Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name J.R.Dilworth 'Andrew R. Cowley' 'Paul Donnelly' 'Susan J. Ross' _publ_contact_author_name 'Jonathan Dilworth' _publ_contact_author_address ; Department of Chemistry University of Oxford Chemistry Research Laboratory 12 Mansfield Road Oxford OX1 3TA UNITED KINGDOM ; _publ_contact_author_email JON.DILWORTH@CHEM.OX.AC.UK _publ_section_title ; Rhenium diazenide ternary complexes with dithiocarbamate ligands: towards new rhenium radiopharmaceuticals ; # Attachment 'ARC368.CIF' data_CRYSTALS_cif_arc368 _database_code_depnum_ccdc_archive 'CCDC 617262' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 12.0739(2) _cell_angle_alpha 90 _cell_length_b 11.4142(2) _cell_angle_beta 99.3207(7) _cell_length_c 25.3935(4) _cell_angle_gamma 90 _cell_volume 3453.4 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C30 H35 N5 O1 P1 Re1 S4 ' _chemical_formula_moiety ' C30 H35 N5 O1 P1 Re1 S4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 827.06 _cell_measurement_reflns_used 44526 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' needle ' _exptl_crystal_colour ' red-brown ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1643.969 _exptl_absorpt_coefficient_mu 3.838 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.83 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 44526 _reflns_number_total 7868 # 8255 unique reflections including systematic absences _diffrn_reflns_av_R_equivalents 0.069 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_gt 4725 _diffrn_reflns_theta_min 5.13 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _refine_diff_density_min -1.16 _refine_diff_density_max 1.16 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 4725 _refine_ls_number_parameters 378 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0403 _refine_ls_goodness_of_fit_ref 1.0398 _refine_ls_shift/su_max 0.014285 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 0.585 0.310 0.376 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.607358(18) 0.30695(2) 0.137687(8) 0.0292 1.0000 Uani N1 0.4629(4) 0.2809(4) 0.12729(18) 0.0330 1.0000 Uani N2 0.3572(4) 0.2627(5) 0.1167(2) 0.0380 1.0000 Uani C1 0.2996(5) 0.2323(5) 0.1589(2) 0.0335 1.0000 Uani N3 0.1877(4) 0.2248(5) 0.1419(2) 0.0449 1.0000 Uani C2 0.1245(5) 0.1978(7) 0.1797(3) 0.0512 1.0000 Uani C3 0.1675(6) 0.1737(6) 0.2318(3) 0.0482 1.0000 Uani C4 0.2826(6) 0.1800(6) 0.2476(3) 0.0447 1.0000 Uani C5 0.3506(5) 0.2097(5) 0.2103(2) 0.0347 1.0000 Uani S1 0.81296(12) 0.33763(14) 0.17619(6) 0.0384 1.0000 Uani S2 0.62778(11) 0.34746(13) 0.23372(6) 0.0326 1.0000 Uani C6 0.7703(4) 0.3587(5) 0.2369(2) 0.0313 1.0000 Uani N4 0.8387(4) 0.3800(5) 0.2816(2) 0.0395 1.0000 Uani C7 0.7971(5) 0.3930(6) 0.3322(3) 0.0440 1.0000 Uani C8 0.9601(5) 0.3795(8) 0.2843(3) 0.0546 1.0000 Uani S3 0.59884(13) 0.51932(14) 0.11736(6) 0.0384 1.0000 Uani S4 0.64845(14) 0.33335(14) 0.04953(6) 0.0405 1.0000 Uani C9 0.6346(5) 0.4836(6) 0.0563(2) 0.0380 1.0000 Uani N5 0.6548(4) 0.5584(5) 0.0199(2) 0.0410 1.0000 Uani C10 0.6877(6) 0.5173(7) -0.0302(2) 0.0484 1.0000 Uani C11 0.6434(6) 0.6846(6) 0.0267(3) 0.0499 1.0000 Uani P1 0.65050(12) 0.10357(14) 0.14748(6) 0.0329 1.0000 Uani C12 0.5357(5) 0.0048(6) 0.1201(3) 0.0397 1.0000 Uani C13 0.4697(5) 0.0350(6) 0.0717(2) 0.0428 1.0000 Uani C14 0.3883(6) -0.0397(7) 0.0468(3) 0.0518 1.0000 Uani C15 0.3727(6) -0.1482(7) 0.0695(3) 0.0550 1.0000 Uani C16 0.4370(6) -0.1807(6) 0.1168(3) 0.0506 1.0000 Uani C17 0.5190(5) -0.1049(5) 0.1428(3) 0.0403 1.0000 Uani C18 0.6933(5) 0.0590(5) 0.2172(2) 0.0313 1.0000 Uani C19 0.6140(5) 0.0396(5) 0.2504(3) 0.0380 1.0000 Uani C20 0.6478(6) 0.0221(6) 0.3044(3) 0.0439 1.0000 Uani C21 0.7605(6) 0.0238(6) 0.3261(3) 0.0494 1.0000 Uani C22 0.8391(6) 0.0428(7) 0.2935(3) 0.0538 1.0000 Uani C23 0.8073(5) 0.0608(6) 0.2394(2) 0.0394 1.0000 Uani C24 0.7651(5) 0.0434(6) 0.1156(3) 0.0415 1.0000 Uani C25 0.8326(5) 0.1149(8) 0.0890(3) 0.0527 1.0000 Uani C26 0.9164(6) 0.0683(9) 0.0639(3) 0.0649 1.0000 Uani C27 0.9314(6) -0.0523(11) 0.0643(3) 0.0756 1.0000 Uani C28 0.8668(6) -0.1252(8) 0.0901(3) 0.0676 1.0000 Uani C29 0.7830(5) -0.0760(7) 0.1159(3) 0.0511 1.0000 Uani O1 0.098(1) 0.277(1) 0.0333(5) 0.101(4) 0.711(13) Uiso C30 0.0411(16) 0.3564(18) 0.0479(8) 0.110(6) 0.711(13) Uiso O2 0.8793(11) 0.6159(12) 0.1413(6) 0.038(4) 0.289(13) Uiso C31 0.9287(18) 0.571(2) 0.1016(9) 0.043(6) 0.289(13) Uiso H1 0.1295 0.2589 0.0713 0.1217 0.7108 Uiso H2 0.8599 0.5347 0.1515 0.0450 0.2892 Uiso H21 0.0412 0.1954 0.1688 0.0623 1.0000 Uiso H31 0.1170 0.1520 0.2578 0.0604 1.0000 Uiso H41 0.3165 0.1634 0.2854 0.0549 1.0000 Uiso H51 0.4340 0.2145 0.2206 0.0418 1.0000 Uiso H71 0.8615 0.4087 0.3614 0.0526 1.0000 Uiso H72 0.7430 0.4599 0.3296 0.0526 1.0000 Uiso H73 0.7583 0.3193 0.3403 0.0526 1.0000 Uiso H81 0.9968 0.3975 0.3216 0.0656 1.0000 Uiso H82 0.9819 0.4400 0.2595 0.0656 1.0000 Uiso H83 0.9849 0.3005 0.2738 0.0656 1.0000 Uiso H101 0.6996 0.5862 -0.0530 0.0580 1.0000 Uiso H102 0.7589 0.4713 -0.0221 0.0580 1.0000 Uiso H103 0.6271 0.4665 -0.0497 0.0580 1.0000 Uiso H111 0.6625 0.7262 -0.0053 0.0604 1.0000 Uiso H112 0.6956 0.7108 0.0593 0.0604 1.0000 Uiso H113 0.5644 0.7034 0.0308 0.0604 1.0000 Uiso H131 0.4818 0.1122 0.0549 0.0519 1.0000 Uiso H141 0.3405 -0.0162 0.0126 0.0636 1.0000 Uiso H151 0.3141 -0.2029 0.0512 0.0682 1.0000 Uiso H161 0.4253 -0.2590 0.1327 0.0630 1.0000 Uiso H171 0.5656 -0.1285 0.1773 0.0497 1.0000 Uiso H191 0.5323 0.0383 0.2351 0.0470 1.0000 Uiso H201 0.5904 0.0081 0.3280 0.0543 1.0000 Uiso H211 0.7846 0.0113 0.3653 0.0591 1.0000 Uiso H221 0.9205 0.0436 0.3092 0.0640 1.0000 Uiso H231 0.8654 0.0750 0.2162 0.0478 1.0000 Uiso H251 0.8200 0.2015 0.0881 0.0649 1.0000 Uiso H261 0.9651 0.1206 0.0459 0.0800 1.0000 Uiso H271 0.9902 -0.0869 0.0454 0.0916 1.0000 Uiso H281 0.8792 -0.2118 0.0905 0.0804 1.0000 Uiso H291 0.7358 -0.1285 0.1348 0.0615 1.0000 Uiso H301 -0.0037 0.3949 0.0160 0.1326 0.7108 Uiso H302 0.0915 0.4156 0.0686 0.1326 0.7108 Uiso H303 -0.0109 0.3232 0.0710 0.1326 0.7108 Uiso H311 0.9594 0.6365 0.0820 0.0519 0.2892 Uiso H312 0.9912 0.5177 0.1171 0.0519 0.2892 Uiso H313 0.8721 0.5262 0.0763 0.0519 0.2892 Uiso 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 0.02699(11) 0.03637(13) 0.02573(11) -0.00003(11) 0.00855(7) -0.00700(11) N1 0.043(3) 0.033(3) 0.024(2) 0.0043(18) 0.0088(19) -0.003(2) N2 0.024(2) 0.051(3) 0.038(3) 0.008(2) 0.0039(19) -0.006(2) C1 0.031(3) 0.032(3) 0.038(3) 0.001(2) 0.005(2) -0.005(2) N3 0.033(2) 0.050(3) 0.052(3) 0.007(2) 0.007(2) -0.008(2) C2 0.032(3) 0.061(4) 0.062(4) 0.011(4) 0.014(3) -0.001(3) C3 0.046(3) 0.048(4) 0.057(4) 0.004(3) 0.027(3) -0.002(3) C4 0.051(3) 0.042(4) 0.044(3) 0.004(3) 0.017(3) 0.001(3) C5 0.035(3) 0.029(3) 0.040(3) 0.001(2) 0.007(2) -0.002(2) S1 0.0303(6) 0.0526(9) 0.0348(7) -0.0023(6) 0.0127(6) -0.0094(6) S2 0.0285(6) 0.0398(7) 0.0311(7) -0.0022(6) 0.0097(5) -0.0056(6) C6 0.034(3) 0.025(3) 0.035(3) 0.005(2) 0.007(2) -0.007(2) N4 0.031(2) 0.051(3) 0.036(3) -0.004(2) 0.006(2) -0.010(2) C7 0.036(3) 0.058(4) 0.038(3) -0.006(3) 0.005(3) -0.008(3) C8 0.030(3) 0.085(6) 0.049(4) -0.013(4) 0.007(3) -0.007(3) S3 0.0413(7) 0.0410(8) 0.0346(7) 0.0013(6) 0.0112(6) -0.0074(6) S4 0.0475(8) 0.0449(9) 0.0312(7) -0.0004(6) 0.0128(6) -0.0136(7) C9 0.032(3) 0.046(3) 0.035(3) 0.002(3) 0.003(2) -0.014(3) N5 0.036(2) 0.050(3) 0.036(3) 0.010(2) 0.003(2) -0.010(2) C10 0.048(3) 0.071(5) 0.026(3) 0.006(3) 0.006(3) -0.012(3) C11 0.058(4) 0.044(4) 0.049(4) 0.006(3) 0.012(3) -0.014(3) P1 0.0293(6) 0.0407(8) 0.0309(7) -0.0028(6) 0.0119(5) -0.0009(6) C12 0.033(3) 0.041(3) 0.048(4) -0.008(3) 0.014(3) -0.005(3) C13 0.039(3) 0.057(4) 0.034(3) -0.011(3) 0.010(3) -0.008(3) C14 0.049(4) 0.069(5) 0.041(4) -0.015(3) 0.018(3) -0.008(3) C15 0.049(4) 0.057(4) 0.064(5) -0.033(4) 0.026(4) -0.016(3) C16 0.052(4) 0.043(4) 0.063(4) -0.016(3) 0.027(3) -0.007(3) C17 0.038(3) 0.036(3) 0.050(4) -0.003(3) 0.017(3) -0.001(3) C18 0.034(3) 0.030(3) 0.030(3) -0.002(2) 0.008(2) 0.004(2) C19 0.040(3) 0.032(3) 0.045(3) -0.003(3) 0.017(3) 0.008(2) C20 0.057(4) 0.037(3) 0.042(3) 0.010(3) 0.020(3) 0.004(3) C21 0.061(4) 0.052(4) 0.035(3) 0.006(3) 0.006(3) 0.014(3) C22 0.046(4) 0.065(5) 0.049(4) 0.001(3) 0.003(3) 0.008(3) C23 0.039(3) 0.044(3) 0.036(3) -0.004(3) 0.010(2) 0.006(3) C24 0.026(3) 0.058(4) 0.041(3) -0.018(3) 0.008(2) 0.005(3) C25 0.037(3) 0.083(5) 0.042(4) -0.010(4) 0.018(3) -0.006(3) C26 0.045(4) 0.101(7) 0.055(4) -0.025(5) 0.024(3) -0.010(4) C27 0.036(3) 0.142(9) 0.050(4) -0.037(5) 0.014(3) -0.003(5) C28 0.037(3) 0.090(6) 0.074(5) -0.039(5) 0.003(3) 0.018(4) C29 0.028(3) 0.073(5) 0.052(4) -0.027(4) 0.007(3) -0.005(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 1.747(5) yes Re1 . S1 . 2.5407(14) yes Re1 . S2 . 2.4550(14) yes Re1 . S3 . 2.4771(16) yes Re1 . S4 . 2.3893(14) yes Re1 . P1 . 2.3833(16) yes N1 . N2 . 1.277(7) yes N2 . C1 . 1.411(7) yes C1 . N3 . 1.352(7) yes C1 . C5 . 1.376(8) yes N3 . C2 . 1.354(8) yes C2 . C3 . 1.37(1) yes C2 . H21 . 1.000 no C3 . C4 . 1.38(1) yes C3 . H31 . 1.000 no C4 . C5 . 1.391(8) yes C4 . H41 . 1.000 no C5 . H51 . 1.000 no S1 . C6 . 1.719(6) yes S2 . C6 . 1.715(5) yes C6 . N4 . 1.313(8) yes N4 . C7 . 1.462(8) yes N4 . C8 . 1.456(7) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no C8 . H81 . 1.000 no C8 . H82 . 1.000 no C8 . H83 . 1.000 no S3 . C9 . 1.725(6) yes S4 . C9 . 1.735(7) yes C9 . N5 . 1.310(8) yes N5 . C10 . 1.471(8) yes N5 . C11 . 1.460(9) yes C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no C11 . H111 . 1.000 no C11 . H112 . 1.000 no C11 . H113 . 1.000 no P1 . C12 . 1.833(6) yes P1 . C18 . 1.833(6) yes P1 . C24 . 1.844(6) yes C12 . C13 . 1.395(9) yes C12 . C17 . 1.406(9) yes C13 . C14 . 1.376(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.391(11) yes C14 . H141 . 1.000 no C15 . C16 . 1.372(12) yes C15 . H151 . 1.000 no C16 . C17 . 1.398(9) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C18 . C19 . 1.393(8) yes C18 . C23 . 1.400(8) yes C19 . C20 . 1.382(9) yes C19 . H191 . 1.000 no C20 . C21 . 1.38(1) yes C20 . H201 . 1.000 no C21 . C22 . 1.37(1) yes C21 . H211 . 1.000 no C22 . C23 . 1.38(1) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no C24 . C25 . 1.401(9) yes C24 . C29 . 1.38(1) yes C25 . C26 . 1.387(9) yes C25 . H251 . 1.000 no C26 . C27 . 1.388(14) yes C26 . H261 . 1.000 no C27 . C28 . 1.377(13) yes C27 . H271 . 1.000 no C28 . C29 . 1.408(9) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no O1 . C30 . 1.23(2) yes O1 . H1 . 1.000 no C30 . H301 . 1.00 no C30 . H302 . 1.00 no C30 . H303 . 1.00 no O2 . C31 . 1.35(3) yes O2 . H2 . 1.000 no C31 . H311 . 1.00 no C31 . H312 . 1.00 no C31 . H313 . 1.00 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . S1 . 166.20(15) yes N1 . Re1 . S2 . 96.86(15) yes S1 . Re1 . S2 . 69.94(4) yes N1 . Re1 . S3 . 97.37(15) yes S1 . Re1 . S3 . 87.15(5) yes S2 . Re1 . S3 . 90.96(5) yes N1 . Re1 . S4 . 103.51(15) yes S1 . Re1 . S4 . 90.29(5) yes S2 . Re1 . S4 . 154.73(5) yes S3 . Re1 . S4 . 71.89(5) yes N1 . Re1 . P1 . 92.64(16) yes S1 . Re1 . P1 . 84.88(5) yes S2 . Re1 . P1 . 95.44(5) yes S3 . Re1 . P1 . 167.40(5) yes S4 . Re1 . P1 . 98.37(5) yes Re1 . N1 . N2 . 176.6(4) yes N1 . N2 . C1 . 118.6(5) yes N2 . C1 . N3 . 111.4(5) yes N2 . C1 . C5 . 124.5(5) yes N3 . C1 . C5 . 124.1(5) yes C1 . N3 . C2 . 116.0(6) yes N3 . C2 . C3 . 124.1(6) yes N3 . C2 . H21 . 117.9 no C3 . C2 . H21 . 117.9 no C2 . C3 . C4 . 118.4(6) yes C2 . C3 . H31 . 120.8 no C4 . C3 . H31 . 120.8 no C3 . C4 . C5 . 119.4(6) yes C3 . C4 . H41 . 120.3 no C5 . C4 . H41 . 120.3 no C1 . C5 . C4 . 117.9(5) yes C1 . C5 . H51 . 121.0 no C4 . C5 . H51 . 121.0 no Re1 . S1 . C6 . 87.06(19) yes Re1 . S2 . C6 . 90.0(2) yes S1 . C6 . S2 . 113.0(3) yes S1 . C6 . N4 . 124.3(4) yes S2 . C6 . N4 . 122.7(4) yes C6 . N4 . C7 . 121.4(5) yes C6 . N4 . C8 . 121.8(5) yes C7 . N4 . C8 . 116.4(5) yes N4 . C7 . H71 . 109.5 no N4 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no N4 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no N4 . C8 . H81 . 109.5 no N4 . C8 . H82 . 109.5 no H81 . C8 . H82 . 109.5 no N4 . C8 . H83 . 109.5 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no Re1 . S3 . C9 . 87.0(2) yes Re1 . S4 . C9 . 89.7(2) yes S3 . C9 . S4 . 111.4(3) yes S3 . C9 . N5 . 125.7(5) yes S4 . C9 . N5 . 