Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cmp1 _database_code_depnum_ccdc_archive 'CCDC 651347' _audit_creation_date 2004-06-25T18:59:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #------------------------------------------------ # CHEMICAL INFORMATION #------------------------------------------- _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C31 H26 Cl4 Co N4 O4 Re, C2 H3 N' _chemical_formula_sum 'C33 H29 Cl4 Co N5 O4 Re' _chemical_formula_weight 946.54 #---------------------------------------------- # UNIT CELL INFORMATION #-------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.354(3) _cell_length_b 12.558(3) _cell_length_c 13.514(2) _cell_angle_alpha 82.892(19) _cell_angle_beta 63.258(15) _cell_angle_gamma 69.708(19) _cell_volume 1754.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.26 _cell_measurement_theta_max 20.81 #----------------------------------------------------- # CRYSTAL INFORMATION #--------------------------------------------------- _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_special_details ; ? ; #--------------------------------------------------- # ABSORPTION CORRECTION #-------------------------------------------------- _exptl_absorpt_coefficient_mu 4.268 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'MSC/AFC Diffractometer Software, 1993' _exptl_absorpt_correction_T_min 0.3166 _exptl_absorpt_correction_T_max 0.8826 #----------------------------------------------------- # DATA COLLECTION #----------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 5 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_unetI/netI 0.04 _diffrn_reflns_number 9132 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.69 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.9876 _diffrn_measured_fraction_theta_max 0.9876 _reflns_number_total 8029 _reflns_number_gt 7065 _reflns_threshold_expression >2sigma(I) #----------------------------------------------- # COMPUTER PROGRAMS USED #-------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Software, 1993' _computing_cell_refinement 'MSC/AFC Diffractometer Software, 1993' _computing_data_reduction 'MSC/AFC Diffractometer Software, 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------- # REFINEMENT INFORMATION #------------------------------------------ _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0776P)^2^+15.5133P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8029 _refine_ls_number_parameters 432 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1736 _refine_ls_wR_factor_gt 0.1609 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.793 _refine_diff_density_min -5.399 _refine_diff_density_rms 0.203 #-------------------------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #-------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 1.10045(3) 0.77200(3) 0.70790(2) 0.03705(12) Uani 1 1 d . . . Cl1 Cl 1.3086(2) 0.7322(2) 0.6872(2) 0.0549(5) Uani 1 1 d . . . Cl2 Cl 1.1248(3) 0.5787(2) 0.7075(2) 0.0567(6) Uani 1 1 d . . . Cl3 Cl 1.0111(3) 0.7800(3) 0.90251(19) 0.0639(7) Uani 1 1 d . . . Cl4 Cl 1.1623(2) 0.7846(2) 0.51644(18) 0.0535(5) Uani 1 1 d . . . O1 O 0.9156(6) 0.8133(5) 0.7281(5) 0.0431(13) Uani 1 1 d . . . O2 O 1.0731(6) 0.9420(5) 0.7095(6) 0.0491(15) Uani 1 1 d . . . C1 C 0.8242(8) 0.9053(8) 0.7658(7) 0.0430(18) Uani 1 1 d . . . C2 C 0.843(3) 1.003(3) 0.805(2) 0.056(8) Uani 0.5 1 d P . . H2A H 0.7795 1.072 0.7994 0.067 Uiso 0.5 1 calc PR . . H2B H 0.8224 0.9933 0.8827 0.067 Uiso 0.5 1 calc PR . . C2' C 0.848(3) 1.020(3) 0.754(3) 0.062(8) Uani 0.5 1 d P . . H2C H 0.8431 1.0522 0.6862 0.074 Uiso 0.5 1 calc PR . . H2D H 0.777 1.0697 0.8149 0.074 Uiso 0.5 1 calc PR . . C3 C 0.9708(8) 1.0237(7) 0.7499(7) 0.0426(18) Uani 1 1 d . . . O3 O 0.7124(6) 0.9124(6) 0.7917(6) 0.0479(14) Uani 1 1 d . . . O4 O 0.9702(7) 1.1178(7) 0.7631(7) 0.069(2) Uani 1 1 d . . . Co1 Co 0.65700(9) 0.78429(9) 0.77304(8) 0.0335(2) Uani 1 1 d . . . N11 N 0.7524(6) 0.6219(6) 0.7032(6) 0.0366(14) Uani 1 1 d . . . N12 N 0.7063(7) 0.6988(6) 0.9011(6) 0.0410(15) Uani 1 1 d . . . C11 C 0.7650(9) 0.5808(8) 0.6111(7) 0.0456(19) Uani 1 1 d . . . C12 C 0.8390(11) 0.4699(9) 0.5737(9) 0.058(2) Uani 1 1 d . . . H12 H 0.8469 0.4429 0.5089 0.07 Uiso 1 1 calc R . . C13 C 0.9007(10) 0.3995(9) 0.6312(10) 0.062(3) Uani 1 1 d . . . H13 H 0.9503 0.325 0.6052 0.075 Uiso 1 1 calc R . . C14 C 0.8899(9) 0.4383(7) 0.7291(9) 0.049(2) Uani 1 1 d . . . C15 C 0.9497(10) 0.3697(9) 0.7947(11) 0.063(3) Uani 1 1 d . . . H15 H 1.0036 0.2959 0.7696 0.076 Uiso 1 1 calc R . . C16 C 0.9311(11) 0.4075(10) 0.8901(11) 0.067(3) Uani 1 1 d . . . H16 H 0.9728 0.3608 0.9302 0.08 Uiso 1 1 calc R . . C17 C 0.8476(9) 0.5192(9) 0.9312(9) 0.051(2) Uani 1 1 d . . . C18 C 0.8171(12) 0.5621(12) 1.0345(9) 0.066(3) Uani 1 1 d . . . H18 H 0.8538 0.5185 1.0793 0.079 Uiso 1 1 calc R . . C19 C 0.7342(12) 0.6673(12) 1.0676(8) 0.065(3) Uani 1 1 d . . . H19 H 0.7131 0.6961 1.1364 0.079 Uiso 1 1 calc R . . C110 C 0.6767(10) 0.7370(10) 1.0001(8) 0.054(2) Uani 1 1 d . . . C111 C 0.7878(8) 0.5922(7) 0.8684(7) 0.0407(17) Uani 1 1 d . . . C112 C 0.8120(7) 0.5504(7) 0.7632(7) 0.0375(16) Uani 1 1 d . . . C113 C 0.6909(12) 0.6554(10) 0.5502(10) 0.067(3) Uani 1 1 d . . . H11A H 0.6443 0.7293 0.5867 0.101 Uiso 1 1 calc R . . H11B H 0.6319 0.622 0.5502 0.101 Uiso 1 1 calc R . . H11C H 0.7496 0.6625 0.4752 0.101 Uiso 1 1 calc R . . C114 C 0.5811(13) 0.8508(12) 1.0402(10) 0.078(4) Uani 1 1 d . . . H11D H 0.5543 0.8851 0.9839 0.117 Uiso 1 1 calc R . . H11E H 0.6186 0.8973 1.057 0.117 Uiso 1 1 calc R . . H11F H 0.5082 0.844 1.1059 0.117 Uiso 1 1 calc R . . N21 N 0.4595(6) 0.8177(6) 0.8370(6) 0.0381(14) Uani 1 1 d . . . N22 N 0.6141(6) 0.9030(6) 0.6547(5) 0.0373(14) Uani 1 1 d . . . C21 C 0.3840(8) 0.7671(9) 0.9191(7) 0.046(2) Uani 1 1 d . . . C22 C 0.2508(10) 0.8197(12) 0.9724(9) 0.066(3) Uani 1 1 d . . . H22 H 0.1995 0.7849 1.0301 0.079 Uiso 1 1 calc R . . C23 C 0.1978(9) 0.9230(11) 0.9383(10) 0.068(3) Uani 1 1 d . . . H23 H 0.1097 0.9594 0.9753 0.081 Uiso 1 1 calc R . . C24 C 0.2725(8) 0.9763(9) 0.8485(8) 0.051(2) Uani 1 1 d . . . C25 C 0.2232(9) 1.0834(10) 0.8043(10) 0.065(3) Uani 1 1 d . . . H25 H 0.1359 1.1242 0.8386 0.078 Uiso 1 1 calc R . . C26 C 0.3004(11) 1.1248(10) 0.7154(10) 0.063(3) Uani 1 1 d . . . H26 H 0.265 1.1933 0.6888 0.076 Uiso 1 1 calc R . . C27 C 0.4349(9) 1.0676(8) 0.6600(8) 0.047(2) Uani 1 1 d . . . C28 C 0.5197(11) 1.1058(8) 0.5632(9) 0.054(2) Uani 1 1 d . . . H28 H 0.489 1.1737 0.5331 0.064 Uiso 1 1 calc R . . C29 C 0.6459(10) 1.0434(9) 0.5146(8) 0.052(2) Uani 1 1 d . . . H29 H 0.7018 1.0664 0.4494 0.063 Uiso 1 1 calc R . . C210 C 0.6914(8) 0.9426(8) 0.5642(7) 0.0425(18) Uani 1 1 d . . . C211 C 0.4866(7) 0.9646(7) 0.7026(7) 0.0365(16) Uani 1 1 d . . . C212 C 0.4053(7) 0.9183(7) 0.7987(6) 0.0370(16) Uani 1 1 d . . . C213 C 0.4415(11) 0.6507(10) 0.9522(10) 0.068(3) Uani 1 1 d . . . H21A H 0.533 0.6258 0.9092 0.101 Uiso 1 1 calc R . . H21B H 0.4072 0.5988 0.9392 0.101 Uiso 1 1 calc R . . H21C H 0.4213 0.6529 1.0295 0.101 Uiso 1 1 calc R . . C214 C 0.8311(9) 0.8781(10) 0.5143(8) 0.058(3) Uani 1 1 d . . . H21D H 0.8476 0.8125 0.5568 0.087 Uiso 1 1 calc R . . H21E H 0.8773 0.9258 0.5144 0.087 Uiso 1 1 calc R . . H21F H 0.8587 0.8544 0.4394 0.087 Uiso 1 1 calc R . . C32 C 0.493(2) 0.584(3) 0.3733(18) 0.183(7) Uani 1 1 d D . . H32A H 0.4205 0.5897 0.4438 0.274 Uiso 1 1 calc R . . H32B H 0.5382 0.632 0.375 0.274 Uiso 1 1 calc R . . H32C H 0.5499 0.5065 0.3584 0.274 Uiso 1 1 calc R . . C31 C 0.451(2) 0.618(3) 0.2882(19) 0.183(7) Uani 1 1 d D . . N31 N 0.416(2) 0.649(3) 0.2226(17) 0.183(7) Uani 1 1 d D . . 