Uani 0.20 1 d PDU . . F7A F 1.0210(12) 1.2744(7) 0.0725(7) 0.021(3) Uani 0.20 1 d PDU . . F8A F 0.9846(13) 1.3568(10) 0.1924(8) 0.028(3) Uani 0.20 1 d PDU . . F6B F 1.075(2) 1.4061(10) 0.2228(7) 0.088(10) Uani 0.20 1 d PD . . F7B F 0.9068(12) 1.3115(10) 0.1527(10) 0.041(4) Uani 0.20 1 d PDU . . F8B F 1.0680(16) 1.2851(10) 0.1112(12) 0.049(5) Uani 0.20 1 d PDU . . F1 F 0.1751(6) 0.4017(4) 0.8623(3) 0.0457(16) Uani 0.60 1 d P . . F2 F 0.0034(6) 0.4087(4) 0.9114(4) 0.0542(17) Uani 0.60 1 d P . . F3 F 0.1494(6) 0.5338(4) 0.9198(4) 0.0553(17) Uani 0.60 1 d P . . F4 F 0.1820(8) 0.4513(5) 0.9953(3) 0.074(3) Uani 0.60 1 d P . . B1 B 0.1275(13) 0.4463(7) 0.9215(5) 0.039(3) Uani 0.60 1 d P . . C51 C 0.4506(15) 0.5382(9) 0.2292(7) 0.047(4) Uani 0.50 1 d P . . H51A H 0.4309 0.5891 0.2599 0.071 Uiso 0.50 1 calc PR . . H51B H 0.5351 0.5451 0.2492 0.071 Uiso 0.50 1 calc PR . . H51C H 0.3953 0.4838 0.2348 0.071 Uiso 0.50 1 calc PR . . C52 C 0.3352(18) 0.5073(13) 0.1774(15) 0.093(7) Uani 0.50 1 d PD . . H52A H 0.3266 0.4508 0.1869 0.140 Uiso 0.50 1 calc PR . . H52B H 0.2646 0.5000 0.1387 0.140 Uiso 0.50 1 calc PR . . H52C H 0.3393 0.5519 0.2275 0.140 Uiso 0.50 1 calc PR . . 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 V2 0.0170(4) 0.0303(5) 0.0188(4) 0.0033(4) 0.0017(3) 0.0110(4) V1 0.0159(4) 0.0301(5) 0.0176(4) 0.0017(4) 0.0020(3) 0.0106(4) Cl1 0.101(2) 0.132(3) 0.161(3) 0.097(3) -0.012(2) -0.011(2) Cl2 0.149(3) 0.140(4) 0.170(4) 0.049(3) 0.067(3) -0.022(3) S1 0.0164(6) 0.0356(8) 0.0207(6) 0.0040(5) 0.0021(5) 0.0087(6) S2 0.0182(6) 0.0399(8) 0.0233(6) 0.0035(6) 0.0027(5) 0.0152(6) S3 0.0217(7) 0.0313(8) 0.0251(6) 0.0046(6) 0.0028(5) 0.0101(6) S4 0.0162(6) 0.0320(7) 0.0200(6) 0.0037(5) 0.0032(5) 0.0102(5) S5 0.0216(6) 0.0338(8) 0.0238(6) 0.0014(6) 0.0023(5) 0.0140(6) S6 0.0175(6) 0.0360(8) 0.0218(6) -0.0016(6) -0.0002(5) 0.0126(6) S7 0.0217(6) 0.0365(8) 0.0214(6) 0.0068(6) 0.0075(5) 0.0161(6) S8 0.0211(6) 0.0327(7) 0.0245(6) 0.0059(6) 0.0083(5) 0.0137(6) S9 0.0156(6) 0.0320(7) 0.0240(6) 0.0014(5) -0.0010(5) 0.0115(5) S10 0.0176(6) 0.0353(8) 0.0220(6) 0.0020(5) 0.0008(5) 0.0137(6) S11 0.0254(7) 0.0364(8) 0.0261(7) 0.0102(6) 0.0058(5) 0.0149(6) S12 0.0343(8) 0.0398(9) 0.0298(7) 0.0058(6) 0.0035(6) 0.0234(7) F5 0.067(5) 0.050(5) 0.040(4) 0.023(4) -0.003(4) 0.042(4) N1 0.030(2) 0.031(3) 0.017(2) 0.0022(19) 0.0044(18) 0.010(2) N2 0.025(2) 0.030(3) 0.025(2) 0.006(2) 0.0056(18) 0.011(2) N3 0.015(2) 0.030(2) 0.021(2) 0.0014(18) -0.0002(16) 0.0094(18) N4 0.050(3) 0.034(3) 0.031(3) 0.007(2) 0.005(2) 0.020(3) C1 0.020(3) 0.031(3) 0.023(2) 0.005(2) 0.005(2) 0.011(2) C2 0.036(3) 0.031(3) 0.024(3) 0.004(2) 0.010(2) 0.014(3) C3 0.156(10) 0.028(4) 0.099(7) 0.013(4) 0.087(7) 0.032(5) C4 0.227(14) 0.041(5) 0.118(9) 0.027(6) 0.114(10) 0.060(7) C6 0.027(3) 0.035(3) 0.026(3) 0.005(2) 0.000(2) 0.009(2) C7 0.046(5) 0.106(8) 0.093(6) 0.070(6) 0.020(4) 0.032(5) C8 0.044(5) 0.139(10) 0.149(10) 0.103(9) 0.003(6) 0.031(6) C9 0.064(7) 0.253(18) 0.167(12) 0.176(13) 0.038(7) 0.046(9) C10 0.019(3) 0.033(3) 0.018(2) 0.003(2) 0.0009(19) 0.012(2) C11 0.033(3) 0.037(3) 0.033(3) 0.014(3) 0.010(2) 0.012(3) C12 0.054(5) 0.073(5) 0.027(3) 0.017(3) 0.008(3) 0.007(4) C13 0.068(5) 0.077(6) 0.031(3) 0.015(4) 0.021(3) 0.007(4) C14 0.090(7) 0.127(9) 0.043(5) 0.017(5) 0.005(5) 0.046(7) C15 0.031(3) 0.036(3) 0.035(3) 0.011(3) 0.006(2) 0.017(3) C16 0.041(4) 0.039(4) 0.044(4) 0.006(3) 0.009(3) 0.016(3) C17 0.053(5) 0.046(4) 0.054(4) -0.003(4) 0.008(4) 0.002(4) C18 0.079(6) 0.049(5) 0.060(5) -0.002(4) 0.017(4) 0.032(4) C19 0.017(2) 0.037(3) 0.021(2) 0.007(2) 0.005(2) 0.013(2) C20 0.022(3) 0.037(3) 0.026(3) -0.002(2) -0.003(2) 0.012(2) C21 0.029(3) 0.037(4) 0.043(3) 0.008(3) -0.005(3) 0.010(3) C22 0.066(5) 0.050(4) 0.045(4) 0.021(3) 0.013(4) 0.016(4) C23 0.061(5) 0.040(4) 0.067(5) 0.014(4) -0.002(4) 0.025(4) C24 0.018(3) 0.034(3) 0.024(3) 0.000(2) 0.001(2) 0.008(2) C25 0.032(3) 0.046(4) 0.025(3) 0.007(3) 0.004(2) 0.019(3) C26 0.046(4) 0.073(5) 0.025(3) 0.003(3) -0.007(3) 0.032(4) C27 0.066(5) 0.070(5) 0.037(4) 0.026(4) 0.009(3) 0.023(4) C28 0.030(3) 0.028(3) 0.026(3) 0.004(2) -0.006(2) 0.010(2) C29 0.049(4) 0.037(4) 0.041(3) 0.017(3) 0.005(3) 0.016(3) C30 0.052(5) 0.199(13) 0.041(4) -0.023(6) 0.007(4) 0.041(7) C31 0.097(8) 0.127(10) 0.047(5) -0.012(6) 0.015(5) -0.052(7) C32 0.065(6) 0.131(9) 0.053(5) 0.009(5) 0.017(4) 0.037(6) C33 0.063(4) 0.035(4) 0.042(3) 0.008(3) 0.008(3) 0.030(3) C34 0.081(6) 0.034(4) 0.053(4) 0.009(3) 0.025(4) 0.016(4) C35 0.116(8) 0.056(6) 0.102(7) 0.018(5) 0.043(7) 0.045(6) C36 0.092(8) 0.079(7) 0.113(8) 0.016(6) 0.033(7) 0.023(6) C37 0.086(7) 0.095(8) 0.110(9) 0.040(7) 0.031(7) -0.001(6) B2 0.042(6) 0.031(6) 0.042(6) 0.015(4) -0.008(4) 0.013(4) F6A 0.017(3) 0.018(3) 0.018(3) 0.011(2) -0.002(2) 0.004(2) F7A 0.019(6) 0.015(6) 0.021(6) -0.005(5) -0.008(5) 0.008(5) F8A 0.035(5) 0.028(5) 0.035(5) 0.026(4) 0.003(4) 0.016(4) F6B 0.19(3) 0.016(10) 0.030(10) 0.004(8) -0.050(13) 0.014(13) F7B 0.052(6) 0.039(6) 0.042(6) 0.021(4) 0.010(4) 0.021(4) F8B 0.044(8) 0.040(8) 0.076(10) 0.019(7) 0.023(7) 0.031(7) F1 0.082(5) 0.018(3) 0.027(3) 0.004(2) -0.007(3) 0.010(3) F2 0.063(4) 0.036(4) 0.038(3) 0.001(3) -0.014(3) -0.004(3) F3 0.066(4) 0.020(3) 0.076(5) 0.016(3) 0.003(4) 0.013(3) F4 0.109(6) 0.087(6) 0.026(3) 0.000(3) -0.031(4) 0.059(5) B1 0.075(9) 0.023(6) 0.007(4) 0.000(4) -0.019(5) 0.013(6) C51 0.081(11) 0.036(8) 0.029(6) 0.020(6) 0.030(7) 0.011(7) C52 0.100(16) 0.056(12) 0.138(19) 0.057(13) 0.024(15) 0.023(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V2 S1 2.3837(17) . ? V2 S4 2.4033(14) . ? V2 S3 2.4217(16) . ? V2 S11 2.4363(16) . ? V2 S10 2.4430(15) . ? V2 S2 2.4486(15) . ? V2 S12 2.4672(17) . ? V2 S9 2.4731(15) . ? V1 S1 2.3727(15) . ? V1 S4 2.4012(14) . ? V1 S6 2.4134(14) . ? V1 S3 2.4241(17) . ? V1 S7 2.4348(16) . ? V1 S2 2.4467(15) . ? V1 S5 2.4787(15) . ? V1 S8 2.5050(16) . ? Cl1 C37 1.739(11) . ? Cl2 C37 1.723(12) . ? S1 S2 2.007(2) . ? S3 S4 2.0033(19) . ? S5 C1 1.715(5) . ? S6 C1 1.718(5) . ? S7 C10 1.714(5) . ? S8 C10 1.724(5) . ? S9 C19 1.718(5) . ? S10 C19 1.712(5) . ? S11 C28 1.725(6) . ? S12 C28 1.717(6) . ? F5 B2 1.390(13) . ? N1 C1 1.321(6) . ? N1 C6 1.457(7) . ? N1 C2 1.480(7) . ? N2 C10 1.309(7) . ? N2 C15 1.471(7) . ? N2 C11 1.485(7) . ? N3 C19 1.338(7) . ? N3 C20 1.454(7) . ? N3 C24 1.473(6) . ? N4 C28 1.303(8) . ? N4 C29 1.471(8) . ? N4 C33 