# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chi-Chiu Ko' _publ_contact_author_email VINCCKO@CITYU.EDU.HK _publ_section_title ; Synthesis, Characterisation and Photophysical Studies of Leucotriarylmethanes-Containing Ligands and Their Rhenium(I) Tricarbonyl Diimine Complexes ; loop_ _publ_author_name 'Chi-Chiu Ko.' 'Wing-Kin Chu.' 'Hua Feng.' 'Chi-On Ng.' # Attachment '2.cif' data_Complex_2 _database_code_depnum_ccdc_archive 'CCDC 760665' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H32 F6 N6 O3 P Re' _chemical_formula_sum 'C38 H32 F6 N6 O3 P Re' _chemical_formula_weight 951.88 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 16.7916(4) _cell_length_b 11.0807(3) _cell_length_c 26.4430(7) _cell_angle_alpha 90.00 _cell_angle_beta 128.189(2) _cell_angle_gamma 90.00 _cell_volume 3867.04(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5598 _cell_measurement_theta_min 3.145 _cell_measurement_theta_max 28.0723 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.635 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 3.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.77101 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Mo)' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13037 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0945 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6579 _reflns_number_gt 3976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford, 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford, 2009)' _computing_data_reduction 'CrysAlisPro (Oxford, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0389P)^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 6579 _refine_ls_number_parameters 498 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0776 _refine_ls_goodness_of_fit_ref 0.846 _refine_ls_restrained_S_all 0.905 _refine_ls_shift/su_max 0.002 _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 Re1 Re 0.66817(2) -0.10107(2) 0.456276(13) 0.04325(10) Uani 1 1 d . . . O1 O 0.5910(4) -0.3599(5) 0.4124(3) 0.092(2) Uani 1 1 d . . . O2 O 0.4490(4) -0.0171(5) 0.3589(3) 0.0767(17) Uani 1 1 d . . . O3 O 0.6205(5) -0.1202(6) 0.5507(3) 0.106(2) Uani 1 1 d . . . N1 N 0.7190(4) -0.0825(5) 0.3986(3) 0.0475(14) Uani 1 1 d . . . N2 N 0.8277(4) -0.1507(5) 0.5211(3) 0.0450(14) Uani 1 1 d . . . N3 N 0.7258(4) 0.0839(4) 0.4889(2) 0.0365(13) Uani 1 1 d . . . N4 N 1.2860(5) 0.3558(8) 0.7413(4) 0.103(3) Uani 1 1 d . . . N5 N 0.6590(5) 0.6771(6) 0.6525(3) 0.0683(19) Uani 1 1 d . . . N6 N 0.8165(5) 0.5803(5) 0.4718(3) 0.0613(17) Uani 1 1 d . . . C1 C 0.6222(6) -0.2644(8) 0.4297(4) 0.059(2) Uani 1 1 d . . . C2 C 0.5329(6) -0.0485(6) 0.3957(4) 0.0509(18) Uani 1 1 d . . . C3 C 0.6382(6) -0.1157(7) 0.5150(4) 0.065(2) Uani 1 1 d . . . C4 C 0.6644(6) -0.0467(7) 0.3371(3) 0.062(2) Uani 1 1 d . . . H4A H 0.5967 -0.0263 0.3154 0.074 Uiso 1 1 calc R . . C5 C 0.7044(9) -0.0388(8) 0.3042(4) 0.084(3) Uani 1 1 d . . . H5A H 0.6636 -0.0148 0.2613 0.101 Uiso 1 1 calc R . . C6 C 0.8041(9) -0.0667(8) 0.3354(5) 0.081(3) Uani 1 1 d . . . H6A H 0.8318 -0.0605 0.3141 0.097 Uiso 1 1 calc R . . C7 C 0.8638(6) -0.1042(7) 0.3991(4) 0.063(2) Uani 1 1 d . . . C8 C 0.9670(8) -0.1337(8) 0.4352(6) 0.085(3) Uani 1 1 d . . . H8A H 0.9978 -0.1295 0.4157 0.102 Uiso 1 1 calc R . . C9 C 1.0225(7) -0.1676(8) 0.4970(6) 0.089(3) Uani 1 1 d . . . H9A H 1.0904 -0.1870 0.5192 0.107 Uiso 1 1 calc R . . C10 C 0.9792(6) -0.1743(7) 0.5294(5) 0.068(2) Uani 1 1 d . . . C11 C 1.0303(6) -0.2104(8) 0.5937(5) 0.081(3) Uani 1 1 d . . . H11A H 1.0984 -0.2316 0.6188 0.097 Uiso 1 1 calc R . . C12 C 0.9821(7) -0.2144(7) 0.6191(4) 0.078(3) Uani 1 1 d . . . H12A H 1.0172 -0.2374 0.6618 0.093 Uiso 1 1 calc R . . C13 C 0.8798(6) -0.1845(7) 0.5823(4) 0.059(2) Uani 1 1 d . . . H13A H 0.8474 -0.1882 0.6008 0.071 Uiso 1 1 calc R . . C14 C 0.8753(5) -0.1443(6) 0.4949(3) 0.0464(17) Uani 1 1 d . . . C15 C 0.8191(5) -0.1109(6) 0.4299(4) 0.0513(18) Uani 1 1 d . . . C16 C 0.7823(5) 0.1109(6) 0.5522(3) 0.0493(17) Uani 1 1 d . . . H16A H 0.7937 0.0508 0.5806 0.059 Uiso 1 1 calc R . . C17 C 0.8234(5) 0.2231(6) 0.5764(3) 0.0493(18) Uani 1 1 d . . . H17A H 0.8624 0.2371 0.6204 0.059 Uiso 1 1 calc R . . C18 C 0.8074(4) 0.3154(5) 0.5359(3) 0.0318(15) Uani 1 1 d . . . C19 C 0.7481(5) 0.2885(6) 0.4718(3) 0.0404(16) Uani 1 1 d . . . H19A H 0.7339 0.3482 0.4425 0.049 Uiso 1 1 calc R . . C20 C 0.7087(5) 0.1738(6) 0.4498(3) 0.0392(16) Uani 1 1 d . . . H20A H 0.6685 0.1588 0.4058 0.047 Uiso 1 1 calc R . . C21 C 0.9735(5) 0.4243(6) 0.6141(3) 0.0397(17) Uani 1 1 d . . . C22 C 1.0350(6) 0.4467(7) 0.5972(4) 0.059(2) Uani 1 1 d . . . H22A H 1.0063 0.4763 0.5563 0.071 Uiso 1 1 calc R . . C23 C 1.1389(6) 0.4261(7) 0.6398(4) 0.066(2) Uani 1 1 d . . . H23A H 1.1788 0.4438 0.6274 0.079 Uiso 1 1 calc R . . C24 C 1.1833(6) 0.3797(8) 0.7001(4) 0.072(2) Uani 1 1 d . . . C25 C 1.1221(6) 0.3576(7) 0.7177(4) 0.063(2) Uani 1 1 d . . . H25A H 1.1506 0.3279 0.7586 0.075 Uiso 1 1 calc R . . C26 C 1.0196(5) 0.3792(6) 0.6751(3) 0.0534(19) Uani 1 1 d . . . H26A H 0.9800 0.3629 0.6879 0.064 Uiso 1 1 calc R . . C27 C 1.3488(7) 0.3828(11) 0.7242(6) 0.152(5) Uani 1 1 d . . . H27A H 1.3078 0.4098 0.6803 0.228 Uiso 1 1 calc R . . H27B H 1.3855 0.3117 0.7288 0.228 Uiso 1 1 calc R . . H27C H 1.3958 0.4452 0.7518 0.228 Uiso 1 1 calc R . . C28 C 1.3322(7) 0.3153(12) 0.8060(5) 0.143(5) Uani 1 1 d . . . H28A H 1.2805 0.3020 0.8106 0.215 Uiso 1 1 calc R . . H28B H 1.3785 0.3757 0.8362 0.215 Uiso 1 1 calc R . . H28C H 1.3682 0.2414 0.8141 0.215 Uiso 1 1 calc R . . C29 C 0.8076(5) 0.4986(6) 0.5917(3) 0.0376(16) Uani 1 1 d . . . C30 C 0.8606(5) 0.5690(6) 0.6472(3) 0.0481(18) Uani 1 1 d . . . H30A H 0.9303 