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 0.03726(18) 0.04604(19) 0.03075(17) -0.00137(12) -0.01353(13) -0.01786(14) Cl1 0.0423(11) 0.0651(14) 0.0606(14) -0.0013(11) -0.0251(10) -0.0163(10) Cl2 0.0671(15) 0.0446(11) 0.0623(14) 0.0032(10) -0.0275(12) -0.0242(11) Cl3 0.0739(16) 0.0897(19) 0.0325(10) 0.0047(11) -0.0202(11) -0.0369(15) Cl4 0.0592(13) 0.0700(15) 0.0341(10) -0.0030(9) -0.0173(9) -0.0270(12) O1 0.037(3) 0.051(3) 0.046(3) -0.005(3) -0.016(3) -0.020(3) O2 0.041(3) 0.039(3) 0.066(4) -0.018(3) -0.017(3) -0.014(3) C1 0.041(4) 0.052(5) 0.046(4) 0.003(4) -0.019(4) -0.026(4) C2 0.040(11) 0.057(17) 0.067(17) -0.023(14) -0.010(14) -0.020(11) C2' 0.047(14) 0.051(12) 0.10(3) 0.004(18) -0.04(2) -0.018(10) C3 0.043(4) 0.046(4) 0.039(4) -0.007(3) -0.009(3) -0.023(4) O3 0.042(3) 0.055(4) 0.059(4) 0.002(3) -0.027(3) -0.022(3) O4 0.050(4) 0.063(4) 0.088(6) -0.024(4) -0.011(4) -0.029(4) Co1 0.0238(4) 0.0394(5) 0.0342(5) -0.0038(4) -0.0110(4) -0.0074(4) N11 0.034(3) 0.039(3) 0.037(3) -0.006(3) -0.017(3) -0.008(3) N12 0.038(3) 0.051(4) 0.034(3) -0.002(3) -0.013(3) -0.017(3) C11 0.047(5) 0.050(5) 0.041(4) -0.009(4) -0.018(4) -0.015(4) C12 0.062(6) 0.055(6) 0.054(6) -0.018(5) -0.022(5) -0.013(5) C13 0.052(6) 0.051(5) 0.074(7) -0.022(5) -0.021(5) -0.006(4) C14 0.040(4) 0.036(4) 0.071(6) -0.004(4) -0.027(4) -0.009(3) C15 0.053(6) 0.042(5) 0.103(9) 0.005(5) -0.048(6) -0.006(4) C16 0.065(7) 0.060(6) 0.096(9) 0.031(6) -0.057(7) -0.023(5) C17 0.047(5) 0.062(6) 0.057(5) 0.017(4) -0.031(4) -0.027(4) C18 0.067(7) 0.102(9) 0.050(6) 0.024(6) -0.037(5) -0.045(7) C19 0.074(7) 0.109(10) 0.033(4) 0.007(5) -0.026(5) -0.049(7) C110 0.061(6) 0.079(7) 0.036(4) 0.001(4) -0.021(4) -0.037(5) C111 0.041(4) 0.048(4) 0.040(4) 0.006(3) -0.024(4) -0.016(4) C112 0.030(3) 0.039(4) 0.047(4) 0.002(3) -0.018(3) -0.013(3) C113 0.084(8) 0.072(7) 0.057(6) -0.014(5) -0.045(6) -0.015(6) C114 0.086(9) 0.088(9) 0.049(6) -0.032(6) -0.016(6) -0.024(7) N21 0.025(3) 0.051(4) 0.038(3) -0.005(3) -0.010(3) -0.015(3) N22 0.029(3) 0.047(4) 0.033(3) -0.006(3) -0.013(3) -0.009(3) C21 0.039(4) 0.066(6) 0.036(4) 0.001(4) -0.010(3) -0.030(4) C22 0.041(5) 0.097(9) 0.054(6) -0.008(6) -0.002(4) -0.038(6) C23 0.027(4) 0.089(8) 0.069(7) -0.022(6) -0.005(4) -0.013(5) C24 0.030(4) 0.066(6) 0.050(5) -0.018(4) -0.015(4) -0.006(4) C25 0.034(5) 0.076(7) 0.075(7) -0.026(6) -0.029(5) 0.012(5) C26 0.054(6) 0.062(6) 0.072(7) -0.016(5) -0.043(6) 0.010(5) C27 0.046(5) 0.047(5) 0.055(5) -0.010(4) -0.035(4) -0.002(4) C28 0.070(6) 0.048(5) 0.058(6) 0.013(4) -0.043(5) -0.018(5) C29 0.064(6) 0.060(6) 0.046(5) 0.012(4) -0.030(5) -0.030(5) C210 0.042(4) 0.055(5) 0.035(4) 0.002(3) -0.017(3) -0.020(4) C211 0.031(4) 0.042(4) 0.038(4) -0.011(3) -0.018(3) -0.006(3) C212 0.029(3) 0.047(4) 0.036(4) -0.012(3) -0.016(3) -0.007(3) C213 0.062(6) 0.076(7) 0.064(7) 0.026(6) -0.019(5) -0.042(6) C214 0.037(5) 0.081(7) 0.045(5) 0.011(5) -0.010(4) -0.020(5) C32 0.123(10) 0.32(2) 0.101(11) -0.017(14) -0.021(8) -0.093(13) C31 0.123(10) 0.32(2) 0.101(11) -0.017(14) -0.021(8) -0.093(13) N31 0.123(10) 0.32(2) 0.101(11) -0.017(14) -0.021(8) -0.093(13) #--------------------------------------------- # MOLECULAR GEOMETRY #-------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O2 2.043(6) . ? Re1 O1 2.052(6) . ? Re1 Cl1 2.332(2) . ? Re1 Cl2 2.340(2) . ? Re1 Cl4 2.347(2) . ? Re1 Cl3 2.350(2) . ? O1 C1 1.262(11) . ? O2 C3 1.252(11) . ? C1 O3 1.235(10) . ? C1 C2 1.52(3) . ? C1 C2' 1.54(4) . ? C2 C3 1.51(3) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C2' C3 1.52(3) . ? C2' H2C 0.97 . ? C2' H2D 0.97 . ? C3 O4 1.214(11) . ? O3 Co1 2.035(6) . ? Co1 N11 2.061(7) . ? Co1 N21 2.088(6) . ? Co1 N12 2.133(7) . ? Co1 N22 2.165(7) . ? N11 C11 1.330(10) . ? N11 C112 1.380(10) . ? N12 C110 1.324(11) . ? N12 C111 1.346(11) . ? C11 C12 1.381(13) . ? C11 C113 1.511(14) . ? C12 C13 1.364(16) . ? C12 H12 0.93 . ? C13 C14 1.400(15) . ? C13 H13 0.93 . ? C14 C112 1.394(11) . ? C14 C15 1.425(14) . ? C15 C16 1.322(18) . ? C15 H15 0.93 . ? C16 C17 1.420(16) . ? C16 H16 0.93 . ? C17 C18 1.398(15) . ? C17 C111 1.417(12) . ? C18 C19 1.338(18) . ? C18 H18 0.93 . ? C19 C110 1.433(16) . ? C19 H19 0.93 . ? C110 C114 1.475(17) . ? C111 C112 1.442(12) . ? C113 H11A 0.96 . ? C113 H11B 0.96 . ? C113 H11C 0.96 . ? C114 H11D 0.96 . ? C114 H11E 0.96 . ? C114 H11F 0.96 . ? N21 C21 1.345(11) . ? N21 C212 1.371(11) . ? N22 C210 1.335(11) . ? N22 C211 1.363(10) . ? C21 C22 1.400(14) . ? C21 C213 1.499(15) . ? C22 C23 1.363(18) . ? C22 H22 0.93 . ? C23 C24 1.412(16) . ? C23 H23 0.93 . ? C24 C212 1.405(11) . ? C24 C25 1.448(16) . ? C25 C26 1.335(18) . ? C25 H25 0.93 . ? C26 C27 1.422(14) . ? C26 H26 0.93 . ? C27 C211 1.410(12) . ? C27 C28 1.414(15) . ? C28 C29 1.354(15) . ? C28 H28 0.93 . ? C29 C210 1.416(13) . ? C29 H29 0.93 . ? C210 C214 1.486(13) . ? C211 C212 1.441(12) . ? C213 H21A 0.96 . ? C213 H21B 0.96 . ? C213 H21C 0.96 . ? C214 H21D 0.96 . ? C214 H21E 0.96 . ? C214 H21F 0.96 . ? C32 C31 1.43(4) . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? C31 N31 1.13(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 88.1(2) . . ? O2 Re1 Cl1 89.84(19) . . ? O1 Re1 Cl1 177.80(18) . . ? O2 Re1 Cl2 178.16(18) . . ? O1 Re1 Cl2 90.11(19) . . ? Cl1 Re1 Cl2 91.99(10) . . ? O2 Re1 Cl4 86.6(2) . . ? O1 Re1 Cl4 87.22(18) . . ? Cl1 Re1 Cl4 93.33(9) . . ? Cl2 Re1 Cl4 93.55(10) . . ? O2 Re1 Cl3 88.8(2) . . ? O1 Re1 Cl3 85.88(19) . . ? Cl1 Re1 Cl3 93.41(10) . . ? Cl2 Re1 Cl3 90.88(11) . . ? Cl4 Re1 Cl3 171.80(10) . . ? C1 O1 Re1 128.4(5) . . ? C3 O2 Re1 129.5(6) . . ? O3 C1 O1 121.5(8) . . ? O3 C1 C2 116.7(14) . . ? O1 C1 C2 120.4(14) . . ? O3 C1 C2' 115.1(15) . . ? O1 C1 C2' 121.6(15) . . ? C3 C2 C1 121(2) . . ? C3 C2 H2A 107 . . ? C1 C2 H2A 107 . . ? C3 C2 H2B 107 . . ? C1 C2 H2B 107 . . ? H2A C2 H2B 106.7 . . ? C3 C2' C1 120(2) . . ? C3 C2' H2C 107.4 . . ? C1 C2' H2C 107.4 . . ? C3 C2' H2D 107.4 . . ? C1 C2' H2D 107.4 . . ? H2C C2' H2D 106.9 . . ? O4 C3 O2 121.7(8) . . ? O4 C3 C2 117.2(14) . . ? O2 C3 C2 120.1(14) . . ? O4 C3 C2' 115.0(16) . . ? O2 C3 C2' 121.0(16) . . ? C1 O3 Co1 124.9(6) . . ? O3 Co1 N11 134.7(3) . . ? O3 Co1 N21 116.0(3) . . ? N11 Co1 N21 109.3(3) . . ? O3 Co1 N12 88.4(3) . . ? N11 Co1 N12 80.1(3) . . ? N21 Co1 N12 104.7(3) . . ? O3 Co1 N22 78.7(3) . . ? N11 Co1 N22 110.5(3) . . ? N21 Co1 N22 79.5(3) . . ? N12 Co1 N22 166.9(3) . . ? C11 N11 C112 118.7(7) . . ? C11 N11 Co1 129.3(6) . . ? C112 N11 Co1 112.0(5) . . ? C110 N12 C111 117.9(8) . . ? C110 N12 Co1 130.2(7) . . ? C111 N12 Co1 111.8(5) . . ? N11 C11 C12 121.1(9) . . ? N11 C11 C113 119.1(8) . . ? C12 C11 C113 119.8(9) . . ? C13 C12 C11 120.5(9) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.7(9) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C112 C14 C13 115.9(9) . . ? C112 C14 C15 120.0(9) . . ? C13 C14 C15 124.1(9) . . ? C16 C15 C14 122.3(10) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 120.0(9) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C18 