1.481(7) . ? C2 C3 1.460(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C52 1.334(15) . ? C3 C51 1.395(15) . ? C3 C4 1.548(10) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.532(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C9 1.391(14) . ? C7 C8 1.520(10) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 C12 1.503(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C14 1.452(12) . ? C12 C13 1.536(9) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.523(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.514(9) . ? C16 C17 1.524(9) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C20 C21 1.516(9) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.523(9) . ? C21 C23 1.549(9) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.525(7) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C27 1.500(10) . ? C25 C26 1.526(8) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 C30 1.493(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.372(14) . ? C30 C32 1.492(11) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.512(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.500(11) . ? C34 C36 1.576(12) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? B2 F8A 1.235(13) . ? B2 F8B 1.280(14) . ? B2 F6B 1.453(14) . ? B2 F7A 1.473(13) . ? B2 F6A 1.511(13) . ? B2 F7B 1.631(14) . ? F1 B1 1.378(13) . ? F2 B1 1.369(15) . ? F3 B1 1.414(12) . ? F4 B1 1.375(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? 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 S1 V2 S4 87.71(5) . . ? S1 V2 S3 104.28(5) . . ? S4 V2 S3 49.06(5) . . ? S1 V2 S11 160.33(6) . . ? S4 V2 S11 89.21(5) . . ? S3 V2 S11 88.15(6) . . ? S1 V2 S10 85.85(5) . . ? S4 V2 S10 147.53(6) . . ? S3 V2 S10 162.26(6) . . ? S11 V2 S10 86.37(5) . . ? S1 V2 S2 49.05(5) . . ? S4 V2 S2 105.23(5) . . ? S3 V2 S2 82.11(5) . . ? S11 V2 S2 149.79(6) . . ? S10 V2 S2 94.29(5) . . ? S1 V2 S12 125.28(6) . . ? S4 V2 S12 128.82(6) . . ? S3 V2 S12 82.72(6) . . ? S11 V2 S12 70.72(5) . . ? S10 V2 S12 79.55(5) . . ? S2 V2 S12 79.68(5) . . ? S1 V2 S9 79.99(5) . . ? S4 V2 S9 77.30(5) . . ? S3 V2 S9 125.33(5) . . ? S11 V2 S9 80.38(5) . . ? S10 V2 S9 70.24(5) . . ? S2 V2 S9 128.21(6) . . ? S12 V2 S9 139.18(6) . . ? S1 V1 S4 88.01(5) . . ? S1 V1 S6 157.93(6) . . ? S4 V1 S6 87.91(5) . . ? S1 V1 S3 104.55(5) . . ? S4 V1 S3 49.06(5) . . ? S6 V1 S3 88.94(6) . . ? S1 V1 S7 85.92(5) . . ? S4 V1 S7 149.21(6) . . ? S6 V1 S7 86.54(5) . . ? S3 V1 S7 160.71(6) . . ? S1 V1 S2 49.18(5) . . ? S4 V1 S2 105.35(5) . . ? S6 V1 S2 152.14(6) . . ? S3 V1 S2 82.10(5) . . ? S7 V1 S2 93.26(5) . . ? S1 V1 S5 127.50(5) . . ? S4 V1 S5 127.05(6) . . ? S6 V1 S5 71.04(5) . . ? S3 V1 S5 81.61(5) . . ? S7 V1 S5 79.19(5) . . ? S2 V1 S5 81.55(5) . . ? S1 V1 S8 78.22(5) . . ? S4 V1 S8 79.21(5) . . ? S6 V1 S8 79.71(5) . . ? S3 V1 S8 127.50(5) . . ? S7 V1 S8 70.00(5) . . ? S2 V1 S8 126.30(6) . . ? S5 V1 S8 138.43(6) . . ? S2 S1 V1 67.33(6) . . ? S2 S1 V2 67.16(6) . . ? V1 S1 V2 76.20(5) . . ? S1 S2 V1 63.49(5) . . ? S1 S2 V2 63.79(5) . . ? V1 S2 V2 73.67(4) . . ? S4 S3 V2 64.99(6) . . ? S4 S3 V1 64.88(6) . . ? V2 S3 V1 74.55(5) . . ? S3 S4 V1 66.07(6) . . ? S3 S4 V2 65.95(5) . . ? V1 S4 V2 75.30(4) . . ? C1 S5 V1 87.50(18) . . ? C1 S6 V1 89.57(18) . . ? C10 S7 V1 90.53(19) . . ? C10 S8 V1 87.98(19) . . ? C19 S9 V2 88.57(18) . . ? C19 S10 V2 89.70(18) . . ? C28 S11 V2 89.5(2) . . ? C28 S12 V2 88.69(19) . . ? C1 N1 C6 121.3(4) . . ? C1 N1 C2 121.3(4) . . ? C6 N1 C2 117.4(4) . . ? C10 N2 C15 120.4(4) . . ? C10 N2 C11 120.5(4) . . ? C15 N2 C11 119.1(5) . . ? C19 N3 C20 121.5(4) . . ? C19 N3 C24 121.2(4) . . ? C20 N3 C24 117.3(4) . . ? C28 N4 C29 122.0(5) . . ? C28 N4 C33 121.5(5) . . ? C29 N4 C33 116.5(5) . . ? N1 C1 S5 125.1(4) . . ? N1 C1 S6 123.0(4) . . ? S5 C1 S6 111.8(3) . . ? C3 C2 N1 113.4(5) . . ? C3 C2 H2A 108.9 . . ? N1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? N1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C52 C3 C51 62.9(12) . . ? C52 C3 C2 132.5(11) . . ? C51 C3 C2 120.3(9) . . ? C52 C3 C4 111.4(12) . . ? C51 C3 C4 113.7(10) . . ? C2 C3 C4 108.9(7) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C6 C7 114.1(5) . . ? N1 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? N1 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C9 C7 C8 114.4(9) . . ? C9 C7 C6 119.9(8) . . ? C8 C7 C6 108.0(6) . . ? C9 C7 H7 104.3 . . ? C8 C7 H7 104.2 . . ? C6 C7 H7 104.3 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 S7 125.3(4) . . ? N2 C10 S8 123.6(4) . . ? S7 C10 S8 111.1(3) . . ? N2 C11 C12 113.1(5) . . ? N2 C11 H11A 109.0 . . ? C12 C11 H11A 109.0 . . ? N2 C11 H11B 109.0 . . ? C12 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C14 C12 C11 115.8(7) . . ? C14 C12 C13 112.1(7) . . ? C11 C12 C13 109.1(6) . . ? C14 C12 H12 106.4 . . ? C11 C12 H12 106.4 . . ? C13 C12 H12 106.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C16 113.1(5) . . ? N2 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N2 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C18 C16 C15 110.0(5) . . ? C18 C16 C17 111.3(6) . . ? C15 C16 C17 112.3(5) . . ? C18 C16 H16 107.7 . . ? C15 C16 H16 107.7 . . ? C17 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C19 S10 125.9(4) . . ? N3 C19 S9 123.0(4) . . ? S10 C19 S9 111.1(3) . . ? N3 C20 C21 114.1(4) . . ? N3 C20 H20A 108.7 . . ? C21 C20 H20A 108.7 . . ? N3 C20 H20B 108.7 . . ? C21 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? C20 C21 C22 113.8(5) . . ? C20 C21 C23 108.3(5) . . ? C22 C21 C23 110.2(6) . . ? C20 C21 H21 108.2 . . ? C22 C21 H21 108.2 . . ? C23 C21 H21 108.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C24 C25 113.2(4) . . ? N3 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N3 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C27 C25 C24 111.9(5) . . ? C27 C25 C26 111.8(6) . . ? C24 C25 C26 108.8(5) . . ? C27 C25 H25 108.1 . . ? C24 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 S12 124.6(4) . . ? N4 C28 S11 124.3(5) . . ? S12 C28 S11 111.0(3) . . ? N4 C29 C30 115.3(6) . . ? N4 C29 H29A 108.4 . . ? C30 C29 H29A 108.4 . . ? N4 C29 H29B 108.4 . . ? C30 C29 H29B 108.4 . . ? H29A C29 H29B 107.5 . . ? C31 C30 C32 116.6(9) . . ? C31 C30 C29 120.6(10) . . ? C32 C30 C29 110.9(7) . . ? C31 C30 H30 101.6 . . ? C32 C30 H30 101.6 . . ? C29 C30 H30 101.