data_global _audit_creation_method 'APEX3 v2016.9-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_CW_FS_040717 _chemical_name_systematic ? _chemical_name_common FS-III-162 _chemical_formula_moiety ? _chemical_formula_sum 'C62.50 H138 Cl3.50 N5.50 P6 Re3' _chemical_formula_iupac ? _chemical_formula_weight 1835.27 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4165(8) _cell_length_b 33.602(2) _cell_length_c 19.7243(14) _cell_angle_alpha 90 _cell_angle_beta 101.313(2) _cell_angle_gamma 90 _cell_volume 8069.5(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.4190 _cell_measurement_theta_max 25.5538 _cell_measurement_temperature 100.(2) _exptl_crystal_description Plate _exptl_crystal_colour 'clear dark brown' _exptl_crystal_size_max 0.217 _exptl_crystal_size_mid 0.085 _exptl_crystal_size_min 0.064 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 4.761 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.75 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'microfucus sealed tube' _diffrn_source_type 'INCOATEC microfocus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'Bruker D8 Venture CMOS' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 10.4167 _diffrn_reflns_number 143213 _diffrn_reflns_av_R_equivalents 0.1745 _diffrn_reflns_av_unetI/netI 0.0971 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.45 _diffrn_reflns_theta_full 26.45 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _refine_special_details ; ; _reflns_number_total 16610 _reflns_number_gt 11420 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_gt 0.1178 _refine_ls_wR_factor_ref 0.1328 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.070 _refine_ls_number_reflns 16610 _refine_ls_number_parameters 963 _refine_ls_number_restraints 469 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+101.1971P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.340 _refine_diff_density_min -1.787 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker Instrument Service vV6.2.4' _computing_cell_refinement 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V8.37A (Bruker AXS Inc., 2015)' _computing_structure_solution 'SHELXT-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 807)' _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Re Re1 0.63631(3) 0.62363(2) 0.92749(2) 0.01904(10) Uani d . . . 1 . . Re Re2 0.83523(3) 0.69445(2) 0.77134(2) 0.02071(10) Uani d . . . 1 . . Cl Cl1 0.5649(2) 0.56664(8) 0.85367(14) 0.0344(6) Uani d . . . 1 . . Cl Cl2 1.0231(2) 0.68398(9) 0.83609(13) 0.0352(6) Uani d . . . 1 . . P P1 0.7849(2) 0.58939(8) 1.00115(14) 0.0235(6) Uani d . . . 1 . . P P2 0.4606(2) 0.65573(8) 0.89515(13) 0.0222(6) Uani d . . . 1 . . P P3 0.8384(2) 0.64346(8) 0.68593(13) 0.0273(6) Uani d . . . 1 . . P P4 0.8374(2) 0.76130(8) 0.81528(14) 0.0275(6) Uani d . . . 1 . . N N1 0.6339(6) 0.6522(2) 1.0125(4) 0.0209(18) Uani d . . . 1 . . N N2 0.7417(7) 0.7202(2) 0.6927(4) 0.027(2) Uani d . . . 1 . . N N3 0.7133(6) 0.6461(2) 0.8650(4) 0.0187(17) Uani d . . . 1 . . N N4 0.7700(6) 0.6654(2) 0.8345(4) 0.0207(18) Uani d . . . 1 . . N N5 0.5447(7) 0.5337(3) 0.2246(4) 0.038(2) Uani d . . D 1 . . C C1 0.7135(8) 0.6487(3) 1.0780(5) 0.025(2) Uani d . . . 1 . . H H1A 0.6747 0.6528 1.1168 0.03 Uiso calc U . R 1 . . H H1B 0.769 0.6701 1.0803 0.03 Uiso calc U . R 1 . . C C2 0.7716(9) 0.6088(3) 1.0869(5) 0.033(3) Uani d . . . 1 . . H H2A 0.7292 0.5899 1.1098 0.039 Uiso calc U . R 1 . . H H2B 0.8454 0.612 1.1165 0.039 Uiso calc U . R 1 . . C C3 0.7733(9) 0.5341(3) 1.0148(6) 0.036(3) Uani d . . . 1 . . C C4 0.6517(9) 0.5255(3) 1.0171(7) 0.045(3) Uani d . . . 1 . . H H4A 0.6052 0.533 0.9728 0.068 Uiso calc U . R 1 . . H H4B 0.6302 0.541 1.0544 0.068 Uiso calc U . R 1 . . H H4C 0.6425 0.4971 1.0255 0.068 Uiso calc U . R 1 . . C C5 0.8460(10) 0.5173(3) 1.0817(6) 0.046(3) Uani d . . . 1 . . H H5A 0.8254 0.4896 1.0882 0.069 Uiso calc U . R 1 . . H H5B 0.8351 0.5333 1.1214 0.069 Uiso calc U . R 1 . . H H5C 0.9234 0.5185 1.0777 0.069 Uiso calc U . R 1 . . C C6 0.8008(10) 0.5116(4) 0.9519(7) 0.049(3) Uani d . . . 1 . . H H6A 0.7761 0.484 0.9525 0.074 Uiso calc U . R 1 . . H H6B 0.8804 0.5122 0.9542 0.074 Uiso calc U . R 1 . . H H6C 0.7635 0.5245 0.9091 0.074 Uiso calc U . R 1 . . C C7 0.9302(7) 0.6038(3) 0.9950(5) 0.024(2) Uani d . . . 1 . . C C8 0.9356(8) 0.6494(3) 1.0065(5) 0.029(2) Uani d . . . 1 . . H H8A 1.0049 0.6596 0.9968 0.043 Uiso calc U . R 1 . . H H8B 0.9314 0.6553 1.0546 0.043 Uiso calc U . R 1 . . H H8C 0.8739 0.6621 0.9754 0.043 Uiso calc U . R 1 . . C C9 0.9513(9) 0.5942(3) 0.9228(6) 0.035(3) Uani d . . . 1 . . H H9A 0.899 0.6089 0.8881 0.053 Uiso calc U . R 1 . . H H9B 0.9419 0.5656 0.9142 0.053 Uiso calc U . R 1 . . H H9C 1.0264 0.602 0.9201 0.053 Uiso calc U . R 1 . . C C10 1.0210(9) 0.5844(4) 1.0490(6) 0.041(3) Uani d . . . 1 . . H H10A 1.0239 0.5558 1.0395 0.062 Uiso calc U . R 1 . . H H10B 1.0051 0.5883 1.0953 0.062 Uiso calc U . R 1 . . H H10C 1.0919 0.5966 1.0467 0.062 Uiso calc U . R 1 . . C C11 0.5580(8) 0.6853(3) 1.0203(5) 0.028(2) Uani d . . . 1 . . H H11A 0.6018 0.7083 1.0419 0.034 Uiso calc U . R 1 . . H H11B 0.5097 0.6767 1.052 0.034 Uiso calc U . R 1 . . C C12 0.4880(8) 0.6985(3) 0.9535(5) 0.027(2) Uani d . . . 1 . . H H12A 0.5263 0.7195 0.9323 0.032 Uiso calc U . R 1 . . H H12B 0.418 0.7096 0.962 0.032 Uiso calc U . R 1 . . C C13 0.3472(8) 0.6272(3) 0.9277(5) 0.026(2) Uani d . . . 1 . . C C14 0.2707(9) 0.6550(3) 0.9589(6) 0.037(3) Uani d . . . 1 . . H H14A 0.2405 0.6754 0.9249 0.055 Uiso calc U . R 1 . . H H14B 0.3126 0.6679 1.0004 0.055 Uiso calc U . R 1 . . H H14C 0.2106 0.6394 0.9711 0.055 Uiso calc U . R 1 . . C C15 0.2788(8) 0.6019(3) 0.8699(6) 0.039(3) Uani d . . . 1 . . H H15A 0.2305 0.6193 0.8375 0.058 Uiso calc U . R 1 . . H H15B 0.2344 0.5828 0.8901 0.058 Uiso calc U . R 1 . . H H15C 0.3281 0.5875 0.8454 0.058 Uiso calc U . R 1 . . C C16 0.4017(8) 0.5990(3) 0.9847(6) 0.033(3) Uani d . . . 1 . . H H16A 0.4424 0.5785 0.9649 0.049 Uiso calc U . R 1 . . H H16B 0.3453 0.5863 1.0059 0.049 Uiso calc U . R 1 . . H H16C 0.4524 0.6139 1.0199 0.049 Uiso calc U . R 1 . . C C17 0.4070(8) 0.6777(3) 0.8067(5) 0.027(2) Uani d . . . 1 . . C C18 0.3028(9) 0.7024(3) 0.8031(6) 0.040(3) Uani d . . . 1 . . H H18A 0.2855 0.7162 0.7586 0.059 Uiso calc U . R 1 . . H H18B 0.3142 0.7219 0.8407 0.059 Uiso calc U . R 1 . . H H18C 0.2417 0.6848 0.8078 0.059 Uiso calc U . R 1 . . C C19 0.3903(9) 0.6444(4) 0.7519(6) 0.039(3) Uani d . . . 1 . . H H19A 0.3845 0.6562 0.7058 0.058 Uiso calc U . R 1 . . H H19B 0.3228 0.6298 0.754 0.058 Uiso calc U . R 1 . . H H19C 0.4531 0.6262 0.761 0.058 Uiso calc U . R 1 . . C C20 0.4961(9) 0.7052(3) 0.7901(6) 0.035(3) Uani d . . . 1 . . H H20A 0.5648 0.6903 0.7936 0.052 Uiso calc U . R 1 . . H H20B 0.5073 0.7274 0.823 0.052 Uiso calc U . R 1 . . H H20C 0.4735 0.7156 0.743 0.052 Uiso calc U . R 1 . . C C21 0.6951(9) 0.7021(3) 0.6256(5) 0.035(3) Uani d . . . 1 . . H H21A 0.6855 0.7228 0.5893 0.042 Uiso calc U . R 1 . . H H21B 0.6217 0.691 0.6272 0.042 Uiso calc U . R 1 . . C C22 0.7679(9) 0.6694(3) 0.6072(5) 0.033(3) Uani d . . . 1 . . H H22A 0.823 0.6809 0.5827 0.04 Uiso calc U . R 1 . . H H22B 0.7228 0.6501 0.5758 0.04 Uiso calc U . R 1 . . C C23 0.7517(9) 0.5979(3) 0.6881(5) 0.033(3) Uani d . . . 1 . . C C24 0.6353(9) 0.6130(3) 0.6859(6) 0.037(3) Uani d . . . 1 . . H H24A 0.6032 0.6218 0.6389 0.055 Uiso calc U . R 1 . . H H24B 0.6374 0.6355 0.7179 0.055 Uiso calc U . R 1 . . H H24C 0.5904 0.5916 0.6996 0.055 Uiso calc U . R 1 . . C C25 0.7880(10) 0.5748(3) 0.7559(6) 0.042(3) Uani d . . . 1 . . H H25A 0.749 0.5493 0.7529 0.062 Uiso calc U . R 1 . . H H25B 0.7708 0.5903 0.7944 0.062 Uiso calc U . R 1 . . H H25C 0.8673 0.5699 0.7636 0.062 Uiso calc U . R 1 . . C C26 0.7490(11) 0.5693(4) 0.6273(6) 0.046(3) Uani d . . . 1 . . H H26A 0.7404 0.5845 0.5842 0.069 Uiso calc U . R 1 . . H H26B 0.6872 0.5509 0.6247 0.069 Uiso calc U . R 1 . . H H26C 0.8178 0.5542 0.6341 0.069 Uiso calc U . R 1 . . C C27 0.9750(9) 0.6301(4) 0.6623(5) 0.038(3) Uani d . . . 1 . . C C28 1.0400(10) 0.6695(4) 0.6635(7) 0.051(3) Uani d . . . 1 . . H H28A 1.1106 0.6642 0.6502 0.077 Uiso calc U . R 1 . . H H28B 1.0529 0.6807 0.7103 0.077 Uiso calc U . R 1 . . H H28C 0.9978 0.6884 0.631 0.077 Uiso calc U . R 1 . . C C29 0.9631(10) 0.6120(4) 0.5890(6) 0.052(4) Uani d . . . 1 . . H H29A 0.9176 0.6295 0.5553 0.077 Uiso calc U . R 1 . . H H29B 0.9282 0.5857 0.588 0.077 Uiso calc U . R 1 . . H H29C 1.0359 0.6092 0.5773 0.077 Uiso calc U . R 1 . . C C30 1.0354(9) 0.6012(4) 0.7158(6) 0.048(3) Uani d . . . 1 . . H H30A 0.9947 0.5761 0.713 0.073 Uiso calc U . R 1 . . H H30B 1.0415 0.6126 0.7621 0.073 Uiso calc U . R 1 . . H H30C 1.1091 0.5963 0.7067 0.073 Uiso calc U . R 1 . . C C31 0.6936(9) 0.7606(3) 0.6929(5) 0.032(3) Uani d . . . 