C17 C111 116.7(10) . . ? C18 C17 C16 123.0(10) . . ? C111 C17 C16 120.3(10) . . ? C19 C18 C17 118.6(10) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C110 122.0(10) . . ? C18 C19 H19 119 . . ? C110 C19 H19 119 . . ? N12 C110 C19 120.3(10) . . ? N12 C110 C114 118.6(10) . . ? C19 C110 C114 121.2(10) . . ? N12 C111 C17 124.5(8) . . ? N12 C111 C112 116.6(7) . . ? C17 C111 C112 118.8(8) . . ? N11 C112 C14 123.1(8) . . ? N11 C112 C111 118.3(7) . . ? C14 C112 C111 118.6(8) . . ? C11 C113 H11A 109.5 . . ? C11 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C11 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C110 C114 H11D 109.5 . . ? C110 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C110 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? C21 N21 C212 119.8(7) . . ? C21 N21 Co1 129.3(6) . . ? C212 N21 Co1 109.7(5) . . ? C210 N22 C211 118.2(8) . . ? C210 N22 Co1 130.4(6) . . ? C211 N22 Co1 108.6(5) . . ? N21 C21 C22 121.1(10) . . ? N21 C21 C213 120.1(8) . . ? C22 C21 C213 118.8(9) . . ? C23 C22 C21 118.8(10) . . ? C23 C22 H22 120.6 . . ? C21 C22 H22 120.6 . . ? C22 C23 C24 122.0(9) . . ? C22 C23 H23 119 . . ? C24 C23 H23 119 . . ? C212 C24 C23 116.0(10) . . ? C212 C24 C25 118.5(9) . . ? C23 C24 C25 125.4(9) . . ? C26 C25 C24 121.3(9) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 122.2(10) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C211 C27 C28 117.8(8) . . ? C211 C27 C26 117.9(10) . . ? C28 C27 C26 124.3(10) . . ? C29 C28 C27 119.8(9) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C210 119.1(9) . . ? C28 C29 H29 120.4 . . ? C210 C29 H29 120.4 . . ? N22 C210 C29 122.8(8) . . ? N22 C210 C214 118.4(8) . . ? C29 C210 C214 118.9(8) . . ? N22 C211 C27 122.3(8) . . ? N22 C211 C212 116.8(7) . . ? C27 C211 C212 120.9(7) . . ? N21 C212 C24 122.0(8) . . ? N21 C212 C211 119.0(7) . . ? C24 C212 C211 119.0(8) . . ? C21 C213 H21A 109.5 . . ? C21 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? C21 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C210 C214 H21D 109.5 . . ? C210 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? C210 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C31 C32 178(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Re1 O1 C1 -21.3(8) . . . . ? Cl2 Re1 O1 C1 158.6(7) . . . . ? Cl4 Re1 O1 C1 -107.9(7) . . . . ? Cl3 Re1 O1 C1 67.7(7) . . . . ? O1 Re1 O2 C3 23.0(8) . . . . ? Cl1 Re1 O2 C3 -156.4(8) . . . . ? Cl4 Re1 O2 C3 110.3(8) . . . . ? Cl3 Re1 O2 C3 -63.0(8) . . . . ? Re1 O1 C1 O3 -167.0(6) . . . . ? Re1 O1 C1 C2 -0.8(18) . . . . ? Re1 O1 C1 C2' 29.1(18) . . . . ? O3 C1 C2 C3 -160.2(19) . . . . ? O1 C1 C2 C3 33(3) . . . . ? C2' C1 C2 C3 -68(5) . . . . ? O3 C1 C2' C3 165.1(19) . . . . ? O1 C1 C2' C3 -30(3) . . . . ? C2 C1 C2' C3 65(4) . . . . ? Re1 O2 C3 O4 165.8(8) . . . . ? Re1 O2 C3 C2 -1.9(18) . . . . ? Re1 O2 C3 C2' -32.0(19) . . . . ? C1 C2 C3 O4 160.2(19) . . . . ? C1 C2 C3 O2 -32(3) . . . . ? C1 C2 C3 C2' 68(5) . . . . ? C1 C2' C3 O4 -165.6(19) . . . . ? C1 C2' C3 O2 31(3) . . . . ? C1 C2' C3 C2 -64(5) . . . . ? O1 C1 O3 Co1 -2.9(13) . . . . ? C2 C1 O3 Co1 -169.6(15) . . . . ? C2' C1 O3 Co1 162.0(15) . . . . ? C1 O3 Co1 N11 -5.0(9) . . . . ? C1 O3 Co1 N21 175.0(7) . . . . ? C1 O3 Co1 N12 69.4(8) . . . . ? C1 O3 Co1 N22 -112.7(8) . . . . ? O3 Co1 N11 C11 -109.5(8) . . . . ? N21 Co1 N11 C11 70.5(8) . . . . ? N12 Co1 N11 C11 172.8(8) . . . . ? N22 Co1 N11 C11 -15.2(8) . . . . ? O3 Co1 N11 C112 68.9(7) . . . . ? N21 Co1 N11 C112 -111.1(5) . . . . ? N12 Co1 N11 C112 -8.8(5) . . . . ? N22 Co1 N11 C112 163.2(5) . . . . ? O3 Co1 N12 C110 48.1(8) . . . . ? N11 Co1 N12 C110 -175.9(8) . . . . ? N21 Co1 N12 C110 -68.4(8) . . . . ? N22 Co1 N12 C110 38.8(16) . . . . ? O3 Co1 N12 C111 -126.5(6) . . . . ? N11 Co1 N12 C111 9.5(6) . . . . ? N21 Co1 N12 C111 117.0(6) . . . . ? N22 Co1 N12 C111 -135.8(10) . . . . ? C112 N11 C11 C12 -1.8(13) . . . . ? Co1 N11 C11 C12 176.5(7) . . . . ? C112 N11 C11 C113 174.8(9) . . . . ? Co1 N11 C11 C113 -6.9(13) . . . . ? N11 C11 C12 C13 0.3(16) . . . . ? C113 C11 C12 C13 -176.3(11) . . . . ? C11 C12 C13 C14 0.1(17) . . . . ? C12 C13 C14 C112 1.0(16) . . . . ? C12 C13 C14 C15 179.1(11) . . . . ? C112 C14 C15 C16 2.1(17) . . . . ? C13 C14 C15 C16 -175.9(11) . . . . ? C14 C15 C16 C17 1.1(18) . . . . ? C15 C16 C17 C18 175.8(11) . . . . ? C15 C16 C17 C111 -2.5(16) . . . . ? C111 C17 C18 C19 0.5(15) . . . . ? C16 C17 C18 C19 -177.9(11) . . . . ? C17 C18 C19 C110 -0.4(17) . . . . ? C111 N12 C110 C19 2.2(13) . . . . ? Co1 N12 C110 C19 -172.2(7) . . . . ? C111 N12 C110 C114 -176.0(9) . . . . ? Co1 N12 C110 C114 9.6(14) . . . . ? C18 C19 C110 N12 -0.9(16) . . . . ? C18 C19 C110 C114 177.2(11) . . . . ? C110 N12 C111 C17 -2.2(13) . . . . ? Co1 N12 C111 C17 173.1(7) . . . . ? C110 N12 C111 C112 176.3(8) . . . . ? Co1 N12 C111 C112 -8.4(9) . . . . ? C18 C17 C111 N12 0.9(14) . . . . ? C16 C17 C111 N12 179.3(9) . . . . ? C18 C17 C111 C112 -177.6(8) . . . . ? C16 C17 C111 C112 0.8(13) . . . . ? C11 N11 C112 C14 3.1(12) . . . . ? Co1 N11 C112 C14 -175.5(7) . . . . ? C11 N11 C112 C111 -174.0(8) . . . . ? Co1 N11 C112 C111 7.4(9) . . . . ? C13 C14 C112 N11 -2.6(13) . . . . ? C15 C14 C112 N11 179.3(9) . . . . ? C13 C14 C112 C111 174.5(9) . . . . ? C15 C14 C112 C111 -3.6(13) . . . . ? N12 C111 C112 N11 0.9(11) . . . . ? C17 C111 C112 N11 179.4(8) . . . . ? N12 C111 C112 C14 -176.4(8) . . . . ? C17 C111 C112 C14 2.2(12) . . . . ? O3 Co1 N21 C21 -116.7(7) . . . . ? N11 Co1 N21 C21 63.3(8) . . . . ? N12 Co1 N21 C21 -21.2(8) . . . . ? N22 Co1 N21 C21 171.5(8) . . . . ? O3 Co1 N21 C212 51.0(6) . . . . ? N11 Co1 N21 C212 -129.0(5) . . . . ? N12 Co1 N21 C212 146.5(5) . . . . ? N22 Co1 N21 C212 -20.8(5) . . . . ? O3 Co1 N22 C210 62.0(7) . . . . ? N11 Co1 N22 C210 -71.7(8) . . . . ? N21 Co1 N22 C210 -178.5(8) . . . . ? N12 Co1 N22 C210 71.5(14) . . . . ? O3 Co1 N22 C211 -98.1(5) . . . . ? N11 Co1 N22 C211 128.2(5) . . . . ? N21 Co1 N22 C211 21.4(5) . . . . ? N12 Co1 N22 C211 -88.6(12) . . . . ? C212 N21 C21 C22 -5.1(13) . . . . ? Co1 N21 C21 C22 161.5(7) . . . . ? C212 N21 C21 C213 172.8(9) . . . . ? Co1 N21 C21 C213 -20.6(13) . . . . ? N21 C21 C22 C23 1.4(16) . . . . ? C213 C21 C22 C23 -176.6(11) . . . . ? C21 C22 C23 C24 2.3(18) . . . . ? C22 C23 C24 C212 -2.0(16) . . . . ? C22 C23 C24 C25 177.4(11) . . . . ? C212 C24 C25 C26 2.8(15) . . . . ? C23 C24 C25 C26 -176.5(11) . . . . ? C24 C25 C26 C27 -1.0(17) . . . . ? C25 C26 C27 C211 -0.8(15) . . . . ? C25 C26 C27 C28 177.5(10) . . . . ? C211 C27 C28 C29 0.4(13) . . . . ? C26 C27 C28 C29 -177.9(10) . . . . ? C27 C28 C29 C210 -2.3(14) . . . . ? C211 N22 C210 C29 -2.0(12) . . . . ? Co1 N22 C210 C29 -160.5(7) . . . . ? C211 N22 C210 C214 177.6(8) . . . . ? Co1 N22 C210 C214 19.1(12) . . . . ? C28 C29 C210 N22 3.3(14) . . . . ? C28 C29 C210 C214 -176.3(9) . . . . ? C210 N22 C211 C27 -0.1(11) . . . . ? Co1 N22 C211 C27 162.8(6) . . . . ? C210 N22 C211 C212 178.6(7) . . . . ? Co1 N22 C211 C212 -18.5(8) . . . . ? C28 C27 C211 N22 0.9(12) . . . . ? C26 C27 C211 N22 179.3(8) . . . . ? C28 C27 C211 C212 -177.8(8) . . . . ? C26 C27 C211 C212 0.6(12) . . . . ? C21 N21 C212 C24 5.4(12) . . . . ? Co1 N21 C212 C24 -163.6(6) . . . . ? C21 N21 C212 C211 -173.0(7) . . . . ? Co1 N21 C212 C211 17.9(8) . . . . ? C23 C24 C212 N21 -1.9(13) . . . . ? C25 C24 C212 N21 178.7(8) . . . . ? C23 C24 C212 C211 176.6(8) . . . . ? C25 C24 C212 C211 -2.8(12) . . . . ? N22 C211 C212 N21 1.0(10) . . . . ? C27 C211 C212 N21 179.7(7) . . . . ? N22 C211 C212 C24 -177.5(7) . . . . ? C27 C211 C212 C24 1.2(11) . . . . ? data_cmp2 _database_code_depnum_ccdc_archive 'CCDC 651348' _audit_creation_date 2004-06-25T19:54:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #-------------------------------------------------------- # CHEMICAL INFORMATION #--------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H26 Cl4 Fe N4 O4 Re, C2 H3 N' _chemical_formula_sum 'C33 H29 Cl4 Fe N5 O4 Re' _chemical_formula_weight 943.46 #------------------------------------------------- # UNIT CELL INFORMATION #--------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4923(14) _cell_length_b 12.6021(12) _cell_length_c 13.5093(13) _cell_angle_alpha 82.143(9) _cell_angle_beta 62.813(7) _cell_angle_gamma 69.561(9) _cell_volume 1772.