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 C34 113.1(6) . . ? N4 C33 H33A 109.0 . . ? C34 C33 H33A 109.0 . . ? N4 C33 H33B 109.0 . . ? C34 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C35 C34 C33 108.5(7) . . ? C35 C34 C36 111.3(8) . . ? C33 C34 C36 114.1(7) . . ? C35 C34 H34 107.6 . . ? C33 C34 H34 107.6 . . ? C36 C34 H34 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Cl2 C37 Cl1 112.0(6) . . ? Cl2 C37 H37A 109.2 . . ? Cl1 C37 H37A 109.2 . . ? Cl2 C37 H37B 109.2 . . ? Cl1 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? F8A B2 F8B 114.7(14) . . ? F8A B2 F5 114.6(11) . . ? F8B B2 F5 126.2(12) . . ? F8A B2 F6B 47.7(11) . . ? F8B B2 F6B 122.0(13) . . ? F5 B2 F6B 106.6(10) . . ? F8A B2 F7A 120.5(12) . . ? F8B B2 F7A 32.1(9) . . ? F5 B2 F7A 101.9(9) . . ? F6B B2 F7A 151.4(12) . . ? F8A B2 F6A 114.6(11) . . ? F8B B2 F6A 71.0(11) . . ? F5 B2 F6A 105.9(10) . . ? F6B B2 F6A 73.2(12) . . ? F7A B2 F6A 97.0(9) . . ? F8A B2 F7B 39.5(9) . . ? F8B B2 F7B 97.8(11) . . ? F5 B2 F7B 106.8(9) . . ? F6B B2 F7B 87.2(11) . . ? F7A B2 F7B 86.8(10) . . ? F6A B2 F7B 145.6(11) . . ? F2 B1 F4 110.0(10) . . ? F2 B1 F1 112.3(8) . . ? F4 B1 F1 111.0(9) . . ? F2 B1 F3 106.0(9) . . ? F4 B1 F3 107.6(8) . . ? F1 B1 F3 109.9(9) . . ? C3 C51 H51A 109.5 . . ? C3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C3 C52 H52A 109.5 . . ? C3 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C3 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.255 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.123 #===END data_c:complex_1b _database_code_depnum_ccdc_archive 'CCDC 614333' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H148 B2 Cl4 F8 N8 S24 V4' _chemical_formula_weight 2438.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7389(13) _cell_length_b 20.7238(18) _cell_length_c 21.4366(18) _cell_angle_alpha 79.133(2) _cell_angle_beta 76.828(2) _cell_angle_gamma 73.115(2) _cell_volume 6047.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4287 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.52 _exptl_crystal_description Block _exptl_crystal_colour green _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_max 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2548 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.879984 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; 'SQUEEZE was used to remove unresolvable electron density..' ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35554 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.1145 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 26.50 _reflns_number_total 24378 _reflns_number_gt 13383 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1140P)^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 24378 _refine_ls_number_parameters 1158 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1386 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.1991 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.021 _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 V1 V 0.41435(8) 1.28128(6) 0.29401(5) 0.0335(3) Uani 1 1 d . . . Cl1 Cl 0.8354(3) 1.17512(17) 0.31745(15) 0.1168(12) Uani 1 1 d . . . S1 S 0.42207(13) 1.29254(9) 0.17852(7) 0.0401(5) Uani 1 1 d . . . F1 F 0.9562(3) 0.7961(2) 0.1253(2) 0.0555(12) Uani 1 1 d . . . N1 N 0.4166(4) 1.4609(3) 0.3655(2) 0.0293(12) Uani 1 1 d . . . C1 C 0.4189(5) 1.4051(4) 0.3430(3) 0.0360(17) Uani 1 1 d . . . B1 B 0.8751(6) 0.7904(4) 0.1056(4) 0.0365(19) Uani 1 1 d . . . V2 V 0.55647(8) 1.19728(6) 0.20145(5) 0.0339(3) Uani 1 1 d . . . Cl2 Cl 0.8928(4) 1.03551(19) 0.3706(3) 0.236(3) Uani 1 1 d . . . S2 S 0.38552(13) 1.20918(9) 0.22942(7) 0.0379(4) Uani 1 1 d . . . F2 F 0.8213(3) 0.8541(2) 0.0897(3) 0.0729(15) Uani 1 1 d . . . N2 N 0.1355(4) 1.2763(3) 0.4083(2) 0.0298(12) Uani 1 1 d . . . C2 C 0.4166(4) 1.4589(3) 0.4350(3) 0.0316(15) Uani 1 1 d . . . H2A H 0.4658 1.4798 0.4387 0.038 Uiso 1 1 calc R . . H2B H 0.4341 1.4118 0.4541 0.038 Uiso 1 1 calc R . . B2 B 0.1367(6) 0.7018(4) 0.3914(4) 0.0313(17) Uani 1 1 d . . . V3 V 0.48544(7) 1.55801(5) 0.03515(4) 0.0160(2) Uani 1 1 d . . . Cl3 Cl 0.8531(3) 1.5268(2) -0.09358(19) 0.1375(14) Uani 1 1 d . B . S3 S 0.58481(13) 1.26786(9) 0.26680(7) 0.0365(4) Uani 1 1 d . . . F3 F 0.8220(4) 0.7577(3) 0.1560(2) 0.0691(15) Uani 1 1 d . . . N3 N 0.8368(4) 1.2164(3) 0.0984(3) 0.0365(14) Uani 1 1 d . . . C3 C 0.3218(4) 1.4942(3) 0.4732(3) 0.0269(14) Uani 1 1 d . . . H3 H 0.3085 1.5429 0.4572 0.032 Uiso 1 1 calc R . . V4 V 0.51799(7) 0.94044(4) 0.46598(4) 0.0152(2) Uani 1 1 d . . . S4 S 0.54766(12) 1.18480(8) 0.31731(7) 0.0335(4) Uani 1 1 d . . . F4 F 0.9040(4) 0.7549(3) 0.0542(2) 0.0732(15) Uani 1 1 d . . . N4 N 0.5772(4) 1.0158(3) 0.1263(2) 0.0299(12) Uani 1 1 d . . . C4 C 0.2390(5) 1.4684(4) 0.4654(3) 0.0389(17) Uani 1 1 d . . . H4B H 0.2512 1.4205 0.4802 0.058 Uiso 1 1 calc R . . H4A H 0.2335 1.4764 0.4207 0.058 Uiso 1 1 calc R . . H4C H 0.1800 1.4921 0.4904 0.058 Uiso 1 1 calc R . . S5 S 0.41556(13) 1.40293(9) 0.26349(7) 0.0373(4) Uani 1 1 d . . . F5 F 0.1152(4) 0.7322(3) 0.4460(2) 0.0743(16) Uani 1 1 d . . . N5 N 0.2412(3) 1.6721(2) 0.1564(2) 0.0197(10) Uani 1 1 d . . . C5 C 0.3317(5) 1.4851(4) 0.5440(3) 0.0343(16) Uani 1 1 d . . . H5C H 0.3404 1.4380 0.5615 0.051 Uiso 1 1 calc R . . H5B H 0.2744 1.5117 0.5680 0.051 Uiso 1 1 calc R . . H5A H 0.3864 1.4998 0.5469 0.051 Uiso 1 1 calc R . . S6 S 0.42008(13) 1.32764(8) 0.38834(7) 0.0369(4) Uani 1 1 d . . . F6 F 0.1921(4) 0.7348(2) 0.3430(2) 0.0634(14) Uani 1 1 d . . . N6 N 0.6882(3) 1.6611(2) 0.0554(2) 0.0234(11) Uani 1 1 d . . . C6 C 0.4031(5) 1.5281(3) 0.3269(3) 0.0339(16) Uani 1 1 d . . . H6B H 0.3409 1.5567 0.3439 0.041 Uiso 1 1 calc R . . H6A H 0.4024 1.5233 0.2828 0.041 Uiso 1 1 calc R . . S7 S 0.24224(13) 1.33647(9) 0.30828(8) 0.0395(5) Uani 1 1 d . . . F7 F 0.1875(3) 0.6349(2) 0.4024(2) 0.0665(13) Uani 1 1 d . . . N7 N 0.3221(4) 0.8311(2) 0.4461(2) 0.0255(11) Uani 1 1 d . . . C7 C 0.4805(5) 1.5631(4) 0.3259(3) 0.0428(18) Uani 1 1 d . . . H7 H 0.4786 1.5698 0.3702 0.051 Uiso 1 1 calc R . . S8 S 0.32499(12) 1.21344(8) 0.38176(7) 0.0341(4) Uani 1 1 d . . . F8 F 0.0536(3) 0.7025(2) 0.3731(2) 0.0547(12) Uani 1 1 d . . . N8 N 0.7596(3) 0.8262(2) 0.3435(2) 0.0172(10) Uani 1 1 d . . . C8 C 0.5800(6) 1.5225(5) 0.3000(4) 0.066(3) Uani 1 1 d . . . H8C H 0.5932 1.4786 0.3255 0.099 Uiso 1 1 calc R . . H8B H 0.6264 1.5459 0.3022 0.099 Uiso 1 1 calc R . . H8A H 0.5840 1.5170 0.2559 0.099 Uiso 1 1 calc