1 . . H H31A 0.6139 0.7589 0.6735 0.038 Uiso calc U . R 1 . . H H31B 0.727 0.778 0.6622 0.038 Uiso calc U . R 1 . . C C32 0.7096(9) 0.7795(3) 0.7634(5) 0.033(3) Uani d . . . 1 . . H H32A 0.6474 0.7726 0.7859 0.04 Uiso calc U . R 1 . . H H32B 0.7124 0.8088 0.7592 0.04 Uiso calc U . R 1 . . C C33 0.9487(10) 0.7934(3) 0.7882(6) 0.038(3) Uani d . . . 1 . . C C34 1.0529(11) 0.7933(4) 0.8437(7) 0.060(4) Uani d . . . 1 . . H H34A 1.1152 0.8018 0.8235 0.089 Uiso calc U . R 1 . . H H34B 1.0665 0.7663 0.8625 0.089 Uiso calc U . R 1 . . H H34C 1.0442 0.8116 0.8809 0.089 Uiso calc U . R 1 . . C C35 0.9104(12) 0.8359(4) 0.7702(7) 0.059(4) Uani d . . . 1 . . H H35A 0.9713 0.8515 0.7589 0.089 Uiso calc U . R 1 . . H H35B 0.8859 0.848 0.8097 0.089 Uiso calc U . R 1 . . H H35C 0.8494 0.8356 0.7302 0.089 Uiso calc U . R 1 . . C C36 0.9772(10) 0.7740(4) 0.7237(6) 0.048(3) Uani d . . . 1 . . H H36A 0.9107 0.7719 0.6878 0.072 Uiso calc U . R 1 . . H H36B 1.0077 0.7475 0.7354 0.072 Uiso calc U . R 1 . . H H36C 1.0315 0.7904 0.7067 0.072 Uiso calc U . R 1 . . C C37 0.8261(10) 0.7737(3) 0.9061(5) 0.035(3) Uani d . . . 1 . . C C38 0.8157(12) 0.8186(3) 0.9185(6) 0.054(4) Uani d . . . 1 . . H H38A 0.8865 0.8316 0.9186 0.081 Uiso calc U . R 1 . . H H38B 0.7945 0.8229 0.9633 0.081 Uiso calc U . R 1 . . H H38C 0.7597 0.83 0.8817 0.081 Uiso calc U . R 1 . . C C39 0.9218(11) 0.7560(4) 0.9570(5) 0.047(3) Uani d . . . 1 . . H H39A 0.9329 0.7283 0.9442 0.07 Uiso calc U . R 1 . . H H39B 0.9058 0.7568 1.0037 0.07 Uiso calc U . R 1 . . H H39C 0.9884 0.7714 0.9559 0.07 Uiso calc U . R 1 . . C C40 0.7224(10) 0.7537(3) 0.9207(6) 0.040(3) Uani d . . . 1 . . H H40A 0.6576 0.7655 0.8912 0.06 Uiso calc U . R 1 . . H H40B 0.7183 0.7575 0.9694 0.06 Uiso calc U . R 1 . . H H40C 0.7248 0.7251 0.9107 0.06 Uiso calc U . R 1 . . Re Re3 0.56845(5) 0.56782(2) 0.31589(3) 0.02476(14) Uani d U P D 0.8 A 1 C C41 0.6329(10) 0.5096(4) 0.2092(6) 0.033(3) Uani d U P D 0.8 A 1 H H41A 0.6872 0.527 0.1933 0.039 Uiso calc U P R 0.8 A 1 H H41B 0.6031 0.4911 0.171 0.039 Uiso calc U P R 0.8 A 1 C C60 0.4239(17) 0.6703(6) 0.3022(11) 0.060(5) Uani d U P . 0.8 A 1 H H60A 0.5001 0.6622 0.3199 0.09 Uiso calc U P R 0.8 A 1 H H60B 0.3794 0.6645 0.3369 0.09 Uiso calc U P R 0.8 A 1 H H60C 0.4215 0.6989 0.2923 0.09 Uiso calc U P R 0.8 A 1 C C59 0.453(2) 0.6557(7) 0.1858(15) 0.063(6) Uani d U P . 0.8 A 1 H H59A 0.4257 0.6415 0.1424 0.095 Uiso calc U P R 0.8 A 1 H H59B 0.5278 0.6465 0.2054 0.095 Uiso calc U P R 0.8 A 1 H H59C 0.4547 0.6843 0.1767 0.095 Uiso calc U P R 0.8 A 1 C C58 0.2630(15) 0.6607(6) 0.2056(11) 0.066(5) Uani d U P . 0.8 A 1 H H58A 0.2618 0.6729 0.1603 0.099 Uiso calc U P R 0.8 A 1 H H58B 0.2384 0.6801 0.2363 0.099 Uiso calc U P R 0.8 A 1 H H58C 0.214 0.6376 0.2001 0.099 Uiso calc U P R 0.8 A 1 C C57 0.379(2) 0.6475(4) 0.2365(13) 0.051(4) Uani d U P D 0.8 A 1 C C42 0.6892(12) 0.4861(4) 0.2701(6) 0.031(3) Uani d U P D 0.8 A 1 H H42A 0.7614 0.4768 0.2622 0.038 Uiso calc U P R 0.8 A 1 H H42B 0.6445 0.4624 0.2759 0.038 Uiso calc U P R 0.8 A 1 C C51 0.4733(10) 0.5496(5) 0.1635(6) 0.038(4) Uani d U P D 0.8 A 1 H H51A 0.4572 0.528 0.1288 0.046 Uiso calc U P R 0.8 A 1 H H51B 0.5136 0.5706 0.1438 0.046 Uiso calc U P R 0.8 A 1 C C50 0.9400(15) 0.5046(5) 0.3885(11) 0.054(5) Uani d U P . 0.8 B 1 H H50A 0.9343 0.4844 0.3522 0.081 Uiso calc U P R 0.8 B 1 H H50B 0.9301 0.492 0.4317 0.081 Uiso calc U P R 0.8 B 1 H H50C 1.0126 0.5171 0.3955 0.081 Uiso calc U P R 0.8 B 1 C C49 0.8689(13) 0.5540(5) 0.2968(9) 0.051(4) Uani d U P . 0.8 B 1 H H49A 0.8643 0.533 0.262 0.076 Uiso calc U P R 0.8 B 1 H H49B 0.941 0.5669 0.303 0.076 Uiso calc U P R 0.8 B 1 H H49C 0.8112 0.5738 0.2814 0.076 Uiso calc U P R 0.8 B 1 C C48 0.8605(13) 0.5697(5) 0.4163(9) 0.053(4) Uani d U P . 0.8 B 1 H H48A 0.7968 0.5871 0.4021 0.08 Uiso calc U P R 0.8 B 1 H H48B 0.928 0.5847 0.4158 0.08 Uiso calc U P R 0.8 B 1 H H48C 0.8614 0.5597 0.4631 0.08 Uiso calc U P R 0.8 B 1 C C46 0.7490(19) 0.4396(5) 0.4117(11) 0.075(5) Uani d U P D 0.8 C 1 H H46A 0.7343 0.4303 0.3636 0.113 Uiso calc U P R 0.8 C 1 H H46B 0.722 0.4199 0.4409 0.113 Uiso calc U P R 0.8 C 1 H H46C 0.8282 0.4432 0.4276 0.113 Uiso calc U P R 0.8 C 1 C C45 0.7157(18) 0.4971(6) 0.4876(8) 0.059(5) Uani d U P D 0.8 C 1 H H45A 0.7954 0.499 0.5035 0.088 Uiso calc U P R 0.8 C 1 H H45B 0.6845 0.4803 0.5195 0.088 Uiso calc U P R 0.8 C 1 H H45C 0.6834 0.5238 0.4861 0.088 Uiso calc U P R 0.8 C 1 C C44 0.5648(14) 0.4718(6) 0.4038(10) 0.075(5) Uani d U P D 0.8 C 1 H H44A 0.5385 0.4628 0.3562 0.112 Uiso calc U P R 0.8 C 1 H H44B 0.5276 0.4966 0.4115 0.112 Uiso calc U P R 0.8 C 1 H H44C 0.5488 0.4514 0.4359 0.112 Uiso calc U P R 0.8 C 1 C C52 0.3663(11) 0.5666(5) 0.1744(6) 0.040(3) Uani d U P D 0.8 A 1 H H52A 0.3122 0.545 0.1745 0.047 Uiso calc U P R 0.8 A 1 H H52B 0.3368 0.5853 0.1365 0.047 Uiso calc U P R 0.8 A 1 C C53 0.2661(16) 0.5761(5) 0.2919(9) 0.047(4) Uani d U P D 0.8 A 1 C C54 0.1570(13) 0.5786(6) 0.2409(9) 0.063(5) Uani d U P D 0.8 A 1 H H54A 0.1502 0.6048 0.2185 0.095 Uiso calc U P R 0.8 A 1 H H54B 0.0965 0.5748 0.2656 0.095 Uiso calc U P R 0.8 A 1 H H54C 0.1539 0.5578 0.2057 0.095 Uiso calc U P R 0.8 A 1 C C55 0.250(2) 0.5997(6) 0.3548(9) 0.049(5) Uani d U P D 0.8 A 1 H H55A 0.2257 0.6266 0.3406 0.074 Uiso calc U P R 0.8 A 1 H H55B 0.3202 0.601 0.388 0.074 Uiso calc U P R 0.8 A 1 H H55C 0.1951 0.5866 0.3763 0.074 Uiso calc U P R 0.8 A 1 C C56 0.2881(18) 0.5331(5) 0.3149(12) 0.081(5) Uani d U P D 0.8 A 1 H H56A 0.2231 0.5222 0.3295 0.121 Uiso calc U P R 0.8 A 1 H H56B 0.3509 0.5321 0.3536 0.121 Uiso calc U P R 0.8 A 1 H H56C 0.3044 0.5173 0.2763 0.121 Uiso calc U P R 0.8 A 1 Cl Cl3 0.5366(4) 0.57989(14) 0.4289(2) 0.0622(11) Uani d U P D 0.8 A 1 Re Re3A 0.5424(2) 0.55450(8) 0.32151(16) 0.02476(14) Uani d U P D 0.2 A 2 C C41A 0.607(3) 0.4970(9) 0.230(3) 0.033(3) Uani d U P D 0.2 A 2 H H41D 0.6032 0.4869 0.1819 0.039 Uiso calc U P R 0.2 A 2 H H41E 0.5691 0.4773 0.2538 0.039 Uiso calc U P R 0.2 A 2 C C42A 0.726(3) 0.4970(16) 0.2644(14) 0.022(7) Uani d U P D 0.2 A 2 H H42D 0.7705 0.5149 0.2411 0.026 Uiso calc U P R 0.2 A 2 H H42E 0.7578 0.4699 0.268 0.026 Uiso calc U P R 0.2 A 2 C C51A 0.445(3) 0.5336(15) 0.174(3) 0.038(4) Uani d U P D 0.2 A 2 H H51D 0.3889 0.5162 0.1878 0.046 Uiso calc U P R 0.2 A 2 H H51E 0.4582 0.5248 0.1281 0.046 Uiso calc U P R 0.2 A 2 C C50A 0.959(6) 0.507(2) 0.360(4) 0.037(9) Uani d U P . 0.2 B 2 H H50D 0.9454 0.4798 0.3734 0.056 Uiso calc U P R 0.2 B 2 H H50E 1.0255 0.5173 0.3906 0.056 Uiso calc U P R 0.2 B 2 H H50F 0.9694 0.5076 0.3121 0.056 Uiso calc U P R 0.2 B 2 C C49A 0.892(4) 0.5747(15) 0.346(3) 0.031(7) Uani d U P . 0.2 B 2 H H49D 0.8632 0.5787 0.2964 0.047 Uiso calc U P R 0.2 B 2 H H49E 0.972 0.5751 0.3549 0.047 Uiso calc U P R 0.2 B 2 H H49F 0.8646 0.596 0.3722 0.047 Uiso calc U P R 0.2 B 2 C C48A 0.892(5) 0.5485(17) 0.456(3) 0.038(8) Uani d U P . 0.2 B 2 H H48D 0.9559 0.5664 0.4627 0.057 Uiso calc U P R 0.2 B 2 H H48E 0.9117 0.5243 0.484 0.057 Uiso calc U P R 0.2 B 2 H H48F 0.831 0.5619 0.4714 0.057 Uiso calc U P R 0.2 B 2 C C46A 0.794(4) 0.4529(18) 0.435(4) 0.051(8) Uani d U P D 0.2 C 2 H H46D 0.8109 0.441 0.393 0.077 Uiso calc U P R 0.2 C 2 H H46E 0.7808 0.4317 0.4666 0.077 Uiso calc U P R 0.2 C 2 H H46F 0.856 0.4692 0.4576 0.077 Uiso calc U P R 0.2 C 2 C C45A 0.674(7) 0.490(2) 0.488(2) 0.041(9) Uani d U P D 0.2 C 2 H H45D 0.6827 0.5194 0.4936 0.061 Uiso calc U P R 0.2 C 2 H H45E 0.729 0.4769 0.5225 0.061 Uiso calc U P R 0.2 C 2 H H45F 0.6004 0.4827 0.493 0.061 Uiso calc U P R 0.2 C 2 C C44A 0.607(4) 0.4506(15) 0.375(3) 0.044(8) Uani d U P D 0.2 C 2 H H44D 0.5684 0.4639 0.333 0.066 Uiso calc U P R 0.2 C 2 H H44E 0.5536 0.4427 0.4033 0.066 Uiso calc U P R 0.2 C 2 H H44F 0.6445 0.4269 0.3625 0.066 Uiso calc U P R 0.2 C 2 C C52A 0.412(5) 0.5764(15) 0.1723(15) 0.034(7) Uani d U P D 0.2 A 2 H H52D 0.3429 0.5801 0.1378 0.04 Uiso calc U P R 0.2 A 2 H H52E 0.4694 0.5929 0.158 0.04 Uiso calc U P R 0.2 A 2 C C53A 0.252(6) 0.5826(15) 0.284(3) 0.038(6) Uani d U P D 0.2 A 2 C C54A 0.154(5) 0.604(2) 0.240(3) 0.044(10) Uani d U P D 0.2 A 2 H H54D 0.1556 0.5998 0.1908 0.067 Uiso calc U P R 0.2 A 2 H H54E 0.1581 0.6322 0.2505 0.067 Uiso calc U P R 0.2 A 2 H H54F 0.0862 0.5927 0.25 0.067 Uiso calc U P R 0.2 A 2 C C55A 0.271(8) 0.589(3) 0.361(3) 0.038(10) Uani d U P D 0.2 A 2 H H55D 0.2818 0.6174 0.3718 0.056 Uiso calc U P R 0.2 A 2 H H55E 0.3359 0.5741 0.384 0.056 Uiso calc U P R 0.2 A 2 H H55F 0.2065 0.5795 0.3787 0.056 Uiso calc U P R 0.2 A 2 C C56A 0.236(5) 0.5388(16) 0.265(3) 0.043(9) Uani d U P D 0.2 A 2 H H56D 0.196 0.5363 0.2176 0.064 Uiso calc U P R 0.2 A 2 H H56E 0.1947 0.526 0.2967 0.064 Uiso calc U P R 0.2 A 2 H H56F 0.3083 0.5259 0.2698 0.064 Uiso calc U P R 0.2 A 2 C C58A 0.298(5) 0.6759(17) 0.248(3) 0.032(8) Uani d U P . 