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 18.77 _cell_measurement_theta_max 19.95 #------------------------------------------------- # CRYSTAL INFORMATION #------------------------------------------------- _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 926 _exptl_special_details ; ? ; #-------------------------------------------- # ABSORPTION CORRECTION #--------------------------------------------------- _exptl_absorpt_coefficient_mu 4.168 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'MSC/AFC Diffractometer Software, 1993' _exptl_absorpt_correction_T_min 0.4222 _exptl_absorpt_correction_T_max 0.8852 #------------------------------------------------- # DATA COLLECTION #--------------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_number 9232 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 8117 _reflns_number_gt 6932 _reflns_threshold_expression >2sigma(I) #------------------------------------------------- # COMPUTER PROGRAMS USED #------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Software, 1993' _computing_cell_refinement 'MSC/AFC Diffractometer Software, 1993' _computing_data_reduction 'MSC/AFC Diffractometer Software, 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------- # REFINEMENT INFORMATION #------------------------------------------------ _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+1.0365P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8117 _refine_ls_number_parameters 431 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.04 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.728 _refine_diff_density_min -1.452 _refine_diff_density_rms 0.093 #------------------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #--------------------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 1.098437(13) 0.771660(12) 0.709243(11) 0.03758(5) Uani 1 1 d . . . Cl1 Cl 1.30505(10) 0.73026(10) 0.68770(10) 0.0559(2) Uani 1 1 d . . . Cl2 Cl 1.12236(12) 0.57909(9) 0.70727(10) 0.0599(3) Uani 1 1 d . . . Cl3 Cl 1.00812(12) 0.78017(12) 0.90459(9) 0.0646(3) Uani 1 1 d . . . Cl4 Cl 1.16069(11) 0.78432(10) 0.51728(8) 0.0553(2) Uani 1 1 d . . . O1 O 0.9147(3) 0.8140(2) 0.7297(2) 0.0449(6) Uani 1 1 d . . . O2 O 1.0717(3) 0.9383(2) 0.7122(2) 0.0472(6) Uani 1 1 d . . . C1 C 0.8246(4) 0.9065(3) 0.7674(3) 0.0449(8) Uani 1 1 d . . . C2 C 0.8405(14) 1.0020(12) 0.8099(10) 0.052(3) Uani 0.5 1 d PU . . H2A H 0.8217 0.9888 0.8876 0.062 Uiso 0.5 1 calc PR . . H2B H 0.7759 1.0713 0.8072 0.062 Uiso 0.5 1 calc PR . . C2' C 0.8466(15) 1.0198(12) 0.7562(14) 0.069(4) Uani 0.5 1 d PU . . H2C H 0.7762 1.0684 0.8182 0.083 Uiso 0.5 1 calc PR . . H2D H 0.8414 1.0537 0.6889 0.083 Uiso 0.5 1 calc PR . . C3 C 0.9690(4) 1.0237(3) 0.7520(3) 0.0446(8) Uani 1 1 d . . . O3 O 0.7129(3) 0.9141(2) 0.7916(2) 0.0494(6) Uani 1 1 d . . . O4 O 0.9689(3) 1.1169(3) 0.7642(3) 0.0688(9) Uani 1 1 d . . . Fe1 Fe 0.65658(4) 0.78759(4) 0.77364(4) 0.03401(11) Uani 1 1 d . . . N11 N 0.7537(3) 0.6199(2) 0.7057(3) 0.0383(6) Uani 1 1 d . . . N12 N 0.7063(3) 0.6997(3) 0.9046(3) 0.0426(7) Uani 1 1 d . . . C11 C 0.7678(4) 0.5783(3) 0.6128(3) 0.0494(9) Uani 1 1 d . . . C12 C 0.8417(5) 0.4669(4) 0.5752(4) 0.0654(12) Uani 1 1 d . . . H12 H 0.8501 0.4404 0.5102 0.078 Uiso 1 1 calc . . . C13 C 0.9013(5) 0.3973(4) 0.6338(5) 0.0670(13) Uani 1 1 d . . . H13 H 0.9503 0.3228 0.609 0.08 Uiso 1 1 calc . . . C14 C 0.8893(4) 0.4372(3) 0.7310(4) 0.0525(10) Uani 1 1 d . . . C15 C 0.9482(5) 0.3675(4) 0.7970(5) 0.0683(14) Uani 1 1 d . . . H15 H 1.0008 0.2935 0.7733 0.082 Uiso 1 1 calc . . . C16 C 0.9284(5) 0.4077(4) 0.8922(5) 0.0715(15) Uani 1 1 d . . . H16 H 0.9693 0.3614 0.9329 0.086 Uiso 1 1 calc . . . C17 C 0.8460(4) 0.5200(4) 0.9338(4) 0.0566(11) Uani 1 1 d . . . C18 C 0.8161(6) 0.5635(5) 1.0369(4) 0.0731(15) Uani 1 1 d . . . H18 H 0.8524 0.5196 1.0818 0.088 Uiso 1 1 calc . . . C19 C 0.7344(5) 0.6691(5) 1.0703(4) 0.0685(14) Uani 1 1 d . . . H19 H 0.7148 0.6975 1.1387 0.082 Uiso 1 1 calc . . . C110 C 0.6776(5) 0.7382(4) 1.0034(3) 0.0559(11) Uani 1 1 d . . . C111 C 0.7878(4) 0.5925(3) 0.8700(3) 0.0423(8) Uani 1 1 d . . . C112 C 0.8127(3) 0.5493(3) 0.7655(3) 0.0396(8) Uani 1 1 d . . . C113 C 0.6958(6) 0.6524(4) 0.5509(4) 0.0712(14) Uani 1 1 d . . . H11A H 0.6498 0.7262 0.5864 0.107 Uiso 1 1 calc R . . H11B H 0.6371 0.6192 0.5513 0.107 Uiso 1 1 calc R . . H11C H 0.7546 0.6591 0.4754 0.107 Uiso 1 1 calc R . . C114 C 0.5833(6) 0.8532(5) 1.0428(4) 0.0808(16) Uani 1 1 d . . . H11D H 0.5546 0.8866 0.9874 0.121 Uiso 1 1 calc R . . H11E H 0.6226 0.8998 1.0557 0.121 Uiso 1 1 calc R . . H11F H 0.5121 0.8474 1.1109 0.121 Uiso 1 1 calc R . . N21 N 0.4574(3) 0.8216(3) 0.8341(2) 0.0408(7) Uani 1 1 d . . . N22 N 0.6127(3) 0.9086(2) 0.6537(2) 0.0366(6) Uani 1 1 d . . . C21 C 0.3810(4) 0.7716(4) 0.9153(3) 0.0521(10) Uani 1 1 d . . . C22 C 0.2485(5) 0.8252(5) 0.9652(4) 0.0710(14) Uani 1 1 d . . . H22 H 0.1965 0.7905 1.0231 0.085 Uiso 1 1 calc . . . C23 C 0.1960(4) 0.9263(6) 0.9303(5) 0.0760(16) Uani 1 1 d . . . H23 H 0.1083 0.9614 0.965 0.091 Uiso 1 1 calc . . . C24 C 0.2717(4) 0.9785(4) 0.8429(4) 0.0548(11) Uani 1 1 d . . . C25 C 0.2231(4) 1.0839(5) 0.7978(5) 0.0672(14) Uani 1 1 d . . . H25 H 0.1361 1.1228 0.8306 0.081 Uiso 1 1 calc . . . C26 C 0.3001(5) 1.1274(4) 0.7097(5) 0.0696(15) Uani 1 1 d . . . H26 H 0.2657 1.1961 0.6827 0.083 Uiso 1 1 calc . . . C27 C 0.4349(4) 1.0699(3) 0.6560(4) 0.0492(9) Uani 1 1 d . . . C28 C 0.5211(5) 1.1082(4) 0.5598(4) 0.0609(12) Uani 1 1 d . . . H28 H 0.4915 1.1756 0.5284 0.073 Uiso 1 1 calc . . . C29 C 0.6460(5) 1.0475(4) 0.5134(4) 0.0562(11) Uani 1 1 d . . . H29 H 0.702 1.0716 0.4485 0.067 Uiso 1 1 calc . . . C210 C 0.6915(4) 0.9474(3) 0.5634(3) 0.0421(8) Uani 1 1 d . . . C211 C 0.4858(3) 0.9680(3) 0.6993(3) 0.0380(7) Uani 1 1 d . . . C212 C 0.4037(3) 0.9218(3) 0.7945(3) 0.0393(8) Uani 1 1 d . . . C213 C 0.4384(5) 0.6574(5) 0.9520(5) 0.0770(15) Uani 1 1 d . . . H21A H 0.5293 0.6337 0.9098 0.115 Uiso 1 1 calc R . . H21B H 0.4063 0.6038 0.9401 0.115 Uiso 1 1 calc R . . H21C H 0.4165 0.6616 1.0297 0.115 Uiso 1 1 calc R . . C214 C 0.8300(4) 0.8840(4) 0.5140(4) 0.0599(12) Uani 1 1 d . . . H21D H 0.8461 0.8187 0.5574 0.09 Uiso 1 1 calc R . . H21E H 0.8752 0.932 0.5138 0.09 Uiso 1 1 calc R . . H21F H 0.8582 0.8604 0.4391 0.09 Uiso 1 1 calc R . . N31 N 0.4197(10) 