122.9(5) yes C9 . N5 . C10 . 120.7(6) yes C9 . N5 . C11 . 121.8(6) yes C10 . N5 . C11 . 117.5(5) yes N5 . C10 . H101 . 109.5 no N5 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no N5 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no N5 . C11 . H111 . 109.5 no N5 . C11 . H112 . 109.5 no H111 . C11 . H112 . 109.5 no N5 . C11 . H113 . 109.5 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no Re1 . P1 . C12 . 114.8(2) yes Re1 . P1 . C18 . 113.18(18) yes C12 . P1 . C18 . 105.8(3) yes Re1 . P1 . C24 . 118.9(2) yes C12 . P1 . C24 . 100.3(3) yes C18 . P1 . C24 . 101.9(3) yes P1 . C12 . C13 . 118.1(5) yes P1 . C12 . C17 . 122.8(5) yes C13 . C12 . C17 . 118.7(6) yes C12 . C13 . C14 . 121.0(7) yes C12 . C13 . H131 . 119.5 no C14 . C13 . H131 . 119.5 no C13 . C14 . C15 . 119.8(7) yes C13 . C14 . H141 . 120.1 no C15 . C14 . H141 . 120.1 no C14 . C15 . C16 . 120.5(6) yes C14 . C15 . H151 . 119.8 no C16 . C15 . H151 . 119.8 no C15 . C16 . C17 . 120.2(7) yes C15 . C16 . H161 . 119.9 no C17 . C16 . H161 . 119.9 no C12 . C17 . C16 . 119.8(6) yes C12 . C17 . H171 . 120.1 no C16 . C17 . H171 . 120.1 no P1 . C18 . C19 . 121.0(4) yes P1 . C18 . C23 . 119.4(4) yes C19 . C18 . C23 . 119.0(5) yes C18 . C19 . C20 . 120.2(6) yes C18 . C19 . H191 . 119.9 no C20 . C19 . H191 . 119.9 no C19 . C20 . C21 . 120.5(6) yes C19 . C20 . H201 . 119.8 no C21 . C20 . H201 . 119.8 no C20 . C21 . C22 . 119.6(6) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 120.2 no C21 . C22 . C23 . 121.0(6) yes C21 . C22 . H221 . 119.5 no C23 . C22 . H221 . 119.5 no C18 . C23 . C22 . 119.7(6) yes C18 . C23 . H231 . 120.1 no C22 . C23 . H231 . 120.1 no P1 . C24 . C25 . 122.1(5) yes P1 . C24 . C29 . 119.6(5) yes C25 . C24 . C29 . 118.3(6) yes C24 . C25 . C26 . 121.6(8) yes C24 . C25 . H251 . 119.2 no C26 . C25 . H251 . 119.2 no C25 . C26 . C27 . 118.8(8) yes C25 . C26 . H261 . 120.6 no C27 . C26 . H261 . 120.6 no C26 . C27 . C28 . 121.3(7) yes C26 . C27 . H271 . 119.4 no C28 . C27 . H271 . 119.4 no C27 . C28 . C29 . 119.1(8) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.5 no C24 . C29 . C28 . 121.0(7) yes C24 . C29 . H291 . 119.5 no C28 . C29 . H291 . 119.5 no C30 . O1 . H1 . 90.2 no O1 . C30 . H301 . 109.5 no O1 . C30 . H302 . 109.5 no H301 . C30 . H302 . 109.4 no O1 . C30 . H303 . 109.5 no H301 . C30 . H303 . 109.4 no H302 . C30 . H303 . 109.5 no C31 . O2 . H2 . 89.6 no O2 . C31 . H311 . 109.5 no O2 . C31 . H312 . 109.5 no H311 . C31 . H312 . 109.5 no O2 . C31 . H313 . 109.5 no H311 . C31 . H313 . 109.5 no H312 . C31 . H313 . 109.5 no # Attachment 'ARC491.CIF' data_CRYSTALS_cif_arc491 _database_code_depnum_ccdc_archive 'CCDC 617263' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 11.4395(3) _cell_angle_alpha 78.9889(10) _cell_length_b 12.0609(3) _cell_angle_beta 75.1100(10) _cell_length_c 14.2850(4) _cell_angle_gamma 86.1885(13) _cell_volume 1869.3 _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C34 H37 Cl2 N5 O2 P1 Re1 S4 ' _chemical_formula_moiety ' C34 H37 Cl2 N5 O2 P1 Re1 S4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 964.02 _cell_measurement_reflns_used 27572 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' brown ' _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_meas ? _exptl_crystal_F_000 958.528 _exptl_absorpt_coefficient_mu 3.699 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 27572 _reflns_number_total 8511 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_gt 5554 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _refine_diff_density_min -1.20 _refine_diff_density_max 0.96 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 5554 _refine_ls_number_parameters 437 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0382 _refine_ls_goodness_of_fit_ref 1.0793 _refine_ls_shift/su_max 0.029246 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 0.199 0.0258 -.00981 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.38751(2) 0.23497(2) 0.238704(18) 0.0198 1.0000 Uani N1 0.2721(4) 0.2374(4) 0.1779(3) 0.0212 1.0000 Uani N2 0.1885(4) 0.2392(5) 0.1365(4) 0.0340 1.0000 Uani C1 0.0674(6) 0.2395(12) 0.2035(7) 0.024(3) 0.58(2) Uiso N3 0.0538(8) 0.2337(11) 0.3001(7) 0.040(3) 0.58(2) Uiso C2 -0.061(1) 0.2276(16) 0.3586(8) 0.065(5) 0.58(2) Uiso C3 -0.1629(9) 0.2333(13) 0.3243(9) 0.051(4) 0.58(2) Uiso C4 -0.1537(8) 0.243(1) 0.2297(9) 0.030(3) 0.58(2) Uiso C5 -0.0335(8) 0.2462(13) 0.1651(8) 0.047(4) 0.58(2) Uiso C51 0.0678(7) 0.240(2) 0.1806(8) 0.035(5) 0.42(2) Uiso N53 -0.0071(9) 0.2549(12) 0.1230(9) 0.035(4) 0.42(2) Uiso C52 -0.125(1) 0.2592(16) 0.1697(12) 0.044(5) 0.42(2) Uiso C53 -0.168(1) 0.2596(17) 0.2693(12) 0.042(6) 0.42(2) Uiso C54 -0.0936(12) 0.2361(19) 0.328(1) 0.053(6) 0.42(2) Uiso C55 0.0323(11) 0.223(2) 0.2818(9) 0.045(5) 0.42(2) Uiso S1 0.56672(12) 0.27926(12) 0.1095(1) 0.0227 1.0000 Uani S2 0.47808(13) 0.05547(13) 0.18906(11) 0.0254 1.0000 Uani C6 0.5863(5) 0.1367(5) 0.1021(4) 0.0230 1.0000 Uani N4 0.6756(4) 0.0966(4) 0.0372(4) 0.0249 1.0000 Uani C7 0.6890(6) -0.0229(5) 0.0293(5) 0.0315 1.0000 Uani C8 0.8213(6) -0.0582(6) 0.0129(5) 0.0347 1.0000 Uani O1 0.8940(4) 0.0118(4) -0.0710(3) 0.0371 1.0000 Uani C9 0.8862(6) 0.1256(6) -0.0551(6) 0.0395 1.0000 Uani C10 0.7576(6) 0.1709(5) -0.0430(5) 0.0326 1.0000 Uani S3 0.50839(13) 0.21638(13) 0.36711(11) 0.0259 1.0000 Uani S4 0.26901(13) 0.13901(14) 0.40002(11) 0.0279 1.0000 Uani C11 0.3867(5) 0.1498(5) 0.4512(4) 0.0259 1.0000 Uani N5 0.3836(5) 0.1108(5) 0.5452(4) 0.0297 1.0000 Uani C12 0.4726(6) 0.1399(6) 0.5933(5) 0.0370 1.0000 Uani C13 0.4105(7) 0.2123(7) 0.6670(6) 0.0463 1.0000 Uani O2 0.3085(5) 0.1582(5) 0.7371(4) 0.0500 1.0000 Uani C14 0.2225(7) 0.1309(7) 0.6888(5) 0.0421 1.0000 Uani C15 0.2777(6) 0.0559(6) 0.6158(4) 0.0347 1.0000 Uani P1 0.34805(13) 0.42598(13) 0.26023(11) 0.0212 1.0000 Uani C16 0.2334(5) 0.4955(5) 0.1978(4) 0.0232 1.0000 Uani C17 0.2459(6) 0.4867(5) 0.0997(4) 0.0272 1.0000 Uani C18 0.1572(6) 0.5304(6) 0.0512(5) 0.0320 1.0000 Uani C19 0.0556(6) 0.5834(6) 0.0998(5) 0.0363 1.0000 Uani C20 0.0433(6) 0.5947(6) 0.1969(5) 0.0337 1.0000 Uani C21 0.1328(5) 0.5522(5) 0.2449(4) 0.0277 1.0000 Uani C22 0.2928(5) 0.4558(5) 0.3850(4) 0.0237 1.0000 Uani C23 0.3508(6) 0.5257(6) 0.4239(5) 0.0368 1.0000 Uani C24 0.3024(8) 0.5472(7) 0.5192(6) 0.0505 1.0000 Uani C25 0.1951(7) 0.4984(7) 0.5743(5) 0.0465 1.0000 Uani C26 0.1361(6) 0.4269(6) 0.5367(5) 0.0351 1.0000 Uani C27 0.1856(6) 0.4038(5) 0.4433(4) 0.0284 1.0000 Uani C28 0.4804(5) 0.5174(5) 0.2076(4) 0.0236 1.0000 Uani C29 0.5895(6) 0.4867(5) 0.2328(5) 0.0300 1.0000 Uani C30 0.6908(5) 0.5509(6) 0.1924(5) 0.0343 1.0000 Uani C31 0.6875(6) 0.6475(6) 0.1234(5) 0.0316 1.0000 Uani C32 0.5812(6) 0.6796(6) 0.0951(5) 0.0341 1.0000 Uani C33 0.4783(6) 0.6153(6) 0.1375(5) 0.0335 1.0000 Uani C34 0.8369(9) 0.0780(8) 0.6938(7) 0.0607 1.0000 Uani Cl1 0.7434(3) 0.1983(3) 0.6886(2) 0.0845 1.0000 Uani Cl2 0.9692(3) 0.0950(4) 0.6013(3) 0.1281 1.0000 Uani H21 -0.0712 0.2183 0.4313 0.0776 0.5836 Uiso H31 -0.2445 0.2301 0.3715 0.0609 0.5836 Uiso H41 -0.2272 0.2482 0.2033 0.0362 0.5836 Uiso H51 -0.0227 0.2532 0.0925 0.0562 0.5836 Uiso H521 -0.1862 0.2623 0.1299 0.0530 0.4164 Uiso H531 -0.2546 0.2778 0.2972 0.0504 0.4164 Uiso H541 -0.1239 0.2278 0.4007 0.0631 0.4164 Uiso H551 0.0927 0.2024 0.3223 0.0541 0.4164 Uiso H71 0.6414 -0.0693 0.0915 0.0372 1.0000 Uiso H72 0.6583 -0.0351 -0.0274 0.0372 1.0000 Uiso H81 0.8494 -0.0521 0.0724 0.0393 1.0000 Uiso H82 0.8303 -0.1383 0.0024 0.0393 1.0000 Uiso H91 0.9403 0.1736 -0.1127 0.0452 1.0000 Uiso H92 0.9128 0.1281 0.0059 0.0452 1.0000 Uiso H101 0.7530 0.2485 -0.0271 0.0363 1.0000 Uiso H102 0.7330 0.1741 -0.1058 0.0363 1.0000 Uiso H121 0.5059 0.0695 0.6277 0.0437 1.0000 Uiso H122 0.5400 0.1825 0.5432 0.0437 1.0000 Uiso H131 0.4697 0.2293 0.7029 0.0565 1.0000 Uiso H132 0.3826 0.2844 0.6311 0.0565 1.0000 Uiso H141 0.1533 0.0911 0.7392 0.0493 1.0000 Uiso H142 0.1922 0.2023 0.6535 0.0493 1.0000 Uiso H151 0.3031 -0.0179 0.6512 0.0377 1.0000 Uiso H152 0.2170 0.0423 0.5800 0.0377 1.0000 Uiso H171 0.3195 0.4486 0.0639 0.0320 1.0000 Uiso H181 0.1673 0.5232 -0.0191 0.0399 1.0000 Uiso H191 -0.0089 0.6135 0.0654 0.0431 1.0000 Uiso H201 -0.0301 0.6336 0.2324 0.0395 1.0000 Uiso H211 0.1243 0.5627 0.3141 0.0323 1.0000 Uiso H231 0.4283 0.5616 0.3834 0.0436 1.0000 Uiso H241 0.3454 0.5974 0.5470 0.0627 1.0000 Uiso H251 0.1593 0.5146 0.6420 0.0524 1.0000 Uiso H261 0.0579 0.3922 0.5770 0.0405 1.0000 Uiso H271 0.1449 0.3499 0.4172 0.0335 1.0000 Uiso H291 0.5941 0.4160 0.2815 0.0365 1.0000 Uiso H301 0.7673 0.5277 0.2130 0.0406 1.0000 Uiso H311 0.7615 0.6941 0.0939 0.0371 1.0000 Uiso H321 0.5786 0.7489 0.0444 0.0415 1.0000 Uiso H331 0.4016 0.6393 0.1175 0.0402 1.0000 Uiso H341 0.8577 0.0622 0.7589 0.0747 1.0000 Uiso H342 0.7924 0.0127 0.6869 0.0747 1.0000 Uiso 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 0.01636(11) 0.02583(12) 0.01658(11) -0.00336(8) -0.00339(7) -0.00005(8) N1 0.020(2) 0.026(3) 0.017(2) -0.0037(19) -0.0029(18) -0.0024(19) N2 0.037(3) 0.034(3) 0.034(3) -0.007(2) -0.013(2) -0.001(2) S1 0.0185(7) 0.0250(7) 0.0221(7) -0.0027(6) -0.0022(5) 0.0006(5) S2 0.0242(7) 0.0239(7) 0.0240(7) -0.0011(6) -0.0012(6) 0.0006(6) C6 0.020(3) 0.032(3) 0.018(3) -0.002(2) -0.010(2) 0.002(2) N4 0.024(3) 0.025(3) 0.023(3) -0.007(2) -0.001(2) 0.004(2) C7 0.037(4) 0.029(3) 0.027(3) -0.009(3) -0.003(3) 0.003(3) C8 0.041(4) 0.027(3) 0.030(3) -0.006(3) 0.001(3) 0.006(3) O1 0.033(2) 0.033(3) 0.037(3) -0.009(2) 0.005(2) 0.006(2) C9 0.028(3) 0.033(4) 0.051(4) -0.013(3) 0.002(3) 0.006(3) C10 0.035(3) 0.027(3) 0.030(3) -0.005(3) 0.004(3) 0.003(3) S3 0.0199(7) 0.0341(8) 0.0229(7) -0.0008(6) -0.0072(6) -0.0011(6) S4 0.0232(7) 0.0398(9) 0.0190(7) -0.0016(6) -0.0034(6) -0.0059(6) C11 0.029(3) 0.030(3) 0.019(3) -0.004(2) -0.006(2) -0.001(3) N5 0.025(3) 0.040(3) 0.022(3) -0.001(2) -0.005(2) -0.003(2) C12 0.038(4) 0.044(4) 0.027(3) 0.002(3) -0.011(3) -0.001(3) C13 0.050(5) 0.051(5) 0.040(4) -0.007(4) -0.018(4) 0.006(4) O2 0.054(3) 0.065(4) 0.031(3) -0.016(3) -0.006(2) 0.003(3) C14 0.046(4) 0.050(4) 0.027(4) -0.003(3) -0.007(3) 0.002(3) C15 0.036(4) 0.042(4) 0.017(3) 0.009(3) 0.001(3) -0.002(3) P1 0.0183(7) 0.0272(8) 0.0183(7) -0.0044(6) -0.0048(6) 0.0004(6) C16 0.022(3) 0.029(3) 0.017(3) 0.004(2) -0.006(2) -0.002(2) C17 0.031(3) 0.025(3) 0.024(3) -0.003(2) -0.004(2) -0.001(3) C18 0.040(4) 0.034(4) 0.025(3) -0.006(3) -0.015(3) 0.002(3) C19 0.028(3) 0.038(4) 0.042(4) 0.004(3) -0.015(3) -0.001(3) C20 0.029(3) 0.038(4) 0.031(4) -0.003(3) -0.008(3) 0.007(3) C21 0.023(3) 0.034(3) 0.023(3) -0.002(3) -0.006(2) 0.006(3) C22 0.024(3) 0.030(3) 0.018(3) -0.003(2) -0.008(2) 0.004(2) C23 0.041(4) 0.046(4) 0.022(3) -0.011(3) -0.001(3) -0.007(3) C24 0.064(5) 0.060(5) 0.032(4) -0.022(4) -0.009(4) -0.009(4) C25 0.054(5) 0.055(5) 0.022(3) -0.007(3) 0.005(3) 0.002(4) C26 0.036(4) 0.042(4) 0.024(3) -0.006(3) -0.002(3) 0.005(3) C27 0.028(3) 0.033(3) 0.022(3) -0.007(3) -0.003(2) 0.001(3) C28 0.023(3) 0.031(3) 0.019(3) -0.010(2) -0.005(2) 0.000(2) C29 0.025(3) 0.031(3) 0.035(4) -0.002(3) -0.012(3) -0.003(3) C30 0.017(3) 0.038(4) 0.047(4) -0.002(3) -0.009(3) -0.003(3) C31 0.028(3) 0.032(4) 0.032(4) -0.008(3) 0.001(3) -0.013(3) C32 0.035(4) 0.040(4) 0.029(3) 0.002(3) -0.013(3) -0.014(3) C33 0.033(4) 0.032(4) 0.035(4) -0.004(3) -0.010(3) -0.001(3) C34 0.074(6) 0.052(5) 0.061(6) -0.022(4) -0.013(5) -0.015(5) Cl1 0.0872(19) 0.089(2) 0.0847(19) -0.0269(16) -0.0313(16) 0.0202(16) Cl2 0.0528(17) 0.190(4) 0.130(3) -0.019(3) -0.0109(18) 0.008(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 1.753(5) yes Re1 . S1 . 2.3912(14) yes Re1 . S2 . 2.4847(15) yes Re1 . S3 . 2.5362(15) yes Re1 . S4 . 2.4641(15) yes Re1 . P1 . 2.3804(16) yes N1 . N2 . 1.244(7) yes N2 . C1 . 1.467(7) yes N2 . C51 . 1.362(8) yes C1 . N3 . 1.337(8) yes C1 . C5 . 1.392(8) yes N3 . C2 . 1.359(9) yes C2 . C3 . 1.371(9) yes C2 . H21 . 1.000 no C3 . C4 . 1.311(9) yes C3 . H31 . 1.000 no C4 . C5 . 1.444(8) yes C4 . H41 . 1.000 no C5 . H51 . 1.000 no C51 . N53 . 1.314(8) yes C51 . C55 . 1.376(9) yes N53 . C52 . 1.349(9) yes C52 . C53 . 1.379(9) yes C52 . H521 . 1.000 no C53 . C54 . 1.315(9) yes C53 . H531 . 1.000 no C54 . C55 . 1.432(9) yes C54 . H541 . 1.000 no C55 . H551 . 1.000 no S1 . C6 . 1.739(6) yes S2 . C6 . 1.715(6) yes C6 . N4 . 1.325(7) yes N4 . C7 . 1.462(8) yes N4 . C10 . 