0.2 A 2 H H58D 0.3135 0.6948 0.2869 0.048 Uiso calc U P R 0.2 A 2 H H58E 0.2341 0.6596 0.2528 0.048 Uiso calc U P R 0.2 A 2 H H58F 0.2822 0.6905 0.2046 0.048 Uiso calc U P R 0.2 A 2 C C57A 0.399(7) 0.6484(6) 0.250(5) 0.032(6) Uani d U P D 0.2 A 2 C C59A 0.444(7) 0.668(2) 0.193(4) 0.029(9) Uani d U P . 0.2 A 2 H H59D 0.4831 0.6475 0.1704 0.044 Uiso calc U P R 0.2 A 2 H H59E 0.4957 0.6887 0.212 0.044 Uiso calc U P R 0.2 A 2 H H59F 0.3841 0.6789 0.1588 0.044 Uiso calc U P R 0.2 A 2 C C60A 0.477(5) 0.6686(19) 0.320(3) 0.026(8) Uani d U P . 0.2 A 2 H H60D 0.5508 0.6573 0.3272 0.04 Uiso calc U P R 0.2 A 2 H H60E 0.444 0.663 0.3603 0.04 Uiso calc U P R 0.2 A 2 H H60F 0.4808 0.6975 0.3136 0.04 Uiso calc U P R 0.2 A 2 Cl Cl3A 0.6073(18) 0.6010(6) 0.4091(11) 0.088(5) Uani d U P D 0.2 A 2 Cl Cl4 0.6699(8) 0.6107(3) 0.2620(5) 0.0622(11) Uani d . P D 0.4 D 3 N N6 0.643(3) 0.6069(9) 0.3007(16) 0.0622(11) Uani d . P D 0.4 E 4 N N6A 0.465(9) 0.524(3) 0.360(3) 0.088(5) Uani d . P D 0.1 F 5 Cl Cl4A 0.437(3) 0.4994(8) 0.340(2) 0.088(5) Uani d . P D 0.1 G 6 P P5 0.7092(2) 0.51670(8) 0.34984(14) 0.0322(6) Uani d U . D 1 . . P P6 0.3901(2) 0.59319(9) 0.25859(15) 0.0336(7) Uani d U . D 1 . . C C43 0.6908(10) 0.4790(3) 0.4162(6) 0.047(3) Uani d U . D 1 . . C C47 0.8533(9) 0.5355(3) 0.3675(6) 0.041(2) Uani d U . . 1 . . C C61 1.186(2) 0.7423(9) 1.0824(15) 0.106(11) Uani d U P D 0.5 . . H H61A 1.1205 0.7288 1.0565 0.16 Uiso calc U P R 0.5 . . H H61B 1.1658 0.7569 1.1212 0.16 Uiso calc U P R 0.5 . . H H61C 1.2424 0.7226 1.1001 0.16 Uiso calc U P R 0.5 . . C C62 1.227(2) 0.7702(9) 1.0368(14) 0.108(11) Uani d U P D 0.5 . . H H62A 1.2184 0.7577 0.9906 0.13 Uiso calc U P R 0.5 . . H H62B 1.1799 0.7941 1.0318 0.13 Uiso calc U P R 0.5 . . C C63 1.339(2) 0.7833(11) 1.0563(15) 0.124(12) Uani d U P D 0.5 . . H H63A 1.3876 0.7614 1.047 0.149 Uiso calc U P R 0.5 . . H H63B 1.3553 0.7881 1.1068 0.149 Uiso calc U P R 0.5 . . C C64 1.368(3) 0.8193(9) 1.0218(18) 0.140(12) Uani d U P D 0.5 . . H H64A 1.3022 0.8287 0.9893 0.168 Uiso calc U P R 0.5 . . H H64B 1.3896 0.8403 1.0571 0.168 Uiso calc U P R 0.5 . . C C65 1.455(3) 0.8148(13) 0.9843(18) 0.141(14) Uani d U P D 0.5 . . H H65A 1.4251 0.8051 0.9376 0.212 Uiso calc U P R 0.5 . . H H65B 1.509 0.7956 1.0083 0.212 Uiso calc U P R 0.5 . . H H65C 1.4911 0.8405 0.9815 0.212 Uiso calc U P R 0.5 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Re1 0.01751(19) 0.0183(2) 0.0216(2) -0.00031(16) 0.00478(15) -0.00009(16) Re2 0.0196(2) 0.0254(2) 0.01685(19) -0.00245(17) 0.00277(15) -0.00052(16) Cl1 0.0362(15) 0.0267(14) 0.0393(15) -0.0040(12) 0.0051(12) -0.0052(12) Cl2 0.0187(13) 0.0542(18) 0.0311(14) -0.0039(12) 0.0010(11) 0.0004(12) P1 0.0195(13) 0.0214(14) 0.0293(15) 0.0026(10) 0.0044(11) 0.0008(11) P2 0.0161(13) 0.0243(14) 0.0260(14) -0.0009(10) 0.0034(10) 0.0031(11) P3 0.0250(14) 0.0360(16) 0.0206(14) 0.0035(12) 0.0041(11) -0.0055(12) P4 0.0331(16) 0.0262(15) 0.0232(14) -0.0110(12) 0.0054(12) -0.0006(11) N1 0.019(4) 0.023(4) 0.021(4) 0.005(3) 0.005(3) 0.000(3) N2 0.044(5) 0.012(4) 0.024(5) 0.000(4) 0.004(4) -0.005(3) N3 0.015(4) 0.022(4) 0.019(4) -0.002(3) 0.000(3) -0.002(3) N4 0.015(4) 0.024(4) 0.021(4) 0.005(3) 0.000(3) -0.005(3) N5 0.040(6) 0.051(6) 0.021(5) 0.016(5) 0.000(4) 0.001(4) C1 0.024(5) 0.034(6) 0.016(5) 0.004(4) 0.001(4) -0.001(4) C2 0.025(6) 0.039(7) 0.032(6) -0.001(5) 0.002(5) 0.004(5) C3 0.034(6) 0.020(6) 0.052(7) 0.002(5) 0.004(5) 0.011(5) C4 0.032(7) 0.037(7) 0.068(9) 0.010(5) 0.012(6) 0.028(6) C5 0.047(8) 0.027(6) 0.062(9) 0.005(5) 0.006(6) 0.021(6) C6 0.044(8) 0.033(7) 0.071(9) 0.008(6) 0.013(7) -0.009(6) C7 0.009(5) 0.033(6) 0.029(6) 0.005(4) -0.004(4) 0.005(4) C8 0.026(6) 0.034(6) 0.029(6) -0.010(5) 0.011(5) -0.010(5) C9 0.032(6) 0.035(6) 0.040(7) 0.003(5) 0.010(5) 0.010(5) C10 0.028(6) 0.049(8) 0.047(7) 0.008(5) 0.008(5) 0.015(6) C11 0.030(6) 0.023(6) 0.035(6) 0.005(4) 0.014(5) -0.009(4) C12 0.023(5) 0.026(6) 0.034(6) -0.004(4) 0.011(4) 0.001(5) C13 0.019(5) 0.030(6) 0.030(6) -0.001(4) 0.008(4) 0.009(5) C14 0.024(6) 0.037(7) 0.050(7) 0.003(5) 0.008(5) 0.004(5) C15 0.014(5) 0.047(7) 0.053(8) -0.006(5) 0.003(5) 0.000(6) C16 0.027(6) 0.030(6) 0.045(7) -0.007(5) 0.012(5) 0.008(5) C17 0.013(5) 0.032(6) 0.032(6) -0.003(4) -0.001(4) 0.012(5) C18 0.031(6) 0.048(8) 0.040(7) 0.007(5) 0.009(5) 0.020(6) C19 0.029(6) 0.056(8) 0.032(6) -0.006(6) 0.008(5) -0.004(6) C20 0.030(6) 0.038(7) 0.036(6) -0.005(5) 0.005(5) 0.010(5) C21 0.044(7) 0.038(7) 0.020(5) 0.008(5) -0.001(5) 0.003(5) C22 0.040(7) 0.047(7) 0.012(5) -0.001(5) 0.007(5) -0.008(5) C23 0.046(7) 0.025(6) 0.021(5) 0.000(5) -0.009(5) -0.008(4) C24 0.036(6) 0.034(7) 0.039(7) -0.012(5) 0.004(5) -0.007(5) C25 0.053(8) 0.038(7) 0.035(7) 0.010(6) 0.013(6) -0.004(5) C26 0.058(8) 0.042(7) 0.038(7) 0.008(6) 0.010(6) -0.013(6) C27 0.030(6) 0.056(8) 0.027(6) 0.009(6) 0.005(5) -0.012(5) C28 0.045(8) 0.071(10) 0.045(8) 0.000(7) 0.027(6) 0.001(7) C29 0.043(7) 0.084(10) 0.032(7) 0.020(7) 0.015(6) -0.012(6) C30 0.026(6) 0.074(9) 0.045(8) 0.018(6) 0.006(5) -0.008(7) C31 0.043(7) 0.030(6) 0.019(5) -0.003(5) -0.005(5) 0.007(4) C32 0.042(7) 0.023(6) 0.034(6) -0.001(5) 0.006(5) 0.004(5) C33 0.044(7) 0.041(7) 0.032(6) -0.027(6) 0.012(5) 0.002(5) C34 0.057(9) 0.060(9) 0.061(9) -0.046(7) 0.010(7) 0.001(7) C35 0.085(11) 0.045(8) 0.049(8) -0.035(8) 0.019(8) 0.004(6) C36 0.049(8) 0.059(8) 0.038(7) -0.031(7) 0.015(6) 0.003(6) C37 0.060(8) 0.021(6) 0.023(6) -0.011(5) 0.007(5) -0.010(4) C38 0.105(12) 0.030(7) 0.031(7) -0.023(7) 0.022(7) -0.014(5) C39 0.069(9) 0.053(8) 0.012(5) -0.011(7) -0.008(5) 0.015(5) C40 0.052(8) 0.036(7) 0.037(7) -0.013(6) 0.021(6) -0.009(5) Re3 0.0214(4) 0.0241(4) 0.0293(3) -0.0007(2) 0.0063(2) -0.0101(3) C41 0.018(6) 0.058(8) 0.026(5) 0.001(5) 0.016(4) -0.009(5) C60 0.073(12) 0.043(8) 0.069(9) 0.009(8) 0.025(8) 0.012(6) C59 0.069(11) 0.060(13) 0.066(10) 0.003(9) 0.025(8) 0.017(9) C58 0.065(8) 0.059(10) 0.078(11) 0.020(6) 0.021(7) 0.033(8) C57 0.059(9) 0.037(6) 0.062(10) 0.015(5) 0.020(7) 0.018(5) C42 0.036(7) 0.030(7) 0.030(5) -0.005(5) 0.013(4) -0.010(4) C51 0.026(6) 0.057(8) 0.030(7) 0.003(5) 0.002(5) -0.009(6) C50 0.036(7) 0.033(7) 0.086(13) 0.000(6) -0.003(7) -0.009(7) C49 0.049(9) 0.037(8) 0.069(7) 0.002(6) 0.017(6) -0.008(6) C48 0.044(8) 0.041(7) 0.068(8) 0.001(6) -0.005(7) -0.020(6) C46 0.130(13) 0.036(7) 0.065(12) 0.009(8) 0.033(10) 0.001(6) C45 0.094(14) 0.044(10) 0.040(6) -0.001(9) 0.019(6) -0.001(6) C44 0.089(8) 0.078(11) 0.061(10) -0.017(7) 0.025(6) -0.012(9) C52 0.028(7) 0.055(8) 0.034(6) 0.008(5) 0.002(5) 0.003(5) C53 0.042(6) 0.048(7) 0.055(7) -0.003(5) 0.017(5) -0.001(5) C54 0.041(7) 0.085(12) 0.066(9) 0.004(7) 0.017(6) -0.020(8) C55 0.060(12) 0.043(10) 0.050(8) 0.002(8) 0.025(7) 0.013(6) C56 0.081(12) 0.058(7) 0.106(13) -0.003(7) 0.025(10) 0.009(7) Cl3 0.066(3) 0.058(2) 0.060(3) 0.017(2) 0.006(2) 0.001(2) Re3A 0.0214(4) 0.0241(4) 0.0293(3) -0.0007(2) 0.0063(2) -0.0101(3) C41A 0.018(6) 0.058(8) 0.026(5) 0.001(5) 0.016(4) -0.009(5) C42A 0.019(8) 0.015(16) 0.034(7) 0.000(7) 0.009(5) -0.007(8) C51A 0.026(6) 0.057(8) 0.030(7) 0.003(5) 0.002(5) -0.009(6) C50A 0.039(11) 0.032(13) 0.039(19) 0.006(10) 0.002(11) -0.011(12) C49A 0.030(14) 0.026(8) 0.036(14) 0.003(8) 0.002(11) -0.011(8) C48A 0.046(16) 0.023(16) 0.044(9) 0.003(12) 0.006(7) -0.010(8) C46A 0.071(11) 0.039(14) 0.044(16) 0.000(10) 0.013(9) 0.000(11) C45A 0.06(2) 0.023(18) 0.037(8) -0.011(14) 0.013(10) -0.003(8) C44A 0.063(13) 0.027(12) 0.045(13) 0.002(10) 0.015(10) -0.010(10) C52A 0.017(17) 0.054(10) 0.030(8) 0.000(9) 0.005(8) -0.003(6) C53A 0.033(8) 0.041(13) 0.041(13) 0.010(7) 0.011(8) 0.006(10) C54A 0.037(11) 0.041(18) 0.053(19) 0.007(11) 0.005(11) 0.009(14) C55A 0.030(18) 0.04(2) 0.041(13) 0.007(15) 0.011(9) 0.006(11) C56A 0.050(16) 0.041(13) 0.037(19) 0.006(9) 0.008(13) 0.007(11) C58A 0.031(14) 0.037(13) 0.027(18) 0.013(9) 0.004(12) 0.005(11) C57A 0.033(13) 0.039(7) 0.025(13) 0.013(6) 0.006(10) 0.007(6) C59A 0.030(18) 0.032(15) 0.026(14) 0.018(11) 0.006(12) 0.007(10) C60A 0.029(16) 0.026(14) 0.025(14) 0.020(10) 0.005(11) 0.009(9) Cl3A 0.070(11) 0.078(11) 0.115(11) 0.001(8) 0.012(9) -0.012(9) Cl4 0.066(3) 0.058(2) 0.060(3) 0.017(2) 0.006(2) 0.001(2) N6 0.066(3) 0.058(2) 0.060(3) 0.017(2) 0.006(2) 0.001(2) N6A 0.070(11) 0.078(11) 0.115(11) 0.001(8) 0.012(9) -0.012(9) Cl4A 0.070(11) 0.078(11) 0.115(11) 0.001(8) 0.012(9) -0.012(9) P5 0.0407(16) 0.0278(15) 0.0282(15) 0.0092(12) 0.0071(12) -0.0058(12) P6 0.0336(16) 0.0381(16) 0.0300(15) 0.0138(13) 0.0087(12) 0.0074(12) C43 0.073(6) 0.032(5) 0.038(5) -0.006(4) 0.013(4) -0.005(4) C47 0.037(4) 0.029(5) 0.055(5) -0.001(3) 0.008(4) -0.009(4) C61 0.13(2) 0.12(2) 0.046(16) 0.087(17) -0.039(14) 0.001(14) C62 0.14(2) 0.12(2) 0.046(16) 0.083(17) -0.035(14) -0.007(13) C63 0.15(2) 0.16(2) 0.046(17) 0.065(18) -0.038(14) -0.013(16) C64 0.17(3) 0.18(2) 0.05(2) 0.05(2) -0.043(16) 0.004(16) C65 0.18(3) 0.16(3) 0.06(2) 0.05(2) -0.037(18) -0.01(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 N3 . 