0.5777 0.6712 0.058 Uiso 1 1 calc R . . C31 C 0.8119(6) 0.6254(6) 0.6667(3) 0.057(2) Uani 1 1 d . . . H31A H 0.8499 0.6705 0.7044 0.069 Uiso 1 1 calc R . . C32 C 0.7067(6) 0.6181(7) 0.6324(3) 0.0510(18) Uani 1 1 d . . . C33 C 0.6542(5) 0.5501(7) 0.5763(4) 0.063(2) Uani 1 1 d . . . H33A H 0.5841 0.5437 0.5513 0.076 Uiso 1 1 calc R . . C34 C 0.7031(6) 0.4925(7) 0.5573(3) 0.057(2) Uani 1 1 d . . . H34A H 0.6652 0.4472 0.5196 0.068 Uiso 1 1 calc R . . C35 C 0.7163(7) 0.7470(9) 0.7109(4) 0.098(3) Uani 1 1 d . . . H35A H 0.7874 0.7371 0.7322 0.147 Uiso 1 1 calc R . . H35B H 0.7013 0.7198 0.7386 0.147 Uiso 1 1 calc R . . H35C H 0.6985 0.8306 0.7007 0.147 Uiso 1 1 calc R . . C36 C 0.5498(6) 0.6768(8) 0.6120(4) 0.086(3) Uani 1 1 d . . . H36A H 0.5234 0.6261 0.5753 0.128 Uiso 1 1 calc R . . H36B H 0.5250 0.7576 0.5979 0.128 Uiso 1 1 calc R . . H36C H 0.5284 0.6466 0.6359 0.128 Uiso 1 1 calc R . . C37 C 0.8562(5) 0.4392(6) 0.5647(3) 0.0375(16) Uani 1 1 d . . . C38 C 0.8332(5) 0.5192(6) 0.5116(3) 0.0441(17) Uani 1 1 d . . . F1 F 0.4968(3) 0.1620(4) 0.2913(2) 0.0812(14) Uani 1 1 d . . . F2 F 0.3790(4) 0.2612(6) 0.2009(3) 0.121(2) Uani 1 1 d . . . F3 F 0.4972(5) 0.3628(6) 0.2910(3) 0.135(2) Uani 1 1 d U . . F4 F 0.9882(5) 0.0203(5) 0.8044(2) 0.1192(19) Uani 1 1 d U . . F5 F 1.0000 -0.1230(12) 0.7500 0.198(5) Uani 1 2 d SU . . F6 F 0.8893(7) 0.0066(10) 0.6997(4) 0.208(3) Uani 1 1 d U . . F7 F 1.0000 0.1554(10) 0.7500 0.175(4) Uani 1 2 d SU . . P1 P 1.0000 0.0173(3) 0.7500 0.0784(10) Uani 1 2 d S . . P2 P 0.5000 0.2619(3) 0.2500 0.0752(10) Uani 1 2 d S . . 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 Re1 0.03916(16) 0.03435(15) 0.04332(16) -0.00058(18) 0.01904(13) -0.00106(18) O1 0.065(4) 0.046(3) 0.107(5) -0.011(3) 0.024(4) -0.016(3) O2 0.051(3) 0.078(4) 0.080(4) 0.022(3) 0.030(3) 0.012(3) O3 0.127(6) 0.116(6) 0.119(5) 0.023(5) 0.099(5) 0.007(5) N1 0.054(4) 0.038(4) 0.042(3) -0.016(3) 0.025(3) -0.004(3) N2 0.045(4) 0.028(3) 0.047(3) 0.002(3) 0.021(3) 0.002(3) N3 0.044(3) 0.032(3) 0.038(3) 0.002(3) 0.028(3) 0.004(3) N4 0.037(4) 0.121(7) 0.104(6) -0.018(6) 0.020(5) -0.001(5) N5 0.071(5) 0.081(5) 0.073(4) -0.013(4) 0.054(4) 0.003(4) N6 0.079(5) 0.044(4) 0.054(4) 0.006(3) 0.038(4) -0.003(4) C1 0.038(4) 0.059(5) 0.057(5) 0.001(5) 0.018(4) 0.005(4) C2 0.057(5) 0.037(4) 0.060(5) 0.003(4) 0.036(4) 0.002(4) C3 0.068(5) 0.044(5) 0.085(6) 0.006(5) 0.048(5) 0.003(4) C4 0.064(6) 0.065(6) 0.044(5) -0.005(4) 0.028(5) 0.006(4) C5 0.120(9) 0.079(7) 0.056(5) -0.010(5) 0.056(6) 0.000(7) C6 0.121(9) 0.071(7) 0.092(7) -0.016(6) 0.086(7) -0.009(6) C7 0.075(6) 0.041(4) 0.095(6) -0.020(5) 0.064(6) -0.004(5) C8 0.088(8) 0.065(7) 0.135(9) -0.025(7) 0.085(8) -0.012(6) C9 0.061(6) 0.063(6) 0.141(9) -0.033(7) 0.061(7) 0.003(5) C10 0.047(5) 0.040(5) 0.096(7) -0.008(5) 0.034(5) 0.003(4) C11 0.038(5) 0.052(5) 0.094(8) -0.005(6) 0.011(5) 0.007(5) C12 0.065(6) 0.050(5) 0.061(6) -0.001(5) 0.011(5) 0.007(5) C13 0.051(5) 0.049(5) 0.050(5) 0.002(4) 0.018(4) 0.012(4) C14 0.048(5) 0.025(3) 0.057(5) -0.012(4) 0.028(4) -0.005(3) C15 0.053(5) 0.031(4) 0.066(5) -0.014(4) 0.035(4) -0.005(4) C16 0.061(4) 0.039(4) 0.037(4) 0.009(4) 0.025(4) 0.003(4) C17 0.065(5) 0.042(4) 0.026(4) -0.001(4) 0.021(4) -0.006(4) C18 0.032(4) 0.033(4) 0.028(4) -0.002(3) 0.017(3) 0.004(3) C19 0.042(4) 0.039(4) 0.034(4) 0.006(4) 0.020(3) 0.008(4) C20 0.043(4) 0.041(4) 0.026(3) -0.003(3) 0.018(3) 0.005(4) C21 0.040(4) 0.038(4) 0.041(4) -0.003(3) 0.024(3) -0.002(3) C22 0.062(5) 0.052(5) 0.060(5) -0.012(4) 0.037(5) -0.002(4) C23 0.038(4) 0.074(6) 0.084(6) -0.019(5) 0.037(5) -0.010(5) C24 0.036(5) 0.061(6) 0.080(6) -0.014(5) 0.016(5) 0.000(5) C25 0.044(5) 0.072(6) 0.050(4) -0.002(4) 0.018(4) 0.007(4) C26 0.049(4) 0.050(5) 0.057(5) 0.004(4) 0.031(4) 0.000(4) C27 0.040(6) 0.164(12) 0.205(13) -0.014(10) 0.052(8) -0.008(7) C28 0.060(7) 0.162(12) 0.114(9) -0.022(9) 0.007(7) 0.026(8) C29 0.035(4) 0.037(4) 0.035(4) -0.004(3) 0.019(3) 0.005(3) C30 0.041(4) 0.051(5) 0.048(4) -0.018(4) 0.026(4) -0.005(4) C31 0.063(5) 0.057(5) 0.048(4) -0.026(4) 0.033(4) -0.004(4) C32 0.056(5) 0.050(5) 0.056(4) -0.001(4) 0.040(4) 0.004(4) C33 0.040(4) 0.083(6) 0.062(5) -0.028(5) 0.029(4) 0.001(4) C34 0.055(5) 0.063(5) 0.046(4) -0.015(4) 0.028(4) 0.003(4) C35 0.098(7) 0.113(8) 0.112(8) -0.050(7) 0.079(7) -0.010(6) C36 0.073(6) 0.114(8) 0.093(6) -0.018(6) 0.063(6) 0.009(6) C37 0.044(4) 0.034(4) 0.031(4) 0.006(3) 0.021(3) -0.001(3) C38 0.043(4) 0.036(4) 0.046(4) -0.004(4) 0.024(4) -0.004(4) F1 0.102(4) 0.083(3) 0.079(3) 0.022(3) 0.066(3) 0.010(3) F2 0.104(4) 0.151(6) 0.098(4) 0.026(4) 0.058(4) 0.045(4) F3 0.194(5) 0.125(4) 0.115(3) -0.018(3) 0.110(3) 0.011(3) F4 0.159(4) 0.126(4) 0.089(3) 0.013(3) 0.085(3) 0.013(3) F5 0.237(7) 0.181(7) 0.179(6) 0.000 0.130(5) 0.000 F6 0.179(5) 0.285(6) 0.176(5) 0.005(4) 0.117(4) -0.005(4) F7 0.244(6) 0.157(6) 0.159(5) 0.000 0.142(5) 0.000 P1 0.100(3) 0.063(2) 0.053(2) 0.000 0.038(2) 0.000 P2 0.118(3) 0.068(2) 0.065(2) 0.000 0.069(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.888(8) . ? Re1 C3 1.913(9) . ? Re1 C1 1.922(9) . ? Re1 N1 2.168(5) . ? Re1 N2 2.177(5) . ? Re1 N3 2.202(5) . ? O1 C1 1.144(8) . ? O2 C2 1.166(8) . ? O3 C3 1.151(8) . ? N1 C4 1.343(8) . ? N1 C15 1.375(8) . ? N2 C13 1.331(8) . ? N2 C14 1.345(8) . ? N3 C20 1.333(7) . ? N3 C16 1.352(7) . ? N4 C24 1.382(10) . ? N4 C27 1.412(12) . ? N4 C28 1.445(12) . ? N5 C32 1.370(8) . ? N5 C35 1.439(9) . ? N5 C36 1.442(9) . ? N6 C38 1.130(7) . ? C4 C5 1.392(10) . ? C4 H4A 0.9300 . ? C5 C6 1.368(11) . ? C5 H5A 0.9300 . ? C6 C7 1.387(11) . ? C6 H6A 0.9300 . ? C7 C8 1.407(12) . ? C7 C15 1.410(9) . ? C8 C9 1.340(12) . ? C8 H8A 0.9300 . ? C9 C10 1.426(12) . ? C9 