0.6481(12) 0.2247(8) 0.196(3) Uani 1 1 d . . . C31 C 0.4561(12) 0.6140(15) 0.2901(10) 0.196(3) Uani 1 1 d . . . C32 C 0.4902(10) 0.5862(13) 0.3725(9) 0.196(3) Uani 1 1 d . . . H32A H 0.5594 0.6128 0.3572 0.294 Uiso 1 1 calc R . . H32B H 0.5167 0.5053 0.3787 0.294 Uiso 1 1 calc R . . H32C H 0.4192 0.6204 0.441 0.294 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.04355(9) 0.03576(8) 0.03643(8) 0.00314(5) -0.01845(6) -0.01594(6) Cl1 0.0480(5) 0.0566(6) 0.0658(6) 0.0032(5) -0.0302(5) -0.0135(5) Cl2 0.0767(7) 0.0386(5) 0.0681(7) 0.0066(5) -0.0329(6) -0.0233(5) Cl3 0.0785(8) 0.0816(8) 0.0380(5) 0.0099(5) -0.0247(5) -0.0353(7) Cl4 0.0692(6) 0.0619(6) 0.0373(4) 0.0016(4) -0.0210(4) -0.0276(5) O1 0.0473(14) 0.0403(14) 0.0545(15) -0.0005(12) -0.0252(12) -0.0182(12) O2 0.0450(14) 0.0428(14) 0.0571(16) -0.0025(12) -0.0187(12) -0.0221(12) C1 0.051(2) 0.0394(19) 0.052(2) 0.0010(17) -0.0262(18) -0.0183(17) C2 0.047(5) 0.050(7) 0.067(7) -0.015(6) -0.026(6) -0.017(5) C2' 0.056(6) 0.036(5) 0.132(14) 0.000(8) -0.055(10) -0.016(4) C3 0.048(2) 0.043(2) 0.046(2) -0.0020(16) -0.0188(17) -0.0206(17) O3 0.0452(15) 0.0478(15) 0.0650(17) 0.0040(13) -0.0290(13) -0.0205(13) O4 0.0573(18) 0.0461(17) 0.098(3) -0.0199(17) -0.0192(17) -0.0235(15) Fe1 0.0325(2) 0.0305(2) 0.0387(2) 0.00193(19) -0.0169(2) -0.00841(19) N11 0.0446(16) 0.0320(14) 0.0435(16) 0.0026(12) -0.0246(13) -0.0116(13) N12 0.0498(18) 0.0455(17) 0.0389(15) 0.0064(13) -0.0234(14) -0.0192(15) C11 0.061(2) 0.045(2) 0.047(2) -0.0034(17) -0.0263(19) -0.0171(19) C12 0.078(3) 0.046(2) 0.068(3) -0.016(2) -0.029(3) -0.014(2) C13 0.068(3) 0.039(2) 0.088(4) -0.015(2) -0.031(3) -0.007(2) C14 0.050(2) 0.0292(18) 0.083(3) 0.0052(19) -0.034(2) -0.0123(16) C15 0.067(3) 0.034(2) 0.116(4) 0.018(3) -0.057(3) -0.015(2) C16 0.081(3) 0.050(3) 0.111(4) 0.042(3) -0.069(3) -0.029(2) C17 0.067(3) 0.057(2) 0.073(3) 0.032(2) -0.049(2) -0.036(2) C18 0.088(4) 0.098(4) 0.067(3) 0.038(3) -0.055(3) -0.053(3) C19 0.086(3) 0.099(4) 0.043(2) 0.013(2) -0.036(2) -0.047(3) C110 0.071(3) 0.070(3) 0.039(2) 0.0039(19) -0.025(2) -0.036(2) C111 0.049(2) 0.0417(19) 0.048(2) 0.0162(16) -0.0288(17) -0.0229(17) C112 0.0400(18) 0.0297(16) 0.053(2) 0.0076(15) -0.0238(16) -0.0135(14) C113 0.107(4) 0.060(3) 0.065(3) 0.000(2) -0.058(3) -0.020(3) C114 0.098(4) 0.084(4) 0.051(3) -0.017(3) -0.023(3) -0.025(3) N21 0.0337(14) 0.0502(18) 0.0392(15) 0.0005(13) -0.0128(12) -0.0187(13) N22 0.0351(14) 0.0359(15) 0.0402(15) 0.0015(12) -0.0190(12) -0.0100(12) C21 0.047(2) 0.067(3) 0.046(2) 0.0006(19) -0.0138(17) -0.032(2) C22 0.049(3) 0.099(4) 0.061(3) -0.010(3) -0.005(2) -0.041(3) C23 0.032(2) 0.101(4) 0.081(3) -0.024(3) -0.009(2) -0.018(2) C24 0.0349(19) 0.067(3) 0.062(2) -0.019(2) -0.0221(18) -0.0067(19) C25 0.042(2) 0.069(3) 0.083(3) -0.022(3) -0.035(2) 0.010(2) C26 0.069(3) 0.054(3) 0.091(4) -0.014(3) -0.057(3) 0.010(2) C27 0.055(2) 0.040(2) 0.062(2) -0.0027(18) -0.040(2) -0.0047(17) C28 0.089(3) 0.045(2) 0.071(3) 0.018(2) -0.057(3) -0.023(2) C29 0.075(3) 0.055(2) 0.057(2) 0.022(2) -0.039(2) -0.035(2) C210 0.0446(19) 0.043(2) 0.0431(19) 0.0071(16) -0.0218(16) -0.0179(16) C211 0.0366(17) 0.0379(18) 0.0447(18) -0.0046(15) -0.0239(15) -0.0076(14) C212 0.0327(17) 0.0454(19) 0.0460(19) -0.0091(16) -0.0218(15) -0.0095(15) C213 0.077(3) 0.080(4) 0.076(3) 0.030(3) -0.028(3) -0.047(3) C214 0.041(2) 0.077(3) 0.050(2) 0.012(2) -0.0112(18) -0.021(2) N31 0.142(5) 0.324(10) 0.111(5) -0.001(7) -0.031(4) -0.095(6) C31 0.142(5) 0.324(10) 0.111(5) -0.001(7) -0.031(4) -0.095(6) C32 0.142(5) 0.324(10) 0.111(5) -0.001(7) -0.031(4) -0.095(6) #---------------------------------------- # MOLECULAR GEOMETRY #----------------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O2 2.011(3) . ? Re1 O1 2.058(3) . ? Re1 Cl1 2.3310(11) . ? Re1 Cl2 2.3417(10) . ? Re1 Cl4 2.3422(10) . ? Re1 Cl3 2.3497(11) . ? O1 C1 1.268(5) . ? O2 C3 1.287(5) . ? C1 O3 1.249(5) . ? C1 C2 1.508(14) . ? C1 C2' 1.521(14) . ? C2 C3 1.538(15) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C2' C3 1.522(14) . ? C2' H2C 0.97 . ? C2' H2D 0.97 . ? C3 O4 1.208(5) . ? O3 Fe1 2.035(3) . ? Fe1 N11 2.122(3) . ? Fe1 N21 2.129(3) . ? Fe1 N12 2.175(3) . ? Fe1 N22 2.192(3) . ? N11 C11 1.340(5) . ? N11 C112 1.369(4) . ? N12 C110 1.328(5) . ? N12 C111 1.364(5) . ? C11 C12 1.394(6) . ? C11 C113 1.506(6) . ? C12 C13 1.357(7) . ? C12 H12 0.93 . ? C13 C14 1.395(7) . ? C13 H13 0.93 . ? C14 C112 1.399(5) . ? C14 C15 1.430(6) . ? C15 C16 1.332(8) . ? C15 H15 0.93 . ? C16 C17 1.431(7) . ? C16 H16 0.93 . ? C17 C18 1.403(7) . ? C17 C111 1.415(5) . ? C18 C19 1.346(8) . ? C18 H18 0.93 . ? C19 C110 1.421(7) . ? C19 H19 0.93 . ? C110 C114 1.489(7) . ? C111 C112 1.441(5) . ? C113 H11A 0.96 . ? C113 H11B 0.96 . ? C113 H11C 0.96 . ? C114 H11D 0.96 . ? C114 H11E 0.96 . ? C114 H11F 0.96 . ? N21 C21 1.337(5) . ? N21 C212 1.372(5) . ? N22 C210 1.332(5) . ? N22 C211 1.363(4) . ? C21 C22 1.405(7) . ? C21 C213 1.496(7) . ? C22 C23 1.346(8) . ? C22 H22 0.93 . ? C23 C24 1.386(8) . ? C23 H23 0.93 . ? C24 C212 1.405(5) . ? C24 C25 1.434(7) . ? C25 C26 1.337(8) . ? C25 H25 0.93 . ? C26 C27 1.436(7) . ? C26 H26 0.93 . ? C27 C211 1.401(5) . ? C27 C28 1.411(7) . ? C28 C29 1.348(7) . ? C28 H28 0.93 . ? C29 C210 1.410(6) . ? C29 H29 0.93 . ? C210 C214 1.484(5) . ? C211 C212 1.433(5) . ? C213 H21A 0.96 . ? C213 H21B 0.96 . ? C213 H21C 0.96 . ? C214 H21D 0.96 . ? C214 H21E 0.96 . ? C214 H21F 0.96 . ? N31 C31 1.140(14) . ? C31 C32 1.329(14) . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 87.91(11) . . ? O2 Re1 Cl1 90.12(8) . . ? O1 Re1 Cl1 177.98(7) . . ? O2 Re1 Cl2 178.09(8) . . ? O1 Re1 Cl2 90.19(8) . . ? Cl1 Re1 Cl2 91.78(4) . . ? O2 Re1 Cl4 87.70(9) . . ? O1 Re1 Cl4 87.22(8) . . ? Cl1 Re1 Cl4 93.17(4) . . ? Cl2 Re1 Cl4 92.42(4) . . ? O2 Re1 Cl3 87.54(9) . . ? O1 Re1 Cl3 85.64(8) . . ? Cl1 Re1 Cl3 93.81(4) . . ? Cl2 Re1 Cl3 92.11(5) . . ? Cl4 Re1 Cl3 171.55(4) . . ? C1 O1 Re1 128.0(2) . . ? C3 O2 Re1 131.0(2) . . ? O3 C1 O1 120.7(3) . . ? O3 C1 C2 116.1(6) . . ? O1 C1 C2 121.7(6) . . ? O3 C1 C2' 114.4(6) . . ? O1 C1 C2' 122.8(7) . . ? C1 C2 C3 119.3(9) . . ? C1 C2 H2A 107.5 . . ? C3 C2 H2A 107.5 . . ? C1 C2 H2B 107.5 . . ? C3 C2 H2B 107.5 . . ? H2A C2 H2B 107 . . ? C1 C2' C3 119.5(9) . . ? C1 C2' H2C 107.4 . . ? C3 C2' H2C 107.4 . . ? C1 C2' H2D 107.4 . . ? C3 C2' H2D 107.4 . . ? H2C C2' H2D 107 . . ? O4 C3 O2 122.8(4) . . ? O4 C3 C2' 115.2(6) . . ? O2 C3 C2' 120.1(6) . . ? O4 C3 C2 117.3(6) . . ? O2 C3 C2 118.6(6) . . ? C1 O3 Fe1 125.6(3) . . ? O3 Fe1 N11 134.23(12) . . ? O3 Fe1 N21 117.03(12) . . ? N11 Fe1 N21 108.74(12) . . ? O3 Fe1 N12 87.89(12) . . ? N11 Fe1 N12 78.86(12) . . ? N21 Fe1 N12 106.55(12) . . ? O3 Fe1 N22 79.20(11) . . ? N11 Fe1 N22 112.00(11) . . ? N21 Fe1 N22 77.63(11) . . ? N12 Fe1 N22 166.86(12) . . ? C11 N11 C112 118.3(3) . . ? C11 N11 Fe1 128.7(3) . . ? C112 N11 Fe1 112.9(2) . . ? C110 N12 C111 119.2(4) . . ? C110 N12 Fe1 129.8(3) . . ? C111 N12 Fe1 110.7(2) . . ? N11 C11 C12 121.9(4) . . ? N11 C11 C113 118.8(4) . . ? C12 C11 C113 119.1(4) . . ? C13 C12 C11 119.8(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C112 117.6(4) . . ? C13 C14 C15 122.8(4) . . ? C112 C14 C15 119.6(4) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 122.0(4) . . ? C15 C16 H16 119 . . ? C17 C16 H16 119 . . ? C18 C17 C111 