1.861(8) ? Re1 N1 . 1.937(7) ? Re1 P2 . 2.405(3) ? Re1 P1 . 2.406(3) ? Re1 Cl1 . 2.463(3) ? Re2 N4 . 1.886(8) ? Re2 N2 . 1.949(8) ? Re2 P4 . 2.406(3) ? Re2 P3 . 2.409(3) ? Re2 Cl2 . 2.455(3) ? P1 C2 . 1.851(11) ? P1 C3 . 1.888(11) ? P1 C7 . 1.895(10) ? P2 C12 . 1.831(10) ? P2 C17 . 1.892(10) ? P2 C13 . 1.915(10) ? P3 C22 . 1.845(11) ? P3 C23 . 1.878(11) ? P3 C27 . 1.898(11) ? P4 C32 . 1.817(11) ? P4 C37 . 1.871(10) ? P4 C33 . 1.910(10) ? N1 C1 . 1.469(12) ? N1 C11 . 1.486(11) ? N2 C21 . 1.469(12) ? N2 C31 . 1.482(13) ? N3 N4 . 1.202(10) ? N5 C51A . 1.432(18) ? N5 C41 . 1.441(12) ? N5 C51 . 1.449(12) ? N5 C41A . 1.451(18) ? N5 Re3A . 2.041(9) ? N5 Re3 . 2.106(9) ? C1 C2 . 1.516(14) ? C3 C6 . 1.546(16) ? C3 C4 . 1.547(15) ? C3 C5 . 1.551(15) ? C7 C9 . 1.531(14) ? C7 C10 . 1.537(13) ? C7 C8 . 1.546(14) ? C11 C12 . 1.496(14) ? C13 C16 . 1.525(14) ? C13 C15 . 1.538(14) ? C13 C14 . 1.542(14) ? C17 C20 . 1.525(13) ? C17 C18 . 1.526(14) ? C17 C19 . 1.541(15) ? C21 C22 . 1.513(14) ? C23 C24 . 1.525(15) ? C23 C26 . 1.530(14) ? C23 C25 . 1.536(15) ? C27 C30 . 1.520(16) ? C27 C28 . 1.547(17) ? C27 C29 . 1.549(15) ? C31 C32 . 1.507(14) ? C33 C34 . 1.523(17) ? C33 C35 . 1.526(17) ? C33 C36 . 1.531(16) ? C37 C39 . 1.518(16) ? C37 C40 . 1.529(15) ? C37 C38 . 1.539(15) ? Re3 Cl3 . 2.374(5) ? Re3 P6 . 2.434(3) ? Re3 P5 . 2.449(3) ? C41 C42 . 1.493(14) ? C60 C57 . 1.52(3) ? C59 C57 . 1.51(4) ? C58 C57 . 1.51(3) ? C57 P6 . 1.875(12) ? C42 P5 . 1.854(10) ? C51 C52 . 1.499(14) ? C50 C47 . 1.49(2) ? C49 C47 . 1.57(2) ? C48 C47 . 1.490(18) ? C46 C43 . 1.519(14) ? C45 C43 . 1.510(13) ? C44 C43 . 1.554(14) ? C52 P6 . 1.857(11) ? C53 C55 . 1.517(14) ? C53 C56 . 1.521(15) ? C53 C54 . 1.524(14) ? C53 P6 . 1.88(2) ? Re3A Cl3A . 2.351(14) ? Re3A P5 . 2.401(4) ? Re3A P6 . 2.426(4) ? C41A C42A . 1.50(2) ? C42A P5 . 1.859(17) ? C51A C52A . 1.50(2) ? C50A C47 . 1.65(6) ? C49A C47 . 1.49(5) ? C48A C47 . 1.78(6) ? C46A C43 . 1.537(18) ? C45A C43 . 1.514(18) ? C44A C43 . 1.524(18) ? C52A P6 . 1.862(17) ? C53A C56A . 1.518(18) ? C53A C55A . 1.520(18) ? C53A C54A . 1.524(18) ? C53A P6 . 1.91(8) ? C58A C57A . 1.56(10) ? C57A C59A . 1.50(12) ? C57A C60A . 1.67(9) ? C57A P6 . 1.868(17) ? P5 C47 . 1.864(12) ? P5 C43 . 1.868(12) ? C61 C62 . 1.462(14) ? C62 C63 . 1.435(18) ? C63 C64 . 1.469(19) ? C64 C65 . 1.43(2) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 Re1 N1 . . 118.0(3) ? N3 Re1 P2 . . 101.5(2) ? N1 Re1 P2 . . 80.8(2) ? N3 Re1 P1 . . 99.3(2) ? N1 Re1 P1 . . 81.6(2) ? P2 Re1 P1 . . 157.38(9) ? N3 Re1 Cl1 . . 95.5(2) ? N1 Re1 Cl1 . . 146.3(2) ? P2 Re1 Cl1 . . 89.39(9) ? P1 Re1 Cl1 . . 97.45(9) ? N4 Re2 N2 . . 119.3(3) ? N4 Re2 P4 . . 102.8(2) ? N2 Re2 P4 . . 80.5(2) ? N4 Re2 P3 . . 99.3(2) ? N2 Re2 P3 . . 81.3(2) ? P4 Re2 P3 . . 156.28(9) ? N4 Re2 Cl2 . . 94.0(2) ? N2 Re2 Cl2 . . 146.6(3) ? P4 Re2 Cl2 . . 90.23(10) ? P3 Re2 Cl2 . . 96.76(9) ? C2 P1 C3 . . 101.2(5) ? C2 P1 C7 . . 103.0(5) ? C3 P1 C7 . . 111.2(5) ? C2 P1 Re1 . . 100.8(3) ? C3 P1 Re1 . . 119.1(4) ? C7 P1 Re1 . . 117.7(3) ? C12 P2 C17 . . 105.2(5) ? C12 P2 C13 . . 103.9(5) ? C17 P2 C13 . . 110.8(4) ? C12 P2 Re1 . . 98.0(3) ? C17 P2 Re1 . . 123.8(3) ? C13 P2 Re1 . . 112.0(3) ? C22 P3 C23 . . 102.9(5) ? C22 P3 C27 . . 101.8(5) ? C23 P3 C27 . . 110.9(5) ? C22 P3 Re2 . . 100.5(3) ? C23 P3 Re2 . . 118.4(3) ? C27 P3 Re2 . . 118.6(4) ? C32 P4 C37 . . 104.1(5) ? C32 P4 C33 . . 104.6(5) ? C37 P4 C33 . . 109.7(5) ? C32 P4 Re2 . . 99.5(4) ? C37 P4 Re2 . . 123.7(3) ? C33 P4 Re2 . . 112.6(4) ? C1 N1 C11 . . 107.3(7) ? C1 N1 Re1 . . 126.9(6) ? C11 N1 Re1 . . 125.3(6) ? C21 N2 C31 . . 107.1(8) ? C21 N2 Re2 . . 126.9(6) ? C31 N2 Re2 . . 125.6(6) ? N4 N3 Re1 . . 167.9(7) ? N3 N4 Re2 . . 168.4(7) ? C41 N5 C51 . . 113.5(9) ? C51A N5 C41A . . 115.(3) ? C51A N5 Re3A . . 119.(2) ? C41A N5 Re3A . . 109.(2) ? C41 N5 Re3 . . 120.1(7) ? C51 N5 Re3 . . 118.1(8) ? N1 C1 C2 . . 113.2(8) ? C1 C2 P1 . . 109.4(7) ? C6 C3 C4 . . 107.7(10) ? C6 C3 C5 . . 108.8(9) ? C4 C3 C5 . . 108.4(9) ? C6 C3 P1 . . 109.3(8) ? C4 C3 P1 . . 106.9(7) ? C5 C3 P1 . . 115.5(8) ? C9 C7 C10 . . 108.6(8) ? C9 C7 C8 . . 109.6(8) ? C10 C7 C8 . . 108.3(9) ? C9 C7 P1 . . 110.1(7) ? C10 C7 P1 . . 115.1(7) ? C8 C7 P1 . . 105.0(6) ? N1 C11 C12 . . 113.7(8) ? C11 C12 P2 . . 109.0(7) ? C16 C13 C15 . . 107.6(9) ? C16 C13 C14 . . 107.6(8) ? C15 C13 C14 . . 109.7(8) ? C16 C13 P2 . . 108.0(6) ? C15 C13 P2 . . 111.3(7) ? C14 C13 P2 . . 112.4(7) ? C20 C17 C18 . . 107.8(9) ? C20 C17 C19 . . 107.0(9) ? C18 C17 C19 . . 111.4(9) ? C20 C17 P2 . . 107.2(7) ? C18 C17 P2 . . 113.4(7) ? C19 C17 P2 . . 109.7(7) ? N2 C21 C22 . . 111.7(8) ? C21 C22 P3 . . 110.4(7) ? C24 C23 C26 . . 108.2(9) ? C24 C23 C25 . . 107.9(9) ? C26 C23 C25 . . 108.8(9) ? C24 C23 P3 . . 105.7(7) ? C26 C23 P3 . . 114.7(8) ? C25 C23 P3 . . 111.1(7) ? C30 C27 C28 . . 110.5(10) ? C30 C27 C29 . . 109.9(10) ? C28 C27 C29 . . 107.8(10) ? C30 C27 P3 . . 108.9(8) ? C28 C27 P3 . . 106.4(8) ? C29 C27 P3 . . 113.4(8) ? N2 C31 C32 . . 114.1(8) ? C31 C32 P4 . . 108.7(8) ? C34 C33 C35 . . 110.7(10) ? C34 C33 C36 . . 107.1(11) ? C35 C33 C36 . . 108.4(10) ? C34 C33 P4 . . 110.9(8) ? C35 C33 P4 . . 112.6(9) ? C36 C33 P4 . . 106.9(7) ? C39 C37 C40 . . 106.4(9) ? C39 C37 C38 . . 111.0(10) ? C40 C37 C38 . . 107.6(10) ? C39 C37 P4 . . 110.5(8) ? C40 C37 P4 . . 107.8(7) ? C38 C37 P4 . . 113.2(8) ? N5 Re3 Cl3 . . 151.0(3) ? N5 Re3 P6 . . 80.3(2) ? Cl3 Re3 P6 . . 94.13(13) ? N5 Re3 P5 . . 79.9(2) ? Cl3 Re3 P5 . . 96.01(12) ? P6 Re3 P5 . . 155.26(10) ? N5 C41 C42 . . 112.5(10) ? C59 C57 C58 . . 109.6(19) ? C59 C57 C60 . . 108.(2) ? C58 C57 C60 . . 111.(2) ? C59 C57 P6 . . 107.7(16) ? C58 C57 P6 . . 113.5(15) ? C60 C57 P6 . . 107.1(13) ? C41 C42 P5 . . 110.7(9) ? N5 C51 C52 . . 115.9(11) ? C51 C52 P6 . . 108.8(9) ? C55 C53 C56 . . 107.2(16) ? C55 C53 C54 . . 105.7(17) ? C56 C53 C54 . . 109.5(16) ? C55 C53 P6 . . 111.8(14) ? C56 C53 P6 . . 106.5(13) ? C54 C53 P6 . . 115.8(13) ? N5 Re3A Cl3A . . 148.2(7) ? N5 Re3A P5 . . 82.3(3) ? Cl3A Re3A P5 . . 91.4(6) ? N5 Re3A P6 . . 81.8(3) ? Cl3A Re3A P6 . . 98.1(6) ? P5 Re3A P6 . . 162.38(17) ? N5 C41A C42A . . 120.(3) ? C41A C42A P5 . . 98.(3) ? N5 C51A C52A . . 102.(3) ? C51A C52A P6 . . 111.(3) ? C56A C53A C55A . . 111.(6) ? C56A C53A C54A . . 105.(5) ? C55A C53A C54A . . 117.(6) ? C56A C53A P6 . . 102.(4) ? C55A C53A P6 . . 106.(5) ? C54A C53A P6 . . 115.(5) ? C59A C57A C58A . . 99.(4) ? C59A C57A C60A . . 102.(6) ? C58A C57A C60A . . 96.(5) ? C59A C57A P6 . . 122.(6) ? C58A C57A P6 . . 122.(5) ? C60A C57A P6 . . 111.(4) ? C42 P5 C47 . . 108.1(6) ? C42A P5 C47 . . 91.0(14) ? C42 P5 C43 . . 101.7(5) ? C42A P5 C43 . . 116.3(18) ? C47 P5 C43 . . 110.1(6) ? C42A P5 Re3A . . 102.8(14) ? C47 P5 Re3A . . 128.1(4) ? C43 P5 Re3A . . 107.7(4) ? C42 P5 Re3 . . 100.8(4) ? C47 P5 Re3 . . 114.9(4) ? C43 P5 Re3 . . 119.3(4) ? C52A P6 C57A . . 101.(4) ? C52 P6 C57 . . 105.6(10) ? C52 P6 C53 . . 99.6(7) ? C57 P6 C53 . . 110.6(11) ? C52A P6 C53A . . 119.(2) ? C57A P6 C53A . . 107.(4) ? C52A P6 Re3A . . 93.9(16) ? C57A P6 Re3A . . 122.(3) ? C53A P6 Re3A . . 114.6(15) ? C52 P6 Re3 . . 102.5(4) ? C57 P6 Re3 . . 117.9(8) ? C53 P6 Re3 . . 117.6(5) ? C45 C43 C46 . . 113.1(15) ? C45A C43 C44A . . 117.(4) ? C45A C43 C46A . . 100.(5) ? C44A C43 C46A . . 103.(4) ? C45 C43 C44 . . 103.0(13) ? C46 C43 C44 . . 109.3(14) ? C45 C43 P5 . . 110.4(10) ? C45A C43 P5 . . 122.(3) ? C46 C43 P5 . . 115.2(10) ? C44A C43 P5 . . 103.(2) ? C46A C43 P5 . . 110.(3) ? C44 C43 P5 . . 104.7(10) ? C48 C47 C50 . . 114.0(13) ? C48 C47 C49 . . 105.3(12) ? C50 C47 C49 . . 108.3(12) ? C49A C47 C50A . . 100.(3) ? C49A C47 C48A . . 91.(3) ? C50A C47 C48A . . 99.(3) ? C48 C47 P5 . . 108.4(9) ? C49A C47 P5 . . 126.(2) ? C50 C47 P5 . . 115.5(10) ? C49 C47 P5 . . 104.4(9) ? C50A C47 P5 . . 123.(3) ? C48A C47 P5 . . 109.(2) ? C63 C62 C61 . . 118.2(19) ? C62 C63 C64 . . 116.(2) ? C65 C64 C63 . . 116.(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 Re1 N3 N4 . . . . 10.(3) ? P2 Re1 N3 N4 . . . . 96.(3) ? P1 Re1 N3 N4 . . . . -75.(3) ? Cl1 Re1 N3 N4 . . . . -174.(3) ? Re1 N3 N4 Re2 . . . . -140.(3) ? N2 Re2 N4 N3 . . . . 25.(4) ? P4 Re2 N4 N3 . . . . 112.(3) ? P3 Re2 N4 N3 . . . . -60.(3) ? Cl2 Re2 N4 N3 . . . . -157.(3) ? C11 N1 C1 C2 . . . . 161.1(8) ? Re1 N1 C1 C2 . . . . -25.7(12) ? N1 C1 C2 P1 . . . . 31.1(10) ? C3 P1 C2 C1 . . . . -146.8(7) ? C7 P1 C2 C1 . . . . 98.1(7) ? Re1 P1 C2 C1 . . . . -24.0(7) ? C2 P1 C3 C6 . . . . -171.1(8) ? C7 P1 C3 C6 . . . . -62.3(9) ? Re1 P1 C3 C6 . . . . 79.6(8) ? C2 P1 C3 C4 . . . . 72.7(9) ? C7 P1 C3 C4 . . . . -178.5(8) ? Re1 P1 C3 C4 . . . . -36.6(9) ? C2 P1 C3 C5 . . . . -48.0(9) ? C7 P1 C3 C5 . . . . 60.8(10) ? Re1 P1 C3 C5 . . . . -157.3(7) ? C2 P1 C7 C9 . . . . -173.4(7) ? C3 P1 C7 C9 . . . . 78.9(8) ? Re1 P1 C7 C9 . . . . -63.6(8) ? C2 P1 C7 C10 . . . . 