H9A 0.9300 . ? C10 C11 1.409(11) . ? C10 C14 1.421(10) . ? C11 C12 1.334(11) . ? C11 H11A 0.9300 . ? C12 C13 1.393(10) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.406(9) . ? C16 C17 1.373(9) . ? C16 H16A 0.9300 . ? C17 C18 1.382(8) . ? C17 H17A 0.9300 . ? C18 C19 1.365(8) . ? C18 C37 1.537(9) . ? C19 C20 1.384(8) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.378(9) . ? C21 C26 1.381(9) . ? C21 C37 1.560(8) . ? C22 C23 1.392(10) . ? C22 H22A 0.9300 . ? C23 C24 1.375(11) . ? C23 H23A 0.9300 . ? C24 C25 1.387(10) . ? C25 C26 1.375(9) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.391(8) . ? C29 C30 1.391(8) . ? C29 C37 1.527(8) . ? C30 C31 1.360(9) . ? C30 H30A 0.9300 . ? C31 C32 1.403(9) . ? C31 H31A 0.9300 . ? C32 C33 1.389(9) . ? C33 C34 1.360(8) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.495(9) . ? F1 P2 1.578(5) . ? F2 P2 1.598(6) . ? F3 P2 1.577(6) . ? F4 P1 1.571(5) . ? F5 P1 1.554(13) . ? F6 P1 1.477(9) . ? F7 P1 1.530(11) . ? P1 F6 1.477(9) 2_756 ? P1 F4 1.571(5) 2_756 ? P2 F3 1.577(6) 2_655 ? P2 F1 1.578(5) 2_655 ? P2 F2 1.598(6) 2_655 ? 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 C2 Re1 C3 86.1(3) . . ? C2 Re1 C1 88.8(3) . . ? C3 Re1 C1 88.3(3) . . ? C2 Re1 N1 99.5(2) . . ? C3 Re1 N1 173.9(3) . . ? C1 Re1 N1 94.3(3) . . ? C2 Re1 N2 174.4(3) . . ? C3 Re1 N2 98.7(3) . . ? C1 Re1 N2 94.1(3) . . ? N1 Re1 N2 75.5(2) . . ? C2 Re1 N3 93.0(3) . . ? C3 Re1 N3 91.9(3) . . ? C1 Re1 N3 178.2(3) . . ? N1 Re1 N3 85.31(18) . . ? N2 Re1 N3 84.13(19) . . ? C4 N1 C15 117.5(6) . . ? C4 N1 Re1 127.6(5) . . ? C15 N1 Re1 114.9(4) . . ? C13 N2 C14 119.2(6) . . ? C13 N2 Re1 126.3(5) . . ? C14 N2 Re1 114.5(4) . . ? C20 N3 C16 116.4(6) . . ? C20 N3 Re1 124.1(4) . . ? C16 N3 Re1 119.5(4) . . ? C24 N4 C27 121.5(9) . . ? C24 N4 C28 119.1(9) . . ? C27 N4 C28 119.0(8) . . ? C32 N5 C35 120.6(7) . . ? C32 N5 C36 119.4(7) . . ? C35 N5 C36 119.9(6) . . ? O1 C1 Re1 177.3(7) . . ? O2 C2 Re1 178.8(6) . . ? O3 C3 Re1 177.6(7) . . ? N1 C4 C5 123.0(8) . . ? N1 C4 H4A 118.5 . . ? C5 C4 H4A 118.5 . . ? C6 C5 C4 119.5(8) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C7 119.8(8) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C6 C7 C8 123.8(8) . . ? C6 C7 C15 118.3(8) . . ? C8 C7 C15 117.9(8) . . ? C9 C8 C7 121.9(9) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C10 121.2(9) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C11 C10 C14 115.5(8) . . ? C11 C10 C9 125.7(9) . . ? C14 C10 C9 118.9(9) . . ? C12 C11 C10 120.7(8) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C11 C12 C13 120.8(8) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? N2 C13 C12 121.0(8) . . ? N2 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? N2 C14 C15 118.7(6) . . ? N2 C14 C10 122.9(7) . . ? C15 C14 C10 118.4(7) . . ? N1 C15 C14 116.3(6) . . ? N1 C15 C7 122.0(7) . . ? C14 C15 C7 121.7(7) . . ? N3 C16 C17 122.9(6) . . ? N3 C16 H16A 118.6 . . ? C17 C16 H16A 118.6 . . ? C16 C17 C18 120.5(6) . . ? C16 C17 H17A 119.7 . . ? C18 C17 H17A 119.7 . . ? C19 C18 C17 116.4(6) . . ? C19 C18 C37 124.5(6) . . ? C17 C18 C37 119.2(5) . . ? C18 C19 C20 121.0(6) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? N3 C20 C19 122.8(6) . . ? N3 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? C22 C21 C26 117.0(6) . . ? C22 C21 C37 121.3(6) . . ? C26 C21 C37 121.5(5) . . ? C21 C22 C23 121.6(7) . . ? C21 C22 H22A 119.2 . . ? C23 C22 H22A 119.2 . . ? C24 C23 C22 120.6(7) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 N4 120.2(8) . . ? C23 C24 C25 118.2(7) . . ? N4 C24 C25 121.6(9) . . ? C26 C25 C24 120.4(7) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C21 122.2(6) . . ? C25 C26 H26A 118.9 . . ? C21 C26 H26A 118.9 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 116.3(6) . . ? C34 C29 C37 119.7(6) . . ? C30 C29 C37 123.8(6) . . ? C31 C30 C29 121.0(6) . . ? C31 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C30 C31 C32 122.7(6) . . ? C30 C31 H31A 118.6 . . ? C32 C31 H31A 118.6 . . ? N5 C32 C33 122.4(7) . . ? N5 C32 C31 121.7(7) . . ? C33 C32 C31 115.8(6) . . ? C34 C33 C32 121.4(7) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C33 C34 C29 122.7(7) . . ? C33 C34 H34A 118.6 . . ? C29 C34 H34A 118.6 . . ? N5 C35 H35A 109.5 . . ? N5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C29 106.3(5) . . ? C38 C37 C18 108.3(5) . . ? C29 C37 C18 110.0(5) . . ? C38 C37 C21 108.0(5) . . ? C29 C37 C21 114.6(5) . . ? C18 C37 C21 109.4(5) . . ? N6 C38 C37 179.4(9) . . ? F6 P1 F6 170.8(9) . 2_756 ? F6 P1 F7 94.6(4) . . ? F6 P1 F7 94.6(4) 2_756 . ? F6 P1 F5 85.4(4) . . ? F6 P1 F5 85.4(4) 2_756 . ? F7 P1 F5 180.000(9) . . ? F6 P1 F4 91.4(4) . . ? F6 P1 F4 88.8(4) 2_756 . ? F7 P1 F4 88.8(3) . . ? F5 P1 F4 91.2(3) . . ? F6 P1 F4 88.8(4) . 2_756 ? F6 P1 F4 91.4(4) 2_756 2_756 ? F7 P1 F4 88.8(3) . 2_756 ? F5 P1 F4 91.2(3) . 2_756 ? F4 P1 F4 177.6(5) . 2_756 ? F3 P2 F3 89.7(5) 2_655 . ? F3 P2 F1 89.7(3) 2_655 2_655 ? F3 P2 F1 179.4(3) . 2_655 ? F3 P2 F1 179.4(3) 2_655 . ? F3 P2 F1 89.7(3) . . ? F1 P2 F1 90.9(4) 2_655 . ? F3 P2 F2 90.0(3) 2_655 2_655 ? F3 P2 F2 90.4(3) . 2_655 ? F1 P2 F2 89.4(3) 2_655 2_655 ? F1 P2 F2 90.2(3) . 