R . . S9 S 0.64338(13) 1.26846(8) 0.11580(7) 0.0385(4) Uani 1 1 d . . . C9 C 0.4557(6) 1.6338(4) 0.2852(3) 0.054(2) Uani 1 1 d . . . H9B H 0.5031 1.6574 0.2848 0.080 Uiso 1 1 calc R . . H9C H 0.3932 1.6596 0.3039 0.080 Uiso 1 1 calc R . . H9A H 0.4554 1.6283 0.2418 0.080 Uiso 1 1 calc R . . S10 S 0.72828(12) 1.14393(8) 0.18559(7) 0.0356(4) Uani 1 1 d . . . C10 C 0.2202(5) 1.2751(3) 0.3714(3) 0.0288(14) Uani 1 1 d . . . S11 S 0.55209(13) 1.15099(9) 0.10631(7) 0.0395(5) Uani 1 1 d . . . C11 C 0.0513(5) 1.3302(3) 0.3948(3) 0.0332(15) Uani 1 1 d . . . H11B H -0.0059 1.3150 0.4159 0.040 Uiso 1 1 calc R . . H11A H 0.0524 1.3372 0.3486 0.040 Uiso 1 1 calc R . . S12 S 0.55956(13) 1.07531(9) 0.23081(7) 0.0344(4) Uani 1 1 d . . . C12 C 0.0421(5) 1.3981(3) 0.4159(3) 0.0377(17) Uani 1 1 d . . . H12 H 0.0989 1.4140 0.3931 0.045 Uiso 1 1 calc R . . S13 S 0.63216(10) 1.47296(7) 0.00553(7) 0.0202(3) Uani 1 1 d . . . C13 C -0.0460(5) 1.4489(4) 0.3953(4) 0.053(2) Uani 1 1 d . . . H13A H -0.0423 1.4502 0.3498 0.080 Uiso 1 1 calc R . . H13B H -0.0487 1.4932 0.4042 0.080 Uiso 1 1 calc R . . H13C H -0.1029 1.4356 0.4187 0.080 Uiso 1 1 calc R . . S14 S 0.53495(10) 1.43803(7) 0.07493(6) 0.0198(3) Uani 1 1 d . . . C14 C 0.0394(6) 1.3921(4) 0.4880(3) 0.0461(19) Uani 1 1 d . . . H14C H -0.0186 1.3805 0.5114 0.069 Uiso 1 1 calc R . . H14A H 0.0408 1.4348 0.4985 0.069 Uiso 1 1 calc R . . H14B H 0.0944 1.3574 0.4995 0.069 Uiso 1 1 calc R . . S15 S 0.37022(11) 1.66835(7) 0.04470(6) 0.0211(3) Uani 1 1 d . . . C15 C 0.1254(5) 1.2258(3) 0.4673(3) 0.0366(16) Uani 1 1 d . . . H15B H 0.0718 1.2467 0.4990 0.044 Uiso 1 1 calc R . . H15A H 0.1834 1.2145 0.4856 0.044 Uiso 1 1 calc R . . S16 S 0.36768(10) 1.55166(7) 0.13772(6) 0.0190(3) Uani 1 1 d . . . C16 C 0.1088(6) 1.1601(4) 0.4551(4) 0.050(2) Uani 1 1 d . . . H16 H 0.1654 1.1373 0.4257 0.060 Uiso 1 1 calc R . . S17 S 0.58993(11) 1.63342(7) -0.02331(6) 0.0212(3) Uani 1 1 d . . . C17 C 0.1004(6) 1.1140(4) 0.5205(4) 0.064(2) Uani 1 1 d . . . H17C H 0.0452 1.1357 0.5499 0.096 Uiso 1 1 calc R . . H17A H 0.1576 1.1066 0.5380 0.096 Uiso 1 1 calc R . . H17B H 0.0933 1.0712 0.5143 0.096 Uiso 1 1 calc R . . S18 S 0.56612(11) 1.58361(8) 0.11030(6) 0.0217(3) Uani 1 1 d . . . C18 C 0.0240(7) 1.1701(5) 0.4273(4) 0.074(3) Uani 1 1 d . . . H18A H 0.0171 1.1268 0.4224 0.110 Uiso 1 1 calc R . . H18B H 0.0308 1.1973 0.3858 0.110 Uiso 1 1 calc R . . H18C H -0.0321 1.1929 0.4554 0.110 Uiso 1 1 calc R . . S19 S 0.46343(10) 1.05945(7) 0.42441(6) 0.0188(3) Uani 1 1 d . . . C19 C 0.7492(5) 1.2111(3) 0.1298(3) 0.0338(16) Uani 1 1 d . . . S20 S 0.36777(10) 1.02348(7) 0.49430(7) 0.0194(3) Uani 1 1 d . . . C20 C 0.9239(5) 1.1639(3) 0.1143(4) 0.0432(18) Uani 1 1 d . . . H20B H 0.9159 1.1527 0.1609 0.052 Uiso 1 1 calc R . . H20A H 0.9789 1.1832 0.0999 0.052 Uiso 1 1 calc R . . S21 S 0.41797(11) 0.86138(7) 0.52460(6) 0.0207(3) Uani 1 1 d . . . C21 C 0.9467(6) 1.0985(4) 0.0849(4) 0.052(2) Uani 1 1 d . . . H21 H 0.8945 1.0764 0.1041 0.062 Uiso 1 1 calc R . . S22 S 0.44039(11) 0.91172(8) 0.39114(6) 0.0221(3) Uani 1 1 d . . . C22 C 0.9522(6) 1.1103(4) 0.0133(4) 0.055(2) Uani 1 1 d . . . H22B H 1.0065 1.1283 -0.0072 0.082 Uiso 1 1 calc R . . H22A H 0.8941 1.1422 0.0030 0.082 Uiso 1 1 calc R . . H22C H 0.9597 1.0681 -0.0020 0.082 Uiso 1 1 calc R . . S23 S 0.63703(11) 0.83146(7) 0.45810(6) 0.0202(3) Uani 1 1 d . . . C23 C 1.0380(6) 1.0528(4) 0.1052(5) 0.071(3) Uani 1 1 d . . . H23A H 1.0532 1.0102 0.0888 0.107 Uiso 1 1 calc R . . H23C H 1.0291 1.0451 0.1515 0.107 Uiso 1 1 calc R . . H23B H 1.0900 1.0741 0.0883 0.107 Uiso 1 1 calc R . . S24 S 0.63569(10) 0.94714(7) 0.36331(6) 0.0195(3) Uani 1 1 d . . . C24 C 0.8518(6) 1.2737(4) 0.0492(4) 0.068(3) Uani 1 1 d . . . H24B H 0.7904 1.2987 0.0370 0.082 Uiso 1 1 calc R . . H24A H 0.8944 1.2560 0.0112 0.082 Uiso 1 1 calc R . . C25 C 0.8984(15) 1.3276(6) 0.0724(8) 0.214(12) Uani 1 1 d D . . H25 H 0.9628 1.3065 0.0828 0.257 Uiso 1 1 calc R . . C26 C 0.8982(10) 1.3814(5) 0.0136(9) 0.223(12) Uani 1 1 d . . . H26A H 0.9580 1.3696 -0.0162 0.335 Uiso 1 1 calc R . . H26B H 0.8907 1.4247 0.0268 0.335 Uiso 1 1 calc R . . H26C H 0.8456 1.3839 -0.0070 0.335 Uiso 1 1 calc R . . C27 C 0.8220(13) 1.3508(8) 0.1309(9) 0.526(16) Uani 1 1 d D . . H27C H 0.8529 1.3569 0.1635 0.789 Uiso 1 1 calc R . . H27B H 0.7869 1.3169 0.1481 0.789 Uiso 1 1 calc R . . H27A H 0.7783 1.3930 0.1180 0.789 Uiso 1 1 calc R . . C28 C 0.5641(4) 1.0708(4) 0.1502(3) 0.0337(16) Uani 1 1 d . . . C29 C 0.5821(4) 1.0167(4) 0.0569(3) 0.0308(15) Uani 1 1 d . . . H29B H 0.5529 1.0626 0.0387 0.037 Uiso 1 1 calc R . . H29A H 0.5442 0.9875 0.0517 0.037 Uiso 1 1 calc R . . C30 C 0.6847(4) 0.9934(3) 0.0185(3) 0.0296(14) Uani 1 1 d . . . H30 H 0.7087 0.9445 0.0315 0.036 Uiso 1 1 calc R . . C31 C 0.7547(5) 1.0291(4) 0.0313(3) 0.0392(17) Uani 1 1 d . . . H31A H 0.8173 1.0128 0.0059 0.059 Uiso 1 1 calc R . . H31C H 0.7587 1.0195 0.0763 0.059 Uiso 1 1 calc R . . H31B H 0.7319 1.0773 0.0197 0.059 Uiso 1 1 calc R . . C32 C 0.6785(5) 1.0041(4) -0.0529(3) 0.0351(16) Uani 1 1 d . . . H32C H 0.6537 1.0516 -0.0666 0.053 Uiso 1 1 calc R . . H32A H 0.6363 0.9792 -0.0593 0.053 Uiso 1 1 calc R . . H32B H 0.7416 0.9881 -0.0779 0.053 Uiso 1 1 calc R . . C33 C 0.5967(5) 0.9478(3) 0.1656(3) 0.0325(15) Uani 1 1 d . . . H33B H 0.6059 0.9528 0.2076 0.039 Uiso 1 1 calc R . . H33A H 0.6561 0.9191 0.1447 0.039 Uiso 1 1 calc R . . C34 C 0.5157(5) 0.9129(4) 0.1749(3) 0.0368(17) Uani 1 1 d . . . H34 H 0.5102 0.9051 0.1324 0.044 Uiso 1 1 calc R . . C35 C 0.4199(5) 0.9560(4) 0.2050(3) 0.0460(19) Uani 1 1 d . . . H35C H 0.4219 0.9606 0.2483 0.069 Uiso 1 1 calc R . . H35B H 0.3698 0.9346 0.2057 0.069 Uiso 1 1 calc R . . H35A H 0.4069 1.0001 0.1800 0.069 Uiso 1 1 calc R . . C36 C 0.5462(6) 0.8436(4) 0.2154(3) 0.049(2) Uani 1 1 d . . . H36A H 0.6078 0.8185 0.1947 0.073 Uiso 1 1 calc R . . H36B H 0.4992 0.8186 0.2192 0.073 Uiso 1 1 calc R . . H36C H 0.5505 0.8502 0.2576 0.073 Uiso 1 1 calc R . . C37 C 0.3141(4) 1.6359(3) 0.1184(2) 0.0184(12) Uani 1 1 d . . . C38 C 0.1962(4) 1.7447(3) 0.1368(3) 0.0232(13) Uani 1 1 d . . . H38B H 0.1268 1.7519 0.1450 0.028 Uiso 1 1 calc R . . H38A H 0.2170 1.7555 0.0906 0.028 Uiso 1 1 calc R . . C39 C 0.2210(5) 1.7939(3) 0.1721(3) 0.0316(15) Uani 1 1 d . . . H39 H 0.1965 1.7848 0.2185 0.038 Uiso 1 1 calc R . . C40 C 0.3281(5) 1.7859(4) 0.1616(4) 0.053(2) Uani 1 1 d . . . H40B