63.5(9) ? C3 P1 C7 C10 . . . . -44.2(9) ? Re1 P1 C7 C10 . . . . 173.3(7) ? C2 P1 C7 C8 . . . . -55.5(7) ? C3 P1 C7 C8 . . . . -163.2(7) ? Re1 P1 C7 C8 . . . . 54.3(7) ? C1 N1 C11 C12 . . . . 167.2(8) ? Re1 N1 C11 C12 . . . . -6.1(12) ? N1 C11 C12 P2 . . . . 31.3(10) ? C17 P2 C12 C11 . . . . -165.0(7) ? C13 P2 C12 C11 . . . . 78.5(7) ? Re1 P2 C12 C11 . . . . -36.6(7) ? C12 P2 C17 C20 . . . . 59.3(8) ? C13 P2 C17 C20 . . . . 170.9(7) ? Re1 P2 C17 C20 . . . . -51.5(8) ? C12 P2 C17 C18 . . . . -59.5(8) ? C13 P2 C17 C18 . . . . 52.1(9) ? Re1 P2 C17 C18 . . . . -170.3(6) ? C12 P2 C17 C19 . . . . 175.2(7) ? C13 P2 C17 C19 . . . . -73.2(8) ? Re1 P2 C17 C19 . . . . 64.4(7) ? C31 N2 C21 C22 . . . . 157.0(9) ? Re2 N2 C21 C22 . . . . -29.8(13) ? N2 C21 C22 P3 . . . . 33.1(11) ? C23 P3 C22 C21 . . . . 98.7(8) ? C27 P3 C22 C21 . . . . -146.4(8) ? Re2 P3 C22 C21 . . . . -24.0(8) ? C22 P3 C23 C24 . . . . -55.4(8) ? C27 P3 C23 C24 . . . . -163.6(7) ? Re2 P3 C23 C24 . . . . 54.4(7) ? C22 P3 C23 C26 . . . . 63.8(9) ? C27 P3 C23 C26 . . . . -44.4(9) ? Re2 P3 C23 C26 . . . . 173.6(7) ? C22 P3 C23 C25 . . . . -172.2(8) ? C27 P3 C23 C25 . . . . 79.6(8) ? Re2 P3 C23 C25 . . . . -62.5(8) ? C22 P3 C27 C30 . . . . -168.7(8) ? C23 P3 C27 C30 . . . . -59.8(9) ? Re2 P3 C27 C30 . . . . 82.2(9) ? C22 P3 C27 C28 . . . . 72.2(8) ? C23 P3 C27 C28 . . . . -178.9(7) ? Re2 P3 C27 C28 . . . . -36.8(9) ? C22 P3 C27 C29 . . . . -46.1(10) ? C23 P3 C27 C29 . . . . 62.8(10) ? Re2 P3 C27 C29 . . . . -155.2(8) ? C21 N2 C31 C32 . . . . 165.3(9) ? Re2 N2 C31 C32 . . . . -8.0(13) ? N2 C31 C32 P4 . . . . 30.5(11) ? C37 P4 C32 C31 . . . . -163.0(7) ? C33 P4 C32 C31 . . . . 81.9(8) ? Re2 P4 C32 C31 . . . . -34.6(8) ? C32 P4 C37 C39 . . . . 173.4(8) ? C33 P4 C37 C39 . . . . -75.1(9) ? Re2 P4 C37 C39 . . . . 61.7(9) ? C32 P4 C37 C40 . . . . 57.6(9) ? C33 P4 C37 C40 . . . . 169.0(8) ? Re2 P4 C37 C40 . . . . -54.2(9) ? C32 P4 C37 C38 . . . . -61.4(10) ? C33 P4 C37 C38 . . . . 50.1(11) ? Re2 P4 C37 C38 . . . . -173.1(8) ? C51 N5 C41 C42 . . . . -166.7(12) ? Re3 N5 C41 C42 . . . . 45.8(15) ? N5 C41 C42 P5 . . . . -41.8(15) ? C41 N5 C51 C52 . . . . 166.2(13) ? Re3 N5 C51 C52 . . . . -45.5(17) ? N5 C51 C52 P6 . . . . 38.1(17) ? C51A N5 C41A C42A . . . . 162.(5) ? Re3A N5 C41A C42A . . . . -61.(5) ? N5 C41A C42A P5 . . . . 57.(5) ? C41A N5 C51A C52A . . . . -170.(4) ? Re3A N5 C51A C52A . . . . 57.(5) ? N5 C51A C52A P6 . . . . -60.(5) ? C41 C42 P5 C47 . . . . -99.3(11) ? C41 C42 P5 C43 . . . . 144.9(10) ? C41 C42 P5 Re3 . . . . 21.7(11) ? C41A C42A P5 C47 . . . . -156.(3) ? C41A C42A P5 C43 . . . . 91.(3) ? C41A C42A P5 Re3A . . . . -26.(3) ? C51 C52 P6 C57 . . . . 107.8(14) ? C51 C52 P6 C53 . . . . -137.5(12) ? C51 C52 P6 Re3 . . . . -16.2(12) ? C51A C52A P6 C57A . . . . 161.(4) ? C51A C52A P6 C53A . . . . -83.(4) ? C51A C52A P6 Re3A . . . . 38.(4) ? C59A C57A P6 C52A . . . . -14.(8) ? C58A C57A P6 C52A . . . . 113.(6) ? C60A C57A P6 C52A . . . . -135.(6) ? C59A C57A P6 C53A . . . . -139.(7) ? C58A C57A P6 C53A . . . . -12.(7) ? C60A C57A P6 C53A . . . . 100.(6) ? C59A C57A P6 Re3A . . . . 87.(7) ? C58A C57A P6 Re3A . . . . -146.(5) ? C60A C57A P6 Re3A . . . . -34.(7) ? C59 C57 P6 C52 . . . . -51.3(19) ? C58 C57 P6 C52 . . . . 70.(2) ? C60 C57 P6 C52 . . . . -166.8(15) ? C59 C57 P6 C53 . . . . -158.2(17) ? C58 C57 P6 C53 . . . . -37.(2) ? C60 C57 P6 C53 . . . . 86.3(17) ? C59 C57 P6 Re3 . . . . 62.4(19) ? C58 C57 P6 Re3 . . . . -176.0(14) ? C60 C57 P6 Re3 . . . . -53.(2) ? C55 C53 P6 C52 . . . . -168.5(12) ? C56 C53 P6 C52 . . . . 74.7(13) ? C54 C53 P6 C52 . . . . -47.4(13) ? C55 C53 P6 C57 . . . . -57.7(14) ? C56 C53 P6 C57 . . . . -174.5(14) ? C54 C53 P6 C57 . . . . 63.4(15) ? C55 C53 P6 Re3 . . . . 81.8(12) ? C56 C53 P6 Re3 . . . . -35.0(14) ? C54 C53 P6 Re3 . . . . -157.1(11) ? C42 P5 C43 C45 . . . . 174.1(12) ? C47 P5 C43 C45 . . . . 59.7(12) ? Re3 P5 C43 C45 . . . . -76.3(12) ? C42A P5 C43 C45A . . . . -179.(4) ? C47 P5 C43 C45A . . . . 80.(4) ? Re3A P5 C43 C45A . . . . -64.(4) ? C42 P5 C43 C46 . . . . 44.4(13) ? C47 P5 C43 C46 . . . . -70.0(13) ? Re3 P5 C43 C46 . . . . 154.0(11) ? C42A P5 C43 C44A . . . . -45.(3) ? C47 P5 C43 C44A . . . . -147.(2) ? Re3A P5 C43 C44A . . . . 69.(2) ? C42A P5 C43 C46A . . . . 64.(3) ? C47 P5 C43 C46A . . . . -38.(3) ? Re3A P5 C43 C46A . . . . 178.(3) ? C42 P5 C43 C44 . . . . -75.7(10) ? C47 P5 C43 C44 . . . . 169.9(9) ? Re3 P5 C43 C44 . . . . 33.9(10) ? C42 P5 C47 C48 . . . . 162.1(10) ? C43 P5 C47 C48 . . . . -87.6(11) ? Re3 P5 C47 C48 . . . . 50.4(11) ? C42A P5 C47 C49A . . . . 86.(3) ? C43 P5 C47 C49A . . . . -155.(3) ? Re3A P5 C47 C49A . . . . -21.(3) ? C42 P5 C47 C50 . . . . -68.5(13) ? C43 P5 C47 C50 . . . . 41.7(12) ? Re3 P5 C47 C50 . . . . 179.8(10) ? C42 P5 C47 C49 . . . . 50.2(9) ? C43 P5 C47 C49 . . . . 160.5(8) ? Re3 P5 C47 C49 . . . . -61.4(9) ? C42A P5 C47 C50A . . . . -51.(3) ? C43 P5 C47 C50A . . . . 67.(3) ? Re3A P5 C47 C50A . . . . -158.(3) ? C42A P5 C47 C48A . . . . -167.(3) ? C43 P5 C47 C48A . . . . -48.(2) ? Re3A P5 C47 C48A . . . . 86.(2) ? C61 C62 C63 C64 . . . . -162.(3) ? C62 C63 C64 C65 . . . . -122.(4) ? _shelx_res_file ; CW_FS_040717_a.res created by SHELXL-2014/7 TITL CW_FS_040717_a.res in P2(1)/c CELL 0.71073 12.4165 33.6022 19.7243 90.000 101.313 90.000 ZERR 4.000 0.0008 0.0021 0.0014 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H CL N P RE UNIT 250 552 14 22 24 12 TEMP -173.150 SIZE 0.064 0.085 0.217 L.S. 20 LIST 6 ACTA CONF FMAP 2 EADP Re3 RE3A EADP Cl3 Cl4 N6 EADP Cl3A Cl4A N6A EADP C41 C41A EADP C51 C51A SADI Re3 Cl3 Re3 Cl4 Re3A Cl3A Re3A Cl4A SADI Re3 N6 Re3A N6A SADI Cl3 Cl4 Cl3A Cl4A SADI Cl3 N6 Cl3A N6A SADI P5 C42 P5 C42A P6 C52 P6 C52A P6 C57 P6 C57A SADI N5 C41 N5 C41A N5 C51 N5 C51A SADI C53 C54 C53 C55 C53 C56 C53A C54A C53A C55A C53A C56A SADI C43 C44 C43 C45 C43 C46 C43 C44A C43 C45A C43 C46A SADI C41 C42 C51 C52 C41A C42A C51A C52A SADI C61 C62 C62 C63 C63 C64 C64 C65 DFIX 1.5 C61 C62 DFIX 2.5 C63 C65 DFIX 2.5 C62 C64 DFIX 2.5 C61 C63 RIGU Re3 > C65 PLAN 20 WGHT 0.027400 101.197098 FVAR 0.11478 RE1 6 0.636311 0.623627 0.927490 11.00000 0.01751 0.01834 = 0.02164 -0.00009 0.00478 -0.00031 RE2 6 0.835233 0.694446 0.771341 11.00000 0.01956 0.02540 = 0.01685 -0.00052 0.00277 -0.00245 CL1 3 0.564908 0.566642 0.853673 11.00000 0.03618 0.02674 = 0.03926 -0.00523 0.00514 -0.00397 CL2 3 1.023050 0.683984 0.836091 11.00000 0.01873 0.05416 = 0.03110 0.00041 0.00095 -0.00394 P1 5 0.784894 0.589387 1.001150 11.00000 0.01947 0.02142 = 0.02933 0.00076 0.00437 0.00259 P2 5 0.460641 0.655729 0.895152 11.00000 0.01612 0.02429 = 0.02595 0.00308 0.00343 -0.00086 P3 5 0.838449 0.643460 0.685931 11.00000 0.02497 0.03601 = 0.02062 -0.00547 0.00409 0.00349 P4 5 0.837379 0.761303 0.815283 11.00000 0.03310 0.02619 = 0.02322 -0.00060 0.00538 -0.01099 N1 4 0.633913 0.652165 1.012498 11.00000 0.01906 0.02275 = 0.02136 -0.00035 0.00531 0.00506 N2 4 0.741726 0.720238 0.692687 11.00000 0.04388 0.01162 = 0.02416 -0.00469 0.00436 -0.00042 N3 4 0.713290 0.646126 0.865034 11.00000 0.01476 0.02159 = 0.01856 -0.00158 0.00011 -0.00167 N4 4 0.770020 0.665394 0.834523 11.00000 0.01490 0.02444 = 0.02108 -0.00477 -0.00027 0.00535 N5 4 0.544722 0.533709 0.224572 11.00000 0.04049 0.05115 = 0.02083 0.00119 0.00049 0.01642 C1 1 0.713476 0.648735 1.078039 11.00000 0.02399 0.03422 = 0.01635 -0.00119 0.00096 0.00384 AFIX 23 H1A 2 0.674731 0.652782 1.116840 11.00000 -1.20000 H1B 2 0.768959 0.670104 1.080302 11.00000 -1.20000 AFIX 0 C2 1 0.771636 0.608847 1.086943 11.00000 0.02475 0.03913 = 0.03227 0.00392 0.00176 -0.00101 AFIX 23 H2A 2 0.729230 0.589859 1.109771 11.00000 -1.20000 H2B 2 0.845362 0.611978 1.116534 11.00000 -1.20000 AFIX 0 C3 1 0.773332 0.534071 1.014770 11.00000 0.03441 0.02023 = 0.05201 0.01072 0.00435 0.00217 C4 1 0.651689 0.525480 1.017078 11.00000 0.03165 0.03736 = 0.06778 0.02827 0.01154 0.00971 AFIX 137 H4A 2 0.605237 0.532952 0.972814 11.00000 -1.50000 H4B 2 0.630250 0.540992 1.054369 11.00000 -1.50000 H4C 2 0.642530 0.497054 1.025513 11.00000 -1.50000 AFIX 0 C5 1 0.845989 0.517328 1.081679 11.00000 0.04694 0.02704 = 0.06222 0.02087 0.00600 0.00461 AFIX 137 H5A 2 0.825391 0.489644 1.088233 11.00000 -1.50000 H5B 2 0.835118 0.533280 1.121386 11.00000 -1.50000 H5C 2 0.923370 0.518478 1.077699 11.00000 -1.50000 AFIX 0 C6 1 0.800846 0.511641 0.951895 11.00000 0.04415 0.03303 = 0.07139 -0.00909 0.01260 0.00790 AFIX 137 H6A 2 0.776093 0.483974 0.952517 11.00000 -1.50000 H6B 2 0.880388 0.512200 0.954168 11.00000 -1.50000 H6C 2 0.763503 0.524528 0.909135 11.00000 -1.50000 AFIX 0 C7 1 0.930170 0.603836 0.994977 11.00000 0.00876 0.03276 = 0.02854 0.00451 -0.00427 0.00453 C8 1 0.935578 0.649367 1.006499 11.00000 0.02556 0.03359 = 0.02919 -0.01001 0.01137 -0.01022 AFIX 137 H8A 2 1.004889 0.659611 0.996795 11.00000 -1.50000 H8B 2 0.931379 