2_655 ? F3 P2 F2 90.4(3) 2_655 . ? F3 P2 F2 90.0(3) . . ? F1 P2 F2 90.2(3) 2_655 . ? F1 P2 F2 89.4(3) . . ? F2 P2 F2 179.5(5) 2_655 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Re1 N1 C4 -1.7(6) . . . . ? C3 Re1 N1 C4 -157(2) . . . . ? C1 Re1 N1 C4 87.8(6) . . . . ? N2 Re1 N1 C4 -179.1(6) . . . . ? N3 Re1 N1 C4 -94.0(6) . . . . ? C2 Re1 N1 C15 178.0(5) . . . . ? C3 Re1 N1 C15 22(3) . . . . ? C1 Re1 N1 C15 -92.4(5) . . . . ? N2 Re1 N1 C15 0.6(4) . . . . ? N3 Re1 N1 C15 85.8(5) . . . . ? C2 Re1 N2 C13 153(2) . . . . ? C3 Re1 N2 C13 2.3(6) . . . . ? C1 Re1 N2 C13 -86.6(6) . . . . ? N1 Re1 N2 C13 180.0(6) . . . . ? N3 Re1 N2 C13 93.3(6) . . . . ? C2 Re1 N2 C14 -27(3) . . . . ? C3 Re1 N2 C14 -177.1(5) . . . . ? C1 Re1 N2 C14 94.0(5) . . . . ? N1 Re1 N2 C14 0.6(4) . . . . ? N3 Re1 N2 C14 -86.0(4) . . . . ? C2 Re1 N3 C20 -53.9(5) . . . . ? C3 Re1 N3 C20 -140.1(5) . . . . ? C1 Re1 N3 C20 124(8) . . . . ? N1 Re1 N3 C20 45.4(5) . . . . ? N2 Re1 N3 C20 121.3(5) . . . . ? C2 Re1 N3 C16 126.0(5) . . . . ? C3 Re1 N3 C16 39.8(5) . . . . ? C1 Re1 N3 C16 -56(8) . . . . ? N1 Re1 N3 C16 -134.7(5) . . . . ? N2 Re1 N3 C16 -58.8(5) . . . . ? C2 Re1 C1 O1 -8(16) . . . . ? C3 Re1 C1 O1 78(16) . . . . ? N1 Re1 C1 O1 -107(16) . . . . ? N2 Re1 C1 O1 177(100) . . . . ? N3 Re1 C1 O1 175(100) . . . . ? C3 Re1 C2 O2 -23(39) . . . . ? C1 Re1 C2 O2 66(39) . . . . ? N1 Re1 C2 O2 160(39) . . . . ? N2 Re1 C2 O2 -173(100) . . . . ? N3 Re1 C2 O2 -114(39) . . . . ? C2 Re1 C3 O3 -77(18) . . . . ? C1 Re1 C3 O3 -166(18) . . . . ? N1 Re1 C3 O3 79(18) . . . . ? N2 Re1 C3 O3 100(18) . . . . ? N3 Re1 C3 O3 16(18) . . . . ? C15 N1 C4 C5 0.8(11) . . . . ? Re1 N1 C4 C5 -179.4(6) . . . . ? N1 C4 C5 C6 -1.0(13) . . . . ? C4 C5 C6 C7 1.0(14) . . . . ? C5 C6 C7 C8 -179.4(8) . . . . ? C5 C6 C7 C15 -0.8(12) . . . . ? C6 C7 C8 C9 178.8(9) . . . . ? C15 C7 C8 C9 0.2(13) . . . . ? C7 C8 C9 C10 -0.6(14) . . . . ? C8 C9 C10 C11 179.1(9) . . . . ? C8 C9 C10 C14 0.0(12) . . . . ? C14 C10 C11 C12 -0.3(12) . . . . ? C9 C10 C11 C12 -179.4(8) . . . . ? C10 C11 C12 C13 0.8(14) . . . . ? C14 N2 C13 C12 -0.7(10) . . . . ? Re1 N2 C13 C12 179.9(5) . . . . ? C11 C12 C13 N2 -0.3(13) . . . . ? C13 N2 C14 C15 178.7(6) . . . . ? Re1 N2 C14 C15 -1.8(7) . . . . ? C13 N2 C14 C10 1.2(10) . . . . ? Re1 N2 C14 C10 -179.4(5) . . . . ? C11 C10 C14 N2 -0.7(10) . . . . ? C9 C10 C14 N2 178.5(7) . . . . ? C11 C10 C14 C15 -178.2(7) . . . . ? C9 C10 C14 C15 0.9(10) . . . . ? C4 N1 C15 C14 178.0(6) . . . . ? Re1 N1 C15 C14 -1.8(8) . . . . ? C4 N1 C15 C7 -0.6(10) . . . . ? Re1 N1 C15 C7 179.6(5) . . . . ? N2 C14 C15 N1 2.4(9) . . . . ? C10 C14 C15 N1 -179.9(6) . . . . ? N2 C14 C15 C7 -179.0(6) . . . . ? C10 C14 C15 C7 -1.3(10) . . . . ? C6 C7 C15 N1 0.6(11) . . . . ? C8 C7 C15 N1 179.3(7) . . . . ? C6 C7 C15 C14 -177.9(7) . . . . ? C8 C7 C15 C14 0.8(11) . . . . ? C20 N3 C16 C17 -2.1(9) . . . . ? Re1 N3 C16 C17 178.0(5) . . . . ? N3 C16 C17 C18 0.8(10) . . . . ? C16 C17 C18 C19 1.0(9) . . . . ? C16 C17 C18 C37 -178.9(6) . . . . ? C17 C18 C19 C20 -1.3(9) . . . . ? C37 C18 C19 C20 178.5(6) . . . . ? C16 N3 C20 C19 1.8(9) . . . . ? Re1 N3 C20 C19 -178.3(4) . . . . ? C18 C19 C20 N3 -0.1(9) . . . . ? C26 C21 C22 C23 -0.7(10) . . . . ? C37 C21 C22 C23 -175.8(6) . . . . ? C21 C22 C23 C24 1.5(12) . . . . ? C22 C23 C24 N4 177.9(7) . . . . ? C22 C23 C24 C25 -1.8(12) . . . . ? C27 N4 C24 C23 2.8(14) . . . . ? C28 N4 C24 C23 175.6(9) . . . . ? C27 N4 C24 C25 -177.5(9) . . . . ? C28 N4 C24 C25 -4.7(14) . . . . ? C23 C24 C25 C26 1.4(12) . . . . ? N4 C24 C25 C26 -178.3(7) . . . . ? C24 C25 C26 C21 -0.7(12) . . . . ? C22 C21 C26 C25 0.3(10) . . . . ? C37 C21 C26 C25 175.3(6) . . . . ? C34 C29 C30 C31 1.8(10) . . . . ? C37 C29 C30 C31 176.1(6) . . . . ? C29 C30 C31 C32 -1.1(11) . . . . ? C35 N5 C32 C33 -179.8(8) . . . . ? C36 N5 C32 C33 -4.8(11) . . . . ? C35 N5 C32 C31 -1.4(11) . . . . ? C36 N5 C32 C31 173.6(7) . . . . ? C30 C31 C32 N5 -179.0(7) . . . . ? C30 C31 C32 C33 -0.5(11) . . . . ? N5 C32 C33 C34 179.8(7) . . . . ? C31 C32 C33 C34 1.3(11) . . . . ? C32 C33 C34 C29 -0.6(12) . . . . ? C30 C29 C34 C33 -0.9(10) . . . . ? C37 C29 C34 C33 -175.5(7) . . . . ? C34 C29 C37 C38 75.1(7) . . . . ? C30 C29 C37 C38 -99.1(7) . . . . ? C34 C29 C37 C18 -42.0(8) . . . . ? C30 C29 C37 C18 143.8(6) . . . . ? C34 C29 C37 C21 -165.7(6) . . . . ? C30 C29 C37 C21 20.2(8) . . . . ? C19 C18 C37 C38 -3.8(8) . . . . ? C17 C18 C37 C38 176.1(5) . . . . ? C19 C18 C37 C29 112.0(6) . . . . ? C17 C18 C37 C29 -68.1(7) . . . . ? C19 C18 C37 C21 -121.3(6) . . . . ? C17 C18 C37 C21 58.6(7) . . . . ? C22 C21 C37 C38 -20.3(8) . . . . ? C26 C21 C37 C38 164.9(6) . . . . ? C22 C21 C37 C29 -138.6(6) . . . . ? C26 C21 C37 C29 46.6(8) . . . . ? C22 C21 C37 C18 97.4(7) . . . . ? C26 C21 C37 C18 -77.4(7) . . . . ? C29 C37 C38 N6 88(81) . . . . ? C18 C37 C38 N6 -154(100) . . . . ? C21 C37 C38 N6 -36(81) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.479 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.097 # Attachment 'revised_3.cif' data_Complex_3 _database_code_depnum_ccdc_archive 'CCDC 760666' #TrackingRef 'revised_3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H30 Br2 F3 N6 O6 Re S' _chemical_formula_sum 'C39 H30 Br2 F3 N6 O6 Re S' _chemical_formula_weight 1113.77 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Br Br -0.2901 2.4595 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 17.4444(3) _cell_length_b 11.1975(2) _cell_length_c 20.8885(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.2079(15) _cell_angle_gamma 90.00 _cell_volume 4079.32(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 18509 _cell_measurement_theta_min 3.0704 _cell_measurement_theta_max 28.0001 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 5.056 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.59388 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET) (compiled Jan 8 2009,16:24:04) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Mo)' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.1270 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62975 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7169 _reflns_number_gt 4632 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford, 