1.471(8) yes C7 . C8 . 1.516(9) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C8 . O1 . 1.427(8) yes C8 . H81 . 1.000 no C8 . H82 . 1.000 no O1 . C9 . 1.426(8) yes C9 . C10 . 1.513(9) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no S3 . C11 . 1.717(6) yes S4 . C11 . 1.711(6) yes C11 . N5 . 1.327(8) yes N5 . C12 . 1.461(9) yes N5 . C15 . 1.465(8) yes C12 . C13 . 1.503(11) yes C12 . H121 . 1.000 no C12 . H122 . 1.000 no C13 . O2 . 1.43(1) yes C13 . H131 . 1.000 no C13 . H132 . 1.000 no O2 . C14 . 1.425(9) yes C14 . C15 . 1.50(1) yes C14 . H141 . 1.000 no C14 . H142 . 1.000 no C15 . H151 . 1.000 no C15 . H152 . 1.000 no P1 . C16 . 1.840(6) yes P1 . C22 . 1.828(6) yes P1 . C28 . 1.842(6) yes C16 . C17 . 1.396(8) yes C16 . C21 . 1.385(8) yes C17 . C18 . 1.392(9) yes C17 . H171 . 1.000 no C18 . C19 . 1.38(1) yes C18 . H181 . 1.000 no C19 . C20 . 1.39(1) yes C19 . H191 . 1.000 no C20 . C21 . 1.392(9) yes C20 . H201 . 1.000 no C21 . H211 . 1.000 no C22 . C23 . 1.379(9) yes C22 . C27 . 1.402(8) yes C23 . C24 . 1.398(9) yes C23 . H231 . 1.000 no C24 . C25 . 1.377(11) yes C24 . H241 . 1.000 no C25 . C26 . 1.389(11) yes C25 . H251 . 1.000 no C26 . C27 . 1.382(9) yes C26 . H261 . 1.000 no C27 . H271 . 1.000 no C28 . C29 . 1.394(8) yes C28 . C33 . 1.398(9) yes C29 . C30 . 1.371(9) yes C29 . H291 . 1.000 no C30 . C31 . 1.381(9) yes C30 . H301 . 1.000 no C31 . C32 . 1.386(9) yes C31 . H311 . 1.000 no C32 . C33 . 1.389(9) yes C32 . H321 . 1.000 no C33 . H331 . 1.000 no C34 . Cl1 . 1.75(1) yes C34 . Cl2 . 1.73(1) yes C34 . H341 . 1.00 no C34 . H342 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . S1 . 104.65(15) yes N1 . Re1 . S2 . 93.40(16) yes S1 . Re1 . S2 . 71.92(5) yes N1 . Re1 . S3 . 164.64(15) yes S1 . Re1 . S3 . 90.70(5) yes S2 . Re1 . S3 . 90.81(5) yes N1 . Re1 . S4 . 95.61(15) yes S1 . Re1 . S4 . 155.36(5) yes S2 . Re1 . S4 . 93.31(5) yes S3 . Re1 . S4 . 69.37(5) yes N1 . Re1 . P1 . 92.62(16) yes S1 . Re1 . P1 . 93.72(5) yes S2 . Re1 . P1 . 165.43(5) yes S3 . Re1 . P1 . 86.85(5) yes S4 . Re1 . P1 . 99.29(5) yes Re1 . N1 . N2 . 178.7(4) yes N1 . N2 . C1 . 113.8(5) yes N1 . N2 . C51 . 126.3(6) yes C1 . N2 . C51 . 12.5(5) yes N2 . C1 . N3 . 120.7(5) yes N2 . C1 . C5 . 119.1(6) yes N3 . C1 . C5 . 120.2(5) yes C1 . N3 . C2 . 117.6(6) yes N3 . C2 . C3 . 124.2(7) yes N3 . C2 . H21 . 117.9 no C3 . C2 . H21 . 117.9 no C2 . C3 . C4 . 120.2(6) yes C2 . C3 . H31 . 119.9 no C4 . C3 . H31 . 119.9 no C3 . C4 . C5 . 117.4(6) yes C3 . C4 . H41 . 121.3 no C5 . C4 . H41 . 121.3 no C1 . C5 . C4 . 120.3(6) yes C1 . C5 . H51 . 119.9 no C4 . C5 . H51 . 119.9 no N2 . C51 . N53 . 117.4(6) yes N2 . C51 . C55 . 118.2(6) yes C51 . N53 . C52 . 115.2(6) yes N53 . C52 . C53 . 123.8(7) yes N53 . C52 . H521 . 118.1 no C53 . C52 . H521 . 118.1 no C52 . C53 . C54 . 120.3(7) yes C52 . C53 . H531 . 119.9 no C54 . C53 . H531 . 119.9 no C53 . C54 . C55 . 117.1(7) yes C53 . C54 . H541 . 121.4 no C55 . C54 . H541 . 121.5 no C51 . C55 . C54 . 118.1(7) yes C51 . C55 . H551 . 120.9 no C54 . C55 . H551 . 120.9 no Re1 . S1 . C6 . 89.2(2) yes Re1 . S2 . C6 . 86.7(2) yes S1 . C6 . S2 . 112.0(3) yes S1 . C6 . N4 . 123.4(5) yes S2 . C6 . N4 . 124.6(5) yes C6 . N4 . C7 . 123.0(5) yes C6 . N4 . C10 . 122.3(5) yes C7 . N4 . C10 . 114.0(5) yes N4 . C7 . C8 . 109.6(5) yes N4 . C7 . H71 . 109.4 no C8 . C7 . H71 . 109.4 no N4 . C7 . H72 . 109.4 no C8 . C7 . H72 . 109.4 no H71 . C7 . H72 . 109.5 no C7 . C8 . O1 . 111.3(5) yes C7 . C8 . H81 . 109.0 no O1 . C8 . H81 . 109.0 no C7 . C8 . H82 . 109.0 no O1 . C8 . H82 . 109.0 no H81 . C8 . H82 . 109.5 no C8 . O1 . C9 . 109.5(5) yes O1 . C9 . C10 . 110.7(6) yes O1 . C9 . H91 . 109.2 no C10 . C9 . H91 . 109.2 no O1 . C9 . H92 . 109.2 no C10 . C9 . H92 . 109.2 no H91 . C9 . H92 . 109.5 no N4 . C10 . C9 . 109.9(5) yes N4 . C10 . H101 . 109.4 no C9 . C10 . H101 . 109.4 no N4 . C10 . H102 . 109.4 no C9 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.5 no Re1 . S3 . C11 . 87.9(2) yes Re1 . S4 . C11 . 90.4(2) yes S3 . C11 . S4 . 112.2(3) yes S3 . C11 . N5 . 124.2(5) yes S4 . C11 . N5 . 123.6(5) yes C11 . N5 . C12 . 123.3(5) yes C11 . N5 . C15 . 123.1(5) yes C12 . N5 . C15 . 112.3(5) yes N5 . C12 . C13 . 108.2(6) yes N5 . C12 . H121 . 109.8 no C13 . C12 . H121 . 109.8 no N5 . C12 . H122 . 109.8 no C13 . C12 . H122 . 109.8 no H121 . C12 . H122 . 109.5 no C12 . C13 . O2 . 112.2(6) yes C12 . C13 . H131 . 108.8 no O2 . C13 . H131 . 108.8 no C12 . C13 . H132 . 108.8 no O2 . C13 . H132 . 108.8 no H131 . C13 . H132 . 109.5 no C13 . O2 . C14 . 110.6(5) yes O2 . C14 . C15 . 111.3(6) yes O2 . C14 . H141 . 109.0 no C15 . C14 . H141 . 109.0 no O2 . C14 . H142 . 109.0 no C15 . C14 . H142 . 109.0 no H141 . C14 . H142 . 109.5 no N5 . C15 . C14 . 109.3(6) yes N5 . C15 . H151 . 109.5 no C14 . C15 . H151 . 109.5 no N5 . C15 . H152 . 109.5 no C14 . C15 . H152 . 109.5 no H151 . C15 . H152 . 109.5 no Re1 . P1 . C16 . 112.6(2) yes Re1 . P1 . C22 . 118.9(2) yes C16 . P1 . C22 . 103.0(3) yes Re1 . P1 . C28 . 113.74(19) yes C16 . P1 . C28 . 103.7(3) yes C22 . P1 . C28 . 103.2(3) yes P1 . C16 . C17 . 118.4(5) yes P1 . C16 . C21 . 123.0(4) yes C17 . C16 . C21 . 118.5(5) yes C16 . C17 . C18 . 120.9(6) yes C16 . C17 . H171 . 119.6 no C18 . C17 . H171 . 119.6 no C17 . C18 . C19 . 120.1(6) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C18 . C19 . C20 . 119.6(6) yes C18 . C19 . H191 . 120.2 no C20 . C19 . H191 . 120.2 no C19 . C20 . C21 . 120.2(6) yes C19 . C20 . H201 . 119.9 no C21 . C20 . H201 . 119.9 no C16 . C21 . C20 . 120.7(6) yes C16 . C21 . H211 . 119.6 no C20 . C21 . H211 . 119.6 no P1 . C22 . C23 . 123.5(5) yes P1 . C22 . C27 . 117.3(5) yes C23 . C22 . C27 . 119.2(5) yes C22 . C23 . C24 . 120.8(6) yes C22 . C23 . H231 . 119.6 no C24 . C23 . H231 . 119.6 no C23 . C24 . C25 . 119.4(7) yes C23 . C24 . H241 . 120.3 no C25 . C24 . H241 . 120.3 no C24 . C25 . C26 . 120.6(6) yes C24 . C25 . H251 . 119.7 no C26 . C25 . H251 . 119.7 no C25 . C26 . C27 . 119.9(6) yes C25 . C26 . H261 . 120.1 no C27 . C26 . H261 . 120.1 no C22 . C27 . C26 . 120.1(6) yes C22 . C27 . H271 . 119.9 no C26 . C27 . H271 . 119.9 no P1 . C28 . C29 . 120.3(5) yes P1 . C28 . C33 . 122.1(5) yes C29 . C28 . C33 . 117.5(6) yes C28 . C29 . C30 . 121.7(6) yes C28 . C29 . H291 . 119.2 no C30 . C29 . H291 . 119.2 no C29 . C30 . C31 . 120.3(6) yes C29 . C30 . H301 . 119.9 no C31 . C30 . H301 . 119.9 no C30 . C31 . C32 . 119.7(6) yes C30 . C31 . H311 . 120.1 no C32 . C31 . H311 . 120.1 no C31 . C32 . C33 . 119.8(6) yes C31 . C32 . H321 . 120.1 no C33 . C32 . H321 . 120.1 no C28 . C33 . C32 . 121.1(6) yes C28 . C33 . H331 . 119.5 no C32 . C33 . H331 . 119.5 no Cl1 . C34 . Cl2 . 111.9(6) yes Cl1 . C34 . H341 . 108.8 no Cl2 . C34 . H341 . 108.9 no Cl1 . C34 . H342 . 108.8 no Cl2 . C34 . H342 . 108.9 no H341 . C34 . H342 . 109.5 no # Attachment 'ARC855.CIF' data_arc855 _database_code_depnum_ccdc_archive 'CCDC 617264' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _chemical_absolute_configuration ad _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 16.1725(4) _cell_angle_alpha 90 _cell_length_b 10.5970(3) _cell_angle_beta 90 _cell_length_c 18.8348(5) _cell_angle_gamma 90 _cell_volume 3227.91(15) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y,z+1/2 x+1/2,-y,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.0185 7.2310 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C31 H32 N4 O1 P1 Re1 S4 ' _chemical_formula_moiety ' C31 H32 N4 O1 P1 Re1 S4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 822.06 _cell_measurement_reflns_used 19830 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _exptl_crystal_description ' plate ' _exptl_crystal_colour ' dark brown ' _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 4.105 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.78 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 19830 _reflns_number_total 6682 #7006 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_theta_min 5.158 _diffrn_reflns_theta_max 27.494 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.494 _diffrn_measured_fraction_theta_full 0.989 _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 _reflns_limit_h_min 0 _reflns_limit_h_max 20 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min -24 _reflns_limit_l_max 24 _refine_diff_density_min -1.38 _refine_diff_density_max 1.52 _refine_ls_number_reflns 4933 _refine_ls_number_restraints 1 _refine_ls_number_parameters 380 #_refine_ls_R_factor_ref 0.0353 _refine_ls_wR_factor_ref 0.0399 _refine_ls_goodness_of_fit_ref 1.0889 #_reflns_number_all 6682 _refine_ls_R_factor_all 0.0569 _refine_ls_wR_factor_all 0.0638 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 4933 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_gt 0.0399 _refine_ls_shift/su_max 0.027354 _refine_ls_abs_structure_Flack 0.346(10) _refine_ls_abs_structure_details 'Flack, 2939 Friedel-pairs' _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.407 0.122 0.188 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 Re 0.596593(14) 0.13745(2) 0.30121(6) 0.0250 1.0000 Uani N1 N 0.5313(4) 0.2180(7) 0.2440(3) 0.0310 1.0000 Uani N2 N 0.4873(4) 0.2766(7) 0.1982(3) 0.0322 1.0000 Uani C1 C 0.4934(5) 0.2331(8) 0.1284(4) 0.0321 1.0000 Uani O1 O 0.5363(4) 0.1430(7) 0.1101(3) 0.0467 1.0000 Uani C2 C 0.4413(5) 0.3061(9) 0.0772(4) 0.0341 1.0000 Uani C3 C 0.4103(6) 0.4243(10) 0.0926(5) 0.0440 1.0000 Uani C4 C 0.3619(7) 0.4884(11) 0.0431(6) 0.0579 1.0000 Uani C5 C 0.3447(10) 0.4324(15) -0.0203(7) 0.0713 1.0000 Uani C6 C 0.3734(9) 0.3142(14) -0.0372(6) 0.0688 1.0000 Uani C7 C 0.4236(6) 0.2510(10) 0.0120(5) 0.0462 1.0000 Uani S1 S 0.49618(14) -0.0064(2) 0.35591(12) 0.0357 1.0000 Uani S2 S 0.55778(14) 0.2237(2) 0.41523(12) 0.0339 1.0000 Uani C8 C 0.4898(5) 0.0995(9) 0.4252(5) 0.0351 1.0000 Uani N3 N 0.4369(5) 0.0883(8) 0.4784(4) 0.0392 1.0000 Uani C9 C 0.4279(7) 0.1825(14) 0.5336(5) 0.0582 1.0000 Uani C10 C 0.3792(7) -0.0184(15) 0.4821(6) 0.0576 1.0000 Uani S3 S 0.70777(14) 0.0044(2) 0.35799(13) 0.0365 1.0000 Uani S4 S 0.64010(13) -0.0276(2) 0.21854(13) 0.0338 1.0000 Uani C11 C 0.7111(5) -0.0826(10) 0.2821(5) 0.0463 1.0000 Uani N4 N 0.7633(5) -0.1749(8) 0.2677(5) 0.0503 1.0000 Uani C12 C 0.7690(7) -0.2339(12) 0.1980(7) 0.0649 1.0000 Uani C13 C 0.8191(7) -0.2177(10) 0.3233(7) 0.0674 1.0000 Uani P1 P 0.70780(12) 0.27490(19) 0.27044(11) 0.0247 1.0000 Uani C14 C 0.7788(5) 0.3391(7) 0.3378(4) 0.0296 1.0000 Uani C15 C 0.8376(5) 0.4276(8) 0.3172(4) 0.0333 1.0000 Uani C16 C 0.8956(6) 0.4731(9) 0.3653(6) 0.0451 1.0000 Uani C17 C 0.8946(6) 0.4320(9) 0.4356(5) 0.0430 1.0000 Uani C18 C 0.8352(6) 0.3460(10) 0.4568(5) 0.0435 1.0000 Uani C19 C 0.7774(5) 0.2973(8) 0.4083(4) 0.0337 1.0000 Uani C20 C 0.7797(5) 0.2081(8) 0.2049(4) 0.0283 1.0000 Uani C21 C 0.7526(5) 0.1789(8) 0.1371(4) 0.0298 1.0000 Uani C22 C 0.8037(5) 0.1191(8) 0.0887(4) 0.0328 1.0000 Uani C23 C 0.8810(7) 0.0789(10) 0.1100(6) 0.0397 1.0000 Uani C24 C 0.9071(5) 0.1029(9) 0.1790(5) 0.0386 1.0000 Uani C25 C 0.8568(5) 0.1668(8) 0.2269(4) 0.0327 1.0000 Uani C26 C 0.6637(5) 0.4198(8) 0.2336(4) 0.0294 1.0000 Uani C27 C 0.6182(6) 0.4922(8) 0.2797(5) 0.0440 1.0000 Uani C28 C 0.5759(6) 0.5972(10) 0.2581(8) 0.0675 1.0000 Uani C29 C 0.5729(7) 0.6261(9) 0.1838(6) 0.0474 1.0000 Uani C30 C 0.6197(9) 0.5523(11) 0.1378(6) 0.0554 1.0000 Uani C31 C 0.6645(7) 0.4528(9) 0.1620(5) 0.0448 1.0000 Uani H31 H 0.4226 0.4642 0.1395 0.0528 1.0000 Uiso H41 H 0.3400 0.5745 0.0540 0.0694 1.0000 Uiso H51 H 0.3100 0.4789 -0.0557 0.0856 1.0000 Uiso H61 H 0.3589 0.2741 -0.0836 0.0826 1.0000 Uiso H71 H 0.4467 0.1660 0.0001 0.0554 1.0000 Uiso H91 H 0.4698 0.2507 0.5264 0.0698 1.0000 Uiso H92 H 0.4367 0.1423 0.5810 0.0698 1.0000 Uiso H93 H 0.3711 0.2195 0.5315 0.0698 1.0000 Uiso H101 H 0.3904 -0.0777 0.4419 0.0691 1.0000 Uiso H102 H 0.3868 -0.0637 0.5282 0.0691 1.0000 Uiso H103 H 0.3212 0.0135 0.4786 0.0691 1.0000 Uiso H121 H 0.7272 -0.1953 0.1655 0.0779 1.0000 Uiso H122 H 0.8257 -0.2204 0.1782 0.0779 1.0000 Uiso H123 H 0.7581 -0.3264 0.2025 0.0779 1.0000 Uiso H131 H 0.8081 -0.1692 0.3678 0.0809 1.0000 Uiso H132 H 0.8776 -0.2037 0.3079 0.0809 1.0000 Uiso H133 H 0.8100 -0.3097 0.3322 0.0809 1.0000 Uiso H151 H 0.8382 0.4590 0.2672 0.0399 1.0000 Uiso H161 H 0.9382 0.5354 0.3494 0.0542 1.0000 Uiso H171 H 0.9363 0.4644 