H 0.3526 1.7957 0.1164 0.080 Uiso 1 1 calc R . . H40C H 0.3596 1.7401 0.1770 0.080 Uiso 1 1 calc R . . H40A H 0.3404 1.8168 0.1849 0.080 Uiso 1 1 calc R . . C41 C 0.1694(5) 1.8654(3) 0.1473(3) 0.0350(16) Uani 1 1 d . . . H41B H 0.1803 1.8972 0.1702 0.052 Uiso 1 1 calc R . . H41C H 0.1015 1.8693 0.1539 0.052 Uiso 1 1 calc R . . H41A H 0.1937 1.8751 0.1019 0.052 Uiso 1 1 calc R . . C42 C 0.2041(4) 1.6399(3) 0.2214(3) 0.0229(13) Uani 1 1 d . . . H42A H 0.1691 1.6752 0.2483 0.027 Uiso 1 1 calc R . . H42B H 0.2584 1.6121 0.2410 0.027 Uiso 1 1 calc R . . C43 C 0.1379(5) 1.5956(3) 0.2204(3) 0.0335(15) Uani 1 1 d . . . H43 H 0.1697 1.5650 0.1877 0.040 Uiso 1 1 calc R . . C44 C 0.0421(5) 1.6378(4) 0.2034(4) 0.066(3) Uani 1 1 d . . . H44C H 0.0006 1.6088 0.2065 0.099 Uiso 1 1 calc R . . H44A H 0.0525 1.6606 0.1600 0.099 Uiso 1 1 calc R . . H44B H 0.0126 1.6710 0.2327 0.099 Uiso 1 1 calc R . . C45 C 0.1248(5) 1.5526(3) 0.2861(3) 0.0420(18) Uani 1 1 d . . . H45B H 0.0997 1.5818 0.3192 0.063 Uiso 1 1 calc R . . H45A H 0.1859 1.5227 0.2932 0.063 Uiso 1 1 calc R . . H45C H 0.0804 1.5263 0.2872 0.063 Uiso 1 1 calc R . . C46 C 0.6246(4) 1.6299(3) 0.0486(3) 0.0198(12) Uani 1 1 d . . . C47 C 0.7165(5) 1.6529(3) 0.1186(3) 0.0299(15) Uani 1 1 d . . . H47A H 0.6600 1.6530 0.1522 0.036 Uiso 1 1 calc R . . H47B H 0.7393 1.6918 0.1207 0.036 Uiso 1 1 calc R . . C48 C 0.7936(7) 1.5890(4) 0.1319(4) 0.057(2) Uani 1 1 d . . . H48 H 0.7642 1.5516 0.1344 0.068 Uiso 1 1 calc R . . C49 C 0.8144(6) 1.5848(4) 0.1994(3) 0.059(2) Uani 1 1 d . . . H49B H 0.8637 1.5440 0.2079 0.088 Uiso 1 1 calc R . . H49A H 0.7567 1.5840 0.2309 0.088 Uiso 1 1 calc R . . H49C H 0.8359 1.6236 0.2017 0.088 Uiso 1 1 calc R . . C50 C 0.8759(8) 1.5759(7) 0.0861(4) 0.119(5) Uani 1 1 d . . . H50C H 0.8665 1.5525 0.0544 0.178 Uiso 1 1 calc R . . H50A H 0.9286 1.5480 0.1063 0.178 Uiso 1 1 calc R . . H50B H 0.8904 1.6180 0.0654 0.178 Uiso 1 1 calc R . . C51 C 0.7325(5) 1.7024(3) 0.0005(3) 0.0375(17) Uani 1 1 d . . . H51B H 0.7543 1.6769 -0.0361 0.045 Uiso 1 1 calc R . . H51A H 0.7891 1.7095 0.0112 0.045 Uiso 1 1 calc R . . C52 C 0.6673(6) 1.7718(4) -0.0201(3) 0.0444(19) Uani 1 1 d . . . H52 H 0.6146 1.7642 -0.0362 0.053 Uiso 1 1 calc R . . C53 C 0.6238(6) 1.8118(4) 0.0358(4) 0.052(2) Uani 1 1 d . . . H53B H 0.5786 1.7905 0.0659 0.078 Uiso 1 1 calc R . . H53A H 0.5912 1.8573 0.0204 0.078 Uiso 1 1 calc R . . H53C H 0.6739 1.8131 0.0570 0.078 Uiso 1 1 calc R . . C54 C 0.7233(7) 1.8123(5) -0.0751(4) 0.077(3) Uani 1 1 d . . . H54A H 0.6801 1.8541 -0.0896 0.116 Uiso 1 1 calc R . . H54B H 0.7513 1.7859 -0.1103 0.116 Uiso 1 1 calc R . . H54C H 0.7735 1.8221 -0.0597 0.116 Uiso 1 1 calc R . . C55 C 0.3834(4) 0.8632(3) 0.4526(3) 0.0203(12) Uani 1 1 d . . . C56 C 0.2824(5) 0.7861(3) 0.4995(3) 0.0295(15) Uani 1 1 d . . . H56B H 0.2262 0.7780 0.4891 0.035 Uiso 1 1 calc R . . H56A H 0.2611 0.8089 0.5379 0.035 Uiso 1 1 calc R . . C57 C 0.3547(5) 0.7161(4) 0.5151(3) 0.0413(18) Uani 1 1 d . . . H57 H 0.4095 0.7242 0.5281 0.050 Uiso 1 1 calc R . . C58 C 0.3035(7) 0.6754(4) 0.5719(4) 0.067(3) Uani 1 1 d . . . H58A H 0.2481 0.6685 0.5603 0.100 Uiso 1 1 calc R . . H58B H 0.2833 0.7000 0.6086 0.100 Uiso 1 1 calc R . . H58C H 0.3469 0.6321 0.5826 0.100 Uiso 1 1 calc R . . C59 C 0.3915(6) 0.6792(4) 0.4573(4) 0.051(2) Uani 1 1 d . . . H59C H 0.3397 0.6665 0.4467 0.077 Uiso 1 1 calc R . . H59B H 0.4415 0.6390 0.4666 0.077 Uiso 1 1 calc R . . H59A H 0.4171 0.7082 0.4214 0.077 Uiso 1 1 calc R . . C60 C 0.2870(4) 0.8425(3) 0.3843(3) 0.0290(14) Uani 1 1 d . . . H60A H 0.2838 0.7995 0.3745 0.035 Uiso 1 1 calc R . . H60B H 0.3323 0.8600 0.3497 0.035 Uiso 1 1 calc R . . C61 C 0.1867(7) 0.8931(4) 0.3877(4) 0.064(3) Uani 1 1 d . . . H61 H 0.1412 0.8671 0.4123 0.076 Uiso 1 1 calc R . . C62 C 0.1669(6) 0.9084(4) 0.3191(4) 0.069(3) Uani 1 1 d . . . H62B H 0.1033 0.9381 0.3187 0.103 Uiso 1 1 calc R . . H62C H 0.1711 0.8667 0.3039 0.103 Uiso 1 1 calc R . . H62A H 0.2136 0.9301 0.2915 0.103 Uiso 1 1 calc R . . C63 C 0.1681(7) 0.9502(5) 0.4200(5) 0.093(4) Uani 1 1 d . . . H63C H 0.1865 0.9356 0.4616 0.140 Uiso 1 1 calc R . . H63A H 0.1006 0.9729 0.4254 0.140 Uiso 1 1 calc R . . H63B H 0.2047 0.9809 0.3950 0.140 Uiso 1 1 calc R . . C64 C 0.6893(4) 0.8619(3) 0.3832(3) 0.0195(12) Uani 1 1 d . . . C65 C 0.8057(4) 0.7534(3) 0.3623(3) 0.0227(13) Uani 1 1 d . . . H65B H 0.7904 0.7431 0.4090 0.027 Uiso 1 1 calc R . . H65A H 0.8752 0.7458 0.3501 0.027 Uiso 1 1 calc R . . C66 C 0.7748(5) 0.7045(3) 0.3320(3) 0.0318(15) Uani 1 1 d . . . H66 H 0.7921 0.7143 0.2849 0.038 Uiso 1 1 calc R . . C67 C 0.6673(5) 0.7112(4) 0.3499(4) 0.0473(19) Uani 1 1 d . . . H67C H 0.6518 0.6781 0.3310 0.071 Uiso 1 1 calc R . . H67A H 0.6331 0.7560 0.3339 0.071 Uiso 1 1 calc R . . H67B H 0.6488 0.7035 0.3960 0.071 Uiso 1 1 calc R . . C68 C 0.8331(5) 0.6327(3) 0.3534(3) 0.0361(17) Uani 1 1 d . . . H68B H 0.8166 0.6222 0.3995 0.054 Uiso 1 1 calc R . . H68A H 0.9008 0.6303 0.3413 0.054 Uiso 1 1 calc R . . H68C H 0.8186 0.6005 0.3329 0.054 Uiso 1 1 calc R . . C69 C 0.7922(4) 0.8569(3) 0.2775(2) 0.0210(12) Uani 1 1 d . . . H69A H 0.7363 0.8855 0.2602 0.025 Uiso 1 1 calc R . . H69B H 0.8228 0.8209 0.2506 0.025 Uiso 1 1 calc R . . C70 C 0.8625(4) 0.8992(3) 0.2734(3) 0.0294(15) Uani 1 1 d . . . H70 H 0.8372 0.9285 0.3077 0.035 Uiso 1 1 calc R . . C71 C 0.8678(5) 0.9447(3) 0.2086(3) 0.0432(18) Uani 1 1 d . . . H71C H 0.8842 0.9172 0.1742 0.065 Uiso 1 1 calc R . . H71B H 0.9161 0.9687 0.2042 0.065 Uiso 1 1 calc R . . H71A H 0.8063 0.9768 0.2066 0.065 Uiso 1 1 calc R . . C72 C 0.9607(5) 0.8550(4) 0.2835(4) 0.0465(19) Uani 1 1 d . . . H72B H 0.9555 0.8298 0.3260 0.070 Uiso 1 1 calc R . . H72A H 1.0040 0.8831 0.2788 0.070 Uiso 1 1 calc R . . H72C H 0.9851 0.8238 0.2519 0.070 Uiso 1 1 calc R . . C73 C 0.8123(7) 1.0940(5) 0.3400(5) 0.079(3) Uani 1 1 d . . . H73A H 0.7522 1.0986 0.3709 0.095 Uiso 1 1 calc R . . H73B H 0.8029 1.0795 0.3020 0.095 Uiso 1 1 calc R . . C74 C 0.8254(8) 1.5844(5) -0.1571(5) 0.086(3) Uani 1 1 d . . . H74A H 0.7557 1.6011 -0.1505 0.103 Uiso 1 1 calc R A 1 H74B H 0.8453 1.5610 -0.1950 0.103 Uiso 1 1 calc R A 1 Cl4A Cl 0.9526(6) 1.6008(5) -0.1972(3) 0.128(3) Uani 0.50 1 d P B 2 Cl4B Cl 0.8727(12) 1.6537(8) -0.1744(5) 0.251(7) Uani 0.50 1 d P B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0352(7) 0.0304(6) 0.0154(5) 0.0006(5) -0.0014(5) 0.0166(5) Cl1 0.171(4) 