2009)' _computing_cell_refinement 'CrysAlisPro (Oxford, 2009)' _computing_data_reduction 'CrysAlisPro (Oxford, 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 (Farrugia, 1997)' _computing_publication_material SHELXL-97 _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^)+(0.0493P)^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 7169 _refine_ls_number_parameters 599 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.825157(13) 1.10319(2) 0.546410(13) 0.04257(10) Uani 1 1 d . . . C1 C 0.8906(4) 1.0440(6) 0.6151(4) 0.0511(17) Uani 1 1 d . . . C2 C 0.9160(4) 1.1113(6) 0.4952(4) 0.062(2) Uani 1 1 d . . . C3 C 0.8483(4) 1.2634(6) 0.5751(4) 0.063(2) Uani 1 1 d . . . C4 C 0.7554(4) 1.1958(5) 0.4156(3) 0.0500(16) Uani 1 1 d . . . H4A H 0.8061 1.1988 0.4028 0.060 Uiso 1 1 calc R . . C5 C 0.6977(4) 1.2288(6) 0.3719(4) 0.0593(19) Uani 1 1 d . . . H5A H 0.7099 1.2520 0.3306 0.071 Uiso 1 1 calc R . . C6 C 0.6245(4) 1.2267(6) 0.3903(3) 0.0579(19) Uani 1 1 d . . . H6A H 0.5858 1.2485 0.3613 0.069 Uiso 1 1 calc R . . C7 C 0.6052(3) 1.1920(5) 0.4525(3) 0.0449(16) Uani 1 1 d . . . C8 C 0.5296(3) 1.1844(5) 0.4763(4) 0.0504(17) Uani 1 1 d . . . C9 C 0.5159(3) 1.1459(5) 0.5352(4) 0.0497(17) Uani 1 1 d . . . C10 C 0.5774(4) 1.1164(5) 0.5797(3) 0.0486(16) Uani 1 1 d . . . C11 C 0.5684(4) 1.0808(6) 0.6436(4) 0.0616(19) Uani 1 1 d . . . H11A H 0.5197 1.0756 0.6606 0.074 Uiso 1 1 calc R . . C12 C 0.6313(4) 1.0542(7) 0.6802(4) 0.070(2) Uani 1 1 d . . . H12A H 0.6256 1.0307 0.7225 0.084 Uiso 1 1 calc R . . C13 C 0.7042(4) 1.0621(6) 0.6547(3) 0.0593(19) Uani 1 1 d . . . H13A H 0.7466 1.0438 0.6807 0.071 Uiso 1 1 calc R . . C14 C 0.6517(4) 1.1229(5) 0.5568(3) 0.0427(15) Uani 1 1 d . . . C15 C 0.6669(3) 1.1590(5) 0.4934(3) 0.0368(14) Uani 1 1 d . . . C16 C 0.7700(3) 0.8371(5) 0.5512(3) 0.0376(14) Uani 1 1 d . . . H16A H 0.7656 0.8554 0.5944 0.045 Uiso 1 1 calc R . . C17 C 0.7499(3) 0.7228(5) 0.5306(3) 0.0400(14) Uani 1 1 d . . . H17A H 0.7311 0.6674 0.5595 0.048 Uiso 1 1 calc R . . C18 C 0.7578(3) 0.6926(5) 0.4674(3) 0.0366(14) Uani 1 1 d . . . C19 C 0.7868(4) 0.7788(6) 0.4279(3) 0.0604(19) Uani 1 1 d . . . H19A H 0.7955 0.7610 0.3852 0.072 Uiso 1 1 calc R . . C20 C 0.8029(4) 0.8901(5) 0.4507(3) 0.0564(18) Uani 1 1 d . . . H20A H 0.8201 0.9475 0.4223 0.068 Uiso 1 1 calc R . . C21 C 0.7355(3) 0.5675(5) 0.4402(3) 0.0412(15) Uani 1 1 d . . . C22 C 0.8058(3) 0.5116(5) 0.4078(3) 0.0425(15) Uani 1 1 d . . . C23 C 0.8056(4) 0.4652(6) 0.3472(3) 0.0529(17) Uani 1 1 d . . . H23A H 0.7616 0.4725 0.3216 0.063 Uiso 1 1 calc R . . C24 C 0.8692(4) 0.4076(6) 0.3228(3) 0.0576(18) Uani 1 1 d . . . H24A H 0.8666 0.3759 0.2817 0.069 Uiso 1 1 calc R . . C25 C 0.9365(4) 0.3964(6) 0.3587(3) 0.0530(17) Uani 1 1 d . . . C26 C 0.9364(4) 0.4448(7) 0.4199(4) 0.066(2) Uani 1 1 d . . . H26A H 0.9805 0.4383 0.4455 0.080 Uiso 1 1 calc R . . C27 C 0.8740(4) 0.5016(6) 0.4436(3) 0.0592(19) Uani 1 1 d . . . H27A H 0.8769 0.5343 0.4845 0.071 Uiso 1 1 calc R . . C28 C 0.9964(4) 0.2851(9) 0.2732(4) 0.102(3) Uani 1 1 d . . . H28A H 0.9544 0.2298 0.2707 0.153 Uiso 1 1 calc R . . H28B H 1.0435 0.2435 0.2658 0.153 Uiso 1 1 calc R . . H28C H 0.9892 0.3460 0.2412 0.153 Uiso 1 1 calc R . . C29 C 1.0679(4) 0.3253(7) 0.3764(4) 0.077(2) Uani 1 1 d . . . H29A H 1.0850 0.4024 0.3907 0.115 Uiso 1 1 calc R . . H29B H 1.1076 0.2875 0.3526 0.115 Uiso 1 1 calc R . . H29C H 1.0558 0.2769 0.4127 0.115 Uiso 1 1 calc R . . C30 C 0.6630(4) 0.5820(5) 0.3969(3) 0.0517(17) Uani 1 1 d . . . C31 C 0.5917(4) 0.5460(6) 0.4178(4) 0.068(2) Uani 1 1 d . . . H31A H 0.5890 0.5072 0.4571 0.081 Uiso 1 1 calc R . . C32 C 0.5244(5) 0.5651(7) 0.3832(5) 0.082(3) Uani 1 1 d . . . H32A H 0.4779 0.5412 0.3999 0.098 Uiso 1 1 calc R . . C33 C 0.5263(6) 0.6192(8) 0.3244(5) 0.087(3) Uani 1 1 d . . . C34 C 0.5978(6) 0.6542(7) 0.3009(4) 0.083(2) Uani 1 1 d . . . H34A H 0.6003 0.6896 0.2607 0.100 Uiso 1 1 calc R . . C35 C 0.6664(5) 0.6360(6) 0.3379(4) 0.070(2) Uani 1 1 d . . . H35A H 0.7133 0.6606 0.3221 0.084 Uiso 1 1 calc R . . C36 C 0.3850(7) 0.6064(10) 0.3135(7) 0.165(6) Uani 1 1 d . . . H36A H 0.3804 0.6362 0.3564 0.247 Uiso 1 1 calc R . . H36B H 0.3807 0.5209 0.3138 0.247 Uiso 1 1 calc R . . H36C H 0.3449 0.6396 0.2868 0.247 Uiso 1 1 calc R . . C37 C 0.4642(8) 0.6831(13) 0.2245(5) 0.182(7) Uani 1 1 d . . . H37A H 0.4954 0.7536 0.2244 0.273 Uiso 1 1 calc R . . H37B H 0.4141 0.7016 0.2074 0.273 Uiso 1 1 calc R . . H37C H 0.4873 0.6227 0.1986 0.273 Uiso 1 1 calc R . . C38 C 0.7167(3) 0.4883(5) 0.4939(3) 0.0429(15) Uani 1 1 d . . . N1 N 0.7154(3) 1.0948(4) 0.5944(2) 0.0416(12) Uani 1 1 d . . . N2 N 0.7410(3) 1.1603(4) 0.4745(2) 0.0380(12) Uani 1 1 d . . . N3 N 0.7950(3) 0.9207(4) 0.5123(2) 0.0373(12) Uani 1 1 d . . . N4 N 0.9995(3) 0.3390(6) 0.3354(3) 0.0710(18) Uani 1 1 d . . . N5 N 0.4579(5) 0.6399(8) 0.2892(4) 0.113(3) Uani 1 1 d . . . N6 N 0.7007(3) 0.4269(5) 0.5339(3) 0.0640(16) Uani 1 1 d . . . Br1 Br 0.41544(4) 1.12659(6) 0.56534(4) 0.0708(2) Uani 1 1 d . . . Br2 Br 0.44818(4) 1.22609(8) 0.41896(5) 0.0810(3) Uani 1 1 d . . . O1 O 0.9299(3) 1.0122(5) 0.6559(3) 0.0742(15) Uani 1 1 d . . . O2 O 0.9678(3) 1.1175(5) 0.4628(3) 0.104(2) Uani 1 1 d . . . O3 O 0.8652(3) 1.3557(5) 0.5914(3) 0.096(2) Uani 1 1 d . . . C2S C 0.2695(9) 0.3438(11) 0.2694(6) 0.065(5) Uani 0.50 1 d PD A -1 F4 F 0.3233(9) 0.3233(12) 0.3132(7) 0.098(5) Uani 0.50 1 d PDU A -1 F5 F 0.2212(10) 0.417(2) 0.2983(9) 0.087(6) Uani 0.50 1 d PDU A -1 F6 F 0.3043(11) 0.416(2) 0.2276(8) 0.090(6) Uani 0.50 1 d PDU A -1 S2 S 0.22913(18) 0.2166(3) 0.23339(17) 0.0405(8) Uani 0.50 1 d PD A -1 O7 O 0.1896(13) 0.157(3) 0.2800(11) 0.046(5) Uani 0.50 1 d PDU A -1 O8 