0.4703 0.0516 1.0000 Uiso H181 H 0.8333 0.3181 0.5075 0.0522 1.0000 Uiso H191 H 0.7358 0.2334 0.4240 0.0404 1.0000 Uiso H211 H 0.6950 0.2016 0.1228 0.0358 1.0000 Uiso H221 H 0.7849 0.1052 0.0387 0.0393 1.0000 Uiso H231 H 0.9178 0.0328 0.0762 0.0476 1.0000 Uiso H241 H 0.9631 0.0738 0.1944 0.0463 1.0000 Uiso H251 H 0.8760 0.1828 0.2765 0.0392 1.0000 Uiso H271 H 0.6158 0.4672 0.3309 0.0528 1.0000 Uiso H281 H 0.5476 0.6528 0.2935 0.0809 1.0000 Uiso H291 H 0.5382 0.6973 0.1656 0.0569 1.0000 Uiso H301 H 0.6203 0.5729 0.0860 0.0665 1.0000 Uiso H311 H 0.6986 0.4025 0.1279 0.0537 1.0000 Uiso 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 0.02400(12) 0.02728(11) 0.02374(11) -0.0005(2) -0.0006(2) -0.00015(12) N1 0.027(3) 0.034(4) 0.032(3) 0.003(3) 0.003(3) 0.010(3) N2 0.025(3) 0.045(4) 0.026(3) 0.004(3) 0.001(3) 0.003(3) C1 0.031(4) 0.030(4) 0.036(4) 0.006(3) -0.007(3) -0.005(3) O1 0.049(4) 0.054(4) 0.037(3) -0.006(3) -0.007(3) 0.023(3) C2 0.022(4) 0.045(5) 0.035(4) 0.010(4) -0.002(3) 0.005(4) C3 0.047(6) 0.044(5) 0.042(5) 0.015(4) 0.008(4) 0.006(5) C4 0.059(7) 0.055(7) 0.060(7) 0.025(5) 0.011(5) 0.010(5) C5 0.095(12) 0.074(9) 0.045(7) 0.021(6) -0.003(7) 0.035(9) C6 0.071(8) 0.094(10) 0.041(6) 0.011(6) -0.020(6) 0.005(7) C7 0.044(6) 0.055(6) 0.039(5) 0.005(4) -0.012(4) 0.004(4) S1 0.0382(11) 0.0365(11) 0.0322(10) -0.0003(9) -0.0008(9) -0.0095(9) S2 0.0364(11) 0.0360(11) 0.0292(10) -0.0039(8) 0.0027(9) -0.0030(9) C8 0.024(4) 0.046(5) 0.035(4) 0.001(4) -0.007(3) -0.004(4) N3 0.038(4) 0.057(5) 0.023(3) 0.000(3) 0.005(3) -0.012(4) C9 0.048(6) 0.097(9) 0.030(5) -0.002(5) 0.004(4) -0.005(6) C10 0.040(6) 0.101(11) 0.032(5) 0.006(6) 0.002(4) -0.033(7) S3 0.0368(11) 0.0308(11) 0.0419(11) 0.0034(9) -0.0096(10) 0.0040(9) S4 0.0313(11) 0.0339(11) 0.0361(10) -0.0069(8) -0.0002(9) 0.0006(9) C11 0.025(4) 0.054(5) 0.059(8) -0.033(5) -0.004(4) -0.007(4) N4 0.021(4) 0.044(4) 0.085(6) -0.011(4) 0.000(4) 0.005(3) C12 0.040(6) 0.061(7) 0.094(9) -0.037(7) 0.012(6) 0.001(5) C13 0.050(6) 0.034(5) 0.118(13) -0.009(6) -0.033(6) 0.001(4) P1 0.0222(9) 0.0264(10) 0.0254(8) 0.0000(8) 0.0004(8) 0.0017(8) C14 0.022(4) 0.033(4) 0.034(4) -0.006(3) 0.005(3) 0.000(3) C15 0.039(4) 0.031(4) 0.030(6) 0.002(3) -0.008(3) -0.008(3) C16 0.028(5) 0.043(5) 0.065(6) -0.013(4) -0.005(4) -0.001(4) C17 0.047(6) 0.036(5) 0.046(5) -0.016(4) -0.016(4) 0.006(4) C18 0.041(5) 0.054(6) 0.036(5) -0.004(4) -0.006(4) 0.001(5) C19 0.036(5) 0.032(5) 0.034(4) 0.000(4) -0.001(4) 0.003(4) C20 0.025(4) 0.032(5) 0.028(4) -0.009(3) -0.001(3) 0.007(3) C21 0.020(4) 0.035(4) 0.034(4) 0.002(3) 0.000(3) 0.002(3) C22 0.034(4) 0.038(5) 0.027(4) -0.002(3) -0.003(3) -0.002(3) C23 0.038(6) 0.046(6) 0.035(5) -0.007(4) 0.011(4) 0.008(5) C24 0.022(4) 0.042(5) 0.052(5) 0.000(4) 0.002(4) 0.000(4) C25 0.028(4) 0.040(5) 0.030(4) 0.002(3) -0.002(3) 0.006(3) C26 0.021(4) 0.034(4) 0.034(4) 0.007(3) -0.002(3) -0.008(3) C27 0.054(5) 0.026(4) 0.052(6) 0.007(3) 0.018(4) 0.004(4) C28 0.036(6) 0.028(5) 0.138(12) -0.004(6) 0.043(6) -0.010(4) C29 0.056(6) 0.030(5) 0.056(6) 0.013(4) -0.003(5) 0.010(4) C30 0.086(10) 0.038(6) 0.042(6) 0.006(5) -0.018(6) 0.014(6) C31 0.062(6) 0.037(5) 0.035(5) 0.000(4) 0.001(4) 0.010(4) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 1.734(7) yes Re1 . S1 . 2.454(2) yes Re1 . S2 . 2.417(2) yes Re1 . S3 . 2.523(2) yes Re1 . S4 . 2.445(2) yes Re1 . P1 . 2.386(2) yes N1 . N2 . 1.279(9) yes N2 . C1 . 1.397(11) yes C1 . O1 . 1.229(11) yes C1 . C2 . 1.495(11) yes C2 . C3 . 1.381(14) yes C2 . C7 . 1.391(13) yes C3 . C4 . 1.394(14) yes C3 . H31 . 1.000 no C4 . C5 . 1.36(2) yes C4 . H41 . 1.000 no C5 . C6 . 1.37(2) yes C5 . H51 . 1.000 no C6 . C7 . 1.401(15) yes C6 . H61 . 1.000 no C7 . H71 . 1.000 no S1 . C8 . 1.724(9) yes S2 . C8 . 1.725(9) yes C8 . N3 . 1.323(11) yes N3 . C9 . 1.449(14) yes N3 . C10 . 1.467(14) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no S3 . C11 . 1.701(8) yes S4 . C11 . 1.758(10) yes C11 . N4 . 1.320(12) yes N4 . C12 . 1.457(15) yes N4 . C13 . 1.454(14) yes C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no P1 . C14 . 1.841(8) yes P1 . C20 . 1.838(8) yes P1 . C26 . 1.830(9) yes C14 . C15 . 1.391(11) yes C14 . C19 . 1.401(12) yes C15 . C16 . 1.390(12) yes C15 . H151 . 1.000 no C16 . C17 . 1.394(15) yes C16 . H161 . 1.000 no C17 . C18 . 1.384(14) yes C17 . H171 . 1.000 no C18 . C19 . 1.404(12) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C20 . C21 . 1.386(11) yes C20 . C25 . 1.383(11) yes C21 . C22 . 1.385(12) yes C21 . H211 . 1.000 no C22 . C23 . 1.380(14) yes C22 . H221 . 1.000 no C23 . C24 . 1.389(15) yes C23 . H231 . 1.000 no C24 . C25 . 1.391(12) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C26 . C27 . 1.374(12) yes C26 . C31 . 1.392(12) yes C27 . C28 . 1.368(15) yes C27 . H271 . 1.000 no C28 . C29 . 1.434(18) yes C28 . H281 . 1.000 no C29 . C30 . 1.391(17) yes C29 . H291 . 1.000 no C30 . C31 . 1.359(15) yes C30 . H301 . 1.000 no C31 . H311 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . S1 . 99.4(2) yes N1 . Re1 . S2 . 102.0(2) yes S1 . Re1 . S2 . 71.95(7) yes N1 . Re1 . S3 . 166.6(2) yes S1 . Re1 . S3 . 86.93(8) yes S2 . Re1 . S3 . 91.14(8) yes N1 . Re1 . S4 . 97.6(2) yes S1 . Re1 . S4 . 90.76(7) yes S2 . Re1 . S4 . 155.66(8) yes S3 . Re1 . S4 . 70.42(7) yes N1 . Re1 . P1 . 90.4(2) yes S1 . Re1 . P1 . 168.54(7) yes S2 . Re1 . P1 . 100.41(7) yes S3 . Re1 . P1 . 84.66(7) yes S4 . Re1 . P1 . 93.73(7) yes Re1 . N1 . N2 . 175.7(6) yes N1 . N2 . C1 . 115.8(7) yes N2 . C1 . O1 . 124.0(8) yes N2 . C1 . C2 . 113.4(7) yes O1 . C1 . C2 . 122.6(8) yes C1 . C2 . C3 . 122.6(8) yes C1 . C2 . C7 . 118.0(8) yes C3 . C2 . C7 . 119.4(8) yes C2 . C3 . C4 . 120.4(10) yes C2 . C3 . H31 . 119.788 no C4 . C3 . H31 . 119.788 no C3 . C4 . C5 . 119.3(11) yes C3 . C4 . H41 . 120.352 no C5 . C4 . H41 . 120.354 no C4 . C5 . C6 . 122.0(12) yes C4 . C5 . H51 . 119.000 no C6 . C5 . H51 . 118.998 no C5 . C6 . C7 . 118.7(11) yes C5 . C6 . H61 . 120.657 no C7 . C6 . H61 . 120.657 no C2 . C7 . C6 . 120.1(10) yes C2 . C7 . H71 . 119.928 no C6 . C7 . H71 . 119.928 no Re1 . S1 . C8 . 87.3(3) yes Re1 . S2 . C8 . 88.5(3) yes S1 . C8 . S2 . 112.1(5) yes S1 . C8 . N3 . 123.6(7) yes S2 . C8 . N3 . 124.3(7) yes C8 . N3 . C9 . 123.1(8) yes C8 . N3 . C10 . 121.1(8) yes C9 . N3 . C10 . 115.7(8) yes N3 . C9 . H91 . 109.466 no N3 . C9 . H92 . 109.467 no H91 . C9 . H92 . 109.476 no N3 . C9 . H93 . 109.466 no H91 . C9 . H93 . 109.475 no H92 . C9 . H93 . 109.477 no N3 . C10 . H101 . 109.467 no N3 . C10 . H102 . 109.466 no H101 . C10 . H102 . 109.474 no N3 . C10 . H103 . 109.468 no H101 . C10 . H103 . 109.477 no H102 . C10 . H103 . 109.476 no Re1 . S3 . C11 . 88.2(3) yes Re1 . S4 . C11 . 89.5(3) yes S3 . C11 . S4 . 111.8(5) yes S3 . C11 . N4 . 126.4(8) yes S4 . C11 . N4 . 121.5(7) yes C11 . N4 . C12 . 122.9(9) yes C11 . N4 . C13 . 118.7(9) yes C12 . N4 . C13 . 118.4(9) yes N4 . C12 . H121 . 109.465 no N4 . C12 . H122 . 109.468 no H121 . C12 . H122 . 109.472 no N4 . C12 . H123 . 109.470 no H121 . C12 . H123 . 109.475 no H122 . C12 . H123 . 109.478 no N4 . C13 . H131 . 109.464 no N4 . C13 . H132 . 109.465 no H131 . C13 . H132 . 109.477 no N4 . C13 . H133 . 109.465 no H131 . C13 . H133 . 109.478 no H132 . C13 . H133 . 109.478 no Re1 . P1 . C14 . 121.9(3) yes Re1 . P1 . C20 . 113.9(3) yes C14 . P1 . C20 . 102.1(3) yes Re1 . P1 . C26 . 108.1(2) yes C14 . P1 . C26 . 101.2(4) yes C20 . P1 . C26 . 108.4(4) yes P1 . C14 . C15 . 119.0(6) yes P1 . C14 . C19 . 121.8(6) yes C15 . C14 . C19 . 119.2(7) yes C14 . C15 . C16 . 120.9(8) yes C14 . C15 . H151 . 119.525 no C16 . C15 . H151 . 119.525 no C15 . C16 . C17 . 120.2(9) yes C15 . C16 . H161 . 119.913 no C17 . C16 . H161 . 119.913 no C16 . C17 . C18 . 119.2(8) yes C16 . C17 . H171 . 120.400 no C18 . C17 . H171 . 120.401 no C17 . C18 . C19 . 121.1(9) yes C17 . C18 . H181 . 119.445 no C19 . C18 . H181 . 119.445 no C14 . C19 . C18 . 119.4(8) yes C14 . C19 . H191 . 120.321 no C18 . C19 . H191 . 120.322 no P1 . C20 . C21 . 120.3(6) yes P1 . C20 . C25 . 119.4(6) yes C21 . C20 . C25 . 119.3(7) yes C20 . C21 . C22 . 121.4(7) yes C20 . C21 . H211 . 119.307 no C22 . C21 . H211 . 119.308 no C21 . C22 . C23 . 119.3(8) yes C21 . C22 . H221 . 120.344 no C23 . C22 . H221 . 120.345 no C22 . C23 . C24 . 119.4(8) yes C22 . C23 . H231 . 120.282 no C24 . C23 . H231 . 120.283 no C23 . C24 . C25 . 121.2(8) yes C23 . C24 . H241 . 119.418 no C25 . C24 . H241 . 119.417 no C20 . C25 . C24 . 119.2(8) yes C20 . C25 . H251 . 120.424 no C24 . C25 . H251 . 120.424 no P1 . C26 . C27 . 115.9(6) yes P1 . C26 . C31 . 125.1(7) yes C27 . C26 . C31 . 118.5(8) yes C26 . C27 . C28 . 122.3(10) yes C26 . C27 . H271 . 118.841 no C28 . C27 . H271 . 118.842 no C27 . C28 . C29 . 118.7(10) yes C27 . C28 . H281 . 120.627 no C29 . C28 . H281 . 120.624 no C28 . C29 . C30 . 118.0(9) yes C28 . C29 . H291 . 120.985 no C30 . C29 . H291 . 121.005 no C29 . C30 . C31 . 121.1(10) yes C29 . C30 . H301 . 119.422 no C31 . C30 . H301 . 119.429 no C26 . C31 . C30 . 121.0(9) yes C26 . C31 . H311 . 119.486 no C30 . C31 . H311 . 119.486 no # Attachment 'arc311.cif' data_CRYSTALS_cif_arc311 _database_code_depnum_ccdc_archive 'CCDC 617265' #====================================================================== # Diffractometer details #====================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #====================================================================== # General computing #====================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #====================================================================== _cell_length_a 33.1722(4) _cell_angle_alpha 90 _cell_length_b 11.2208(2) _cell_angle_beta 129.7968(6) _cell_length_c 25.2507(3) _cell_angle_gamma 90 _cell_volume 7221.3 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C32.50 H37.50 Cl1.00 N4 O1.25 P1 Re1 S4 ' _chemical_formula_moiety ' C32.50 H37.50 Cl1.00 N4 O1.25 P1 Re1 S4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 885.02 _cell_measurement_reflns_used 39920 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 8 _exptl_crystal_description ' block ' _exptl_crystal_colour ' brown ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.628 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3524.931 _exptl_absorpt_coefficient_mu 3.748 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.69 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 39920 _reflns_number_total 8601 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_gt 6310 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -42 _reflns_limit_h_max 33 _reflns_limit_k_min 0 _reflns_limit_k_max 14 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _refine_diff_density_min -1.28 _refine_diff_density_max 0.84 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6310 _refine_ls_number_parameters 430 _refine_ls_R_factor_gt 0.0337 _refine_ls_wR_factor_ref 0.0418 _refine_ls_goodness_of_fit_ref 0.9920 _refine_ls_shift/su_max 0.032790 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 2.71 0.415 2.23 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.363118(6) 0.298368(14) 0.420904(7) 0.0252 1.0000 Uani N1 0.37839(13) 0.2687(3) 0.36651(17) 0.0275 1.0000 Uani N2 0.39188(14) 0.2468(3) 0.33135(17) 0.0321 1.0000 Uani C1 0.35409(16) 0.2163(3) 0.2607(2) 0.0283 1.0000 Uani C2 0.37334(19) 0.1957(4) 0.2259(2) 0.0356 1.0000 Uani C3 0.3386(2) 0.1720(4) 0.1555(2) 0.0380 1.0000 Uani C4 0.28535(19) 0.1677(4) 0.1201(2) 0.0358 1.0000 Uani C5 0.26576(18) 0.1836(4) 0.1547(2) 0.0350 1.0000 Uani C6 0.30036(17) 0.2087(4) 0.2249(2) 0.0304 1.0000 Uani O1 0.25439(14) 0.1443(3) 0.05056(16) 0.0463 1.0000 Uani C7 0.2001(2) 0.1696(5) 0.0092(3) 0.0480 1.0000 Uani S1 0.38372(4) 0.51498(9) 0.43386(5) 0.0320 1.0000 Uani S2 0.44767(4) 0.3298(1) 0.53130(5) 0.0323 1.0000 Uani C8 0.44292(16) 0.4808(4) 0.5125(2) 0.0296 1.0000 Uani N3 0.48089(13) 0.5576(3) 0.55474(18) 0.0321 1.0000 Uani C9 0.52968(17) 0.5191(4) 0.6212(2) 0.0400 1.0000 Uani C10 0.47687(18) 0.6826(4) 0.5356(3) 0.0390 1.0000 Uani S3 0.31987(4) 0.3296(1) 0.47408(5) 0.0311 1.0000 Uani S4 0.26931(4) 0.3409(1) 0.33038(5) 0.0284 1.0000 Uani C11 0.26214(15) 0.3496(4) 0.3917(2) 0.0276 1.0000 Uani N4 0.21617(13) 0.3681(3) 0.37620(17) 0.0319 1.0000 Uani C12 0.20980(18) 0.3676(5) 0.4281(2) 0.0423 1.0000 Uani C13 0.16825(16) 