0.655266 1.054569 11.00000 -1.50000 H8C 2 0.873893 0.662080 0.975436 11.00000 -1.50000 AFIX 0 C9 1 0.951257 0.594213 0.922833 11.00000 0.03172 0.03499 = 0.03993 0.01039 0.01002 0.00304 AFIX 137 H9A 2 0.899036 0.608924 0.888076 11.00000 -1.50000 H9B 2 0.941869 0.565585 0.914163 11.00000 -1.50000 H9C 2 1.026364 0.601970 0.920085 11.00000 -1.50000 AFIX 0 C10 1 1.021003 0.584364 1.048989 11.00000 0.02785 0.04940 = 0.04665 0.01534 0.00770 0.00786 AFIX 137 H10A 2 1.023891 0.555802 1.039458 11.00000 -1.50000 H10B 2 1.005124 0.588326 1.095267 11.00000 -1.50000 H10C 2 1.091894 0.596553 1.046671 11.00000 -1.50000 AFIX 0 C11 1 0.558022 0.685302 1.020306 11.00000 0.02971 0.02286 = 0.03497 -0.00865 0.01432 0.00544 AFIX 23 H11A 2 0.601751 0.708253 1.041888 11.00000 -1.20000 H11B 2 0.509717 0.676744 1.051992 11.00000 -1.20000 AFIX 0 C12 1 0.488025 0.698489 0.953501 11.00000 0.02305 0.02610 = 0.03390 0.00131 0.01126 -0.00369 AFIX 23 H12A 2 0.526310 0.719542 0.932259 11.00000 -1.20000 H12B 2 0.417968 0.709556 0.961990 11.00000 -1.20000 AFIX 0 C13 1 0.347189 0.627242 0.927721 11.00000 0.01899 0.02999 = 0.03003 0.00881 0.00814 -0.00096 C14 1 0.270742 0.655018 0.958883 11.00000 0.02356 0.03692 = 0.04970 0.00394 0.00829 0.00301 AFIX 137 H14A 2 0.240489 0.675390 0.924892 11.00000 -1.50000 H14B 2 0.312551 0.667867 1.000425 11.00000 -1.50000 H14C 2 0.210610 0.639446 0.971133 11.00000 -1.50000 AFIX 0 C15 1 0.278813 0.601909 0.869928 11.00000 0.01394 0.04710 = 0.05345 0.00016 0.00342 -0.00600 AFIX 137 H15A 2 0.230455 0.619273 0.837450 11.00000 -1.50000 H15B 2 0.234355 0.582846 0.890143 11.00000 -1.50000 H15C 2 0.328057 0.587466 0.845363 11.00000 -1.50000 AFIX 0 C16 1 0.401715 0.598976 0.984695 11.00000 0.02656 0.02984 = 0.04454 0.00843 0.01227 -0.00745 AFIX 137 H16A 2 0.442443 0.578475 0.964891 11.00000 -1.50000 H16B 2 0.345323 0.586341 1.005902 11.00000 -1.50000 H16C 2 0.452425 0.613946 1.019913 11.00000 -1.50000 AFIX 0 C17 1 0.406997 0.677735 0.806683 11.00000 0.01343 0.03238 = 0.03203 0.01217 -0.00053 -0.00330 C18 1 0.302797 0.702374 0.803124 11.00000 0.03123 0.04806 = 0.04015 0.02007 0.00927 0.00703 AFIX 137 H18A 2 0.285507 0.716213 0.758576 11.00000 -1.50000 H18B 2 0.314247 0.721943 0.840693 11.00000 -1.50000 H18C 2 0.241720 0.684788 0.807816 11.00000 -1.50000 AFIX 0 C19 1 0.390333 0.644439 0.751911 11.00000 0.02869 0.05612 = 0.03221 -0.00353 0.00763 -0.00571 AFIX 137 H19A 2 0.384494 0.656171 0.705845 11.00000 -1.50000 H19B 2 0.322834 0.629784 0.754030 11.00000 -1.50000 H19C 2 0.453070 0.626185 0.761021 11.00000 -1.50000 AFIX 0 C20 1 0.496095 0.705225 0.790100 11.00000 0.03018 0.03755 = 0.03569 0.00965 0.00471 -0.00460 AFIX 137 H20A 2 0.564824 0.690324 0.793649 11.00000 -1.50000 H20B 2 0.507258 0.727416 0.822973 11.00000 -1.50000 H20C 2 0.473455 0.715599 0.743021 11.00000 -1.50000 AFIX 0 C21 1 0.695055 0.702106 0.625595 11.00000 0.04368 0.03844 = 0.01979 0.00292 -0.00053 0.00772 AFIX 23 H21A 2 0.685539 0.722843 0.589255 11.00000 -1.20000 H21B 2 0.621730 0.691012 0.627191 11.00000 -1.20000 AFIX 0 C22 1 0.767869 0.669355 0.607189 11.00000 0.04045 0.04744 = 0.01223 -0.00784 0.00716 -0.00125 AFIX 23 H22A 2 0.822975 0.680879 0.582742 11.00000 -1.20000 H22B 2 0.722810 0.650082 0.575787 11.00000 -1.20000 AFIX 0 C23 1 0.751697 0.597868 0.688056 11.00000 0.04627 0.02503 = 0.02100 -0.00842 -0.00871 -0.00010 C24 1 0.635308 0.613035 0.685904 11.00000 0.03568 0.03431 = 0.03931 -0.00727 0.00429 -0.01159 AFIX 137 H24A 2 0.603246 0.621782 0.638876 11.00000 -1.50000 H24B 2 0.637441 0.635468 0.717891 11.00000 -1.50000 H24C 2 0.590448 0.591602 0.699561 11.00000 -1.50000 AFIX 0 C25 1 0.787984 0.574752 0.755880 11.00000 0.05283 0.03789 = 0.03547 -0.00383 0.01280 0.00951 AFIX 137 H25A 2 0.748998 0.549260 0.752939 11.00000 -1.50000 H25B 2 0.770824 0.590348 0.794387 11.00000 -1.50000 H25C 2 0.867282 0.569900 0.763586 11.00000 -1.50000 AFIX 0 C26 1 0.749027 0.569307 0.627327 11.00000 0.05769 0.04208 = 0.03762 -0.01327 0.00986 0.00789 AFIX 137 H26A 2 0.740367 0.584539 0.584226 11.00000 -1.50000 H26B 2 0.687170 0.550883 0.624743 11.00000 -1.50000 H26C 2 0.817833 0.554206 0.634116 11.00000 -1.50000 AFIX 0 C27 1 0.974960 0.630114 0.662265 11.00000 0.02981 0.05589 = 0.02747 -0.01200 0.00550 0.00937 C28 1 1.040013 0.669452 0.663531 11.00000 0.04455 0.07116 = 0.04530 0.00065 0.02653 -0.00047 AFIX 137 H28A 2 1.110641 0.664185 0.650176 11.00000 -1.50000 H28B 2 1.052864 0.680714 0.710258 11.00000 -1.50000 H28C 2 0.997751 0.688382 0.630961 11.00000 -1.50000 AFIX 0 C29 1 0.963094 0.611953 0.588998 11.00000 0.04251 0.08370 = 0.03161 -0.01216 0.01538 0.01968 AFIX 137 H29A 2 0.917631 0.629472 0.555272 11.00000 -1.50000 H29B 2 0.928245 0.585736 0.588021 11.00000 -1.50000 H29C 2 1.035900 0.609159 0.577342 11.00000 -1.50000 AFIX 0 C30 1 1.035432 0.601209 0.715757 11.00000 0.02558 0.07380 = 0.04548 -0.00850 0.00557 0.01811 AFIX 137 H30A 2 0.994739 0.576082 0.713030 11.00000 -1.50000 H30B 2 1.041461 0.612646 0.762055 11.00000 -1.50000 H30C 2 1.109090 0.596259 0.706682 11.00000 -1.50000 AFIX 0 C31 1 0.693596 0.760578 0.692892 11.00000 0.04251 0.03023 = 0.01858 0.00743 -0.00502 -0.00284 AFIX 23 H31A 2 0.613904 0.758941 0.673478 11.00000 -1.20000 H31B 2 0.727001 0.777984 0.662165 11.00000 -1.20000 AFIX 0 C32 1 0.709581 0.779483 0.763448 11.00000 0.04249 0.02313 = 0.03411 0.00368 0.00600 -0.00085 AFIX 23 H32A 2 0.647399 0.772582 0.785897 11.00000 -1.20000 H32B 2 0.712376 0.808803 0.759172 11.00000 -1.20000 AFIX 0 C33 1 0.948662 0.793413 0.788217 11.00000 0.04361 0.04075 = 0.03175 0.00205 0.01239 -0.02656 C34 1 1.052909 0.793265 0.843728 11.00000 0.05745 0.06021 = 0.06070 0.00149 0.01045 -0.04595 AFIX 137 H34A 2 1.115168 0.801803 0.823485 11.00000 -1.50000 H34B 2 1.066473 0.766322 0.862480 11.00000 -1.50000 H34C 2 1.044184 0.811575 0.880946 11.00000 -1.50000 AFIX 0 C35 1 0.910390 0.835939 0.770156 11.00000 0.08532 0.04508 = 0.04932 0.00397 0.01929 -0.03458 AFIX 137 H35A 2 0.971315 0.851490 0.758907 11.00000 -1.50000 H35B 2 0.885895 0.848029 0.809742 11.00000 -1.50000 H35C 2 0.849379 0.835609 0.730218 11.00000 -1.50000 AFIX 0 C36 1 0.977192 0.774048 0.723718 11.00000 0.04927 0.05877 = 0.03846 0.00346 0.01510 -0.03145 AFIX 137 H36A 2 0.910665 0.771852 0.687786 11.00000 -1.50000 H36B 2 1.007660 0.747458 0.735419 11.00000 -1.50000 H36C 2 1.031513 0.790439 0.706666 11.00000 -1.50000 AFIX 0 C37 1 0.826064 0.773682 0.906131 11.00000 0.06039 0.02108 = 0.02343 -0.00963 0.00688 -0.01123 C38 1 0.815742 0.818613 0.918549 11.00000 0.10479 0.03027 = 0.03117 -0.01430 0.02223 -0.02293 AFIX 137 H38A 2 0.886475 0.831566 0.918605 11.00000 -1.50000 H38B 2 0.794469 0.822908 0.963278 11.00000 -1.50000 H38C 2 0.759710 0.829978 0.881672 11.00000 -1.50000 AFIX 0 C39 1 0.921782 0.755985 0.957008 11.00000 0.06878 0.05290 = 0.01246 0.01493 -0.00752 -0.01054 AFIX 137 H39A 2 0.932942 0.728323 0.944229 11.00000 -1.50000 H39B 2 0.905767 0.756803 1.003702 11.00000 -1.50000 H39C 2 0.988418 0.771405 0.955932 11.00000 -1.50000 AFIX 0 C40 1 0.722362 0.753652 0.920669 11.00000 0.05215 0.03645 = 0.03695 -0.00940 0.02094 -0.01322 AFIX 137 H40A 2 0.657565 0.765523 0.891225 11.00000 -1.50000 H40B 2 0.718294 0.757470 0.969360 11.00000 -1.50000 H40C 2 0.724762 0.725125 0.910739 11.00000 -1.50000 AFIX 0 PART 1 10.8 RE3 6 0.568447 0.567820 0.315890 10.80000 0.02138 0.02412 = 0.02931 -0.01013 0.00628 -0.00072 C41 1 0.632876 0.509601 0.209177 10.80000 0.01841 0.05844 = 0.02614 -0.00920 0.01559 0.00070 AFIX 23 H41A 2 0.687247 0.527039 0.193301 10.80000 -1.20000 H41B 2 0.603111 0.491128 0.170986 10.80000 -1.20000 AFIX 0 C60 1 0.423949 0.670301 0.302187 10.80000 0.07251 0.04342 = 0.06897 0.01202 0.02508 0.00900 AFIX 137 H60A 2 0.500098 0.662210 0.319910 10.80000 -1.50000 H60B 2 0.379397 0.664534 0.336883 10.80000 -1.50000 H60C 2 0.421488 0.698902 0.292281 10.80000 -1.50000 AFIX 0 C59 1 0.453338 0.655690 0.185784 10.80000 0.06909 0.06004 = 0.06595 0.01703 0.02455 0.00324 AFIX 137 H59A 2 0.425709 0.641523 0.142431 10.80000 -1.50000 H59B 2 0.527844 0.646503 0.205405 10.80000 -1.50000 H59C 2 0.454652 0.684342 0.176707 10.80000 -1.50000 AFIX 0 C58 1 0.263036 0.660684 0.205562 10.80000 0.06481 0.05915 = 0.07761 0.03278 0.02103 0.02015 AFIX 137 H58A 2 0.261760 0.672882 0.160281 10.80000 -1.50000 H58B 2 0.238398 0.680132 0.236278 10.80000 -1.50000 H58C 2 0.213969 0.637568 0.200132 10.80000 -1.50000 AFIX 0 C57 1 0.378902 0.647505 0.236460 10.80000 0.05867 0.03718 = 0.06187 0.01795 0.02017 0.01504 C42 1 0.689190 0.486100 0.270141 10.80000 0.03648 0.03037 = 0.02974 -0.01035 0.01300 -0.00450 AFIX 23 H42A 2 0.761371 0.476839 0.262170 10.80000 -1.20000 H42B 2 0.644526 0.462389 0.275912 10.80000 -1.20000 AFIX 0 C51 1 0.473258 0.549552 0.163548 10.80000 0.02585 0.05724 = 0.03034 -0.00894 0.00182 0.00327 AFIX 23 H51A 2 0.457162 0.528014 0.128784 10.80000 -1.20000 