O 0.2915(13) 0.158(3) 0.2053(11) 0.043(5) Uani 0.50 1 d PDU A -1 O9 O 0.1805(8) 0.2614(12) 0.1839(7) 0.056(4) Uani 0.50 1 d PDU A -1 C1S C 0.6711(9) 0.9900(16) 0.2384(7) 0.068(5) Uani 0.50 1 d PDU B -1 F1 F 0.6353(9) 0.9044(16) 0.2048(7) 0.185(8) Uani 0.50 1 d PDU B -1 F2 F 0.6529(9) 1.0866(16) 0.2089(10) 0.227(12) Uani 0.50 1 d PDU B -1 F3 F 0.6335(10) 0.9882(13) 0.2903(7) 0.188(8) Uani 0.50 1 d PDU B -1 S1 S 0.7648(8) 0.9732(8) 0.2449(9) 0.182(6) Uani 0.50 1 d PDU B -1 O4 O 0.7939(14) 1.071(2) 0.2770(10) 0.234(15) Uani 0.50 1 d PDU B -1 O5 O 0.7813(15) 0.8632(16) 0.2783(8) 0.219(12) Uani 0.50 1 d PDU B -1 O6 O 0.7910(11) 0.9632(13) 0.1819(5) 0.123(6) Uani 0.50 1 d PDU 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 Re1 0.04553(16) 0.03529(13) 0.04666(16) -0.00057(15) -0.00452(11) 0.00086(12) C1 0.050(4) 0.037(4) 0.067(5) -0.005(4) 0.006(4) -0.001(3) C2 0.070(5) 0.042(4) 0.074(5) 0.022(4) -0.008(4) 0.004(4) C3 0.089(5) 0.036(4) 0.061(5) 0.002(4) -0.039(4) -0.005(4) C4 0.068(4) 0.038(4) 0.044(4) 0.004(3) 0.006(4) -0.002(3) C5 0.079(5) 0.051(4) 0.048(5) 0.009(4) -0.007(4) 0.002(4) C6 0.080(6) 0.047(4) 0.046(5) 0.002(4) -0.020(4) 0.006(4) C7 0.050(4) 0.027(3) 0.057(5) -0.008(3) -0.008(3) 0.001(3) C8 0.046(4) 0.034(3) 0.071(5) -0.001(4) -0.016(4) -0.002(3) C9 0.049(4) 0.028(3) 0.072(5) -0.010(3) -0.005(4) 0.006(3) C10 0.050(4) 0.041(4) 0.055(4) -0.009(4) 0.009(3) 0.001(3) C11 0.057(4) 0.068(5) 0.060(5) 0.000(4) 0.009(4) 0.007(4) C12 0.081(6) 0.076(5) 0.055(5) 0.006(4) 0.016(5) 0.020(4) C13 0.064(5) 0.074(5) 0.040(4) -0.006(4) 0.000(4) 0.017(4) C14 0.055(4) 0.029(3) 0.044(4) -0.008(3) -0.006(3) 0.006(3) C15 0.047(4) 0.023(3) 0.040(4) -0.004(3) -0.001(3) 0.002(3) C16 0.047(4) 0.041(3) 0.025(3) -0.003(3) 0.004(3) -0.007(3) C17 0.049(4) 0.043(4) 0.028(4) 0.007(3) 0.003(3) 0.002(3) C18 0.053(4) 0.027(3) 0.030(4) 0.001(3) -0.002(3) 0.005(3) C19 0.103(5) 0.047(4) 0.032(4) -0.004(3) 0.012(4) -0.004(4) C20 0.094(5) 0.031(3) 0.045(4) 0.002(4) 0.017(4) -0.004(3) C21 0.060(4) 0.035(3) 0.028(3) -0.001(3) -0.001(3) 0.007(3) C22 0.057(4) 0.033(3) 0.038(4) -0.003(3) 0.000(3) 0.004(3) C23 0.061(4) 0.047(4) 0.050(4) -0.008(4) -0.008(3) 0.005(3) C24 0.068(5) 0.060(4) 0.044(4) -0.017(4) -0.001(4) 0.006(4) C25 0.058(4) 0.049(4) 0.052(4) -0.002(4) 0.009(4) 0.002(4) C26 0.057(4) 0.082(5) 0.059(5) -0.015(4) -0.006(4) 0.022(4) C27 0.065(4) 0.072(5) 0.040(4) -0.022(4) -0.006(3) 0.011(4) C28 0.073(5) 0.143(9) 0.092(7) -0.063(7) 0.022(5) 0.020(5) C29 0.063(5) 0.085(6) 0.083(6) -0.014(5) 0.023(5) 0.010(4) C30 0.071(5) 0.037(4) 0.046(4) -0.009(3) -0.007(3) 0.011(3) C31 0.077(5) 0.041(4) 0.084(6) 0.001(4) -0.027(5) 0.002(4) C32 0.075(5) 0.072(6) 0.096(7) -0.003(5) -0.032(5) 0.004(4) C33 0.102(7) 0.069(6) 0.088(7) -0.025(5) -0.038(6) 0.028(5) C34 0.131(8) 0.069(5) 0.049(5) -0.003(4) -0.008(5) 0.032(6) C35 0.096(6) 0.062(5) 0.051(5) -0.003(4) -0.016(4) 0.033(4) C36 0.100(8) 0.154(11) 0.237(16) 0.011(11) -0.089(9) -0.031(7) C37 0.245(15) 0.211(15) 0.085(9) -0.042(10) -0.091(10) 0.112(12) C38 0.053(4) 0.030(3) 0.045(4) -0.011(3) -0.004(3) 0.001(3) N1 0.046(3) 0.041(3) 0.038(3) -0.003(3) 0.002(2) 0.007(2) N2 0.048(3) 0.025(2) 0.041(3) -0.002(2) -0.003(3) 0.000(2) N3 0.054(3) 0.034(3) 0.024(3) -0.006(2) -0.001(2) 0.011(2) N4 0.052(4) 0.091(5) 0.070(5) -0.025(4) 0.019(3) 0.013(3) N5 0.114(7) 0.113(7) 0.109(7) -0.006(5) -0.057(5) 0.025(5) N6 0.093(4) 0.042(4) 0.057(4) 0.000(3) 0.006(3) -0.006(3) Br1 0.0499(4) 0.0570(5) 0.1058(7) -0.0153(4) 0.0094(4) 0.0058(3) Br2 0.0626(5) 0.0803(6) 0.0987(7) 0.0074(5) -0.0320(4) 0.0092(4) O1 0.065(3) 0.084(4) 0.073(4) 0.018(3) -0.020(3) 0.003(3) O2 0.076(4) 0.106(5) 0.133(6) 0.037(4) 0.046(4) 0.005(3) O3 0.145(5) 0.047(3) 0.093(5) -0.004(3) -0.058(4) -0.011(3) C2S 0.071(14) 0.086(11) 0.040(12) -0.001(9) 0.017(9) -0.022(10) F4 0.098(8) 0.107(12) 0.087(10) -0.009(9) -0.045(7) -0.027(9) F5 0.091(11) 0.078(10) 0.093(13) -0.037(11) 0.017(8) 0.001(8) F6 0.103(13) 0.072(9) 0.095(13) -0.009(10) 0.024(9) -0.038(10) S2 0.040(2) 0.0442(17) 0.037(2) -0.0009(16) 0.0021(15) -0.0039(15) O7 0.044(11) 0.058(8) 0.037(11) 0.000(9) -0.008(8) -0.008(9) O8 0.042(11) 0.060(8) 0.028(9) -0.010(9) -0.009(7) 0.005(9) O9 0.053(7) 0.072(9) 0.043(7) -0.002(7) -0.011(5) 0.003(7) C1S 0.142(17) 0.049(9) 0.013(9) -0.002(9) 0.022(10) 0.009(12) F1 0.173(14) 0.24(2) 0.148(14) -0.082(14) 0.058(12) -0.044(13) F2 0.194(19) 0.22(2) 0.28(3) 0.100(18) 0.120(18) 0.092(16) F3 0.31(2) 0.137(13) 0.128(14) -0.024(11) 0.131(15) -0.038(14) S1 0.369(19) 0.115(6) 0.060(6) -0.004(9) -0.011(9) 0.055(17) O4 0.22(3) 0.32(3) 0.17(2) -0.17(2) 0.085(18) -0.08(2) O5 0.28(3) 0.25(2) 0.132(18) 0.147(17) 0.08(2) 0.06(2) O6 0.227(17) 0.093(10) 0.051(9) 0.010(8) 0.025(10) 0.022(12) _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 Re1 C3 1.931(7) . ? Re1 C1 1.932(8) . ? Re1 C2 1.933(9) . ? Re1 N2 2.174(5) . ? Re1 N1 2.182(5) . ? Re1 N3 2.224(4) . ? C1 O1 1.139(8) . ? C2 O2 1.143(8) . ? C3 O3 1.126(7) . ? C4 N2 1.323(7) . ? C4 C5 1.394(9) . ? C4 H4A 0.9300 . ? C5 C6 1.342(9) . ? C5 H5A 0.9300 . ? C6 C7 1.404(9) . ? C6 H6A 0.9300 . ? C7 C15 1.409(8) . ? C7 C8 1.421(9) . ? C8 C9 1.330(9) . ? C8 Br2 1.898(6) . ? C9 C10 1.443(9) . ? C9 Br1 1.887(6) . ? C10 C14 1.393(9) . ? C10 C11 1.403(9) . ? C11 C12 1.357(10) . ? C11 H11A 0.9300 . ? C12 C13 1.393(9) . ? C12 H12A 0.9300 . ? C13 N1 1.329(8) . ? C13 H13A 0.9300 . ? C14 N1 1.383(7) . ? C14 C15 1.416(8) . ? C15 N2 1.359(7) . ? C16 N3 1.320(7) . ? C16 C17 1.393(8) . ? C16 H16A 0.9300 . ? C17 C18 1.372(8) . ? C17 H17A 0.9300 . ? C18 C19 1.374(8) . ? C18 C21 1.558(8) . ? C19 C20 1.361(8) . ? C19 H19A 0.9300 . ? C20 N3 1.341(8) . ? C20 H20A 0.9300 . ? C21 C38 