0.3758(5) 0.3039(2) 0.0382 1.0000 Uani P1 0.35365(4) 0.09295(9) 0.43114(5) 0.0264 1.0000 Uani C14 0.38006(16) -0.0084(4) 0.4030(2) 0.0294 1.0000 Uani C15 0.42844(17) 0.0201(4) 0.4206(2) 0.0356 1.0000 Uani C16 0.45180(18) -0.0552(5) 0.4045(2) 0.0424 1.0000 Uani C17 0.4276(2) -0.1629(5) 0.3708(2) 0.0484 1.0000 Uani C18 0.3800(2) -0.1931(4) 0.3531(2) 0.0437 1.0000 Uani C19 0.35610(18) -0.1164(4) 0.3690(2) 0.0359 1.0000 Uani C20 0.28557(16) 0.0433(4) 0.3827(2) 0.0293 1.0000 Uani C21 0.25221(18) 0.0391(4) 0.3108(2) 0.0348 1.0000 Uani C22 0.19860(17) 0.0164(4) 0.2720(2) 0.0384 1.0000 Uani C23 0.17861(17) 0.0004(4) 0.3053(3) 0.0425 1.0000 Uani C24 0.21104(19) 0.0060(5) 0.3763(3) 0.0438 1.0000 Uani C25 0.26478(17) 0.0263(4) 0.4156(2) 0.0372 1.0000 Uani C26 0.38671(16) 0.0306(4) 0.5182(2) 0.0324 1.0000 Uani C27 0.3914(2) -0.0924(5) 0.5274(2) 0.0433 1.0000 Uani C28 0.4173(2) -0.1420(5) 0.5925(3) 0.0531 1.0000 Uani C29 0.43915(19) -0.0688(6) 0.6488(3) 0.0540 1.0000 Uani C30 0.4348(2) 0.0529(6) 0.6405(3) 0.0570 1.0000 Uani C31 0.40854(18) 0.1036(5) 0.5752(2) 0.0430 1.0000 Uani C32 0.5789(6) 0.587(2) 0.3436(9) 0.0939 0.499(6) Uani Cl1 0.5683(2) 0.6718(4) 0.2801(3) 0.1006 0.499(6) Uani Cl2 0.57376(19) 0.4283(5) 0.3220(3) 0.0972 0.499(6) Uani O2 0.5000 0.5112(12) 0.2500 0.0617 0.501(6) Uani C33 0.5463(7) 0.5763(15) 0.3059(8) 0.0728 0.501(6) Uani C34 0.5822(6) 0.488(2) 0.3564(8) 0.0757 0.501(6) Uani H21 0.4120 0.1981 0.2514 0.0482 1.0000 Uiso H31 0.3523 0.1579 0.1305 0.0501 1.0000 Uiso H51 0.2273 0.1769 0.1294 0.0429 1.0000 Uiso H61 0.2865 0.2216 0.2499 0.0401 1.0000 Uiso H71 0.1822 0.1487 -0.0399 0.0553 1.0000 Uiso H72 0.1952 0.2563 0.0125 0.0553 1.0000 Uiso H73 0.1847 0.1216 0.0257 0.0553 1.0000 Uiso H91 0.5273 0.4323 0.6279 0.0421 1.0000 Uiso H92 0.5352 0.5657 0.6591 0.0421 1.0000 Uiso H93 0.5598 0.5329 0.6219 0.0421 1.0000 Uiso H101 0.4419 0.6971 0.4895 0.0440 1.0000 Uiso H102 0.4807 0.7346 0.5708 0.0440 1.0000 Uiso H103 0.5053 0.7017 0.5335 0.0440 1.0000 Uiso H121 0.2450 0.3621 0.4750 0.0538 1.0000 Uiso H122 0.1920 0.4428 0.4246 0.0538 1.0000 Uiso H123 0.1880 0.2975 0.4205 0.0538 1.0000 Uiso H131 0.1778 0.3754 0.2734 0.0441 1.0000 Uiso H132 0.1492 0.4512 0.2965 0.0441 1.0000 Uiso H133 0.1452 0.3060 0.2924 0.0441 1.0000 Uiso H151 0.4462 0.0964 0.4453 0.0404 1.0000 Uiso H161 0.4861 -0.0330 0.4168 0.0497 1.0000 Uiso H171 0.4448 -0.2181 0.3594 0.0558 1.0000 Uiso H181 0.3627 -0.2700 0.3288 0.0490 1.0000 Uiso H191 0.3216 -0.1386 0.3561 0.0419 1.0000 Uiso H211 0.2668 0.0525 0.2868 0.0383 1.0000 Uiso H221 0.1751 0.0118 0.2205 0.0369 1.0000 Uiso H231 0.1403 -0.0155 0.2779 0.0445 1.0000 Uiso H241 0.1959 -0.0046 0.3998 0.0554 1.0000 Uiso H251 0.2882 0.0286 0.4670 0.0440 1.0000 Uiso H271 0.3761 -0.1458 0.4868 0.0544 1.0000 Uiso H281 0.4201 -0.2306 0.5984 0.0657 1.0000 Uiso H291 0.4581 -0.1042 0.6957 0.0595 1.0000 Uiso H301 0.4505 0.1057 0.6814 0.0619 1.0000 Uiso H311 0.4055 0.1922 0.5697 0.0482 1.0000 Uiso H321 0.6148 0.6035 0.3879 0.0978 0.4995 Uiso H322 0.5522 0.6067 0.3487 0.0978 0.4995 Uiso H331 0.5624 0.6194 0.2888 0.0901 0.5005 Uiso H332 0.5370 0.6349 0.3264 0.0901 0.5005 Uiso H341 0.6150 0.5276 0.3964 0.0937 0.5005 Uiso H342 0.5908 0.4294 0.3351 0.0937 0.5005 Uiso H343 0.5654 0.4449 0.3727 0.0937 0.5005 Uiso 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 0.02400(9) 0.0278(1) 0.02251(9) -0.00268(6) 0.01425(7) -0.00333(6) N1 0.0231(15) 0.0292(17) 0.0234(15) -0.0025(13) 0.0117(13) -0.0033(13) N2 0.0363(19) 0.0348(18) 0.0343(18) -0.0017(16) 0.0268(17) -0.0017(17) C1 0.033(2) 0.0255(19) 0.0307(19) 0.0006(15) 0.0226(18) 0.0026(15) C2 0.040(2) 0.038(2) 0.042(2) 0.0007(19) 0.033(2) 0.0013(18) C3 0.046(3) 0.042(2) 0.037(2) -0.0008(19) 0.032(2) 0.003(2) C4 0.046(3) 0.035(2) 0.031(2) 0.0045(17) 0.027(2) 0.0075(19) C5 0.033(2) 0.038(2) 0.036(2) 0.0002(18) 0.0231(19) 0.0026(17) C6 0.033(2) 0.032(2) 0.036(2) -0.0041(17) 0.0261(19) -0.0036(16) O1 0.0480(19) 0.059(2) 0.0294(16) -0.0021(15) 0.0237(15) 0.0095(17) C7 0.050(3) 0.056(3) 0.032(2) 0.002(2) 0.024(2) 0.001(2) S1 0.0313(5) 0.0313(5) 0.0295(5) -0.0017(4) 0.0177(4) -0.0049(4) S2 0.0259(5) 0.0320(5) 0.0289(5) -0.0005(4) 0.0128(4) -0.0021(4) C8 0.0291(19) 0.036(2) 0.0287(19) -0.0056(16) 0.0210(17) -0.0028(16) N3 0.0274(17) 0.0337(18) 0.0304(17) -0.0024(14) 0.0163(15) -0.0058(14) C9 0.029(2) 0.040(2) 0.036(2) -0.0050(19) 0.0140(19) -0.0082(18) C10 0.033(2) 0.034(2) 0.043(2) -0.0047(18) 0.021(2) -0.0073(17) S3 0.0293(5) 0.0401(5) 0.0234(4) -0.0033(4) 0.0166(4) -0.0025(4) S4 0.0270(5) 0.0353(5) 0.0220(4) -0.0015(4) 0.0152(4) -0.0014(4) C11 0.0285(18) 0.0284(19) 0.0271(18) -0.0029(16) 0.0184(17) 0.0009(16) N4 0.0306(17) 0.039(2) 0.0257(16) 0.0016(14) 0.0179(15) 0.0009(15) C12 0.038(2) 0.059(3) 0.037(2) 0.002(2) 0.028(2) 0.004(2) C13 0.0259(19) 0.049(3) 0.035(2) 0.0019(19) 0.0175(18) 0.0018(18) P1 0.0264(4) 0.0290(5) 0.0220(4) -0.0008(4) 0.0146(4) -0.0024(4) C14 0.034(2) 0.030(2) 0.0258(18) 0.0019(15) 0.0198(17) 0.0034(16) C15 0.032(2) 0.040(2) 0.030(2) 0.0033(17) 0.0169(18) 0.0041(18) C16 0.034(2) 0.054(3) 0.036(2) 0.006(2) 0.021(2) 0.013(2) C17 0.053(3) 0.053(3) 0.033(2) 0.011(2) 0.025(2) 0.025(2) C18 0.058(3) 0.031(2) 0.033(2) 0.0001(18) 0.025(2) 0.007(2) C19 0.041(2) 0.032(2) 0.032(2) 0.0010(17) 0.0221(19) 0.0005(18) C20 0.0262(18) 0.0269(19) 0.0295(19) -0.0008(15) 0.0154(17) -0.0021(15) C21 0.036(2) 0.031(2) 0.029(2) -0.0021(16) 0.0169(18) -0.0061(17) C22 0.028(2) 0.033(2) 0.031(2) -0.0019(17) 0.0083(18) -0.0023(17) C23 0.024(2) 0.041(3) 0.046(3) -0.004(2) 0.015(2) -0.0044(18) C24 0.037(2) 0.051(3) 0.050(3) -0.005(2) 0.031(2) -0.007(2) C25 0.032(2) 0.045(3) 0.033(2) -0.0067(19) 0.0202(19) -0.0059(19) C26 0.0252(19) 0.043(2) 0.0275(19) 0.0021(17) 0.0164(17) -0.0010(17) C27 0.048(3) 0.050(3) 0.038(2) 0.007(2) 0.030(2) -0.001(2) C28 0.055(3) 0.060(4) 0.049(3) 0.020(3) 0.036(3) 0.010(3) C29 0.033(2) 0.085(4) 0.031(2) 0.020(3) 0.014(2) -0.000(2) C30 0.044(3) 0.083(4) 0.028(2) -0.001(2) 0.016(2) -0.019(3) C31 0.037(2) 0.057(3) 0.026(2) -0.000(2) 0.0164(19) -0.010(2) C32 0.047(7) 0.149(6) 0.049(7) -0.033(7) 0.013(6) 0.008(11) Cl1 0.112(4) 0.062(2) 0.179(5) -0.027(3) 0.117(4) -0.018(2) Cl2 0.087(3) 0.107(4) 0.071(3) 0.024(2) 0.039(2) -0.013(2) O2 0.053(6) 0.075(8) 0.044(6) 0.0000 0.026(5) 0.0000 C33 0.074(8) 0.09(1) 0.065(8) -0.022(6) 0.048(6) -0.024(6) C34 0.056(8) 0.127(15) 0.051(8) -0.015(7) 0.038(7) -0.008(8) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 1.773(3) yes Re1 . S1 . 2.4890(11) yes Re1 . S2 . 2.399(1) yes Re1 . S3 . 2.540(1) yes Re1 . S4 . 2.456(1) yes Re1 . P1 . 2.363(1) yes N1 . N2 . 1.248(5) yes N2 . C1 . 1.416(5) yes C1 . C2 . 1.399(6) yes C1 . C6 . 1.392(6) yes C2 . C3 . 1.391(7) yes C2 . H21 . 1.000 no C3 . C4 . 1.377(7) yes C3 . H31 . 1.000 no C4 . C5 . 1.396(6) yes C4 . O1 . 1.377(5) yes C5 . C6 . 1.390(6) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no O1 . C7 . 1.416(6) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no S1 . C8 . 1.719(4) yes S2 . C8 . 1.739(4) yes C8 . N3 . 1.322(5) yes N3 . C9 . 1.465(6) yes N3 . C10 . 1.461(6) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . H101 . 1.000 no C10 . H102 . 1.000 no C10 . H103 . 1.000 no S3 . C11 . 1.716(4) yes S4 . C11 . 1.714(4) yes C11 . N4 . 1.325(5) yes N4 . C12 . 1.455(5) yes N4 . C13 . 1.468(5) yes C12 . H121 . 1.000 no C12 . H122 . 1.000 no C12 . H123 . 1.000 no C13 . H131 . 1.000 no C13 . H132 . 1.000 no C13 . H133 . 1.000 no P1 . C14 . 1.833(4) yes P1 . C20 . 1.836(4) yes P1 . C26 . 1.854(4) yes C14 . C15 . 1.401(6) yes C14 . C19 . 1.401(6) yes C15 . C16 . 1.373(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.398(8) yes C16 . H161 . 1.000 no C17 . C18 . 1.380(8) yes C17 . H171 . 1.000 no C18 . C19 . 1.393(7) yes C18 . H181 . 1.000 no C19 . H191 . 1.000 no C20 . C21 . 1.395(6) yes C20 . C25 . 1.392(6) yes C21 . C22 . 1.399(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.377(7) yes C22 . H221 . 1.000 no C23 . C24 . 1.380(7) yes C23 . H231 . 1.000 no C24 . C25 . 1.396(6) yes C24 . H241 . 1.000 no C25 . H251 . 1.000 no C26 . C27 . 1.392(7) yes C26 . C31 . 1.391(6) yes C27 . C28 . 1.394(7) yes C27 . H271 . 1.000 no C28 . C29 . 1.379(9) yes C28 . H281 . 1.000 no C29 . C30 . 1.375(9) yes C29 . H291 . 1.000 no C30 . C31 . 1.400(7) yes C30 . H301 . 1.000 no C31 . H311 . 1.000 no C32 . Cl1 . 1.70(3) yes C32 . Cl2 . 1.84(2) yes C32 . H321 . 1.000 no C32 . H322 . 1.000 no O2 . C33 . 1.453(16) yes O2 . C33 5_655 1.453(16) yes C33 . C34 . 1.45(3) yes C33 . H331 . 1.000 no C33 . H332 . 1.000 no C34 . H341 . 1.000 no C34 . H342 . 1.000 no C34 . H343 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . S1 . 95.41(11) yes N1 . Re1 . S2 . 103.08(11) yes S1 . Re1 . S2 . 71.66(4) yes N1 . Re1 . S3 . 166.79(11) yes S1 . Re1 . S3 . 89.78(4) yes S2 . Re1 . S3 . 90.08(4) yes N1 . Re1 . S4 . 97.79(11) yes S1 . Re1 . S4 . 90.60(4) yes S2 . Re1 . S4 . 153.61(4) yes S3 . Re1 . S4 . 69.96(3) yes N1 . Re1 . P1 . 91.48(11) yes S1 . Re1 . P1 . 169.36(3) yes S2 . Re1 . P1 . 98.89(4) yes S3 . Re1 . P1 . 85.25(4) yes S4 . Re1 . P1 . 96.51(4) yes Re1 . N1 . N2 . 176.6(3) yes N1 . N2 . C1 . 120.8(3) yes N2 . C1 . C2 . 116.1(4) yes N2 . C1 . C6 . 124.5(4) yes C2 . C1 . C6 . 119.4(4) yes C1 . C2 . C3 . 119.7(4) yes C1 . C2 . H21 . 120.1 no C3 . C2 . H21 . 120.1 no C2 . C3 . C4 . 120.5(4) yes C2 . C3 . H31 . 119.7 no C4 . C3 . H31 . 119.7 no C3 . C4 . C5 . 120.3(4) yes C3 . C4 . O1 . 115.8(4) yes C5 . C4 . O1 . 123.8(4) yes C4 . C5 . C6 . 119.3(4) yes C4 . C5 . H51 . 120.4 no C6 . C5 . H51 . 120.4 no C1 . C6 . C5 . 120.7(4) yes C1 . C6 . H61 . 119.7 no C5 . C6 . H61 . 119.7 no C4 . O1 . C7 . 117.5(4) yes O1 . C7 . H71 . 109.5 no O1 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no O1 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no Re1 . S1 . C8 . 87.04(15) yes Re1 . S2 . C8 . 89.53(14) yes S1 . C8 . S2 . 111.7(2) yes S1 . C8 . N3 . 125.5(3) yes S2 . C8 . N3 . 122.8(3) yes C8 . N3 . C9 . 121.0(4) yes C8 . N3 . C10 . 121.4(4) yes C9 . N3 . C10 . 117.5(3) yes N3 . C9 . H91 . 109.5 no N3 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no N3 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N3 . C10 . H101 . 109.5 no N3 . C10 . H102 . 109.5 no H101 . C10 . H102 . 109.5 no N3 . C10 . H103 . 109.5 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no Re1 . S3 . C11 . 86.97(13) yes Re1 . S4 . C11 . 89.77(14) yes S3 . C11 . S4 . 113.3(2) yes S3 . C11 . N4 . 124.0(3) yes S4 . C11 . N4 . 122.7(3) yes C11 . N4 . C12 . 122.4(3) yes C11 . N4 . C13 . 120.1(3) yes C12 . N4 . C13 . 117.1(3) yes N4 . C12 . H121 . 109.5 no N4 . C12 . H122 . 109.5 no H121 . C12 . H122 . 109.5 no N4 . C12 . H123 . 109.5 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N4 . C13 . H131 . 109.5 no N4 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no N4 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no Re1 . P1 . C14 . 115.66(14) yes Re1 . P1 . C20 . 114.59(14) yes C14 . P1 . C20 . 104.01(19) yes Re1 . P1 . C26 . 118.60(15) yes C14 . P1 . C26 . 99.10(19) yes C20 . P1 . C26 . 102.57(19) yes P1 . C14 . C15 . 118.0(3) yes P1 . C14 . C19 . 123.4(3) yes C15 . C14 . C19 . 118.5(4) yes C14 . C15 . C16 . 121.0(4) yes C14 . C15 . H151 . 119.5 no C16 . C15 . H151 . 119.5 no C15 . C16 . C17 . 120.0(5) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 120.0 no C16 . C17 . C18 . 120.1(5) yes C16 . C17 . H171 . 120.0 no C18 . C17 . H171 . 120.0 no C17 . C18 . C19 . 120.0(5) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.0 no C14 . C19 . C18 . 120.4(4) yes C14 . C19 . H191 . 119.8 no C18 . C19 . H191 . 119.8 no P1 . C20 . C21 . 119.4(3) yes P1 . C20 . C25 . 120.8(3) yes C21 . C20 . C25 . 119.2(4) yes C20 . C21 . C22 . 120.8(4) yes C20 . C21 . H211 . 119.6 no C22 . C21 . H211 . 119.6 no C21 . C22 . C23 . 119.2(4) yes C21 . C22 . H221 . 120.4 no C23 . C22 . H221 . 120.4 no C22 . C23 . C24 . 120.5(4) yes C22 . C23 . H231 . 119.7 no C24 . C23 . H231 . 119.7 no C23 . C24 . C25 . 120.7(4) yes C23 . C24 . H241 . 119.7 no C25 . C24 . H241 . 119.7 no C20 . C25 . C24 . 119.5(4) yes C20 . C25 . H251 . 120.2 no C24 . C25 . H251 . 120.2 no P1 . C26 . C27 . 119.4(3) yes P1 . C26 . C31 . 121.8(4) yes C27 . C26 . C31 . 118.8(4) yes C26 . C27 . C28 . 120.8(5) yes C26 . C27 . H271 . 119.6 no C28 . C27 . H271 . 119.6 no C27 . C28 . C29 . 