116.7(5) . . ? C18 C17 C16 124.0(4) . . ? C111 C17 C16 119.3(4) . . ? C19 C18 C17 119.6(4) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C110 121.5(4) . . ? C18 C19 H19 119.3 . . ? C110 C19 H19 119.3 . . ? N12 C110 C19 120.1(5) . . ? N12 C110 C114 118.7(4) . . ? C19 C110 C114 121.2(4) . . ? N12 C111 C17 123.0(4) . . ? N12 C111 C112 118.7(3) . . ? C17 C111 C112 118.3(4) . . ? N11 C112 C14 122.2(4) . . ? N11 C112 C111 117.5(3) . . ? C14 C112 C111 120.2(4) . . ? C11 C113 H11A 109.5 . . ? C11 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C11 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C110 C114 H11D 109.5 . . ? C110 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C110 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? C21 N21 C212 118.8(3) . . ? C21 N21 Fe1 129.1(3) . . ? C212 N21 Fe1 111.0(2) . . ? C210 N22 C211 119.1(3) . . ? C210 N22 Fe1 128.8(2) . . ? C211 N22 Fe1 109.7(2) . . ? N21 C21 C22 120.5(5) . . ? N21 C21 C213 119.1(4) . . ? C22 C21 C213 120.4(4) . . ? C23 C22 C21 120.7(5) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 120.5(4) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C212 117.1(5) . . ? C23 C24 C25 124.0(4) . . ? C212 C24 C25 118.9(4) . . ? C26 C25 C24 121.4(4) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C25 C26 C27 121.2(4) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C211 C27 C28 116.8(4) . . ? C211 C27 C26 118.8(4) . . ? C28 C27 C26 124.3(4) . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C210 119.8(4) . . ? C28 C29 H29 120.1 . . ? C210 C29 H29 120.1 . . ? N22 C210 C29 121.3(4) . . ? N22 C210 C214 119.4(3) . . ? C29 C210 C214 119.3(4) . . ? N22 C211 C27 122.5(4) . . ? N22 C211 C212 117.4(3) . . ? C27 C211 C212 120.1(3) . . ? N21 C212 C24 122.2(4) . . ? N21 C212 C211 118.2(3) . . ? C24 C212 C211 119.6(4) . . ? C21 C213 H21A 109.5 . . ? C21 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? C21 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? C210 C214 H21D 109.5 . . ? C210 C214 H21E 109.5 . . ? H21D C214 H21E 109.5 . . ? C210 C214 H21F 109.5 . . ? H21D C214 H21F 109.5 . . ? H21E C214 H21F 109.5 . . ? N31 C31 C32 173.1(19) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Re1 O1 C1 -20.5(3) . . . . ? Cl2 Re1 O1 C1 159.3(3) . . . . ? Cl4 Re1 O1 C1 -108.3(3) . . . . ? Cl3 Re1 O1 C1 67.2(3) . . . . ? O1 Re1 O2 C3 21.6(3) . . . . ? Cl1 Re1 O2 C3 -157.9(3) . . . . ? Cl4 Re1 O2 C3 108.9(3) . . . . ? Cl3 Re1 O2 C3 -64.1(3) . . . . ? Re1 O1 C1 O3 -168.6(3) . . . . ? Re1 O1 C1 C2 -3.1(8) . . . . ? Re1 O1 C1 C2' 28.9(9) . . . . ? O3 C1 C2 C3 -158.0(7) . . . . ? O1 C1 C2 C3 35.9(11) . . . . ? O3 C1 C2' C3 166.8(9) . . . . ? O1 C1 C2' C3 -29.6(15) . . . . ? C2 C1 C2' C3 66.8(19) . . . . ? Re1 O2 C3 O4 167.0(3) . . . . ? Re1 O2 C3 C2' -29.7(9) . . . . ? Re1 O2 C3 C2 0.9(7) . . . . ? C1 C2' C3 O4 -166.6(9) . . . . ? C1 C2' C3 O2 28.9(15) . . . . ? C1 C2' C3 C2 -65.5(19) . . . . ? C1 C2 C3 O4 158.5(7) . . . . ? C1 C2 C3 O2 -34.6(11) . . . . ? C1 C2 C3 C2' 66.3(18) . . . . ? O1 C1 O3 Fe1 -1.2(6) . . . . ? C2 C1 O3 Fe1 -167.5(6) . . . . ? C2' C1 O3 Fe1 162.7(7) . . . . ? C1 O3 Fe1 N11 -4.5(4) . . . . ? C1 O3 Fe1 N21 175.3(3) . . . . ? C1 O3 Fe1 N12 67.7(3) . . . . ? C1 O3 Fe1 N22 -114.7(3) . . . . ? O3 Fe1 N11 C11 -110.4(3) . . . . ? N21 Fe1 N11 C11 69.8(4) . . . . ? N12 Fe1 N11 C11 173.7(4) . . . . ? N22 Fe1 N11 C11 -14.0(4) . . . . ? O3 Fe1 N11 C112 66.5(3) . . . . ? N21 Fe1 N11 C112 -113.2(2) . . . . ? N12 Fe1 N11 C112 -9.3(2) . . . . ? N22 Fe1 N11 C112 162.9(2) . . . . ? O3 Fe1 N12 C110 47.7(4) . . . . ? N11 Fe1 N12 C110 -176.4(4) . . . . ? N21 Fe1 N12 C110 -69.9(4) . . . . ? N22 Fe1 N12 C110 36.9(7) . . . . ? O3 Fe1 N12 C111 -126.4(3) . . . . ? N11 Fe1 N12 C111 9.6(2) . . . . ? N21 Fe1 N12 C111 116.0(3) . . . . ? N22 Fe1 N12 C111 -137.1(5) . . . . ? C112 N11 C11 C12 -1.0(6) . . . . ? Fe1 N11 C11 C12 175.9(3) . . . . ? C112 N11 C11 C113 175.6(4) . . . . ? Fe1 N11 C11 C113 -7.6(6) . . . . ? N11 C11 C12 C13 0.3(8) . . . . ? C113 C11 C12 C13 -176.3(5) . . . . ? C11 C12 C13 C14 -0.3(8) . . . . ? C12 C13 C14 C112 1.1(7) . . . . ? C12 C13 C14 C15 179.1(5) . . . . ? C13 C14 C15 C16 -176.4(5) . . . . ? C112 C14 C15 C16 1.6(7) . . . . ? C14 C15 C16 C17 1.5(8) . . . . ? C15 C16 C17 C18 175.9(5) . . . . ? C15 C16 C17 C111 -2.8(7) . . . . ? C111 C17 C18 C19 0.7(7) . . . . ? C16 C17 C18 C19 -178.0(5) . . . . ? C17 C18 C19 C110 -0.1(8) . . . . ? C111 N12 C110 C19 1.9(6) . . . . ? Fe1 N12 C110 C19 -171.7(3) . . . . ? C111 N12 C110 C114 -176.9(4) . . . . ? Fe1 N12 C110 C114 9.5(6) . . . . ? C18 C19 C110 N12 -1.2(8) . . . . ? C18 C19 C110 C114 177.5(5) . . . . ? C110 N12 C111 C17 -1.3(6) . . . . ? Fe1 N12 C111 C17 173.5(3) . . . . ? C110 N12 C111 C112 176.5(4) . . . . ? Fe1 N12 C111 C112 -8.7(4) . . . . ? C18 C17 C111 N12 0.0(6) . . . . ? C16 C17 C111 N12 178.7(4) . . . . ? C18 C17 C111 C112 -177.8(4) . . . . ? C16 C17 C111 C112 0.9(6) . . . . ? C11 N11 C112 C14 1.7(5) . . . . ? Fe1 N11 C112 C14 -175.6(3) . . . . ? C11 N11 C112 C111 -174.9(3) . . . . ? Fe1 N11 C112 C111 7.8(4) . . . . ? C13 C14 C112 N11 -1.8(6) . . . . ? C15 C14 C112 N11 -179.9(4) . . . . ? C13 C14 C112 C111 174.7(4) . . . . ? C15 C14 C112 C111 -3.4(6) . . . . ? N12 C111 C112 N11 0.9(5) . . . . ? C17 C111 C112 N11 178.8(3) . . . . ? N12 C111 C112 C14 -175.8(4) . . . . ? C17 C111 C112 C14 2.1(5) . . . . ? O3 Fe1 N21 C21 -117.0(3) . . . . ? N11 Fe1 N21 C21 62.8(4) . . . . ? N12 Fe1 N21 C21 -20.8(4) . . . . ? N22 Fe1 N21 C21 172.1(4) . . . . ? O3 Fe1 N21 C212 50.5(3) . . . . ? N11 Fe1 N21 C212 -129.7(2) . . . . ? N12 Fe1 N21 C212 146.7(2) . . . . ? N22 Fe1 N21 C212 -20.4(2) . . . . ? O3 Fe1 N22 C210 61.3(3) . . . . ? N11 Fe1 N22 C210 -72.2(3) . . . . ? N21 Fe1 N22 C210 -177.6(3) . . . . ? N12 Fe1 N22 C210 72.3(6) . . . . ? O3 Fe1 N22 C211 -100.4(2) . . . . ? N11 Fe1 N22 C211 126.1(2) . . . . ? N21 Fe1 N22 C211 20.6(2) . . . . ? N12 Fe1 N22 C211 -89.5(5) . . . . ? C212 N21 C21 C22 -5.2(6) . . . . ? Fe1 N21 C21 C22 161.5(3) . . . . ? C212 N21 C21 C213 174.6(4) . . . . ? Fe1 N21 C21 C213 -18.7(6) . . . . ? N21 C21 C22 C23 1.8(8) . . . . ? C213 C21 C22 C23 -178.0(5) . . . . ? C21 C22 C23 C24 1.1(8) . . . . ? C22 C23 C24 C212 -0.5(8) . . . . ? C22 C23 C24 C25 177.5(5) . . . . ? C23 C24 C25 C26 -176.4(5) . . . . ? C212 C24 C25 C26 1.5(7) . . . . ? C24 C25 C26 C27 0.4(8) . . . . ? C25 C26 C27 C211 -1.7(7) . . . . ? C25 C26 C27 C28 177.1(5) . . . . ? C211 C27 C28 C29 0.3(6) . . . . ? C26 C27 C28 C29 -178.5(4) . . . . ? C27 C28 C29 C210 -2.3(7) . . . . ? C211 N22 C210 C29 -1.0(6) . . . . ? Fe1 N22 C210 C29 -161.3(3) . . . . ? C211 N22 C210 C214 179.2(4) . . . . ? Fe1 N22 C210 C214 18.9(5) . . . . ? C28 C29 C210 N22 2.8(7) . . . . ? C28 C29 C210 C214 -177.5(4) . . . . ? C210 N22 C211 C27 -1.1(5) . . . . ? Fe1 N22 C211 C27 162.7(3) . . . . ? C210 N22 C211 C212 178.2(3) . . . . ? Fe1 N22 C211 C212 -18.0(4) . . . . ? C28 C27 C211 N22 1.4(6) . . . . ? C26 C27 C211 N22 -179.6(4) . . . . ? C28 C27 C211 C212 -177.9(4) . . . . ? C26 C27 C211 C212 1.1(6) . . . . ? C21 N21 C212 C24 5.8(5) . . . . ? Fe1 N21 C212 C24 -163.1(3) . . . . ? C21 N21 C212 C211 -173.1(3) . . . . ? Fe1 N21 C212 C211 18.0(4) . . . . ? C23 C24 C212 N21 -3.0(6) . . . . ? C25 C24 C212 N21 178.9(4) . . . . ? C23 C24 C212 C211 175.9(4) . . . . ? C25 C24 C212 C211 -2.1(6) . . . . ? N22 C211 C212 N21 0.5(5) . . . . ? C27 C211 C212 N21 179.8(3) . . . . ? N22 C211 C212 C24 -178.5(3) . . . . ? C27 C211 C212 C24 0.9(5) . . . . ? data_cmp4 _database_code_depnum_ccdc_archive 'CCDC 651349' _audit_creation_date 2004-06-28T15:47:20-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #-------------------------------------------------------- # CHEMICAL INFORMATION #------------------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_sum 'C22 H24.50 Cl4 N4.50 Ni O5.50 Re' _chemical_formula_moiety 'C21 H22 Cl4 N4 Ni O5 Re, (C2 H3 N)0.5, (H2 O)0.5' _chemical_formula_weight 826.67 #---------------------------------------------- # UNIT CELL INFORMATION #------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0455(3) _cell_length_b 13.365(7) _cell_length_c 14.493(8) _cell_angle_alpha 73.86(4) _cell_angle_beta 85.12(4) _cell_angle_gamma 77.55(4) _cell_volume 1461.