1.473(9) . ? C21 C22 1.546(8) . ? C21 C30 1.548(9) . ? C22 C23 1.368(8) . ? C22 C27 1.397(8) . ? C23 C24 1.391(8) . ? C23 H23A 0.9300 . ? C24 C25 1.384(9) . ? C24 H24A 0.9300 . ? C25 N4 1.371(8) . ? C25 C26 1.388(9) . ? C26 C27 1.364(8) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 N4 1.434(9) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N4 1.460(9) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C35 1.376(10) . ? C30 C31 1.388(9) . ? C31 C32 1.381(9) . ? C31 H31A 0.9300 . ? C32 C33 1.371(12) . ? C32 H32A 0.9300 . ? C33 C34 1.406(12) . ? C33 N5 1.408(10) . ? C34 C35 1.426(11) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 N5 1.430(14) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N5 1.441(14) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 N6 1.121(7) . ? C2S F4 1.317(14) . ? C2S F5 1.326(15) . ? C2S F6 1.346(14) . ? C2S S2 1.750(11) . ? S2 O7 1.375(14) . ? S2 O8 1.412(14) . ? S2 O9 1.416(11) . ? C1S F3 1.278(14) . ? C1S F2 1.282(16) . ? C1S F1 1.335(15) . ? C1S S1 1.648(16) . ? S1 O4 1.377(16) . ? S1 O6 1.406(17) . ? S1 O5 1.442(15) . ? 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 C3 Re1 C1 88.4(3) . . ? C3 Re1 C2 87.7(3) . . ? C1 Re1 C2 87.1(3) . . ? C3 Re1 N2 94.3(2) . . ? C1 Re1 N2 173.6(2) . . ? C2 Re1 N2 98.8(2) . . ? C3 Re1 N1 94.4(3) . . ? C1 Re1 N1 98.9(2) . . ? C2 Re1 N1 173.7(2) . . ? N2 Re1 N1 75.13(18) . . ? C3 Re1 N3 178.3(2) . . ? C1 Re1 N3 93.1(2) . . ? C2 Re1 N3 93.2(2) . . ? N2 Re1 N3 84.11(16) . . ? N1 Re1 N3 84.49(17) . . ? O1 C1 Re1 178.1(6) . . ? O2 C2 Re1 177.2(7) . . ? O3 C3 Re1 176.9(7) . . ? N2 C4 C5 122.7(6) . . ? N2 C4 H4A 118.7 . . ? C5 C4 H4A 118.7 . . ? C6 C5 C4 119.1(7) . . ? C6 C5 H5A 120.4 . . ? C4 C5 H5A 120.4 . . ? C5 C6 C7 121.2(6) . . ? C5 C6 H6A 119.4 . . ? C7 C6 H6A 119.4 . . ? C6 C7 C15 116.0(6) . . ? C6 C7 C8 125.7(6) . . ? C15 C7 C8 118.3(6) . . ? C9 C8 C7 122.0(6) . . ? C9 C8 Br2 121.1(5) . . ? C7 C8 Br2 116.8(5) . . ? C8 C9 C10 121.6(6) . . ? C8 C9 Br1 122.1(5) . . ? C10 C9 Br1 116.3(5) . . ? C14 C10 C11 117.7(6) . . ? C14 C10 C9 116.8(6) . . ? C11 C10 C9 125.5(6) . . ? C12 C11 C10 119.5(6) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 120.3(7) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? N1 C13 C12 122.2(6) . . ? N1 C13 H13A 118.9 . . ? C12 C13 H13A 118.9 . . ? N1 C14 C10 122.3(6) . . ? N1 C14 C15 115.7(5) . . ? C10 C14 C15 122.0(6) . . ? N2 C15 C7 122.8(6) . . ? N2 C15 C14 118.1(5) . . ? C7 C15 C14 119.1(6) . . ? N3 C16 C17 123.1(5) . . ? N3 C16 H16A 118.5 . . ? C17 C16 H16A 118.5 . . ? C18 C17 C16 119.6(5) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 116.8(5) . . ? C17 C18 C21 122.9(5) . . ? C19 C18 C21 120.3(5) . . ? C20 C19 C18 120.6(6) . . ? C20 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? N3 C20 C19 123.0(6) . . ? N3 C20 H20A 118.5 . . ? C19 C20 H20A 118.5 . . ? C38 C21 C22 106.3(5) . . ? C38 C21 C30 108.4(5) . . ? C22 C21 C30 115.6(5) . . ? C38 C21 C18 108.7(5) . . ? C22 C21 C18 109.3(5) . . ? C30 C21 C18 108.3(4) . . ? C23 C22 C27 116.8(5) . . ? C23 C22 C21 124.9(5) . . ? C27 C22 C21 118.2(5) . . ? C22 C23 C24 121.9(6) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 121.2(6) . . ? C25 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? N4 C25 C24 121.9(6) . . ? N4 C25 C26 121.7(6) . . ? C24 C25 C26 116.5(6) . . ? C27 C26 C25 122.2(6) . . ? C27 C26 H26A 118.9 . . ? C25 C26 H26A 118.9 . . ? C26 C27 C22 121.3(6) . . ? C26 C27 H27A 119.3 . . ? C22 C27 H27A 119.3 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C35 C30 C31 117.7(7) . . ? C35 C30 C21 121.3(7) . . ? C31 C30 C21 120.9(6) . . ? C32 C31 C30 123.2(8) . . ? C32 C31 H31A 118.4 . . ? C30 C31 H31A 118.4 . . ? C33 C32 C31 120.1(8) . . ? C33 C32 H32A 120.0 . . ? C31 C32 H32A 120.0 . . ? C32 C33 C34 118.3(8) . . ? C32 C33 N5 120.4(10) . . ? C34 C33 N5 121.3(10) . . ? C33 C34 C35 120.7(8) . . ? C33 C34 H34A 119.6 . . ? C35 C34 H34A 119.6 . . ? C30 C35 C34 119.8(8) . . ? C30 C35 H35A 120.1 . . ? C34 C35 H35A 120.1 . . ? N5 C36 H36A 109.5 . . ? N5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 C21 178.1(7) . . ? C13 N1 C14 118.0(5) . . ? C13 N1 Re1 126.5(4) . . ? C14 N1 Re1 115.5(4) . . ? C4 N2 C15 118.3(5) . . ? C4 N2 Re1 126.3(4) . . ? C15 N2 Re1 115.5(4) . . ? C16 N3 C20 116.9(5) . . ? C16 N3 Re1 122.2(4) . . ? C20 N3 Re1 120.9(4) . . ? C25 N4 C28 120.2(6) . . ? C25 N4 C29 119.5(6) . . ? C28 N4 C29 120.1(6) . . ? C33 N5 C36 121.4(10) . . ? C33 N5 C37 117.7(10) . . ? C36 N5 C37 120.5(9) . . ? F4 C2S F5 104.0(12) . . ? F4 C2S F6 103.3(12) . . ? F5 C2S F6 103.0(10) . . ? F4 C2S S2 115.5(10) . . ? F5 C2S S2 116.2(13) . . ? F6 C2S S2 113.3(12) . . ? O7 S2 O8 118.1(6) . . ? O7 S2 O9 112.7(10) . . ? O8 S2 O9 108.5(10) . . ? O7 S2 C2S 107.0(15) . . ? O8 S2 C2S 104.6(15) . . ? O9 S2 C2S 104.8(7) . . ? F3 C1S F2 107.1(14) . . ? F3 C1S F1 101.1(13) . . ? F2 C1S F1 104.2(14) . . ? F3 C1S S1 117.1(13) . . ? F2 C1S S1 111.8(13) . . ? F1 C1S S1 114.4(13) . . ? O4 S1 O6 113.3(14) . . ? O4 S1 O5 112.1(15) . . ? O6 S1 O5 108.6(11) . . ? O4 S1 C1S 107.7(14) . . ? O6 S1 C1S 105.9(13) . . ? O5 S1 C1S 109.0(14) . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Re1 C1 O1 -10(19) . . . . ? C2 Re1 C1 O1 78(19) . . . . ? N2 Re1 C1 O1 -124(18) . . . . ? N1 Re1 C1 O1 -104(19) . . . . ? N3 Re1 C1 O1 171(19) . . . . ? C3 Re1 C2 O2 -95(14) . . . . ? C1 Re1 C2 O2 177(100) . . . . ? N2 Re1 C2 O2 -1(14) . . . . ? N1 Re1 C2 O2 15(15) . . . . ? N3 Re1 C2 O2 84(14) . . . . ? C1 Re1 C3 O3 58(13) . . . . ? C2 Re1 C3 O3 -29(13) . . . . ? N2 Re1 C3 O3 -128(13) . . . . ? N1 Re1 C3 O3 157(13) . . . . ? N3 Re1 C3 O3 -151(9) . . . . ? N2 C4 C5 C6 1.1(10) . . . . ? C4 C5 C6 C7 0.1(10) . . . . ? C5 C6 C7 C15 -0.7(9) . . . . ? C5 C6 C7 C8 -178.7(6) . . . . ? C6 C7 C8 C9 177.1(6) . . . . ? C15 C7 C8 C9 -0.8(9) . . . . ? C6 C7 C8 Br2 -0.6(8) . . . . ? C15 C7 C8 Br2 -178.5(4) . . . . ? C7 C8 C9 C10 3.7(10) . . . . ? Br2 C8 C9 C10 -178.6(4) . . . . ? C7 C8 C9 Br1 -176.1(4) . . . . ? Br2 C8 C9 Br1 1.5(8) . . . . ? C8 C9 C10 C14 -3.9(9) . . . . ? Br1 C9 C10 C14 176.0(4) . . . . ? C8 C9 C10 C11 176.7(6) . . . . ? Br1 C9 C10 C11 -3.4(9) . . . . ? C14 C10 C11 C12 -0.2(10) . . . . ? C9 C10 C11 C12 179.3(6) . . . . ? C10 C11 C12 C13 0.0(11) . . . . ? C11 C12 C13 N1 -0.3(11) . . . . ? C11 C10 C14 N1 0.6(9) . . . . ? C9 C10 C14 N1 -178.8(5) . . . . ? C11 C10 C14 C15 -179.4(6) . . . . ? C9 C10 C14 C15 1.2(8) . . . . ? C6 C7 C15 N2 0.2(8) . . . . ? C8 C7 C15 N2 178.3(5) . . . . ? C6 C7 C15 C14 -180.0(5) . . . . ? C8 C7 C15 C14 -1.8(8) . . . . ? N1 C14 C15 N2 1.4(7) . . . . ? C10 C14 C15 N2 -178.6(5) . . . . ? N1 C14 C15 C7 -178.4(5) . . . . ? C10 C14 C15 C7 1.6(8) . . . . ? N3 C16 C17 C18 1.8(8) . . . . ? C16 C17 C18 C19 0.8(8) . . . . ? C16 C17 C18 C21 -179.0(5) . . . . ? C17 C18 C19 C20 -3.1(10) . . . . ? C21 C18 C19 C20 176.8(6) . . . . ? C18 C19 C20 N3 3.0(11) . . . . ? C17 C18 C21 C38 -8.0(7) . . . . ? C19 C18 C21 C38 172.1(6) . . . . ? C17 C18 C21 C22 -123.7(6) . . . . ? C19 C18 C21 C22 56.5(7) . . . . ? C17 C18 C21 C30 109.6(6) . . . . ? C19 C18 C21 C30 -70.3(7) . . . . ? C38 C21 C22 C23 113.9(7) . . . . ? C30 C21 C22 C23 -6.5(8) . . . . ? C18 C21 C22 C23 -128.9(6) . . . . ? C38 C21 C22 C27 -62.6(7) . . . . ? C30 C21 C22 C27 177.0(6) . . . . ? C18 C21 C22 C27 54.5(7) . . . . ? C27 C22 C23 C24 1.9(10) . . . . ? C21 C22 C23 C24 -174.7(6) . . . . ? C22 C23 C24 C25 -1.1(10) . . . . ? C23 C24 C25 N4 179.5(6) . . . . ? C23 C24 C25 C26 0.4(10) . . . . ? N4 C25 C26 C27 -179.7(7) . . . . ? C24 C25 C26 C27 -0.6(11) . . . . ? C25 C26 C27 C22 1.5(12) . . . . ? C23 C22 C27 C26 -2.0(10) . . . . ? C21 C22 C27 C26 174.8(6) . . . . ? C38 C21 C30 C35 -169.9(6) . . . . ? C22 C21 C30 C35 -50.7(8) . . . . ? C18 C21 C30 C35 72.3(7) . . . . ? C38 C21 C30 C31 13.4(7) . . . . ? C22 C21 C30 C31 132.6(6) . . . . ? C18 C21 C30 C31 -104.4(6) . . . . ? C35 C30 C31 C32 -1.9(10) . . . . ? C21 C30 C31 C32 174.9(6) . . . . ? C30 C31 C32 C33 1.7(12) . . . . ? C31 C32 C33 C34 0.0(12) . . . . ? C31 C32 C33 N5 -179.4(7) . . . . ? C32 C33 C34 C35 -1.3(12) . . . . ? N5 C33 C34 C35 178.1(7) . . . . ? C31 C30 C35 C34 0.6(10) . . . . ? C21 C30 C35 C34 -176.3(6) . . . . ? C33 C34 C35 C30 1.0(11) . . . . ? C22 C21 C38 N6 -108(21) . . . . ? C30 C21 C38 N6 17(21) . . . . ? C18 C21 C38 N6 135(21) . . . . ? C12 C13 N1 C14 0.7(10) . . . . ? C12 C13 N1 Re1 -176.9(5) . . . . ? C10 C14 N1 C13 -0.9(8) . . . . ? C15 C14 N1 C13 179.1(5) . . . . ? C10 C14 N1 Re1 177.0(4) . . . . ? C15 C14 N1 Re1 -3.0(6) . . . . ? C3 Re1 N1 C13 -86.5(6) . . . . ? C1 Re1 N1 C13 2.6(6) . . . . ? C2 Re1 N1 C13 164(2) . . . . ? N2 Re1 N1 C13 -179.7(6) . . . . ? N3 Re1 N1 C13 94.9(5) . . . . ? C3 Re1 N1 C14 95.8(4) . . . . ? C1 Re1 N1 C14 -175.1(4) . . . . ? C2 Re1 N1 C14 -14(2) . . . . ? N2 Re1 N1 C14 2.6(4) . . . . ? N3 Re1 N1 C14 -82.8(4) . . . . ? C5 C4 N2 C15 -1.6(9) . . . . ? C5 C4 N2 Re1 178.7(4) . . . . ? C7 C15 N2 C4 0.9(8) . . . . ? C14 C15 N2 C4 -178.9(5) . . . . ? C7 C15 N2 Re1 -179.3(4) . . . . ? C14 C15 N2 Re1 0.9(6) . . . . ? C3 Re1 N2 C4 84.5(5) . . . . ? C1 Re1 N2 C4 -161.0(19) . . . . ? C2 Re1 N2 C4 -3.8(5) . . . . ? N1 Re1 N2 C4 178.0(5) . . . . ? N3 Re1 N2 C4 -96.2(5) . . . . ? C3 Re1 N2 C15 -95.3(4) . . . . ? C1 Re1 N2 C15 19(2) . . . . ? C2 Re1 N2 C15 176.4(4) . . . . ? N1 Re1 N2 C15 -1.8(4) . . . . ? N3 Re1 N2 C15 84.0(4) . . . . ? C17 C16 N3 C20 -2.0(8) . . . . ? C17 C16 N3 Re1 179.1(4) . . . . ? C19 C20 N3 C16 -0.4(9) . . . . ? C19 C20 N3 Re1 178.5(5) . . . . ? C3 Re1 N3 C16 -100(9) . . . . ? C1 Re1 N3 C16 51.0(5) . . . . ? C2 Re1 N3 C16 138.2(5) . . . . ? N2 Re1 N3 C16 -123.2(4) . . . . ? N1 Re1 N3 C16 -47.7(4) . . . . ? C3 Re1 N3 C20 81(9) . . . . ? C1 Re1 N3 C20 -127.9(5) . . . . ? C2 Re1 N3 C20 -40.6(5) . . . . ? N2 Re1 N3 C20 57.9(5) . . . . ? N1 Re1 N3 C20 133.5(5) . . . . ? C24 C25 N4 C28 -2.0(11) . . . . ? C26 C25 N4 C28 177.1(8) . . . . ? C24 C25 N4 C29 -177.4(7) . . . . ? C26 C25 N4 C29 1.7(11) . . . . ? C32 C33 N5 C36 0.6(14) . . . . ? C34 C33 N5 C36 -178.9(9) . . . . ? C32 C33 N5 C37 -172.3(9) . . . . ? C34 C33 N5 C37 8.3(13) . . . . ? F4 C2S S2 O7 67(2) . . . . ? F5 C2S S2 O7 -55(2) . . . . ? F6 C2S S2 O7 -174.4(19) . . . . ? F4 C2S S2 O8 -59.3(19) . . . . ? F5 C2S S2 O8 178.5(19) . . . . ? F6 C2S S2 O8 60(2) . . . . ? F4 C2S S2 O9 -173.4(15) . . . . ? F5 C2S S2 O9 64.4(16) . . . . ? F6 C2S S2 O9 -54.5(16) . . . . ? F3 C1S S1 O4 -65.7(19) . . . . ? F2 C1S S1 O4 58.3(18) . . . . ? F1 C1S S1 O4 176.3(16) . . . . ? F3 C1S S1 O6 172.7(12) . . . . ? F2 C1S S1 O6 -63.2(17) . . . . ? F1 C1S S1 O6 54.8(15) . . . . ? F3 C1S S1 O5 56.0(19) . . . . ? F2 C1S S1 O5 -179.9(16) . . . . ? F1 C1S S1 O5 -61.9(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.505 _refine_diff_density_min -0.984 _refine_diff_density_rms 0.101 # start Validation Reply Form _vrf_PLAT220_Complex_3 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) 4.92 Ratio. RESPONSE: This is attributed to the diorderness of the terminal methyl groups ; _vrf_PLAT222_Complex_3 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) 6.07 Ratio RESPONSE: This is attributed to the diorderness of the terminal methyl groups ; _vrf_PLAT242_Complex_3 ; PROBLEM: Check Low Ueq as Compared to Neighbors for N5 RESPONSE: This is the result of the disorderness of the terminal methyl groups and the N atom. ; # end Validation Reply Form