119.9(5) yes C27 . C28 . H281 . 120.1 no C29 . C28 . H281 . 120.1 no C28 . C29 . C30 . 120.0(5) yes C28 . C29 . H291 . 120.0 no C30 . C29 . H291 . 120.0 no C29 . C30 . C31 . 120.5(5) yes C29 . C30 . H301 . 119.7 no C31 . C30 . H301 . 119.7 no C26 . C31 . C30 . 120.0(5) yes C26 . C31 . H311 . 120.0 no C30 . C31 . H311 . 120.0 no Cl1 . C32 . Cl2 . 110.0(9) yes Cl1 . C32 . H321 . 109.3 no Cl2 . C32 . H321 . 109.4 no Cl1 . C32 . H322 . 109.3 no Cl2 . C32 . H322 . 109.4 no C33 . O2 . C33 5_655 119.6(17) yes O2 . C33 . C34 . 105.8(14) yes O2 . C33 . H331 . 110.4 no C34 . C33 . H331 . 110.4 no O2 . C33 . H332 . 110.4 no C34 . C33 . H332 . 110.4 no H331 . C33 . H332 . 109.5 no C33 . C34 . H341 . 109.4 no C33 . C34 . H342 . 109.5 no H341 . C34 . H342 . 109.5 no C33 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.6 no # Attachment 'arc312.cif' data_CRYSTALS_cif_arc312 _database_code_depnum_ccdc_archive 'CCDC 617266' #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 13.7100(2) _cell_angle_alpha 90 _cell_length_b 17.5722(2) _cell_angle_beta 93.2214(8) _cell_length_c 20.1587(3) _cell_angle_gamma 90 _cell_volume 4848.9 _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B 'S ' 0.1100 0.1240 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C43 H40 Cl6 N4 O1 P1 Re1 S4 ' _chemical_formula_moiety ' C43 H40 Cl6 N4 O1 P1 Re1 S4 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 1186.95 _cell_measurement_reflns_used 47019 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' fragment ' _exptl_crystal_colour ' brown ' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 2359.180 _exptl_absorpt_coefficient_mu 3.080 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.86 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 47019 _reflns_number_total 11343 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_gt 7348 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _refine_diff_density_min -1.11 _refine_diff_density_max 1.21 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 7348 _refine_ls_number_parameters 541 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0385 _refine_ls_goodness_of_fit_ref 1.0473 _refine_ls_shift/su_max 0.025340 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters (Carruthers & Watkin , 1979) 0.375 0.153 0.147 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.121243(13) 0.229224(9) 0.627646(8) 0.0186 1.0000 Uani N1 0.2054(3) 0.2978(2) 0.60251(18) 0.0212 1.0000 Uani N2 0.2685(3) 0.3451(2) 0.5855(2) 0.0252 1.0000 Uani C1 0.2422(3) 0.4228(3) 0.5771(2) 0.0239 1.0000 Uani C2 0.3104(4) 0.4715(3) 0.5519(3) 0.0320 1.0000 Uani C3 0.2885(4) 0.5482(3) 0.5416(3) 0.0386 1.0000 Uani C4 0.1982(4) 0.5764(3) 0.5558(3) 0.0306 1.0000 Uani C5 0.1287(4) 0.5282(3) 0.5805(2) 0.0297 1.0000 Uani C6 0.1519(4) 0.4520(3) 0.5911(3) 0.0309 1.0000 Uani O1 0.1839(3) 0.6529(2) 0.5449(2) 0.0422 1.0000 Uani C7 0.0908(5) 0.6822(3) 0.5602(3) 0.0466 1.0000 Uani S1 0.07917(9) 0.17540(6) 0.51583(5) 0.0240 1.0000 Uani S2 0.20581(8) 0.11073(6) 0.61827(5) 0.0213 1.0000 Uani C8 0.1509(3) 0.0991(3) 0.5391(2) 0.0231 1.0000 Uani N3 0.1603(3) 0.0371(2) 0.50221(19) 0.0263 1.0000 Uani C9 0.1058(4) 0.0288(3) 0.4379(3) 0.0369 1.0000 Uani C10 0.2299(4) -0.0220(3) 0.5210(2) 0.0271 1.0000 Uani C11 0.1982(4) -0.0961(3) 0.5280(3) 0.0352 1.0000 Uani C12 0.2661(5) -0.1528(3) 0.5445(3) 0.0451 1.0000 Uani C13 0.3644(5) -0.1345(4) 0.5551(3) 0.0431 1.0000 Uani C14 0.3951(4) -0.0600(4) 0.5470(3) 0.0433 1.0000 Uani C15 0.3271(4) -0.0039(3) 0.5303(3) 0.0327 1.0000 Uani S3 -0.02634(9) 0.15914(6) 0.66766(6) 0.0257 1.0000 Uani S4 -0.02440(9) 0.31177(6) 0.61941(6) 0.0263 1.0000 Uani N4 -0.1864(3) 0.2467(2) 0.6599(2) 0.0341 1.0000 Uani C16 -0.0923(3) 0.2402(3) 0.6495(2) 0.0254 1.0000 Uani C17 -0.2383(4) 0.3194(4) 0.6463(4) 0.0505 1.0000 Uani C18 -0.2383(4) 0.1860(4) 0.6898(3) 0.0404 1.0000 Uani C19 -0.2675(5) 0.1238(3) 0.6527(4) 0.0512 1.0000 Uani C20 -0.3145(6) 0.0642(4) 0.6821(6) 0.0734 1.0000 Uani C21 -0.3314(6) 0.0666(7) 0.7480(7) 0.0982 1.0000 Uani C22 -0.3028(6) 0.1298(9) 0.7858(5) 0.1030 1.0000 Uani C23 -0.2556(6) 0.1910(6) 0.7571(4) 0.0723 1.0000 Uani P1 0.16321(9) 0.25756(6) 0.74022(6) 0.0207 1.0000 Uani C24 0.1561(3) 0.1838(3) 0.8050(2) 0.0232 1.0000 Uani C25 0.1376(4) 0.1074(3) 0.7893(2) 0.0256 1.0000 Uani C26 0.1334(4) 0.0536(3) 0.8392(2) 0.0288 1.0000 Uani C27 0.1482(4) 0.0744(3) 0.9051(2) 0.0291 1.0000 Uani C28 0.1667(4) 0.1503(3) 0.9211(2) 0.0343 1.0000 Uani C29 0.1706(4) 0.2049(3) 0.8715(2) 0.0305 1.0000 Uani C30 0.2897(4) 0.2907(3) 0.7568(2) 0.0256 1.0000 Uani C31 0.3166(4) 0.3461(3) 0.8043(3) 0.0376 1.0000 Uani C32 0.4142(5) 0.3650(4) 0.8166(3) 0.0480 1.0000 Uani C33 0.4859(5) 0.3286(4) 0.7828(3) 0.0506 1.0000 Uani C34 0.4599(4) 0.2726(4) 0.7369(3) 0.0457 1.0000 Uani C35 0.3620(4) 0.2544(3) 0.7234(3) 0.0319 1.0000 Uani C36 0.0853(3) 0.3320(3) 0.7722(2) 0.0232 1.0000 Uani C37 -0.0001(4) 0.3122(3) 0.8017(2) 0.0287 1.0000 Uani C38 -0.0661(4) 0.3676(3) 0.8186(3) 0.0353 1.0000 Uani C39 -0.0478(5) 0.4438(3) 0.8050(3) 0.0373 1.0000 Uani C40 0.0356(4) 0.4637(3) 0.7743(2) 0.0343 1.0000 Uani C41 0.1022(4) 0.4087(3) 0.7576(2) 0.0275 1.0000 Uani C42 0.4381(4) 0.2362(3) 0.5492(3) 0.0418 1.0000 Uani Cl1 0.48783(12) 0.1563(1) 0.59180(8) 0.0485 1.0000 Uani Cl2 0.53038(15) 0.30173(12) 0.53429(12) 0.0726 1.0000 Uani Cl3 0.37776(13) 0.2080(1) 0.47438(9) 0.0559 1.0000 Uani C43 0.3895(7) 0.0449(6) 0.8319(5) 0.0868 1.0000 Uani Cl4 0.3854(2) 0.04150(19) 0.74618(13) 0.1063 1.0000 Uani Cl5 0.4510(3) 0.12296(18) 0.86467(17) 0.1214 1.0000 Uani Cl6 0.4352(3) -0.03847(17) 0.86631(17) 0.1248 1.0000 Uani H21 0.3760 0.4516 0.5411 0.0383 1.0000 Uiso H31 0.3385 0.5829 0.5237 0.0463 1.0000 Uiso H51 0.0628 0.5481 0.5906 0.0357 1.0000 Uiso H61 0.1020 0.4173 0.6092 0.0373 1.0000 Uiso H71 0.0882 0.7380 0.5505 0.0558 1.0000 Uiso H72 0.0803 0.6736 0.6083 0.0558 1.0000 Uiso H73 0.0385 0.6556 0.5325 0.0558 1.0000 Uiso H91 0.1223 -0.0211 0.4176 0.0438 1.0000 Uiso H92 0.0341 0.0309 0.4445 0.0438 1.0000 Uiso H93 0.1239 0.0711 0.4077 0.0438 1.0000 Uiso H111 0.1272 -0.1087 0.5213 0.0422 1.0000 Uiso H121 0.2441 -0.2068 0.5488 0.0544 1.0000 Uiso H131 0.4129 -0.1750 0.5685 0.0520 1.0000 Uiso H141 0.4660 -0.0469 0.5531 0.0519 1.0000 Uiso H151 0.3489 0.0499 0.5250 0.0394 1.0000 Uiso H171 -0.3083 0.3139 0.6569 0.0606 1.0000 Uiso H172 -0.2071 0.3606 0.6744 0.0606 1.0000 Uiso H173 -0.2345 0.3329 0.5983 0.0606 1.0000 Uiso H191 -0.2548 0.1216 0.6044 0.0620 1.0000 Uiso H201 -0.3362 0.0191 0.6549 0.0889 1.0000 Uiso H211 -0.3643 0.0228 0.7693 0.1175 1.0000 Uiso H221 -0.3163 0.1315 0.8340 0.1232 1.0000 Uiso H231 -0.2349 0.2367 0.7839 0.0863 1.0000 Uiso H251 0.1274 0.0915 0.7418 0.0305 1.0000 Uiso H261 0.1195 -0.0007 0.8275 0.0344 1.0000 Uiso H271 0.1456 0.0353 0.9410 0.0347 1.0000 Uiso H281 0.1774 0.1657 0.9687 0.0410 1.0000 Uiso H291 0.1837 0.2593 0.8835 0.0363 1.0000 Uiso H311 0.2653 0.3720 0.8295 0.0447 1.0000 Uiso H321 0.4328 0.4053 0.8500 0.0567 1.0000 Uiso H331 0.5561 0.3426 0.7916 0.0601 1.0000 Uiso H341 0.5117 0.2452 0.7133 0.0546 1.0000 Uiso H351 0.3437 0.2148 0.6893 0.0380 1.0000 Uiso H371 -0.0142 0.2575 0.8109 0.0343 1.0000 Uiso H381 -0.1269 0.3529 0.8405 0.0422 1.0000 Uiso H391 -0.0951 0.4839 0.8174 0.0444 1.0000 Uiso H401 0.0482 0.5184 0.7641 0.0407 1.0000 Uiso H411 0.1624 0.4237 0.7350 0.0326 1.0000 Uiso H421 0.3896 0.2611 0.5774 0.0500 1.0000 Uiso H431 0.3202 0.0508 0.8442 0.1038 1.0000 Uiso 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 0.02484(9) 0.01348(8) 0.01727(8) 0.00001(7) -0.00204(6) 0.00097(8) N1 0.0211(19) 0.0226(18) 0.0198(17) 0.0007(14) -0.0009(14) 0.0101(15) N2 0.027(2) 0.0215(18) 0.027(2) 0.0029(16) 0.0032(16) -0.0030(16) C1 0.029(2) 0.018(2) 0.025(2) -0.0002(17) -0.0031(18) -0.0010(18) C2 0.025(2) 0.030(3) 0.041(3) 0.008(2) 0.001(2) -0.004(2) C3 0.037(3) 0.026(3) 0.053(3) 0.009(2) 0.003(3) -0.005(2) C4 0.037(3) 0.018(2) 0.037(3) 0.004(2) -0.003(2) -0.002(2) C5 0.035(3) 0.025(2) 0.029(2) 0.0055(19) 0.004(2) 0.001(2) C6 0.039(3) 0.025(2) 0.030(3) 0.003(2) 0.007(2) -0.002(2) O1 0.047(2) 0.0191(17) 0.060(3) 0.0084(17) 0.0001(19) -0.0005(16) C7 0.056(4) 0.024(3) 0.060(4) 0.006(3) 0.002(3) 0.008(3) S1 0.0325(6) 0.0197(5) 0.0191(5) -0.0009(4) -0.0043(4) 0.0044(4) S2 0.0277(6) 0.0169(5) 0.0187(5) -0.0004(4) -0.0046(4) 0.0027(4) C8 0.024(2) 0.022(2) 0.024(2) -0.0011(18) 0.0001(18) -0.0032(17) N3 0.032(2) 0.0245(19) 0.0218(19) -0.0060(16) -0.0055(16) 0.0068(16) C9 0.049(3) 0.034(3) 0.027(3) -0.010(2) -0.009(2) 0.005(2) C10 0.038(3) 0.022(2) 0.022(2) -0.0018(18) 0.006(2) 0.003(2) C11 0.036(3) 0.025(2) 0.044(3) -0.001(2) 0.002(2) 0.001(2) C12 0.052(4) 0.026(3) 0.057(4) 0.000(3) 0.009(3) 0.006(3) C13 0.046(3) 0.041(3) 0.043(3) 0.003(3) 0.010(3) 0.016(3) C14 0.032(3) 0.048(3) 0.050(3) -0.004(3) 0.001(3) 0.009(3) C15 0.035(3) 0.024(2) 0.040(3) -0.004(2) 0.005(2) 0.004(2) S3 0.0273(6) 0.0202(5) 0.0294(6) 0.0044(4) -0.0009(5) 0.0011(4) S4 0.0308(6) 0.0173(5) 0.0305(6) 0.0030(4) -0.0029(5) 0.0027(4) N4 0.026(2) 0.028(2) 0.047(3) 0.0065(19) -0.0009(19) 0.0059(17) C16 0.028(2) 0.022(2) 0.025(2) 0.0006(18) -0.0048(18) 0.0037(18) C17 0.036(3) 0.037(3) 0.079(5) 0.018(3) 0.001(3) 0.012(3) C18 0.023(3) 0.046(3) 0.052(3) 0.017(3) -0.004(2) 0.004(2) C19 0.055(4) 0.031(3) 0.069(4) 0.002(3) 0.016(3) -0.000(3) C20 0.053(4) 0.042(4) 0.127(8) 0.020(4) 0.025(5) -0.001(3) C21 0.043(5) 0.103(8) 0.15(1) 0.081(8) -0.001(6) -0.009(5) C22 0.045(5) 0.198(13) 0.065(5) 0.072(7) -0.005(4) -0.024(6) C23 0.057(5) 0.118(7) 0.041(4) 0.012(4) -0.007(3) -0.019(5) P1 0.0270(6) 0.0171(5) 0.0176(5) -0.0013(4) -0.0022(4) 0.0010(4) C24 0.029(2) 0.022(2) 0.019(2) 0.0050(17) -0.0026(17) 0.0027(18) C25 0.032(3) 0.020(2) 0.024(2) -0.0014(18) -0.0035(19) 0.0013(18) C26 0.038(3) 0.021(2) 0.028(2) 0.0015(19) -0.002(2) -0.0000(19) C27 0.037(3) 0.027(2) 0.023(2) 0.0049(19) -0.003(2) 0.001(2) C28 0.052(3) 0.033(3) 0.018(2) 0.003(2) -0.002(2) 0.006(2) C29 0.043(3) 0.023(2) 0.025(2) -0.0032(19) -0.003(2) 0.004(2) C30 0.030(2) 0.022(2) 0.024(2) 0.0022(17) -0.0046(18) -0.0038(18) C31 0.040(3) 0.028(2) 0.044(3) -0.008(2) -0.007(2) -0.001(2) C32 0.049(4) 0.041(3) 0.052(4) -0.009(3) -0.019(3) -0.011(3) C33 0.036(3) 0.057(4) 0.057(4) -0.003(3) -0.013(3) -0.009(3) C34 0.035(3) 0.059(4) 0.042(3) -0.005(3) -0.004(2) -0.002(3) C35 0.031(3) 0.036(3) 0.027(2) -0.004(2) -0.003(2) 0.001(2) C36 0.031(2) 0.022(2) 0.0154(19) -0.0054(17) -0.0052(17) 0.0015(18) C37 0.038(3) 0.027(2) 0.021(2) 0.0026(19) -0.0022(19) 0.006(2) C38 0.038(3) 0.041(3) 0.027(3) -0.002(2) -0.002(2) 0.016(2) C39 0.053(4) 0.032(3) 0.025(2) -0.002(2) -0.006(2) 0.023(2) C40 0.055(4) 0.022(2) 0.025(2) -0.0032(19) -0.010(2) 0.008(2) C41 0.041(3) 0.018(2) 0.023(2) -0.0003(18) -0.007(2) 0.0026(19) C42 0.034(3) 0.042(3) 0.049(3) -0.008(3) -0.002(2) 0.005(3) Cl1 0.0480(9) 0.0521(9) 0.0449(8) -0.0021(7) 0.0004(6) 0.0116(7) Cl2 0.0671(12) 0.053(1) 0.0968(15) -0.002(1) -0.0033(11) -0.0233(9) Cl3 0.0516(9) 0.0549(9) 0.059(1) 0.0004(8) -0.0166(8) 0.0013(7) C43 0.063(5) 0.112(8) 0.084(6) 0.005(6) -0.003(5) 0.005(5) Cl4 0.120(2) 0.123(2) 0.0746(15) 0.0142(15) -0.0066(15) 0.0377(18) Cl5 0.163(3) 0.0836(19) 0.116(2) -0.0090(17) -0.006(2) 0.0107(19) Cl6 0.163(3) 0.0879(19) 0.116(2) 0.0334(17) -0.054(2) -0.032(2) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . N1 . 1.762(4) yes Re1 . S1 . 2.4824(11) yes Re1 . S2 . 2.3958(11) yes Re1 . S3 . 2.5387(12) yes Re1 . S4 . 2.4660(12) yes Re1 . P1 . 2.3627(11) yes N1 . N2 . 1.261(5) yes N2 . C1 . 1.420(6) yes C1 . C2 . 1.387(7) yes C1 . C6 . 1.384(7) yes C2 . C3 . 1.393(7) yes C2 . H21 . 1.000 no C3 . C4 . 1.379(8) yes C3 . H31 . 1.000 no C4 . C5 . 1.388(7) yes C4 . O1 . 1.374(6) yes C5 . C6 . 1.391(7) yes C5 . H51 . 1.000 no C6 . H61 . 1.000 no O1 . C7 . 1.426(7) yes C7 . H71 . 1.000 no C7 . H72 . 1.000 no C7 . H73 . 1.000 no S1 . C8 . 1.712(5) yes S2 . C8 . 1.738(5) yes C8 . N3 . 1.330(6) yes N3 . C9 . 1.467(6) yes N3 . C10 . 1.447(6) yes C9 . H91 . 1.000 no C9 . H92 . 1.000 no C9 . H93 . 1.000 no C10 . C11 . 1.381(7) yes C10 . C15 . 1.373(8) yes C11 . C12 . 1.392(8) yes C11 . H111 . 1.000 no C12 . C13 . 1.391(9) yes C12 . H121 . 1.000 no C13 . C14 . 1.388(9) yes C13 . H131 . 1.000 no C14 . C15 . 1.385(8) yes C14 . H141 . 1.000 no C15 . H151 . 1.000 no S3 . C16 . 1.715(5) yes S4 . C16 . 1.697(5) yes N4 . C16 . 