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.16 _cell_measurement_theta_max 13.47 #------------------------------------------------------ # CRYSTAL INFORMATION #-------------------------------------------------- _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.874 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_special_details ; ? ; #----------------------------------------------------- # ABSORPTION CORRECTION #--------------------------------------------------- _exptl_absorpt_coefficient_mu 5.19 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'MSC/AFC Diffractometer Software, 1993' _exptl_absorpt_correction_T_min 0.2306 _exptl_absorpt_correction_T_max 0.7814 #---------------------------------------------- # DATA COLLECTION #----------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 15 _diffrn_reflns_number 6902 _diffrn_reflns_av_R_equivalents 0.1703 _diffrn_reflns_av_unetI/netI 0.2605 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 3 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.59 _diffrn_reflns_theta_full 26.59 _diffrn_measured_fraction_theta_full 0.947 _diffrn_measured_fraction_theta_max 0.947 _reflns_number_total 5787 _reflns_number_gt 2440 _reflns_threshold_expression >2sigma(I) #-------------------------------------------- # COMPUTER PROGRAMS USED #----------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Software, 1993' _computing_cell_refinement 'MSC/AFC Diffractometer Software, 1993' _computing_data_reduction 'MSC/AFC Diffractometer Software, 1993' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #---------------------------------------------- # REFINEMENT INFORMATION #------------------------------------------- _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1702P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5787 _refine_ls_number_parameters 340 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.2427 _refine_ls_R_factor_gt 0.097 _refine_ls_wR_factor_ref 0.3007 _refine_ls_wR_factor_gt 0.2291 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.936 _refine_diff_density_min -3.347 _refine_diff_density_rms 0.308 #----------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #-------------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.42306(11) 0.83368(7) 0.80229(6) 0.0594(4) Uani 1 1 d . . . Cl4 Cl 0.6150(9) 0.9441(6) 0.7240(5) 0.0909(19) Uani 1 1 d . . . Cl3 Cl 0.2279(11) 0.7257(6) 0.8659(5) 0.108(2) Uani 1 1 d . . . Cl2 Cl 0.3955(9) 0.9014(6) 0.9365(5) 0.093(2) Uani 1 1 d . . . Cl1 Cl 0.6544(10) 0.6982(6) 0.8624(5) 0.100(2) Uani 1 1 d . . . O1 O 0.232(2) 0.9531(12) 0.7441(11) 0.074(4) Uani 1 1 d . . . O3 O 0.0237(18) 1.0450(11) 0.6423(11) 0.069(4) Uani 1 1 d . . . C1 C 0.128(3) 0.9616(19) 0.6740(16) 0.068(6) Uani 1 1 d . . . C2 C 0.137(3) 0.8699(18) 0.6346(18) 0.077(7) Uani 1 1 d . . . H2A H 0.0835 0.8959 0.5725 0.093 Uiso 1 1 calc R . . H2B H 0.0689 0.8229 0.6765 0.093 Uiso 1 1 calc R . . C3 C 0.318(3) 0.8022(15) 0.6213(17) 0.065(6) Uani 1 1 d . . . O2 O 0.4309(16) 0.7848(10) 0.6828(10) 0.060(3) Uani 1 1 d . . . O4 O 0.345(2) 0.7647(12) 0.5510(10) 0.076(4) Uani 1 1 d . . . Ni1 Ni -0.0419(3) 1.1821(2) 0.68268(18) 0.0551(7) Uani 1 1 d . . . N11 N -0.159(2) 1.3320(13) 0.6937(12) 0.064(5) Uani 1 1 d . . . N12 N 0.014(2) 1.2741(14) 0.5458(12) 0.064(5) Uani 1 1 d . . . C11 C -0.234(3) 1.367(2) 0.7727(17) 0.077(7) Uani 1 1 d . . . C12 C -0.353(4) 1.468(2) 0.759(3) 0.100(9) Uani 1 1 d . . . H12 H -0.4052 1.4896 0.8118 0.12 Uiso 1 1 calc R . . C13 C -0.386(3) 1.527(2) 0.674(3) 0.092(9) Uani 1 1 d . . . H13 H -0.4606 1.592 0.6693 0.111 Uiso 1 1 calc R . . C14 C -0.322(3) 1.5056(17) 0.5894(18) 0.069(7) Uani 1 1 d . . . C15 C -0.334(4) 1.560(2) 0.496(3) 0.100(9) Uani 1 1 d . . . H15 H -0.4093 1.6256 0.4818 0.12 Uiso 1 1 calc R . . C16 C -0.248(4) 1.530(2) 0.420(2) 0.103(10) Uani 1 1 d . . . H16 H -0.2713 1.5732 0.3584 0.123 Uiso 1 1 calc R . . C17 C -0.121(4) 1.431(2) 0.4326(18) 0.078(7) Uani 1 1 d . . . C18 C -0.015(4) 1.397(3) 0.361(2) 0.095(9) Uani 1 1 d . . . H18 H -0.0267 1.438 0.2972 0.115 Uiso 1 1 calc R . . C19 C 0.103(4) 1.308(2) 0.3815(19) 0.091(8) Uani 1 1 d . . . H19 H 0.1728 1.2875 0.3329 0.109 Uiso 1 1 calc R . . C110 C 0.121(3) 1.247(2) 0.475(2) 0.079(7) Uani 1 1 d . . . C111 C -0.101(3) 1.3653(18) 0.5241(17) 0.070(6) Uani 1 1 d . . . C112 C -0.191(2) 1.3980(17) 0.6025(17) 0.062(6) Uani 1 1 d . . . C113 C -0.186(3) 1.301(2) 0.8681(18) 0.088(7) Uani 1 1 d . . . H11A H -0.1088 1.2371 0.8633 0.105 Uiso 1 1 calc R . . H11B H -0.2862 1.2834 0.9046 0.105 Uiso 1 1 calc R . . H11C H -0.1322 1.3394 0.8996 0.105 Uiso 1 1 calc R . . C114 C 0.256(3) 1.154(2) 0.499(2) 0.103(10) Uani 1 1 d . . . H11D H 0.2511 1.121 0.5669 0.124 Uiso 1 1 calc R . . H11E H 0.3641 1.1749 0.482 0.124 Uiso 1 1 calc R . . H11F H 0.2427 1.1051 0.4644 0.124 Uiso 1 1 calc R . . O1W O -0.2806(18) 1.1758(11) 0.6363(9) 0.064(4) Uani 1 1 d . . . N21 N -0.108(2) 1.0835(14) 0.8132(12) 0.062(4) Uani 1 1 d D . . C21 C -0.122(2) 1.0100(17) 0.8708(14) 0.056(5) Uani 1 1 d D . . C22 C -0.133(4) 0.9066(17) 0.9461(16) 0.098(9) Uani 1 1 d D . . H22A H -0.0771 0.9039 1.0031 0.146 Uiso 1 1 calc R . . H22B H -0.0777 0.8477 0.9215 0.146 Uiso 1 1 calc R . . H22C H -0.25 0.9029 0.9613 0.146 Uiso 1 1 calc R . . N31 N 0.174(3) 1.1860(15) 0.7385(15) 0.081(6) Uani 1 1 d D . . C31 C 0.296(4) 1.189(2) 0.772(2) 0.109(11) Uani 1 1 d D . . C32 C 0.434(3) 1.201(3) 0.832(2) 0.128(12) Uani 1 1 d DU . . H32A H 0.4668 1.136 0.8812 0.192 Uiso 1 1 calc R . . H32B H 0.3914 1.2582 0.8602 0.192 Uiso 1 1 calc R . . H32C H 0.5314 1.2152 0.7909 0.192 Uiso 1 1 calc R . . N41 N 0.804(8) 0.574(5) 0.133(4) 0.15(2) Uiso 0.5 1 d PD . . C41 C 0.891(9) 0.540(6) 0.080(4) 0.14(3) Uiso 0.5 1 d PD . . C42 C 1 0.5 0 0.20(3) Uiso 1 2 d SD . . H42A H 0.9511 0.4479 -0.0163 0.298 Uiso 0.5 1 calc PR . . H42B H 1.1135 0.4686 0.022 0.298 Uiso 0.5 1 calc PR . . H42C H 1.0034 0.5588 -0.0556 0.298 Uiso 0.5 1 calc PR . . O2W O 0.5 0.5 1 0.53(8) Uiso 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0504(5) 0.0707(7) 0.0558(6) -0.0232(4) -0.0075(4) 0.0014(4) Cl4 0.094(5) 0.103(5) 0.090(4) -0.031(4) 0.001(4) -0.044(4) Cl3 0.117(6) 0.118(6) 0.095(5) -0.022(4) 0.018(4) -0.051(5) Cl2 0.095(5) 0.120(5) 0.078(4) -0.053(4) -0.006(3) -0.011(4) Cl1 0.101(5) 0.094(5) 0.094(5) -0.026(4) -0.045(4) 0.025(4) O1 0.069(10) 0.069(9) 0.092(11) -0.050(8) 0.003(8) 