0.094(2) 0.094(2) -0.0081(19) -0.044(2) -0.035(2) S1 0.0425(11) 0.0394(10) 0.0157(7) 0.0011(7) -0.0040(7) 0.0199(8) F1 0.043(3) 0.046(3) 0.086(3) -0.001(2) -0.036(2) -0.011(2) N1 0.031(3) 0.031(3) 0.020(3) 0.003(2) -0.008(2) 0.000(2) C1 0.029(4) 0.044(4) 0.016(3) 0.005(3) 0.004(3) 0.009(3) B1 0.035(5) 0.036(5) 0.039(4) -0.009(4) -0.008(4) -0.007(4) V2 0.0366(7) 0.0303(6) 0.0135(5) 0.0018(4) -0.0001(5) 0.0177(5) Cl2 0.275(6) 0.075(2) 0.432(9) -0.001(4) -0.293(7) -0.004(3) S2 0.0380(10) 0.0406(10) 0.0185(8) -0.0029(7) -0.0039(7) 0.0135(8) F2 0.054(3) 0.050(3) 0.109(4) 0.005(3) -0.041(3) 0.004(2) N2 0.033(3) 0.021(3) 0.026(3) -0.002(2) -0.006(2) 0.006(2) C2 0.029(4) 0.035(4) 0.026(3) 0.004(3) -0.011(3) -0.001(3) B2 0.040(5) 0.027(4) 0.033(4) -0.007(3) -0.010(4) -0.013(4) V3 0.0189(5) 0.0127(5) 0.0155(5) -0.0028(4) -0.0045(4) -0.0015(4) Cl3 0.128(3) 0.140(3) 0.138(3) -0.019(3) -0.044(3) -0.010(3) S3 0.0381(10) 0.0321(9) 0.0224(8) 0.0023(7) -0.0020(7) 0.0107(8) F3 0.095(4) 0.089(4) 0.046(3) -0.013(3) 0.001(3) -0.067(3) N3 0.043(4) 0.022(3) 0.039(3) 0.004(3) -0.015(3) 0.000(3) C3 0.022(3) 0.031(4) 0.028(3) -0.006(3) -0.009(3) -0.001(3) V4 0.0183(5) 0.0109(5) 0.0155(4) -0.0024(4) -0.0041(4) -0.0011(4) S4 0.0346(10) 0.0321(9) 0.0162(7) 0.0025(7) -0.0032(7) 0.0134(7) F4 0.074(4) 0.094(4) 0.062(3) -0.045(3) 0.012(3) -0.036(3) N4 0.023(3) 0.035(3) 0.026(3) -0.006(2) -0.005(2) 0.005(2) C4 0.033(4) 0.051(5) 0.031(4) -0.010(3) -0.005(3) -0.007(3) S5 0.0426(11) 0.0318(9) 0.0190(8) 0.0042(7) -0.0017(7) 0.0108(8) F5 0.077(4) 0.103(4) 0.059(3) -0.046(3) 0.017(3) -0.048(3) N5 0.021(3) 0.020(3) 0.017(2) -0.004(2) -0.002(2) -0.003(2) C5 0.025(4) 0.043(4) 0.033(3) -0.005(3) -0.004(3) -0.006(3) S6 0.0486(11) 0.0289(9) 0.0160(7) 0.0006(7) -0.0026(7) 0.0113(8) F6 0.083(4) 0.075(3) 0.050(3) -0.006(2) -0.002(2) -0.059(3) N6 0.025(3) 0.025(3) 0.020(2) -0.002(2) -0.005(2) -0.007(2) C6 0.028(4) 0.038(4) 0.026(3) 0.015(3) -0.006(3) -0.004(3) S7 0.0379(10) 0.0333(10) 0.0225(8) 0.0058(7) -0.0002(7) 0.0187(8) F7 0.054(3) 0.039(3) 0.095(4) 0.000(3) -0.024(3) 0.009(2) N7 0.027(3) 0.021(3) 0.032(3) -0.006(2) -0.007(2) -0.009(2) C7 0.045(5) 0.059(5) 0.026(3) 0.005(3) -0.011(3) -0.019(4) S8 0.0377(10) 0.0273(9) 0.0186(7) 0.0012(7) -0.0018(7) 0.0151(7) F8 0.047(3) 0.048(3) 0.076(3) 0.003(2) -0.036(2) -0.010(2) N8 0.019(3) 0.014(2) 0.015(2) 0.0001(19) -0.0026(19) 0.001(2) C8 0.038(5) 0.098(7) 0.054(5) 0.021(5) -0.014(4) -0.023(5) S9 0.0447(11) 0.0277(9) 0.0220(8) 0.0052(7) -0.0014(7) 0.0143(8) C9 0.076(6) 0.061(5) 0.031(4) 0.002(4) -0.009(4) -0.036(5) S10 0.0356(10) 0.0276(9) 0.0215(8) 0.0064(7) 0.0024(7) 0.0139(7) C10 0.037(4) 0.020(3) 0.021(3) 0.001(3) -0.010(3) 0.005(3) S11 0.0485(11) 0.0342(10) 0.0149(7) 0.0009(7) -0.0012(7) 0.0150(8) C11 0.028(4) 0.031(4) 0.035(4) -0.006(3) -0.005(3) 0.002(3) S12 0.0408(10) 0.0329(9) 0.0145(7) 0.0009(7) -0.0021(7) 0.0089(8) C12 0.030(4) 0.019(3) 0.052(4) -0.002(3) 0.002(3) 0.004(3) S13 0.0186(7) 0.0194(7) 0.0219(7) -0.0055(6) -0.0058(6) -0.0007(6) C13 0.038(5) 0.029(4) 0.070(5) 0.000(4) 0.003(4) 0.013(3) S14 0.0220(8) 0.0149(7) 0.0211(7) -0.0031(6) -0.0082(6) 0.0012(6) C14 0.051(5) 0.033(4) 0.051(4) -0.008(4) -0.003(4) -0.010(4) S15 0.0267(8) 0.0147(7) 0.0161(7) -0.0006(6) 0.0001(6) -0.0004(6) C15 0.039(4) 0.025(4) 0.038(4) 0.000(3) -0.004(3) -0.002(3) S16 0.0216(8) 0.0138(7) 0.0187(7) -0.0006(6) -0.0024(6) -0.0021(6) C16 0.047(5) 0.042(5) 0.052(5) -0.014(4) -0.005(4) 0.004(4) S17 0.0259(8) 0.0227(8) 0.0156(7) -0.0022(6) -0.0034(6) -0.0076(6) C17 0.063(6) 0.041(5) 0.074(6) 0.007(5) -0.002(5) -0.011(4) S18 0.0267(8) 0.0253(8) 0.0159(7) -0.0024(6) -0.0043(6) -0.0108(7) C18 0.095(8) 0.055(6) 0.078(6) -0.016(5) -0.024(6) -0.020(6) S19 0.0219(8) 0.0134(7) 0.0188(7) -0.0002(6) -0.0064(6) 0.0002(6) C19 0.039(4) 0.030(4) 0.023(3) -0.007(3) 0.000(3) 0.003(3) S20 0.0166(7) 0.0191(7) 0.0231(7) -0.0044(6) -0.0061(6) -0.0026(6) C20 0.036(4) 0.034(4) 0.056(5) 0.011(4) -0.024(4) -0.002(3) S21 0.0264(8) 0.0207(7) 0.0166(7) -0.0023(6) -0.0035(6) -0.0089(6) C21 0.043(5) 0.049(5) 0.053(5) -0.007(4) 0.007(4) -0.006(4) S22 0.0282(8) 0.0245(8) 0.0170(7) -0.0035(6) -0.0053(6) -0.0106(7) C22 0.060(6) 0.047(5) 0.055(5) -0.001(4) -0.006(4) -0.019(4) S23 0.0264(8) 0.0119(7) 0.0166(7) -0.0005(6) -0.0018(6) 0.0011(6) C23 0.041(5) 0.052(5) 0.101(7) -0.011(5) -0.003(5) 0.010(4) S24 0.0213(8) 0.0145(7) 0.0184(7) 0.0013(6) -0.0022(6) -0.0014(6) C24 0.043(5) 0.057(6) 0.089(7) 0.044(5) -0.031(5) -0.008(4) C25 0.32(2) 0.038(7) 0.188(16) -0.043(9) 0.163(16) -0.041(11) C26 0.115(12) 0.037(6) 0.41(3) 0.035(11) 0.100(15) -0.017(7) C27 0.76(3) 0.365(13) 0.75(5) 0.470(18) -0.70(3) -0.514 C28 0.022(3) 0.040(4) 0.025(3) 0.006(3) -0.004(3) 0.006(3) C29 0.026(4) 0.044(4) 0.018(3) -0.005(3) -0.001(3) -0.004(3) C30 0.021(3) 0.037(4) 0.026(3) -0.008(3) -0.002(3) 0.001(3) C31 0.031(4) 0.054(5) 0.031(4) -0.022(3) 0.007(3) -0.009(4) C32 0.028(4) 0.049(4) 0.026(3) -0.007(3) -0.004(3) -0.006(3) C33 0.036(4) 0.035(4) 0.022(3) 0.002(3) -0.011(3) -0.001(3) C34 0.039(4) 0.050(5) 0.023(3) -0.006(3) -0.006(3) -0.013(4) C35 0.043(5) 0.069(6) 0.027(4) -0.002(4) -0.004(3) -0.022(4) C36 0.074(6) 0.044(5) 0.038(4) 0.003(4) -0.014(4) -0.032(4) C37 0.018(3) 0.019(3) 0.019(3) -0.003(2) -0.007(2) -0.003(2) C38 0.023(3) 0.018(3) 0.023(3) -0.005(3) -0.001(3) 0.002(3) C39 0.046(4) 0.018(3) 0.026(3) -0.003(3) -0.012(3) 0.003(3) C40 0.047(5) 0.027(4) 0.096(6) -0.018(4) -0.031(5) -0.005(4) C41 0.043(4) 0.017(3) 0.033(4) -0.001(3) 0.005(3) 0.000(3) C42 0.020(3) 0.023(3) 0.022(3) -0.003(3) 0.000(2) -0.002(3) C43 0.032(4) 0.030(4) 0.038(4) -0.003(3) -0.004(3) -0.011(3) C44 0.036(5) 0.059(5) 0.099(7) 0.035(5) -0.031(5) -0.021(4) C45 0.045(5) 0.031(4) 0.040(4) 0.004(3) 0.008(3) -0.014(3) C46 0.016(3) 0.020(3) 0.022(3) -0.005(2) 0.002(2) -0.005(2) C47 0.036(4) 0.034(4) 0.029(3) -0.013(3) -0.012(3) -0.014(3) C48 0.073(6) 0.049(5) 0.053(5) -0.012(4) -0.034(5) -0.002(4) C49 0.073(6) 0.070(6) 0.044(4) 0.004(4) -0.029(4) -0.029(5) C50 0.083(8) 0.165(12) 0.047(6) -0.007(7) -0.011(6) 0.055(8) C51 0.049(5) 0.036(4) 0.035(4) -0.002(3) -0.007(3) -0.026(4) C52 0.061(5) 0.042(4) 0.040(4) 0.001(4) -0.016(4) -0.026(4) C53 0.062(6) 0.035(4) 0.059(5) -0.008(4) -0.018(4) -0.007(4) C54 0.101(8) 0.068(6) 0.063(6) 0.012(5) -0.008(5) -0.043(6) C55 0.025(3) 0.015(3) 0.020(3) -0.004(2) -0.004(2) -0.003(2) C56 0.038(4) 0.026(3) 