H51B 2 0.513639 0.570610 0.143817 10.80000 -1.20000 AFIX 0 C50 1 0.940019 0.504609 0.388549 10.80000 0.03647 0.03347 = 0.08569 -0.00862 -0.00251 -0.00046 AFIX 137 H50A 2 0.934262 0.484381 0.352222 10.80000 -1.50000 H50B 2 0.930071 0.492049 0.431740 10.80000 -1.50000 H50C 2 1.012614 0.517150 0.395474 10.80000 -1.50000 AFIX 0 C49 1 0.868917 0.554029 0.296831 10.80000 0.04922 0.03721 = 0.06866 -0.00844 0.01718 0.00194 AFIX 137 H49A 2 0.864285 0.532952 0.262038 10.80000 -1.50000 H49B 2 0.940966 0.566932 0.302992 10.80000 -1.50000 H49C 2 0.811194 0.573768 0.281442 10.80000 -1.50000 AFIX 0 C48 1 0.860519 0.569650 0.416339 10.80000 0.04409 0.04063 = 0.06843 -0.01988 -0.00535 0.00125 AFIX 137 H48A 2 0.796805 0.587079 0.402121 10.80000 -1.50000 H48B 2 0.928016 0.584668 0.415835 10.80000 -1.50000 H48C 2 0.861450 0.559691 0.463148 10.80000 -1.50000 AFIX 0 C46 1 0.748992 0.439591 0.411680 10.80000 0.13035 0.03632 = 0.06509 0.00069 0.03321 0.00900 AFIX 137 H46A 2 0.734345 0.430308 0.363646 10.80000 -1.50000 H46B 2 0.721951 0.419863 0.440905 10.80000 -1.50000 H46C 2 0.828247 0.443190 0.427602 10.80000 -1.50000 AFIX 0 C45 1 0.715709 0.497099 0.487591 10.80000 0.09375 0.04426 = 0.04047 -0.00053 0.01916 -0.00149 AFIX 137 H45A 2 0.795437 0.498970 0.503470 10.80000 -1.50000 H45B 2 0.684511 0.480327 0.519535 10.80000 -1.50000 H45C 2 0.683353 0.523762 0.486121 10.80000 -1.50000 AFIX 0 C44 1 0.564776 0.471757 0.403803 10.80000 0.08937 0.07786 = 0.06119 -0.01231 0.02473 -0.01728 AFIX 137 H44A 2 0.538536 0.462774 0.356156 10.80000 -1.50000 H44B 2 0.527588 0.496591 0.411533 10.80000 -1.50000 H44C 2 0.548765 0.451361 0.435936 10.80000 -1.50000 AFIX 0 C52 1 0.366344 0.566592 0.174429 10.80000 0.02806 0.05513 = 0.03389 0.00286 0.00237 0.00841 AFIX 23 H52A 2 0.312164 0.544982 0.174477 10.80000 -1.20000 H52B 2 0.336810 0.585260 0.136497 10.80000 -1.20000 AFIX 0 C53 1 0.266143 0.576054 0.291880 10.80000 0.04227 0.04769 = 0.05513 -0.00104 0.01737 -0.00306 C54 1 0.156953 0.578600 0.240867 10.80000 0.04134 0.08522 = 0.06648 -0.02011 0.01740 0.00358 AFIX 137 H54A 2 0.150243 0.604778 0.218532 10.80000 -1.50000 H54B 2 0.096503 0.574842 0.265578 10.80000 -1.50000 H54C 2 0.153900 0.557815 0.205686 10.80000 -1.50000 AFIX 0 C55 1 0.250400 0.599663 0.354751 10.80000 0.05956 0.04283 = 0.05045 0.01318 0.02459 0.00184 AFIX 137 H55A 2 0.225744 0.626643 0.340552 10.80000 -1.50000 H55B 2 0.320181 0.601038 0.388021 10.80000 -1.50000 H55C 2 0.195104 0.586562 0.376303 10.80000 -1.50000 AFIX 0 C56 1 0.288080 0.533108 0.314893 10.80000 0.08126 0.05752 = 0.10554 0.00854 0.02515 -0.00287 AFIX 137 H56A 2 0.223091 0.522193 0.329528 10.80000 -1.50000 H56B 2 0.350932 0.532123 0.353648 10.80000 -1.50000 H56C 2 0.304351 0.517341 0.276328 10.80000 -1.50000 AFIX 0 CL3 3 0.536554 0.579885 0.428902 10.80000 0.06577 0.05816 = 0.06028 0.00143 0.00638 0.01747 PART 2 10.2 RE3A 6 0.542375 0.554497 0.321506 10.20000 0.02138 0.02412 = 0.02931 -0.01013 0.00628 -0.00072 C41A 1 0.607283 0.496983 0.229528 10.20000 0.01841 0.05844 = 0.02614 -0.00920 0.01559 0.00070 AFIX 23 H41D 2 0.603200 0.486933 0.181910 10.20000 -1.20000 H41E 2 0.569084 0.477325 0.253823 10.20000 -1.20000 AFIX 0 C42A 1 0.725815 0.497018 0.264418 10.20000 0.01906 0.01480 = 0.03371 -0.00732 0.00950 0.00009 AFIX 23 H42D 2 0.770470 0.514908 0.241113 10.20000 -1.20000 H42E 2 0.757808 0.469932 0.268008 10.20000 -1.20000 AFIX 0 C51A 1 0.445059 0.533585 0.173674 10.20000 0.02585 0.05724 = 0.03034 -0.00894 0.00182 0.00327 AFIX 23 H51D 2 0.388897 0.516214 0.187755 10.20000 -1.20000 H51E 2 0.458161 0.524803 0.128070 10.20000 -1.20000 AFIX 0 C50A 1 0.959139 0.507189 0.360154 10.20000 0.03898 0.03200 = 0.03910 -0.01101 0.00238 0.00626 AFIX 137 H50D 2 0.945382 0.479819 0.373367 10.20000 -1.50000 H50E 2 1.025454 0.517344 0.390563 10.20000 -1.50000 H50F 2 0.969400 0.507622 0.312147 10.20000 -1.50000 AFIX 0 C49A 1 0.891570 0.574660 0.345919 10.20000 0.02970 0.02589 = 0.03615 -0.01122 0.00243 0.00337 AFIX 137 H49D 2 0.863154 0.578652 0.296425 10.20000 -1.50000 H49E 2 0.972036 0.575146 0.354927 10.20000 -1.50000 H49F 2 0.864648 0.595957 0.372193 10.20000 -1.50000 AFIX 0 C48A 1 0.892356 0.548471 0.456406 10.20000 0.04610 0.02279 = 0.04422 -0.00959 0.00597 0.00322 AFIX 137 H48D 2 0.955851 0.566374 0.462746 10.20000 -1.50000 H48E 2 0.911742 0.524336 0.483994 10.20000 -1.50000 H48F 2 0.830961 0.561875 0.471430 10.20000 -1.50000 AFIX 0 C46A 1 0.793971 0.452868 0.435051 10.20000 0.07145 0.03926 = 0.04391 0.00006 0.01307 -0.00029 AFIX 137 H46D 2 0.810895 0.441024 0.392955 10.20000 -1.50000 H46E 2 0.780795 0.431688 0.466600 10.20000 -1.50000 H46F 2 0.856016 0.469248 0.457648 10.20000 -1.50000 AFIX 0 C45A 1 0.674251 0.490493 0.487630 10.20000 0.06393 0.02327 = 0.03707 -0.00340 0.01303 -0.01067 AFIX 137 H45D 2 0.682745 0.519352 0.493573 10.20000 -1.50000 H45E 2 0.728953 0.476910 0.522545 10.20000 -1.50000 H45F 2 0.600362 0.482675 0.493029 10.20000 -1.50000 AFIX 0 C44A 1 0.606828 0.450579 0.375060 10.20000 0.06273 0.02672 = 0.04520 -0.01010 0.01511 0.00218 AFIX 137 H44D 2 0.568399 0.463883 0.333002 10.20000 -1.50000 H44E 2 0.553629 0.442726 0.403293 10.20000 -1.50000 H44F 2 0.644465 0.426871 0.362458 10.20000 -1.50000 AFIX 0 C52A 1 0.411679 0.576401 0.172282 10.20000 0.01669 0.05438 = 0.03020 -0.00297 0.00482 0.00020 AFIX 23 H52D 2 0.342911 0.580093 0.137755 10.20000 -1.20000 H52E 2 0.469383 0.592935 0.158028 10.20000 -1.20000 AFIX 0 C53A 1 0.252393 0.582582 0.283764 10.20000 0.03257 0.04077 = 0.04111 0.00627 0.01136 0.00977 C54A 1 0.154318 0.603691 0.239838 10.20000 0.03683 0.04148 = 0.05315 0.00879 0.00487 0.00744 AFIX 137 H54D 2 0.155601 0.599795 0.190764 10.20000 -1.50000 H54E 2 0.158127 0.632201 0.250511 10.20000 -1.50000 H54F 2 0.086162 0.592652 0.249995 10.20000 -1.50000 AFIX 0 C55A 1 0.270771 0.588948 0.361463 10.20000 0.02953 0.04400 = 0.04118 0.00586 0.01123 0.00720 AFIX 137 H55D 2 0.281753 0.617359 0.371758 10.20000 -1.50000 H55E 2 0.335924 0.574089 0.384015 10.20000 -1.50000 H55F 2 0.206487 0.579499 0.378723 10.20000 -1.50000 AFIX 0 C56A 1 0.236445 0.538822 0.265324 10.20000 0.05004 0.04130 = 0.03744 0.00720 0.00838 0.00615 AFIX 137 H56D 2 0.196019 0.536261 0.217590 10.20000 -1.50000 H56E 2 0.194747 0.526045 0.296675 10.20000 -1.50000 H56F 2 0.308275 0.525917 0.269805 10.20000 -1.50000 AFIX 0 C58A 1 0.297861 0.675862 0.248390 10.20000 0.03098 0.03697 = 0.02680 0.00467 0.00415 0.01350 AFIX 137 H58D 2 0.313492 0.694767 0.286903 10.20000 -1.50000 H58E 2 0.234074 0.659601 0.252793 10.20000 -1.50000 H58F 2 0.282153 0.690491 0.204576 10.20000 -1.50000 AFIX 0 C57A 1 0.399467 0.648384 0.249820 10.20000 0.03272 0.03884 = 0.02533 0.00713 0.00612 0.01290 C59A 1 0.444457 0.667523 0.192837 10.20000 0.03015 0.03244 = 0.02576 0.00725 0.00612 0.01751 AFIX 137 H59D 2 0.483055 0.647540 0.170363 10.20000 -1.50000 H59E 2 0.495749 0.688706 0.211971 10.20000 -1.50000 H59F 2 0.384058 0.678867 0.158825 10.20000 -1.50000 AFIX 0 C60A 1 0.476723 0.668627 0.319924 10.20000 0.02899 0.02554 = 0.02461 0.00929 0.00464 0.02005 AFIX 137 H60D 2 0.550804 0.657277 0.327169 10.20000 -1.50000 H60E 2 0.444044 0.663039 0.360286 10.20000 -1.50000 H60F 2 0.480774 0.697475 0.313565 10.20000 -1.50000 AFIX 0 CL3A 3 0.607289 0.600970 0.409110 10.20000 0.07038 0.07761 = 0.11474 -0.01151 0.01155 0.00056 PART 3 10.4 CL4 3 0.669856 0.610719 0.262032 10.40000 0.06577 0.05816 = 0.06028 0.00143 0.00638 0.01747 PART 4 10.4 N6 4 0.643027 0.606856 0.300696 10.40000 0.06577 0.05816 = 0.06028 0.00143 0.00638 0.01747 PART 5 10.1 N6A 4 0.464566 0.524127 0.359736 10.10000 0.07038 0.07761 = 0.11474 -0.01151 0.01155 0.00056 PART 6 10.1 CL4A 3 0.436930 0.499393 0.339998 10.10000 0.07038 0.07761 = 0.11474 -0.01151 0.01155 0.00056 PART 0 P5 5 0.709229 0.516702 0.349841 11.00000 0.04068 0.02784 = 0.02821 -0.00575 0.00706 0.00922 P6 5 0.390100 0.593189 0.258590 11.00000 0.03360 0.03805 = 0.03004 0.00735 0.00874 0.01382 C43 1 0.690779 0.478969 0.416151 11.00000 0.07258 0.03169 = 0.03765 -0.00488 0.01320 -0.00589 C47 1 0.853349 0.535454 0.367539 11.00000 0.03731 0.02873 = 0.05523 -0.00927 0.00801 -0.00104 C61 1 1.185556 0.742335 1.082389 10.50000 0.13102 0.11958 = 0.04559 0.00102 -0.03919 0.08662 AFIX 137 H61A 2 1.120486 0.728755 1.056462 10.50000 -1.50000 H61B 2 1.165779 0.756931 1.121193 10.50000 -1.50000 H61C 2 1.242363 0.722642 1.100057 10.50000 -1.50000 AFIX 0 C62 1 1.227381 0.770196 1.036824 10.50000 0.13706 0.11946 = 0.04564 -0.00728 -0.03518 0.08296 AFIX 23 H62A 2 1.218413 0.757691 0.990608 10.50000 -1.20000 H62B 2 1.179859 0.794098 1.031764 10.50000 -1.20000 AFIX 0 C63 1 1.339242 0.783271 1.056336 10.50000 0.14830 0.15567 = 0.04577 -0.01256 -0.03826 0.06488 AFIX 23 H63A 2 1.387624 0.761358 1.047024 10.50000 -1.20000 H63B 2 1.355293 0.788090 1.106833 10.50000 -1.20000 AFIX 0 C64 1 1.368383 0.819294 1.021758 10.50000 