1.324(6) yes N4 . C17 . 1.481(7) yes N4 . C18 . 1.434(7) yes C17 . H171 . 1.000 no C17 . H172 . 1.000 no C17 . H173 . 1.000 no C18 . C19 . 1.371(9) yes C18 . C23 . 1.39(1) yes C19 . C20 . 1.38(1) yes C19 . H191 . 1.000 no C20 . C21 . 1.361(16) yes C20 . H201 . 1.000 no C21 . C22 . 1.390(17) yes C21 . H211 . 1.000 no C22 . C23 . 1.397(14) yes C22 . H221 . 1.00 no C23 . H231 . 1.00 no P1 . C24 . 1.845(4) yes P1 . C30 . 1.842(5) yes P1 . C36 . 1.829(5) yes C24 . C25 . 1.400(6) yes C24 . C29 . 1.395(6) yes C25 . C26 . 1.383(7) yes C25 . H251 . 1.000 no C26 . C27 . 1.382(7) yes C26 . H261 . 1.000 no C27 . C28 . 1.393(7) yes C27 . H271 . 1.000 no C28 . C29 . 1.388(7) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no C30 . C31 . 1.401(7) yes C30 . C35 . 1.384(7) yes C31 . C32 . 1.387(8) yes C31 . H311 . 1.000 no C32 . C33 . 1.38(1) yes C32 . H321 . 1.000 no C33 . C34 . 1.383(9) yes C33 . H331 . 1.000 no C34 . C35 . 1.393(8) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C36 . C37 . 1.388(7) yes C36 . C41 . 1.401(6) yes C37 . C38 . 1.383(7) yes C37 . H371 . 1.000 no C38 . C39 . 1.392(8) yes C38 . H381 . 1.000 no C39 . C40 . 1.374(9) yes C39 . H391 . 1.000 no C40 . C41 . 1.385(7) yes C40 . H401 . 1.000 no C41 . H411 . 1.000 no C42 . Cl1 . 1.762(6) yes C42 . Cl2 . 1.750(6) yes C42 . Cl3 . 1.750(6) yes C42 . H421 . 1.000 no C43 . Cl4 . 1.73(1) yes C43 . Cl5 . 1.722(11) yes C43 . Cl6 . 1.725(11) yes C43 . H431 . 1.00 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Re1 . S1 . 96.99(12) yes N1 . Re1 . S2 . 104.10(12) yes S1 . Re1 . S2 . 71.70(4) yes N1 . Re1 . S3 . 165.82(12) yes S1 . Re1 . S3 . 87.42(4) yes S2 . Re1 . S3 . 90.08(4) yes N1 . Re1 . S4 . 96.86(12) yes S1 . Re1 . S4 . 90.97(4) yes S2 . Re1 . S4 . 154.09(4) yes S3 . Re1 . S4 . 69.51(4) yes N1 . Re1 . P1 . 90.24(12) yes S1 . Re1 . P1 . 169.77(4) yes S2 . Re1 . P1 . 99.56(4) yes S3 . Re1 . P1 . 87.28(4) yes S4 . Re1 . P1 . 95.35(4) yes Re1 . N1 . N2 . 177.6(3) yes N1 . N2 . C1 . 119.5(4) yes N2 . C1 . C2 . 117.8(4) yes N2 . C1 . C6 . 123.8(4) yes C2 . C1 . C6 . 118.4(4) yes C1 . C2 . C3 . 120.5(5) yes C1 . C2 . H21 . 119.7 no C3 . C2 . H21 . 119.7 no C2 . C3 . C4 . 120.4(5) yes C2 . C3 . H31 . 119.8 no C4 . C3 . H31 . 119.8 no C3 . C4 . C5 . 119.8(5) yes C3 . C4 . O1 . 116.1(5) yes C5 . C4 . O1 . 124.1(5) yes C4 . C5 . C6 . 119.2(5) yes C4 . C5 . H51 . 120.4 no C6 . C5 . H51 . 120.4 no C1 . C6 . C5 . 121.7(5) yes C1 . C6 . H61 . 119.2 no C5 . C6 . H61 . 119.2 no C4 . O1 . C7 . 116.1(4) yes O1 . C7 . H71 . 109.5 no O1 . C7 . H72 . 109.5 no H71 . C7 . H72 . 109.5 no O1 . C7 . H73 . 109.5 no H71 . C7 . H73 . 109.5 no H72 . C7 . H73 . 109.5 no Re1 . S1 . C8 . 87.06(15) yes Re1 . S2 . C8 . 89.29(16) yes S1 . C8 . S2 . 111.9(3) yes S1 . C8 . N3 . 124.1(3) yes S2 . C8 . N3 . 124.0(4) yes C8 . N3 . C9 . 121.0(4) yes C8 . N3 . C10 . 121.7(4) yes C9 . N3 . C10 . 117.1(4) yes N3 . C9 . H91 . 109.5 no N3 . C9 . H92 . 109.5 no H91 . C9 . H92 . 109.5 no N3 . C9 . H93 . 109.5 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no N3 . C10 . C11 . 119.8(5) yes N3 . C10 . C15 . 119.3(4) yes C11 . C10 . C15 . 120.9(5) yes C10 . C11 . C12 . 119.3(5) yes C10 . C11 . H111 . 120.4 no C12 . C11 . H111 . 120.4 no C11 . C12 . C13 . 120.0(5) yes C11 . C12 . H121 . 120.0 no C13 . C12 . H121 . 120.0 no C12 . C13 . C14 . 119.9(5) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.1 no C13 . C14 . C15 . 119.7(5) yes C13 . C14 . H141 . 120.2 no C15 . C14 . H141 . 120.2 no C10 . C15 . C14 . 120.2(5) yes C10 . C15 . H151 . 119.9 no C14 . C15 . H151 . 119.9 no Re1 . S3 . C16 . 87.09(17) yes Re1 . S4 . C16 . 89.89(16) yes C16 . N4 . C17 . 120.5(4) yes C16 . N4 . C18 . 120.9(4) yes C17 . N4 . C18 . 118.4(4) yes S3 . C16 . S4 . 113.5(3) yes S3 . C16 . N4 . 123.0(4) yes S4 . C16 . N4 . 123.5(4) yes N4 . C17 . H171 . 109.5 no N4 . C17 . H172 . 109.5 no H171 . C17 . H172 . 109.5 no N4 . C17 . H173 . 109.5 no H171 . C17 . H173 . 109.5 no H172 . C17 . H173 . 109.5 no N4 . C18 . C19 . 120.1(6) yes N4 . C18 . C23 . 118.5(6) yes C19 . C18 . C23 . 121.4(6) yes C18 . C19 . C20 . 120.0(7) yes C18 . C19 . H191 . 120.0 no C20 . C19 . H191 . 120.0 no C19 . C20 . C21 . 120.3(9) yes C19 . C20 . H201 . 119.8 no C21 . C20 . H201 . 119.8 no C20 . C21 . C22 . 120.0(8) yes C20 . C21 . H211 . 120.0 no C22 . C21 . H211 . 120.0 no C21 . C22 . C23 . 120.8(9) yes C21 . C22 . H221 . 119.6 no C23 . C22 . H221 . 119.6 no C18 . C23 . C22 . 117.5(9) yes C18 . C23 . H231 . 121.2 no C22 . C23 . H231 . 121.2 no Re1 . P1 . C24 . 120.77(15) yes Re1 . P1 . C30 . 114.63(16) yes C24 . P1 . C30 . 100.4(2) yes Re1 . P1 . C36 . 111.95(14) yes C24 . P1 . C36 . 101.4(2) yes C30 . P1 . C36 . 105.8(2) yes P1 . C24 . C25 . 122.0(3) yes P1 . C24 . C29 . 118.9(4) yes C25 . C24 . C29 . 119.1(4) yes C24 . C25 . C26 . 120.4(4) yes C24 . C25 . H251 . 119.8 no C26 . C25 . H251 . 119.8 no C25 . C26 . C27 . 120.6(4) yes C25 . C26 . H261 . 119.7 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 119.3(4) yes C26 . C27 . H271 . 120.3 no C28 . C27 . H271 . 120.3 no C27 . C28 . C29 . 120.7(4) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 119.7 no C24 . C29 . C28 . 119.9(4) yes C24 . C29 . H291 . 120.0 no C28 . C29 . H291 . 120.0 no P1 . C30 . C31 . 123.5(4) yes P1 . C30 . C35 . 117.3(4) yes C31 . C30 . C35 . 119.0(5) yes C30 . C31 . C32 . 120.2(5) yes C30 . C31 . H311 . 119.9 no C32 . C31 . H311 . 119.9 no C31 . C32 . C33 . 120.4(5) yes C31 . C32 . H321 . 119.8 no C33 . C32 . H321 . 119.8 no C32 . C33 . C34 . 119.7(6) yes C32 . C33 . H331 . 120.2 no C34 . C33 . H331 . 120.2 no C33 . C34 . C35 . 120.2(6) yes C33 . C34 . H341 . 119.9 no C35 . C34 . H341 . 119.9 no C30 . C35 . C34 . 120.5(5) yes C30 . C35 . H351 . 119.8 no C34 . C35 . H351 . 119.8 no P1 . C36 . C37 . 119.7(4) yes P1 . C36 . C41 . 120.5(4) yes C37 . C36 . C41 . 119.0(4) yes C36 . C37 . C38 . 120.5(5) yes C36 . C37 . H371 . 119.8 no C38 . C37 . H371 . 119.7 no C37 . C38 . C39 . 120.1(5) yes C37 . C38 . H381 . 120.0 no C39 . C38 . H381 . 120.0 no C38 . C39 . C40 . 119.8(5) yes C38 . C39 . H391 . 120.1 no C40 . C39 . H391 . 120.1 no C39 . C40 . C41 . 120.5(5) yes C39 . C40 . H401 . 119.7 no C41 . C40 . H401 . 119.7 no C36 . C41 . C40 . 120.1(5) yes C36 . C41 . H411 . 120.0 no C40 . C41 . H411 . 120.0 no Cl1 . C42 . Cl2 . 110.1(3) yes Cl1 . C42 . Cl3 . 110.3(3) yes Cl2 . C42 . Cl3 . 110.4(4) yes Cl1 . C42 . H421 . 108.8 no Cl2 . C42 . H421 . 108.6 no Cl3 . C42 . H421 . 108.5 no Cl4 . C43 . Cl5 . 113.5(6) yes Cl4 . C43 . Cl6 . 111.3(6) yes Cl5 . C43 . Cl6 . 111.3(5) yes Cl4 . C43 . H431 . 105.9 no Cl5 . C43 . H431 . 106.0 no Cl6 . C43 . H431 . 108.5 no # Attachment 'arc468.cif' data_CRYSTALS_cif_arc468 _database_code_depnum_ccdc_archive 'CCDC 617267' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #============================================================= _cell_length_a 16.7286(2) _cell_angle_alpha 90 _cell_length_b 9.6479(2) _cell_angle_beta 93.6530(4) _cell_length_c 24.8790(3) _cell_angle_gamma 90 _cell_volume 4007.2 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'P ' 0.0900 0.0950 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _chemical_formula_sum ' C44 H41 Cl2 N4 O1 P2 Re1 ' _chemical_formula_moiety ' C44 H41 Cl2 N4 O1 P2 Re1 ' _chemical_compound_source ; synthesis as described ; _chemical_formula_weight 960.89 _cell_measurement_reflns_used 57704 _cell_measurement_theta_min 5 _cell_measurement_theta_max 28 _cell_measurement_temperature 150 _cell_formula_units_Z 4 _exptl_crystal_description ' block ' _exptl_crystal_colour ' dark red ' _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.14 _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_meas ? _exptl_crystal_F_000 1915.654 _exptl_absorpt_coefficient_mu 3.286 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.77 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 57704 _reflns_number_total 9104 #9635 unique reflections including absences _diffrn_reflns_av_R_equivalents 0.050 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_gt 6807 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _reflns_limit_h_min -21 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _refine_diff_density_min -0.99 _refine_diff_density_max 1.46 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6807 _refine_ls_number_parameters 487 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0311 _refine_ls_goodness_of_fit_ref 1.0528 _refine_ls_shift/su_max 0.004084 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, (Carruthers & Watkin , 1979) 0.256 0.131 0.0559 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Re1 0.323018(8) 0.348856(14) 0.598205(5) 0.0162 1.0000 Uani Cl1 0.36653(5) 0.4631(1) 0.52049(3) 0.0241 1.0000 Uani Cl2 0.33726(6) 0.11725(9) 0.56770(4) 0.0269 1.0000 Uani N1 0.28757(17) 0.3388(3) 0.66474(12) 0.0223 1.0000 Uani N2 0.26927(19) 0.4247(3) 0.70108(12) 0.0247 1.0000 Uani C1 0.2808(2) 0.5574(4) 0.68002(14) 0.0233 1.0000 Uani C2 0.2670(2) 0.6777(4) 0.70820(15) 0.0284 1.0000 Uani C3 0.2802(3) 0.8021(4) 0.68381(17) 0.0324 1.0000 Uani C4 0.3071(3) 0.8042(4) 0.63220(17) 0.0323 1.0000 Uani C5 0.3198(2) 0.6795(4) 0.60569(15) 0.0249 1.0000 Uani N3 0.30736(17) 0.5572(3) 0.62889(11) 0.0190 1.0000 Uani P1 0.18640(5) 0.34513(9) 0.55704(3) 0.0180 1.0000 Uani C6 0.1508(2) 0.5205(4) 0.54336(15) 0.0242 1.0000 Uani C7 0.1586(2) 0.5823(4) 0.49322(17) 0.0312 1.0000 Uani C8 0.1458(3) 0.7245(5) 0.48686(18) 0.0373 1.0000 Uani C9 0.1235(3) 0.8046(5) 0.5296(2) 0.0413 1.0000 Uani C10 0.1147(2) 0.7431(5) 0.57927(19) 0.0361 1.0000 Uani C11 0.1290(2) 0.6034(4) 0.58637(16) 0.0276 1.0000 Uani C12 0.1143(2) 0.2678(4) 0.60075(14) 0.0234 1.0000 Uani C13 0.0364(2) 0.3166(4) 0.60347(16) 0.0293 1.0000 Uani C14 -0.0156(2) 0.2537(5) 0.63781(17) 0.0341 1.0000 Uani C15 0.0092(2) 0.1401(5) 0.66846(16) 0.0346 1.0000 Uani C16 0.0864(3) 0.0888(4) 0.66528(16) 0.0321 1.0000 Uani C17 0.1389(2) 0.1525(4) 0.63129(15) 0.0274 1.0000 Uani C18 0.1680(2) 0.2483(4) 0.49394(14) 0.0231 1.0000 Uani C19 0.0953(2) 0.1807(4) 0.48173(16) 0.0307 1.0000 Uani C20 0.0852(2) 0.0982(5) 0.43564(16) 0.0328 1.0000 Uani C21 0.1460(3) 0.0842(4) 0.40148(16) 0.0323 1.0000 Uani C22 0.2174(2) 0.1551(5) 0.41222(15) 0.0324 1.0000 Uani C23 0.2286(2) 0.2366(5) 0.45833(16) 0.0314 1.0000 Uani P2 0.46212(5) 0.34900(9) 0.63439(3) 0.0176 1.0000 Uani C24 0.5006(2) 0.5258(4) 0.64240(13) 0.0197 1.0000 Uani C25 0.5404(2) 0.5862(4) 0.60071(15) 0.0249 1.0000 Uani C26 0.5591(2) 0.7268(5) 0.60231(16) 0.0312 1.0000 Uani C27 0.5395(2) 0.8079(4) 0.64540(17) 0.0311 1.0000 Uani C28 0.5003(2) 0.7479(4) 0.68735(16) 0.0306 1.0000 Uani C29 0.4803(2) 0.6086(4) 0.68592(14) 0.0235 1.0000 Uani C30 0.4749(2) 0.2673(4) 0.70128(14) 0.0214 1.0000 Uani C31 0.5289(2) 0.3159(4) 0.74159(15) 0.0284 1.0000 Uani C32 0.5383(3) 0.2457(5) 0.79054(16) 0.0360 1.0000 Uani C33 0.4939(3) 0.1268(5) 0.79893(16) 0.0344 1.0000 Uani C34 0.4403(2) 0.0788(4) 0.75920(17) 0.0325 1.0000 Uani C35 0.4302(2) 0.1480(4) 0.70993(15) 0.0257 1.0000 Uani C36 0.5387(2) 0.2612(4) 0.59753(14) 0.0217 1.0000 Uani C37 0.6136(2) 0.2330(4) 0.62323(16) 0.0305 1.0000 Uani C38 0.6721(2) 0.1647(5) 0.59638(18) 0.0382 1.0000 Uani C39 0.6562(2) 0.1239(5) 0.54326(18) 0.0349 1.0000 Uani C40 0.5829(2) 0.1515(4) 0.51741(16) 0.0314 1.0000 Uani C41 0.5238(2) 0.2201(4) 0.54420(15) 0.0280 1.0000 Uani O1 0.6804(2) 0.6002(5) 0.78311(16) 0.0689 1.0000 Uani C42 0.6953(3) 0.5804(6) 0.7365(2) 0.0477 1.0000 Uani N4 0.7593(2) 0.5160(4) 0.71960(16) 0.0413 1.0000 Uani C43 0.8214(3) 0.4644(7) 0.7589(3) 0.0609 1.0000 Uani C44 0.7729(3) 0.4998(7) 0.6630(2) 0.0595 1.0000 Uani H21 0.2479 0.6739 0.7455 0.0343 1.0000 Uiso H31 0.2704 0.8909 0.7031 0.0389 1.0000 Uiso H41 0.3172 0.8945 0.6141 0.0389 1.0000 Uiso H51 0.3388 0.6817 0.5684 0.0300 1.0000 Uiso H71 0.1734 0.5249 0.4619 0.0376 1.0000 Uiso H81 0.1527 0.7689 0.4511 0.0444 1.0000 Uiso H91 0.1139 0.9062 0.5247 0.0492 1.0000 Uiso H101 0.0978 0.8004 0.6101 0.0432 1.0000 Uiso H111 0.1238 0.5607 0.6226 0.0332 1.0000 Uiso H131 0.0176 0.3970 0.5807 0.0353 1.0000 Uiso H141 -0.0710 0.2910 0.6403 0.0413 1.0000 Uiso H151 -0.0283 0.0951 0.6929 0.0418 1.0000 Uiso H161 0.1043 0.0063 0.6872 0.0385 1.0000 Uiso H171 0.1943 0.1151 0.6289 0.0329 1.0000 Uiso H191 0.0504 0.1914 0.5060 0.0366 1.0000 Uiso H201 0.0333 0.0489 0.4275 0.0390 1.0000 