0.030(3) -0.006(3) -0.004(3) -0.018(3) C57 0.048(5) 0.035(4) 0.047(4) 0.002(3) -0.015(4) -0.019(4) C58 0.089(7) 0.042(5) 0.060(5) 0.009(4) 0.002(5) -0.024(5) C59 0.063(6) 0.038(4) 0.055(5) -0.002(4) -0.025(4) -0.008(4) C60 0.034(4) 0.033(4) 0.026(3) -0.010(3) -0.004(3) -0.013(3) C61 0.072(6) 0.060(6) 0.073(6) -0.032(5) -0.047(5) 0.003(5) C62 0.074(6) 0.058(6) 0.090(7) -0.025(5) -0.059(6) 0.003(5) C63 0.081(8) 0.081(7) 0.106(8) -0.048(7) -0.053(6) 0.045(6) C64 0.019(3) 0.020(3) 0.019(3) 0.003(2) -0.009(2) -0.004(2) C65 0.026(3) 0.018(3) 0.019(3) 0.001(2) -0.009(3) 0.003(3) C66 0.052(5) 0.013(3) 0.027(3) -0.001(3) -0.008(3) -0.003(3) C67 0.053(5) 0.028(4) 0.068(5) -0.008(4) -0.030(4) -0.007(4) C68 0.055(5) 0.021(3) 0.023(3) -0.002(3) 0.001(3) -0.002(3) C69 0.018(3) 0.023(3) 0.019(3) -0.002(2) -0.004(2) -0.002(3) C70 0.029(4) 0.028(3) 0.030(3) -0.004(3) 0.003(3) -0.011(3) C71 0.038(4) 0.032(4) 0.053(4) 0.008(3) 0.001(3) -0.014(3) C72 0.028(4) 0.059(5) 0.056(5) 0.008(4) -0.013(3) -0.020(4) C73 0.078(7) 0.075(7) 0.076(7) -0.016(6) -0.011(6) -0.007(6) C74 0.111(9) 0.073(7) 0.081(7) 0.007(6) -0.056(7) -0.016(7) Cl4A 0.129(6) 0.159(7) 0.094(5) 0.061(5) -0.055(5) -0.058(6) Cl4B 0.314(19) 0.342(19) 0.146(9) -0.109(11) 0.018(10) -0.160(16) _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 V1 S3 2.391(2) . ? V1 S2 2.397(2) . ? V1 S1 2.4219(18) . ? V1 S6 2.4242(19) . ? V1 S4 2.4283(19) . ? V1 S7 2.435(2) . ? V1 S5 2.487(2) . ? V1 S8 2.490(2) . ? V1 V2 2.9402(14) . ? Cl1 C73 1.768(10) . ? S1 S2 2.007(3) . ? S1 V2 2.423(2) . ? F1 B1 1.395(9) . ? N1 C1 1.324(8) . ? N1 C6 1.464(7) . ? N1 C2 1.483(7) . ? C1 S6 1.710(7) . ? C1 S5 1.725(6) . ? B1 F2 1.353(9) . ? B1 F4 1.360(8) . ? B1 F3 1.374(9) . ? V2 S3 2.381(2) . ? V2 S2 2.403(2) . ? V2 S10 2.424(2) . ? V2 S4 2.4254(18) . ? V2 S11 2.433(2) . ? V2 S12 2.477(2) . ? V2 S9 2.488(2) . ? Cl2 C73 1.590(10) . ? N2 C10 1.313(8) . ? N2 C11 1.452(8) . ? N2 C15 1.491(8) . ? C2 C3 1.506(8) . ? B2 F8 1.364(8) . ? B2 F5 1.364(8) . ? B2 F6 1.372(8) . ? B2 F7 1.376(9) . ? V3 S13 2.3922(16) 2_685 ? V3 S13 2.4017(17) . ? V3 S18 2.4192(16) . ? V3 S14 2.4233(16) . ? V3 S14 2.4293(16) 2_685 ? V3 S15 2.4325(17) . ? V3 S16 2.4796(16) . ? V3 S17 2.4829(16) . ? V3 V3 2.9510(17) 2_685 ? Cl3 C74 1.674(10) . ? S3 S4 2.002(2) . ? N3 C19 1.338(8) . ? N3 C24 1.466(9) . ? N3 C20 1.482(8) . ? C3 C4 1.520(8) . ? C3 C5 1.528(8) . ? V4 S20 2.3967(16) 2_676 ? V4 S20 2.4084(17) . ? V4 S22 2.4141(16) . ? V4 S19 2.4227(16) . ? V4 S19 2.4273(16) 2_676 ? V4 S23 2.4320(16) . ? V4 S24 2.4814(16) . ? V4 S21 2.4938(16) . ? V4 V4 2.9576(17) 2_676 ? N4 C28 1.282(8) . ? N4 C29 1.469(7) . ? N4 C33 1.485(8) . ? N5 C37 1.320(7) . ? N5 C38 1.480(7) . ? N5 C42 1.484(6) . ? N6 C46 1.331(7) . ? N6 C51 1.462(7) . ? N6 C47 1.473(7) . ? C6 C7 1.513(9) . ? S7 C10 1.716(6) . ? N7 C55 1.311(7) . ? N7 C56 1.462(7) . ? N7 C60 1.482(7) . ? C7 C8 1.502(11) . ? C7 C9 1.546(10) . ? S8 C10 1.724(6) . ? N8 C64 1.316(7) . ? N8 C69 1.471(6) . ? N8 C65 1.485(7) . ? S9 C19 1.713(7) . ? S10 C19 1.708(7) . ? S11 C28 1.731(7) . ? C11 C12 1.519(9) . ? S12 C28 1.734(6) . ? C12 C13 1.511(9) . ? C12 C14 1.518(9) . ? S13 S14 2.004(2) . ? S13 V3 2.3922(16) 2_685 ? S14 V3 2.4293(16) 2_685 ? S15 C37 1.721(5) . ? C15 C16 1.531(10) . ? S16 C37 1.708(6) . ? C16 C18 1.450(11) . ? C16 C17 1.541(10) . ? S17 C46 1.713(6) . ? S18 C46 1.702(5) . ? S19 S20 2.0037(19) . ? S19 V4 2.4273(16) 2_676 ? S20 V4 2.3967(16) 2_676 ? C20 C21 1.518(10) . ? S21 C55 1.724(5) . ? C21 C22 1.495(10) . ? C21 C23 1.508(11) . ? S22 C55 1.714(6) . ? S23 C64 1.705(5) . ? S24 C64 1.729(6) . ? C24 C25 1.67(2) . ? C25 C26 1.52(2) . ? C25 C27 1.531(18) . ? C29 C30 1.534(8) . ? C30 C32 1.525(8) . ? C30 C31 1.528(8) . ? C33 C34 1.525(9) . ? C34 C35 1.509(10) . ? C34 C36 1.532(9) . ? C38 C39 1.541(8) . ? C39 C40 1.507(9) . ? C39 C41 1.513(8) . ? C42 C43 1.528(8) . ? C43 C44 1.513(9) . ? C43 C45 1.521(8) . ? C47 C48 1.503(10) . ? C48 C50 1.370(12) . ? C48 C49 1.527(10) . ? C51 C52 1.530(10) . ? C52 C53 1.501(9) . ? C52 C54 1.536(10) . ? C56 C57 1.560(9) . ? C57 C59 1.491(9) . ? C57 C58 1.526(9) . ? C60 C61 1.540(10) . ? C61 C63 1.410(11) . ? C61 C62 1.521(10) . ? C65 C66 1.519(8) . ? C66 C67 1.515(9) . ? C66 C68 1.532(8) . ? C69 C70 1.518(8) . ? C70 C72 1.510(9) . ? C70 C71 1.524(8) . ? C74 Cl4B 1.719(16) . ? C74 Cl4A 1.974(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 V1 S2 104.13(7) . . ? S3 V1 S1 85.07(7) . . ? S2 V1 S1 49.21(6) . . ? S3 V1 S6 86.10(7) . . ? S2 V1 S6 160.24(8) . . ? S1 V1 S6 150.10(8) . . ? S3 V1 S4 49.09(6) . . ? S2 V1 S4 84.40(7) . . ? S1 V1 S4 105.31(6) . . ? S6 V1 S4 90.02(7) . . ? S3 V1 S7 159.67(8) . . ? S2 V1 S7 87.14(7) . . ? S1 V1 S7 89.95(7) . . ? S6 V1 S7 88.53(7) . . ? S4 V1 S7 150.61(8) . . ? S3 V1 S5 80.87(7) . . ? S2 V1 S5 127.19(7) . . ? S1 V1 S5 79.84(7) . . ? S6 V1 S5 70.57(6) . . ? S4 V1 S5 127.92(8) . . ? S7 V1 S5 78.86(7) . . ? S3 V1 S8 127.53(7) . . ? S2 V1 S8 81.60(7) . . ? S1 V1 S8 128.33(8) . . ? S6 V1 S8 78.79(6) . . ? S4 V1 S8 80.71(6) . . ? S7 V1 S8 70.22(6) . . ? S5 V1 S8 136.61(7) . . ? S3 V1 V2 51.82(5) . . ? S2 V1 V2 52.32(5) . . ? S1 V1 V2 52.64(5) . . ? S6 V1 V2 135.25(7) . . ? S4 V1 V2 52.67(4) . . ? S7 V1 V2 136.21(7) . . ? S5 V1 V2 110.64(6) . . ? S8 V1 V2 112.75(6) . . ? S2 S1 V1 64.76(7) . . ? S2 S1 V2 64.92(7) . . ? V1 S1 V2 74.73(6) . . ? C1 N1 C6 123.4(5) . . ? C1 N1 C2 120.0(5) . . ? C6 N1 C2 116.3(5) . . ? N1 C1 S6 125.2(5) . . ? N1 C1 S5 123.4(5) . . ? S6 C1 S5 111.3(4) . . ? F2 B1 F4 111.0(7) . . ? F2 B1 F3 109.1(7) . . ? F4 B1 F3 110.3(6) . . ? F2 B1 F1 107.9(6) . . ? F4 B1 F1 109.3(6) . . ? F3 B1 F1 109.3(6) . . ? S3 V2 S2 104.25(7) . . ? S3 V2 S1 85.27(7) . . ? S2 V2 S1 49.14(7) . . ? S3 V2 S10 87.06(7) . . ? S2 V2 S10 159.80(8) . . ? S1 V2 S10 150.26(8) . . ? S3 V2 S4 49.23(6) . . ? S2 V2 S4 84.34(6) . . ? S1 V2 S4 105.38(6) . . ? S10 V2 S4 90.91(7) . . ? S3 V2 S11 160.53(8) . . ? S2 V2 S11 86.47(7) . . ? S1 V2 S11 89.91(7) . . ? S10 V2 S11 87.86(7) . . ? S4 V2 S11 149.69(8) . . ? S3 V2 S12 126.44(7) . . ? S2 V2 S12 81.49(7) . . ? S1 V2 S12 128.44(8) . . ? S10 V2 S12 78.34(7) . . ? S4 V2 S12 79.49(6) . . ? S11 V2 S12 70.61(6) . . ? S3 V2 S9 80.66(7) . . ? S2 V2 S9 127.52(7) . . ? S1 V2 S9 80.18(7) . . ? S10 V2 S9 70.23(6) . . ? S4 V2 S9 127.81(8) . . ? S11 V2 S9 79.93(7) . . ? S12 V2 S9 137.34(7) . . ? S3 V2 V1 52.12(5) . . ? S2 V2 V1 52.14(5) . . ? S1 V2 V1 52.62(5) . . ? S10 V2 V1 136.50(7) . . ? S4 V2 V1 52.76(5) . . ? S11 V2 V1 135.65(7) . . ? S12 V2 V1 111.80(6) . . ? S9 V2 V1 110.84(6) . . ? S1 S2 V1 66.03(8) . . ? S1 S2 V2 65.93(8) . . ? V1 S2 V2 75.54(7) . . ? C10 N2 C11 120.2(5) . . ? C10 N2 C15 120.8(5) . . ? C11 N2 C15 118.9(5) . . ? N1 C2 C3 114.7(5) . . ? F8 B2 F5 109.8(6) . . ? F8 B2 F6 110.7(6) . . ? F5 B2 F6 109.8(5) . . ? F8 B2 F7 107.5(6) . . ? F5 B2 F7 110.7(6) . . ? F6 B2 F7 108.4(6) . . ? S13 V3 S13 104.01(5) 2_685 . ? S13 V3 S18 160.34(6) 2_685 . ? S13 V3 S18 86.44(6) . . ? S13 V3 S14 84.79(6) 2_685 . ? S13 V3 S14 49.07(5) . . ? S18 V3 S14 89.95(6) . . ? S13 V3 S14 49.11(5) 2_685 2_685 ? S13 V3 S14 84.45(5) . 