0.16892 0.17627 = 0.04811 0.00358 -0.04292 0.05053 AFIX 23 H64A 2 1.302155 0.828741 0.989312 10.50000 -1.20000 H64B 2 1.389625 0.840264 1.057109 10.50000 -1.20000 AFIX 0 C65 1 1.455216 0.814789 0.984348 10.50000 0.17622 0.16026 = 0.06293 -0.00850 -0.03742 0.04589 AFIX 137 H65A 2 1.425072 0.805114 0.937606 10.50000 -1.50000 H65B 2 1.509033 0.795618 1.008267 10.50000 -1.50000 H65C 2 1.491092 0.840546 0.981516 10.50000 -1.50000 AFIX 0 HKLF 4 REM CW_FS_040717_a.res in P2(1)/c REM R1 = 0.0639 for 11420 Fo > 4sig(Fo) and 0.1113 for all 16610 data REM 963 parameters refined using 469 restraints END WGHT 0.0273 101.3806 REM Highest difference peak 2.340, deepest hole -1.787, 1-sigma level 0.205 Q1 1 0.6211 0.6064 0.9627 11.00000 0.05 2.34 Q2 1 0.8619 0.7039 0.7385 11.00000 0.05 2.14 Q3 1 0.6225 0.6166 0.4535 11.00000 0.05 1.98 Q4 1 0.4949 0.5356 0.3780 11.00000 0.05 1.93 Q5 1 0.4395 0.5184 0.4094 11.00000 0.05 1.86 Q6 1 0.5004 0.5644 0.3113 11.00000 0.05 1.38 Q7 1 0.5627 0.5777 0.3394 11.00000 0.05 1.33 Q8 1 1.3705 0.8459 1.0181 11.00000 0.05 1.31 Q9 1 1.3828 0.7987 1.0029 11.00000 0.05 1.29 Q10 1 0.5673 0.5502 0.3184 11.00000 0.05 1.28 Q11 1 1.4030 0.8424 1.0277 11.00000 0.05 1.23 Q12 1 1.4221 0.8040 1.0074 11.00000 0.05 1.20 Q13 1 1.3106 0.7666 1.0838 11.00000 0.05 1.17 Q14 1 0.7443 0.6930 0.7849 11.00000 0.05 1.02 Q15 1 0.5880 0.5730 0.2878 11.00000 0.05 0.97 Q16 1 0.7177 0.6295 0.9241 11.00000 0.05 0.95 Q17 1 1.2922 0.7827 0.9983 11.00000 0.05 0.94 Q18 1 0.5587 0.5789 0.3045 11.00000 0.05 0.93 Q19 1 1.2807 0.7517 1.0611 11.00000 0.05 0.92 Q20 1 1.2608 0.7886 1.0618 11.00000 0.05 0.92 ; 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130.49 35.50 -6 -21 0 134.19 35.50 -6 -21 0 170.08 29.50 6 21 0 159.88 36.90 6 21 0 130.69 38.60 -6 21 0 164.28 28.90 6 21 0 109.29 29.40 -6 21 0 111.39 34.40 7 -21 0 87.49 36.00 -7 -21 0 87.39 29.80 7 -21 0 95.29 32.90 -7 -21 0 130.49 37.30 -7 21 0 132.89 29.00 -7 21 0 90.29 34.80 7 21 0 84.79 32.10 7 21 0 50.89 37.50 7 21 0 88.59 38.00 -8 -21 0 281.97 46.20 8 -21 0 292.77 50.29 8 -21 0 251.77 46.50 -8 -21 0 308.27 51.79 -8 21 0 347.37 46.30 8 21 0 312.67 47.50 8 21 0 265.77 52.89 -8 21 0 352.06 53.49 9 -21 0 140.29 46.80 9 -21 0 75.19 39.10 -9 -21 0 142.09 39.20 -9 21 0 110.39 33.70 9 21 0 128.09 49.00 -9 21 0 198.68 50.09 10 -21 0 -15.80 37.90 -10 -21 0 35.40 38.10 10 -21 0 49.90 42.80 10 21 0 -69.79 51.09 -10 21 0 110.49 51.29 10 21 0 -20.30 48.90 -10 21 0 16.70 44.60 10 21 0 -26.30 49.80 -11 -21 0 127.49 50.59 11 -21 0 20.50 50.99 11 -21 0 187.58 53.49 11 21 0 73.49 62.69 -11 21 0 137.99 59.49 -11 21 0 88.39 41.40 12 -21 0 -61.09 52.29 -12 -21 0 80.69 53.99 -12 21 0 40.90 53.59 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347.87 49.60 -6 -23 0 361.16 43.00 6 23 0 344.17 56.59 6 23 0 300.57 49.70 -6 23 0 369.06 42.60 6 23 0 280.07 42.90 -6 23 0 367.16 50.39 7 -23 0 181.28 38.80 7 -23 0 123.49 39.90 -7 -23 0 186.88 35.80 -7 23 0 200.38 33.90 7 23 0 217.18 49.40 -7 23 0 232.98 45.20 8 -23 0 54.09 37.90 -8 -23 0 85.99 33.80 8 -23 0 105.49 47.80 -8 23 0 78.09 31.90 -8 23 0 68.19 43.50 8 23 0 59.59 44.90 9 -23 0 25.20 39.80 9 -23 0 58.49 52.99 -9 -23 0 42.90 36.90 -9 23 0 77.59 33.60 -9 23 0 124.29 48.70 9 23 0 10.70 44.90 9 23 0 59.49 45.50 9 23 0 0.30 50.59 10 -23 0 -26.00 46.50 -10 -23 0 -18.80 40.60 10 -23 0 23.20 42.30 -10 23 0 -49.00 36.90 10 23 0 3.40 55.49 -10 23 0 -20.80 55.09 11 -23 0 -17.40 49.10 11 -23 0 21.20 48.90 -11 -23 0 12.80 49.00 -11 23 0 37.90 48.60 -11 23 0 76.49 63.79 11 23 0 -0.60 62.19 12 -23 0 33.20 63.49 12 -23 0 -2.00 61.89 -12 -23 0 147.29 55.39 -12 23 0 22.10 75.29 12 23 0 123.39 76.19 -12 23 0 90.79 53.89 0 24 0 178.88 35.10 0 24 0 138.29 29.20 -1 24 0 63.19 21.60 1 24 0 43.20 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7 24 0 1218.18 124.19 8 -24 0 601.24 83.99 8 -24 0 616.34 78.79 -8 -24 0 635.64 72.49 -8 24 0 695.83 86.19 8 24 0 470.55 73.99 -8 24 0 573.74 68.19 -9 -24 0 23.40 34.70 9 -24 0 -9.00 50.59 9 -24 0 -50.99 39.50 9 24 0 116.99 55.99 -9 24 0 -14.90 48.30 -9 24 0 72.89 34.30 9 24 0 19.00 46.20 9 24 0 52.29 73.49 10 -24 0 -34.30 45.50 -10 -24 0 26.90 40.70 10 -24 0 22.30 54.89 -10 24 0 34.40 57.49 -10 24 0 33.10 42.40 10 24 0 -9.60 57.19 11 -24 0 30.10 53.99 11 -24 0 -18.60 51.49 -11 -24 0 43.20 49.90 -11 24 0 83.69 49.80 11 24 0 173.68 65.89 -11 24 0 2.40 69.09 12 -24 0 273.07 72.79 -12 -24 0 256.87 62.39 -12 24 0 230.28 66.19 -12 24 0 263.97 85.39 12 24 0 141.09 81.29 0 25 0 25.30 28.70 0 25 0 -1.60 23.40 -1 25 0 151.58 29.40 1 25 0 192.58 35.50 1 25 0 183.78 34.30 -1 25 0 169.08 34.80 2 25 0 57.39 16.50 -2 25 0 63.89 23.00 2 25 0 22.90 33.10 2 25 0 53.39 28.40 -2 25 0 60.69 28.30 3 -25 0 145.59 23.70 3 -25 0 197.48 39.10 -3 -25 0 164.98 21.70 3 -25 0 178.28 22.80 -3 -25 0 165.68 21.00 3 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133.69 47.60 9 25 0 125.39 58.89 -9 25 0 137.49 58.59 -9 25 0 220.78 45.90 9 25 0 146.59 62.39 -10 -25 0 -1.20 65.09 10 -25 0 31.40 55.19 10 -25 0 59.99 50.19 10 25 0 -47.30 96.49 -10 25 0 209.28 61.69 -10 25 0 -10.50 40.70 11 -25 0 341.07 70.29 -11 -25 0 379.46 67.79 11 -25 0 419.96 91.19 -11 25 0 334.37 80.89 11 25 0 364.26 82.09 -11 25 0 433.06 68.79 -12 -25 0 106.79 54.99 12 -25 0 -70.79 63.59 12 -25 0 -47.40 61.49 -12 25 0 -49.30 80.39 -12 25 0 -39.70 62.79 12 25 0 -15.30 70.59 0 26 0 421.16 58.29 0 26 0 538.85 65.69 1 26 0 -6.60 29.80 -1 26 0 27.20 30.10 -1 26 0 76.99 24.50 1 26 0 27.50 27.00 -2 26 0 18.80 28.30 2 26 0 63.29 31.60 -2 26 0 -7.10 21.40 2 26 0 11.10 28.60 3 -26 0 218.28 29.30 3 -26 0 183.18 41.60 -3 26 0 207.88 42.00 3 26 0 288.17 50.99 -3 26 0 223.78 28.40 3 26 0 262.87 42.30 3 26 0 235.78 30.30 -3 26 0 239.58 32.20 4 -26 0 171.98 26.40 -4 -26 0 168.28 23.50 4 -26 0 153.08 26.60 4 -26 0 86.09 36.40 -4 26 0 144.39 22.60 4 26 0 89.99 37.10 4 26 0 75.49 41.00 4 26 0 203.28 28.80 -4 26 0 120.99 39.20 -4 26 0 169.18 23.70 -4 26 0 119.09 22.90 5 -26 0 43.00 23.50 5 -26 0 18.20 33.00 -5 -26 0 33.30 22.10 -5 26 0 76.59 16.60 5 26 0 87.99 39.90 5 26 0 101.29 27.70 -5 26 0 93.29 36.90 -5 26 0 87.99 21.50 5 26 0 21.70 37.70 6 -26 0 324.77 53.09 -6 -26 0 337.37 43.10 6 -26 0 329.47 45.40 6 26 0 389.76 59.59 -6 26 0 393.66 56.39 6 26 0 376.26 59.49 -6 26 0 311.77 40.90 -7 -26 0 13.10 28.20 7 -26 0 16.70 30.90 7 -26 0 33.70 37.70 -7 26 0 16.30 41.00 -7 26 0 -17.90 25.10 7 26 0 -58.19 35.30 -8 -26 0 15.80 31.70 8 -26 0 -23.70 38.70 8 -26 0 -40.20 37.50 8 26 0 -12.70 45.80 -8 26 0 -25.80 27.00 -8 26 0 5.70 47.90 9 -26 0 78.89 46.30 9 -26 0 18.70 42.00 -9 -26 0 41.70 37.40 9 26 0 87.69 52.29 -9 26 0 121.29 37.10 -9 26 0 103.59 57.89 10 -26 0 150.78 52.99 -10 -26 0 95.19 44.80 10 -26 0 8.10 49.99 10 26 0 59.69 64.09 -10 26 0 70.89 62.39 -10 26 0 121.29 44.20 -11 -26 0 155.98 51.99 11 -26 0 -20.90 56.59 11 -26 0 89.39 59.69 11 26 0 81.59 66.09 -11 26 0 99.09 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30.10 2 11 -12 60.29 23.60 2 11 -12 67.29 23.20 1 -11 -12 82.19 28.80 1 -11 -12 161.08 29.00 -1 -11 12 125.19 31.50 1 -11 -12 184.38 48.20 -1 -11 12 148.69 23.80 -1 -11 12 121.79 29.70 1 -11 -12 142.39 28.00 1 11 -12 138.09 24.60 1 11 -12 125.79 23.90 1 11 -12 96.89 26.40 1 11 -12 142.49 28.50 -1 11 12 99.19 34.50 -1 11 12 148.79 37.60 -1 11 12 131.29 29.80 0 -11 -12 2003.00 161.68 0 -11 12 2016.40 160.58 0 -11 -12 2030.60 166.58 0 -11 12 1916.01 160.38 0 -11 -12 1901.11 160.48 0 11 12 2028.00 163.38 0 11 12 2071.49 161.88 0 11 -12 2033.40 160.88 0 11 -12 1926.21 161.48 0 11 -12 1944.51 153.08 0 11 -12 1946.71 157.78 1 -11 12 336.87 41.70 -1 -11 -12 263.97 38.80 -1 -11 -12 272.87 40.70 -1 -11 -12 307.07 48.20 1 -11 12 260.17 39.80 -1 -11 -12 243.38 38.40 1 11 12 257.57 38.10 1 11 12 193.88 41.90 -1 11 -12 329.27 41.50 1 11 12 316.77 44.40 -1 11 -12 299.47 40.70 -2 -11 -12 15.70 22.80 -2 -11 -12 19.20 29.50 2 -11 12 30.40 25.70 2 -11 12 14.70 24.70 2 11 12 24.00 26.60 2 11 12 34.60 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343.97 90.29 3 -8 -24 452.45 84.09 -3 -8 24 479.75 80.19 3 -8 -24 133.89 105.49 3 -8 -24 374.26 79.39 3 8 -24 357.46 93.29 -3 8 24 247.78 97.89 3 8 -24 428.66 68.39 2 -8 -24 265.07 69.79 2 -8 -24 354.06 73.59 2 -8 -24 115.59 95.19 2 -8 -24 -26.70 80.29 -2 -8 24 156.28 57.49 2 8 -24 255.87 52.59 2 8 -24 128.59 80.89 1 -8 -24 102.09 70.99 1 -8 -24 120.59 66.79 1 8 -24 246.48 81.09 4 -9 -24 349.27 77.29 -4 -9 24 316.77 82.99 4 -9 -24 264.87 88.59 4 9 -24 410.06 73.39 4 9 -24 439.76 93.99 3 -9 -24 98.49 64.69 -3 -9 24 230.38 68.49 3 -9 -24 141.89 73.79 3 -9 -24 128.09 75.19 3 -9 -24 223.88 94.29 3 9 -24 41.60 79.69 3 9 -24 103.59 107.09 -3 9 24 336.57 99.69 3 9 -24 141.59 56.99 -2 -9 24 -1.60 48.30 2 -9 -24 142.09 88.19 2 -9 -24 9.60 66.59 2 -9 -24 7.30 61.49 2 9 -24 52.09 46.30 2 9 -24 118.29 77.59 3 10 -24 -14.60 78.99 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 72063