Uiso H211 0.1389 0.0232 0.3690 0.0383 1.0000 Uiso H221 0.2610 0.1477 0.3867 0.0389 1.0000 Uiso H231 0.2804 0.2869 0.4659 0.0377 1.0000 Uiso H251 0.5557 0.5284 0.5696 0.0299 1.0000 Uiso H261 0.5869 0.7696 0.5720 0.0374 1.0000 Uiso H271 0.5533 0.9087 0.6464 0.0369 1.0000 Uiso H281 0.4865 0.8059 0.7188 0.0365 1.0000 Uiso H291 0.4514 0.5669 0.7159 0.0282 1.0000 Uiso H311 0.5611 0.4012 0.7355 0.0340 1.0000 Uiso H321 0.5770 0.2809 0.8197 0.0430 1.0000 Uiso H331 0.5010 0.0761 0.8340 0.0415 1.0000 Uiso H341 0.4083 -0.0065 0.7656 0.0392 1.0000 Uiso H351 0.3913 0.1124 0.6810 0.0308 1.0000 Uiso H371 0.6252 0.2626 0.6615 0.0365 1.0000 Uiso H381 0.7255 0.1449 0.6152 0.0457 1.0000 Uiso H391 0.6981 0.0743 0.5238 0.0423 1.0000 Uiso H401 0.5719 0.1222 0.4791 0.0380 1.0000 Uiso H411 0.4706 0.2399 0.5251 0.0335 1.0000 Uiso H421 0.6555 0.6159 0.7081 0.0573 1.0000 Uiso H431 0.8046 0.4819 0.7962 0.0726 1.0000 Uiso H432 0.8729 0.5136 0.7537 0.0726 1.0000 Uiso H433 0.8288 0.3626 0.7536 0.0726 1.0000 Uiso H441 0.7264 0.5389 0.6407 0.0714 1.0000 Uiso H442 0.8229 0.5501 0.6547 0.0714 1.0000 Uiso H443 0.7788 0.3991 0.6545 0.0714 1.0000 Uiso 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 0.01921(7) 0.01518(7) 0.01462(7) -0.00012(6) 0.00317(4) -0.00022(5) Cl1 0.0289(4) 0.0257(4) 0.0181(4) 0.0013(3) 0.0062(3) -0.0021(4) Cl2 0.0348(5) 0.0182(4) 0.0278(4) -0.0040(3) 0.0026(4) 0.0009(3) N1 0.0206(14) 0.0222(15) 0.0240(15) -0.0030(13) -0.0004(11) -0.0010(12) N2 0.0302(16) 0.0236(16) 0.0210(15) -0.0009(12) 0.0083(12) -0.0011(13) C1 0.0232(17) 0.0281(19) 0.0192(16) -0.0031(15) 0.0060(13) -0.0022(15) C2 0.032(2) 0.030(2) 0.0229(18) -0.0064(15) 0.0060(15) 0.0033(16) C3 0.035(2) 0.030(2) 0.032(2) -0.0064(17) 0.0039(17) 0.0041(17) C4 0.041(2) 0.0215(19) 0.035(2) 0.0006(16) 0.0051(18) -0.0003(17) C5 0.0273(18) 0.0180(17) 0.030(2) 0.0032(14) 0.0042(15) -0.0007(14) N3 0.0204(14) 0.0165(14) 0.0200(14) -0.0017(12) 0.0019(11) 0.0014(11) P1 0.0190(4) 0.0189(4) 0.0163(4) -0.0003(3) 0.0026(3) -0.0010(3) C6 0.0213(17) 0.0222(18) 0.0293(19) 0.0040(15) 0.0026(14) -0.0008(14) C7 0.030(2) 0.033(2) 0.031(2) 0.0063(17) 0.0040(16) 0.0002(17) C8 0.038(2) 0.033(2) 0.040(2) 0.0181(19) -0.0053(19) -0.0001(18) C9 0.039(2) 0.027(2) 0.057(3) 0.005(2) -0.003(2) 0.0034(18) C10 0.028(2) 0.032(2) 0.048(3) -0.004(2) 0.0006(18) 0.0086(17) C11 0.0239(18) 0.0290(19) 0.030(2) -0.0021(16) 0.0036(15) 0.0043(15) C12 0.0251(18) 0.0267(19) 0.0189(17) -0.0027(15) 0.0046(13) -0.0042(15) C13 0.0230(18) 0.034(2) 0.031(2) -0.0057(17) 0.0038(15) -0.0031(16) C14 0.0244(19) 0.047(3) 0.032(2) -0.0089(19) 0.0082(16) -0.0042(18) C15 0.032(2) 0.050(3) 0.0230(18) -0.0000(18) 0.0079(15) -0.0177(19) C16 0.037(2) 0.033(2) 0.0255(19) 0.0050(17) 0.0018(16) -0.0114(18) C17 0.0284(18) 0.0295(19) 0.0244(18) 0.0001(16) 0.0040(14) -0.0080(16) C18 0.0289(18) 0.0193(17) 0.0208(17) -0.0016(14) -0.0006(14) 0.0041(15) C19 0.030(2) 0.035(2) 0.0263(19) -0.0048(17) -0.0019(15) 0.0027(17) C20 0.033(2) 0.036(2) 0.029(2) -0.0093(18) -0.0056(16) -0.0032(18) C21 0.041(2) 0.032(2) 0.0223(18) -0.0072(16) -0.0085(16) 0.0073(18) C22 0.035(2) 0.041(2) 0.0205(18) -0.0081(18) 0.0023(15) 0.0019(19) C23 0.033(2) 0.036(2) 0.0254(19) -0.0074(17) 0.0016(15) -0.0016(17) P2 0.0188(4) 0.0182(4) 0.0158(4) -0.0014(3) 0.0025(3) -0.0000(3) C24 0.0220(17) 0.0197(17) 0.0172(16) -0.0020(13) 0.0005(13) 0.0001(13) C25 0.0254(18) 0.027(2) 0.0224(18) -0.0010(15) 0.0026(14) -0.0015(15) C26 0.031(2) 0.035(2) 0.0274(19) 0.0075(17) -0.0001(16) -0.0083(17) C27 0.032(2) 0.0230(19) 0.037(2) -0.0000(16) -0.0056(17) -0.0043(16) C28 0.031(2) 0.030(2) 0.031(2) -0.0093(17) -0.0015(16) 0.0015(17) C29 0.0227(17) 0.0261(18) 0.0218(17) -0.0002(15) 0.0021(14) -0.0023(14) C30 0.0223(17) 0.0239(18) 0.0185(16) 0.0006(14) 0.0049(13) 0.0017(14) C31 0.034(2) 0.030(2) 0.0205(17) -0.0012(15) -0.0013(15) -0.0029(16) C32 0.045(2) 0.037(2) 0.026(2) 0.0002(18) -0.0034(17) 0.0030(19) C33 0.041(2) 0.042(3) 0.0203(18) 0.0116(17) 0.0043(16) 0.0073(19) C34 0.033(2) 0.030(2) 0.035(2) 0.0101(17) 0.0074(17) 0.0031(17) C35 0.0281(18) 0.0242(18) 0.0248(18) 0.0009(16) 0.0015(14) 0.0000(16) C36 0.0229(17) 0.0185(17) 0.0242(17) -0.0008(14) 0.0051(14) 0.0025(14) C37 0.030(2) 0.035(2) 0.0266(19) -0.0072(17) 0.0004(15) 0.0039(17) C38 0.027(2) 0.046(3) 0.041(2) -0.014(2) -0.0012(17) 0.0095(19) C39 0.029(2) 0.035(2) 0.041(2) -0.0130(19) 0.0101(17) 0.0055(17) C40 0.037(2) 0.032(2) 0.0262(19) -0.0067(17) 0.0077(16) 0.0046(18) C41 0.031(2) 0.029(2) 0.0236(18) -0.0041(16) 0.0008(15) 0.0051(16) O1 0.052(2) 0.103(4) 0.053(2) 0.015(2) 0.0199(18) 0.014(2) C42 0.032(2) 0.057(3) 0.054(3) 0.015(3) 0.005(2) 0.005(2) N4 0.035(2) 0.042(2) 0.047(2) 0.0109(18) 0.0015(16) 0.0006(17) C43 0.048(3) 0.064(4) 0.069(4) 0.021(3) -0.005(3) 0.011(3) C44 0.051(3) 0.073(4) 0.054(3) -0.009(3) 0.003(3) -0.003(3) _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Cl1 . 2.3798(8) yes Re1 . Cl2 . 2.3767(9) yes Re1 . N1 . 1.796(3) yes Re1 . N3 . 2.172(3) yes Re1 . P1 . 2.4444(9) yes Re1 . P2 . 2.4409(9) yes N1 . N2 . 1.278(4) yes N2 . C1 . 1.401(5) yes C1 . C2 . 1.383(5) yes C1 . N3 . 1.374(4) yes C2 . C3 . 1.369(6) yes C2 . H21 . 1.000 no C3 . C4 . 1.388(6) yes C3 . H31 . 1.000 no C4 . C5 . 1.395(6) yes C4 . H41 . 1.000 no C5 . N3 . 1.336(5) yes C5 . H51 . 1.000 no P1 . C6 . 1.818(4) yes P1 . C12 . 1.833(4) yes P1 . C18 . 1.836(4) yes C6 . C7 . 1.396(5) yes C6 . C11 . 1.403(5) yes C7 . C8 . 1.396(6) yes C7 . H71 . 1.000 no C8 . C9 . 1.384(7) yes C8 . H81 . 1.000 no C9 . C10 . 1.387(7) yes C9 . H91 . 1.000 no C10 . C11 . 1.378(6) yes C10 . H101 . 1.000 no C11 . H111 . 1.000 no C12 . C13 . 1.391(5) yes C12 . C17 . 1.394(6) yes C13 . C14 . 1.396(6) yes C13 . H131 . 1.000 no C14 . C15 . 1.384(7) yes C14 . H141 . 1.000 no C15 . C16 . 1.389(6) yes C15 . H151 . 1.000 no C16 . C17 . 1.400(5) yes C16 . H161 . 1.000 no C17 . H171 . 1.000 no C18 . C19 . 1.396(5) yes C18 . C23 . 1.393(5) yes C19 . C20 . 1.397(6) yes C19 . H191 . 1.000 no C20 . C21 . 1.373(6) yes C20 . H201 . 1.000 no C21 . C22 . 1.386(6) yes C21 . H211 . 1.000 no C22 . C23 . 1.394(5) yes C22 . H221 . 1.000 no C23 . H231 . 1.000 no P2 . C24 . 1.829(4) yes P2 . C30 . 1.841(4) yes P2 . C36 . 1.830(4) yes C24 . C25 . 1.396(5) yes C24 . C29 . 1.404(5) yes C25 . C26 . 1.391(6) yes C25 . H251 . 1.000 no C26 . C27 . 1.383(6) yes C26 . H261 . 1.000 no C27 . C28 . 1.393(6) yes C27 . H271 . 1.000 no C28 . C29 . 1.385(6) yes C28 . H281 . 1.000 no C29 . H291 . 1.000 no C30 . C31 . 1.388(5) yes C30 . C35 . 1.396(5) yes C31 . C32 . 1.394(6) yes C31 . H311 . 1.000 no C32 . C33 . 1.389(6) yes C32 . H321 . 1.000 no C33 . C34 . 1.372(6) yes C33 . H331 . 1.000 no C34 . C35 . 1.397(5) yes C34 . H341 . 1.000 no C35 . H351 . 1.000 no C36 . C37 . 1.397(5) yes C36 . C41 . 1.392(5) yes C37 . C38 . 1.386(6) yes C37 . H371 . 1.000 no C38 . C39 . 1.389(6) yes C38 . H381 . 1.000 no C39 . C40 . 1.373(6) yes C39 . H391 . 1.000 no C40 . C41 . 1.395(5) yes C40 . H401 . 1.000 no C41 . H411 . 1.000 no O1 . C42 . 1.218(6) yes C42 . N4 . 1.329(6) yes C42 . H421 . 1.000 no N4 . C43 . 1.467(6) yes N4 . C44 . 1.449(7) yes C43 . H431 . 1.000 no C43 . H432 . 1.000 no C43 . H433 . 1.000 no C44 . H441 . 1.000 no C44 . H442 . 1.000 no C44 . H443 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Re1 . Cl2 . 97.71(3) yes Cl1 . Re1 . N1 . 155.5(1) yes Cl2 . Re1 . N1 . 106.8(1) yes Cl1 . Re1 . N3 . 84.65(8) yes Cl2 . Re1 . N3 . 177.61(8) yes N1 . Re1 . N3 . 70.84(12) yes Cl1 . Re1 . P1 . 89.58(3) yes Cl2 . Re1 . P1 . 87.85(3) yes N1 . Re1 . P1 . 91.75(9) yes N3 . Re1 . P1 . 91.74(8) yes Cl1 . Re1 . P2 . 88.03(3) yes Cl2 . Re1 . P2 . 90.33(3) yes N1 . Re1 . P2 . 91.32(9) yes N3 . Re1 . P2 . 90.19(8) yes P1 . Re1 . P2 . 176.78(3) yes Re1 . N1 . N2 . 136.5(3) yes N1 . N2 . C1 . 106.5(3) yes N2 . C1 . C2 . 123.1(3) yes N2 . C1 . N3 . 113.9(3) yes C2 . C1 . N3 . 123.0(3) yes C1 . C2 . C3 . 118.3(3) yes C1 . C2 . H21 . 120.8 no C3 . C2 . H21 . 120.8 no C2 . C3 . C4 . 119.6(4) yes C2 . C3 . H31 . 120.2 no C4 . C3 . H31 . 120.2 no C3 . C4 . C5 . 119.6(4) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 120.2 no C4 . C5 . N3 . 121.6(3) yes C4 . C5 . H51 . 119.2 no N3 . C5 . H51 . 119.2 no Re1 . N3 . C1 . 112.3(2) yes Re1 . N3 . C5 . 129.8(2) yes C1 . N3 . C5 . 117.9(3) yes Re1 . P1 . C6 . 110.54(12) yes Re1 . P1 . C12 . 112.97(12) yes C6 . P1 . C12 . 105.66(17) yes Re1 . P1 . C18 . 117.82(12) yes C6 . P1 . C18 . 106.16(17) yes C12 . P1 . C18 . 102.70(17) yes P1 . C6 . C7 . 121.1(3) yes P1 . C6 . C11 . 119.1(3) yes C7 . C6 . C11 . 118.8(4) yes C6 . C7 . C8 . 119.9(4) yes C6 . C7 . H71 . 120.0 no C8 . C7 . H71 . 120.0 no C7 . C8 . C9 . 120.5(4) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 119.7 no C8 . C9 . C10 . 119.7(4) yes C8 . C9 . H91 . 120.2 no C10 . C9 . H91 . 120.2 no C9 . C10 . C11 . 120.3(4) yes C9 . C10 . H101 . 119.8 no C11 . C10 . H101 . 119.8 no C6 . C11 . C10 . 120.8(4) yes C6 . C11 . H111 . 119.6 no C10 . C11 . H111 . 119.6 no P1 . C12 . C13 . 123.0(3) yes P1 . C12 . C17 . 117.8(3) yes C13 . C12 . C17 . 119.2(3) yes C12 . C13 . C14 . 120.3(4) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 119.8 no C13 . C14 . C15 . 120.3(4) yes C13 . C14 . H141 . 119.8 no C15 . C14 . H141 . 119.8 no C14 . C15 . C16 . 119.9(4) yes C14 . C15 . H151 . 120.1 no C16 . C15 . H151 . 120.1 no C15 . C16 . C17 . 119.9(4) yes C15 . C16 . H161 . 120.0 no C17 . C16 . H161 . 120.0 no C12 . C17 . C16 . 120.4(4) yes C12 . C17 . H171 . 119.8 no C16 . C17 . H171 . 119.8 no P1 . C18 . C19 . 121.3(3) yes P1 . C18 . C23 . 119.8(3) yes C19 . C18 . C23 . 118.9(3) yes C18 . C19 . C20 . 120.2(4) yes C18 . C19 . H191 . 119.9 no C20 . C19 . H191 . 119.9 no C19 . C20 . C21 . 120.5(4) yes C19 . C20 . H201 . 119.7 no C21 . C20 . H201 . 119.7 no C20 . C21 . C22 . 119.7(4) yes C20 . C21 . H211 . 120.2 no C22 . C21 . H211 . 120.2 no C21 . C22 . C23 . 120.4(4) yes C21 . C22 . H221 . 119.8 no C23 . C22 . H221 . 119.8 no C18 . C23 . C22 . 120.2(4) yes C18 . C23 . H231 . 119.9 no C22 . C23 . H231 . 119.9 no Re1 . P2 . C24 . 111.16(11) yes Re1 . P2 . C30 . 112.72(11) yes C24 . P2 . C30 . 106.32(16) yes Re1 . P2 . C36 . 119.74(12) yes C24 . P2 . C36 . 103.52(16) yes C30 . P2 . C36 . 102.12(16) yes P2 . C24 . C25 . 119.3(3) yes P2 . C24 . C29 . 120.9(3) yes C25 . C24 . C29 . 119.0(3) yes C24 . C25 . C26 . 120.2(4) yes C24 . C25 . H251 . 119.9 no C26 . C25 . H251 . 119.9 no C25 . C26 . C27 . 120.7(4) yes C25 . C26 . H261 . 119.7 no C27 . C26 . H261 . 119.7 no C26 . C27 . C28 . 119.4(4) yes C26 . C27 . H271 . 120.3 no C28 . C27 . H271 . 120.3 no C27 . C28 . C29 . 120.6(4) yes C27 . C28 . H281 . 119.7 no C29 . C28 . H281 . 119.7 no C24 . C29 . C28 . 120.1(3) yes C24 . C29 . H291 . 119.9 no C28 . C29 . H291 . 119.9 no P2 . C30 . C31 . 122.8(3) yes P2 . C30 . C35 . 117.4(3) yes C31 . C30 . C35 . 119.8(3) yes C30 . C31 . C32 . 119.9(4) yes C30 . C31 . H311 . 120.0 no C32 . C31 . H311 . 120.0 no C31 . C32 . C33 . 120.1(4) yes C31 . C32 . H321 . 120.0 no C33 . C32 . H321 . 120.0 no C32 . C33 . C34 . 120.1(4) yes C32 . C33 . H331 . 119.9 no C34 . C33 . H331 . 119.9 no C33 . C34 . C35 . 120.5(4) yes C33 . C34 . H341 . 119.7 no C35 . C34 . H341 . 119.7 no C30 . C35 . C34 . 119.6(4) yes C30 . C35 . H351 . 120.2 no C34 . C35 . H351 . 120.2 no P2 . C36 . C37 . 119.8(3) yes P2 . C36 . C41 . 121.4(3) yes C37 . C36 . C41 . 118.8(3) yes C36 . C37 . C38 . 120.8(4) yes C36 . C37 . H371 . 119.6 no C38 . C37 . H371 . 119.6 no C37 . C38 . C39 . 119.6(4) yes C37 . C38 . H381 . 120.2 no C39 . C38 . H381 . 120.2 no C38 . C39 . C40 . 120.2(4) yes C38 . C39 . H391 . 119.9 no C40 . C39 . H391 . 119.9 no C39 . C40 . C41 . 120.5(4) yes C39 . C40 . H401 . 119.8 no C41 . C40 . H401 . 119.8 no C36 . C41 . C40 . 120.1(4) yes C36 . C41 . H411 . 120.0 no C40 . C41 . H411 . 120.0 no O1 . C42 . N4 . 126.3(5) yes O1 . C42 . H421 . 116.8 no N4 . C42 . H421 . 116.8 no C42 . N4 . C43 . 119.9(5) yes C42 . N4 . C44 . 122.5(4) yes C43 . N4 . C44 . 117.6(4) yes N4 . C43 . H431 . 109.5 no N4 . C43 . H432 . 109.5 no H431 . C43 . H432 . 109.5 no N4 . C43 . H433 . 109.5 no H431 . C43 . H433 . 109.5 no H432 . C43 . H433 . 109.5 no N4 . C44 . H441 . 109.5 no N4 . C44 . H442 . 109.5 no H441 . C44 . H442 . 109.5 no N4 . C44 . H443 . 109.5 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no