2_685 ? S18 V3 S14 150.09(6) . 2_685 ? S14 V3 S14 105.09(5) . 2_685 ? S13 V3 S15 86.86(6) 2_685 . ? S13 V3 S15 160.95(6) . . ? S18 V3 S15 88.07(6) . . ? S14 V3 S15 149.21(6) . . ? S14 V3 S15 91.36(6) 2_685 . ? S13 V3 S16 82.28(5) 2_685 . ? S13 V3 S16 125.90(6) . . ? S18 V3 S16 78.13(5) . . ? S14 V3 S16 79.09(5) . . ? S14 V3 S16 129.51(6) 2_685 . ? S15 V3 S16 70.44(5) . . ? S13 V3 S17 126.94(6) 2_685 . ? S13 V3 S17 80.80(6) . . ? S18 V3 S17 70.61(5) . . ? S14 V3 S17 127.73(6) . . ? S14 V3 S17 79.82(5) 2_685 . ? S15 V3 S17 80.18(6) . . ? S16 V3 S17 137.44(6) . . ? S13 V3 V3 52.15(4) 2_685 2_685 ? S13 V3 V3 51.86(4) . 2_685 ? S18 V3 V3 135.47(7) . 2_685 ? S14 V3 V3 52.64(4) . 2_685 ? S14 V3 V3 52.45(4) 2_685 2_685 ? S15 V3 V3 136.46(6) . 2_685 ? S16 V3 V3 111.61(6) . 2_685 ? S17 V3 V3 110.92(6) . 2_685 ? S4 S3 V2 66.53(7) . . ? S4 S3 V1 66.42(8) . . ? V2 S3 V1 76.06(7) . . ? C19 N3 C24 122.7(6) . . ? C19 N3 C20 120.0(6) . . ? C24 N3 C20 117.2(6) . . ? C2 C3 C4 111.9(5) . . ? C2 C3 C5 108.6(5) . . ? C4 C3 C5 111.7(5) . . ? S20 V4 S20 104.02(5) 2_676 . ? S20 V4 S22 159.96(6) 2_676 . ? S20 V4 S22 85.98(6) . . ? S20 V4 S19 84.71(6) 2_676 . ? S20 V4 S19 49.01(5) . . ? S22 V4 S19 89.20(6) . . ? S20 V4 S19 49.08(5) 2_676 2_676 ? S20 V4 S19 84.36(5) . 2_676 ? S22 V4 S19 150.68(6) . 2_676 ? S19 V4 S19 104.85(5) . 2_676 ? S20 V4 S23 87.17(6) 2_676 . ? S20 V4 S23 160.76(6) . . ? S22 V4 S23 88.44(6) . . ? S19 V4 S23 149.39(6) . . ? S19 V4 S23 91.67(6) 2_676 . ? S20 V4 S24 82.27(5) 2_676 . ? S20 V4 S24 125.95(6) . . ? S22 V4 S24 77.83(5) . . ? S19 V4 S24 79.23(5) . . ? S19 V4 S24 129.51(6) 2_676 . ? S23 V4 S24 70.44(5) . . ? S20 V4 S21 127.62(6) 2_676 . ? S20 V4 S21 81.32(6) . . ? S22 V4 S21 70.49(5) . . ? S19 V4 S21 128.00(6) . . ? S19 V4 S21 80.70(5) 2_676 . ? S23 V4 S21 79.45(5) . . ? S24 V4 S21 136.47(6) . . ? S20 V4 V4 52.19(4) 2_676 2_676 ? S20 V4 V4 51.83(4) . 2_676 ? S22 V4 V4 134.76(7) . 2_676 ? S19 V4 V4 52.49(4) . 2_676 ? S19 V4 V4 52.35(4) 2_676 2_676 ? S23 V4 V4 136.79(6) . 2_676 ? S24 V4 V4 111.66(6) . 2_676 ? S21 V4 V4 111.83(6) . 2_676 ? S3 S4 V2 64.24(7) . . ? S3 S4 V1 64.48(7) . . ? V2 S4 V1 74.57(6) . . ? C28 N4 C29 121.2(6) . . ? C28 N4 C33 122.2(5) . . ? C29 N4 C33 116.4(5) . . ? C1 S5 V1 87.9(2) . . ? C37 N5 C38 122.0(4) . . ? C37 N5 C42 119.4(5) . . ? C38 N5 C42 118.5(4) . . ? C1 S6 V1 90.2(2) . . ? C46 N6 C51 120.9(5) . . ? C46 N6 C47 119.8(5) . . ? C51 N6 C47 119.2(5) . . ? N1 C6 C7 113.6(5) . . ? C10 S7 V1 90.4(2) . . ? C55 N7 C56 121.9(5) . . ? C55 N7 C60 120.3(5) . . ? C56 N7 C60 117.7(5) . . ? C8 C7 C6 112.8(7) . . ? C8 C7 C9 111.0(6) . . ? C6 C7 C9 108.1(6) . . ? C10 S8 V1 88.4(2) . . ? C64 N8 C69 120.7(5) . . ? C64 N8 C65 121.6(4) . . ? C69 N8 C65 117.6(4) . . ? C19 S9 V2 88.0(2) . . ? C19 S10 V2 90.2(2) . . ? N2 C10 S7 124.5(5) . . ? N2 C10 S8 124.5(5) . . ? S7 C10 S8 110.9(4) . . ? C28 S11 V2 90.3(2) . . ? N2 C11 C12 115.7(5) . . ? C28 S12 V2 88.8(2) . . ? C13 C12 C14 112.1(6) . . ? C13 C12 C11 108.7(6) . . ? C14 C12 C11 112.1(6) . . ? S14 S13 V3 66.41(6) . 2_685 ? S14 S13 V3 66.02(6) . . ? V3 S13 V3 75.99(5) 2_685 . ? S13 S14 V3 64.90(6) . . ? S13 S14 V3 64.48(6) . 2_685 ? V3 S14 V3 74.91(5) . 2_685 ? C37 S15 V3 89.7(2) . . ? N2 C15 C16 114.1(6) . . ? C37 S16 V3 88.43(19) . . ? C18 C16 C15 114.2(7) . . ? C18 C16 C17 109.9(7) . . ? C15 C16 C17 107.2(6) . . ? C46 S17 V3 87.40(18) . . ? C46 S18 V3 89.76(19) . . ? S20 S19 V4 65.12(6) . . ? S20 S19 V4 64.66(6) . 2_676 ? V4 S19 V4 75.15(5) . 2_676 ? N3 C19 S10 124.2(5) . . ? N3 C19 S9 124.3(5) . . ? S10 C19 S9 111.4(4) . . ? S19 S20 V4 66.26(6) . 2_676 ? S19 S20 V4 65.87(6) . . ? V4 S20 V4 75.98(5) 2_676 . ? N3 C20 C21 115.3(6) . . ? C55 S21 V4 87.80(19) . . ? C22 C21 C23 113.2(7) . . ? C22 C21 C20 113.1(7) . . ? C23 C21 C20 107.2(7) . . ? C55 S22 V4 90.64(19) . . ? C64 S23 V4 90.1(2) . . ? C64 S24 V4 87.95(19) . . ? N3 C24 C25 114.5(9) . . ? C26 C25 C27 113.7(13) . . ? C26 C25 C24 100.9(15) . . ? C27 C25 C24 101.2(13) . . ? N4 C28 S11 125.0(5) . . ? N4 C28 S12 125.0(5) . . ? S11 C28 S12 110.0(4) . . ? N4 C29 C30 114.4(5) . . ? C32 C30 C31 112.0(5) . . ? C32 C30 C29 107.9(5) . . ? C31 C30 C29 113.0(5) . . ? N4 C33 C34 113.1(5) . . ? C35 C34 C33 112.0(6) . . ? C35 C34 C36 112.7(6) . . ? C33 C34 C36 107.3(6) . . ? N5 C37 S16 124.2(4) . . ? N5 C37 S15 124.3(4) . . ? S16 C37 S15 111.4(3) . . ? N5 C38 C39 113.9(5) . . ? C40 C39 C41 110.8(6) . . ? C40 C39 C38 112.1(5) . . ? C41 C39 C38 107.4(5) . . ? N5 C42 C43 113.5(5) . . ? C44 C43 C45 111.6(6) . . ? C44 C43 C42 111.8(6) . . ? C45 C43 C42 108.3(5) . . ? N6 C46 S18 124.1(4) . . ? N6 C46 S17 123.7(4) . . ? S18 C46 S17 112.2(3) . . ? N6 C47 C48 114.0(5) . . ? C50 C48 C47 117.7(8) . . ? C50 C48 C49 112.7(8) . . ? C47 C48 C49 109.3(7) . . ? N6 C51 C52 115.3(6) . . ? C53 C52 C51 111.4(6) . . ? C53 C52 C54 110.4(6) . . ? C51 C52 C54 110.6(7) . . ? N7 C55 S22 124.9(4) . . ? N7 C55 S21 124.1(4) . . ? S22 C55 S21 111.0(3) . . ? N7 C56 C57 114.1(5) . . ? C59 C57 C58 112.0(6) . . ? C59 C57 C56 111.2(6) . . ? C58 C57 C56 108.0(6) . . ? N7 C60 C61 111.5(5) . . ? C63 C61 C62 115.7(8) . . ? C63 C61 C60 118.0(7) . . ? C62 C61 C60 105.8(7) . . ? N8 C64 S23 126.0(4) . . ? N8 C64 S24 122.8(4) . . ? S23 C64 S24 111.2(3) . . ? N8 C65 C66 114.1(5) . . ? C67 C66 C65 112.7(5) . . ? C67 C66 C68 111.7(5) . . ? C65 C66 C68 107.0(5) . . ? N8 C69 C70 114.0(4) . . ? C72 C70 C69 111.6(5) . . ? C72 C70 C71 111.7(5) . . ? C69 C70 C71 109.2(5) . . ? Cl2 C73 Cl1 116.5(6) . . ? Cl3 C74 Cl4B 118.5(8) . . ? Cl3 C74 Cl4A 101.1(6) . . ? Cl4B C74 Cl4A 44.6(6) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.858 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.134 #===END