0.000(7) O3 0.059(9) 0.057(9) 0.086(10) -0.031(7) -0.017(8) 0.018(7) C1 0.062(14) 0.094(18) 0.069(14) -0.054(13) -0.003(11) -0.016(13) C2 0.051(13) 0.081(15) 0.097(17) -0.028(13) -0.036(12) 0.011(11) C3 0.058(13) 0.044(12) 0.081(16) -0.015(11) 0.001(12) 0.008(10) O2 0.040(7) 0.063(9) 0.068(9) -0.017(7) -0.011(7) 0.011(6) O4 0.072(10) 0.088(11) 0.065(9) -0.030(8) -0.015(8) 0.008(8) Ni1 0.0447(14) 0.0617(16) 0.0596(15) -0.0223(12) -0.0076(11) -0.0021(11) N11 0.048(10) 0.066(11) 0.067(11) -0.001(9) -0.028(9) -0.002(8) N12 0.052(10) 0.078(12) 0.070(11) -0.035(9) 0.018(9) -0.019(9) C11 0.081(17) 0.103(19) 0.067(15) -0.045(14) -0.003(12) -0.029(14) C12 0.11(2) 0.079(19) 0.12(3) -0.053(18) 0.02(2) -0.014(17) C13 0.041(13) 0.085(19) 0.15(3) -0.05(2) -0.004(16) 0.019(12) C14 0.058(14) 0.053(13) 0.083(17) 0.017(13) -0.037(12) -0.018(11) C15 0.08(2) 0.078(19) 0.13(3) 0.011(19) -0.033(19) -0.022(15) C16 0.11(3) 0.10(2) 0.08(2) 0.023(17) -0.050(19) -0.05(2) C17 0.091(19) 0.079(17) 0.072(16) -0.011(14) -0.011(14) -0.039(15) C18 0.10(2) 0.12(2) 0.067(17) 0.011(17) -0.024(16) -0.050(19) C19 0.13(3) 0.10(2) 0.061(16) -0.020(15) 0.010(16) -0.06(2) C110 0.035(12) 0.089(17) 0.12(2) -0.040(16) 0.009(13) -0.027(12) C111 0.069(15) 0.065(14) 0.075(16) -0.026(12) -0.003(12) -0.003(12) C112 0.022(9) 0.072(14) 0.097(17) -0.028(12) -0.016(10) -0.004(9) C113 0.078(18) 0.102(19) 0.094(19) -0.046(16) 0.006(14) -0.018(14) C114 0.077(19) 0.14(2) 0.12(2) -0.07(2) 0.057(17) -0.056(19) O1W 0.058(9) 0.074(9) 0.052(8) -0.017(7) -0.009(6) 0.009(7) N21 0.047(10) 0.074(12) 0.055(11) -0.017(9) -0.003(8) 0.007(9) C21 0.038(10) 0.076(15) 0.048(12) -0.024(11) -0.011(9) 0.014(10) C22 0.12(2) 0.079(17) 0.059(14) 0.013(12) 0.031(14) 0.002(15) N31 0.071(14) 0.076(13) 0.084(14) -0.024(11) 0.014(11) 0.012(11) C31 0.09(2) 0.085(19) 0.11(2) 0.018(16) -0.030(18) 0.031(17) C32 0.069(17) 0.21(3) 0.12(2) -0.04(2) -0.036(16) -0.062(19) #--------------------------------------- # MOLECULAR GEOMETRY #--------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O2 2.005(14) . ? Re1 O1 2.009(15) . ? Re1 Cl3 2.321(7) . ? Re1 Cl1 2.334(6) . ? Re1 Cl2 2.339(6) . ? Re1 Cl4 2.367(7) . ? O1 C1 1.34(3) . ? O3 C1 1.24(3) . ? O3 Ni1 2.027(13) . ? C1 C2 1.48(3) . ? C2 C3 1.57(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O4 1.24(2) . ? C3 O2 1.27(3) . ? Ni1 N31 2.00(2) . ? Ni1 N11 2.065(17) . ? Ni1 N21 2.086(18) . ? Ni1 N12 2.093(17) . ? Ni1 O1W 2.114(15) . ? N11 C112 1.38(3) . ? N11 C11 1.40(3) . ? N12 C111 1.34(3) . ? N12 C110 1.35(3) . ? C11 C113 1.45(3) . ? C11 C12 1.45(4) . ? C12 C13 1.28(4) . ? C12 H12 0.9300 . ? C13 C14 1.37(4) . ? C13 H13 0.9300 . ? C14 C15 1.35(4) . ? C14 C112 1.56(3) . ? C15 C16 1.36(4) . ? C15 H15 0.9300 . ? C16 C17 1.46(4) . ? C16 H16 0.9300 . ? C17 C111 1.37(3) . ? C17 C18 1.40(4) . ? C18 C19 1.33(4) . ? C18 H18 0.9300 . ? C19 C110 1.38(3) . ? C19 H19 0.9300 . ? C110 C114 1.44(4) . ? C111 C112 1.41(3) . ? C113 H11A 0.9600 . ? C113 H11B 0.9600 . ? C113 H11C 0.9600 . ? C114 H11D 0.9600 . ? C114 H11E 0.9600 . ? C114 H11F 0.9600 . ? N21 C21 1.12(2) . ? C21 C22 1.52(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N31 C31 1.15(2) . ? C31 C32 1.52(3) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N41 C41 1.13(3) . ? C41 C42 1.54(3) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 87.6(5) . . ? O2 Re1 Cl3 87.4(5) . . ? O1 Re1 Cl3 89.9(5) . . ? O2 Re1 Cl1 90.6(4) . . ? O1 Re1 Cl1 176.8(5) . . ? Cl3 Re1 Cl1 92.7(3) . . ? O2 Re1 Cl2 175.4(4) . . ? O1 Re1 Cl2 87.8(4) . . ? Cl3 Re1 Cl2 92.4(3) . . ? Cl1 Re1 Cl2 93.9(3) . . ? O2 Re1 Cl4 88.0(4) . . ? O1 Re1 Cl4 87.9(5) . . ? Cl3 Re1 Cl4 175.0(2) . . ? Cl1 Re1 Cl4 89.3(3) . . ? Cl2 Re1 Cl4 92.0(3) . . ? C1 O1 Re1 129.7(13) . . ? C1 O3 Ni1 132.1(13) . . ? O3 C1 O1 120.9(18) . . ? O3 C1 C2 119.6(19) . . ? O1 C1 C2 119(2) . . ? C1 C2 C3 117.2(19) . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C3 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? O4 C3 O2 121.5(18) . . ? O4 C3 C2 118(2) . . ? O2 C3 C2 120.1(19) . . ? C3 O2 Re1 130.3(13) . . ? N31 Ni1 O3 101.5(7) . . ? N31 Ni1 N11 93.5(7) . . ? O3 Ni1 N11 163.6(6) . . ? N31 Ni1 N21 89.9(8) . . ? O3 Ni1 N21 83.9(7) . . ? N11 Ni1 N21 102.9(7) . . ? N31 Ni1 N12 94.2(8) . . ? O3 Ni1 N12 92.6(6) . . ? N11 Ni1 N12 79.6(7) . . ? N21 Ni1 N12 175.1(7) . . ? N31 Ni1 O1W 174.8(7) . . ? O3 Ni1 O1W 80.5(6) . . ? N11 Ni1 O1W 85.1(6) . . ? N21 Ni1 O1W 85.5(6) . . ? N12 Ni1 O1W 90.5(6) . . ? C112 N11 C11 119.1(19) . . ? C112 N11 Ni1 108.7(14) . . ? C11 N11 Ni1 130.8(16) . . ? C111 N12 C110 119(2) . . ? C111 N12 Ni1 109.5(14) . . ? C110 N12 Ni1 130.1(17) . . ? N11 C11 C113 118(2) . . ? N11 C11 C12 120(2) . . ? C113 C11 C12 121(2) . . ? C13 C12 C11 120(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 127(2) . . ? C12 C13 H13 116.6 . . ? C14 C13 H13 116.6 . . ? C15 C14 C13 135(3) . . ? C15 C14 C112 111(3) . . ? C13 C14 C112 114(2) . . ? C14 C15 C16 127(3) . . ? C14 C15 H15 116.5 . . ? C16 C15 H15 116.5 . . ? C15 C16 C17 122(3) . . ? C15 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C111 C17 C18 117(3) . . ? C111 C17 C16 117(3) . . ? C18 C17 C16 127(3) . . ? C19 C18 C17 121(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C18 C19 C110 120(3) . . ? C18 C19 H19 120.0 . . ? C110 C19 H19 120.0 . . ? N12 C110 C19 120(2) . . ? N12 C110 C114 120(3) . . ? C19 C110 C114 120(3) . . ? N12 C111 C17 123(2) . . ? N12 C111 C112 116(2) . . ? C17 C111 C112 120(2) . . ? N11 C112 C111 118.0(18) . . ? N11 C112 C14 119(2) . . ? C111 C112 C14 123(2) . . ? C11 C113 H11A 109.5 . . ? C11 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C11 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C110 C114 H11D 109.5 . . ? C110 C114 H11E 109.5 . . ? H11D C114 H11E 109.5 . . ? C110 C114 H11F 109.5 . . ? H11D C114 H11F 109.5 . . ? H11E C114 H11F 109.5 . . ? C21 N21 Ni1 160.6(16) . . ? N21 C21 C22 177(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 N31 Ni1 179(2) . . ? N31 C31 C32 169(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N41 C41 C42 175(9) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Re1 O1 C1 20.5(19) . . . . ? Cl3 Re1 O1 C1 -66.8(19) . . . . ? Cl2 Re1 O1 C1 -159.3(19) . . . . ? Cl4 Re1 O1 C1 108.7(19) . . . . ? Ni1 O3 C1 O1 -5(3) . . . . ? Ni1 O3 C1 C2 174.3(16) . . . . ? Re1 O1 C1 O3 -175.1(15) . . . . ? Re1 O1 C1 C2 6(3) . . . . ? O3 C1 C2 C3 142(2) . . . . ? O1 C1 C2 C3 -39(3) . . . . ? C1 C2 C3 O4 -144(2) . . . . ? C1 C2 C3 O2 38(3) . . . . ? O4 C3 O2 Re1 -179.8(15) . . . . ? C2 C3 O2 Re1 -1(3) . . . . ? O1 Re1 O2 C3 -22.4(18) . . . . ? Cl3 Re1 O2 C3 67.6(18) . . . . ? Cl1 Re1 O2 C3 160.3(18) . . . . ? Cl4 Re1 O2 C3 -110.4(18) . . . . ? C1 O3 Ni1 N31 29(2) . . . . ? C1 O3 Ni1 N11 -176(2) . . . . ? C1 O3 Ni1 N21 -60(2) . . . . ? C1 O3 Ni1 N12 123(2) . . . . ? C1 O3 Ni1 O1W -146(2) . . . . ? N31 Ni1 N11 C112 115.5(13) . . . . ? O3 Ni1 N11 C112 -41(3) . . . . ? N21 Ni1 N11 C112 -153.8(12) . . . . ? N12 Ni1 N11 C112 21.9(12) . . . . ? O1W Ni1 N11 C112 -69.6(12) . . . . ? N31 Ni1 N11 C11 -78.3(19) . . . . ? O3 Ni1 N11 C11 125(3) . . . . ? N21 Ni1 N11 C11 12.4(19) . . . . ? N12 Ni1 N11 C11 -172(2) . . . . ? O1W Ni1 N11 C11 96.6(19) . . . . ? N31 Ni1 N12 C111 -116.9(15) . . . . ? O3 Ni1 N12 C111 141.4(15) . . . . ? N11 Ni1 N12 C111 -24.0(14) . . . . ? O1W Ni1 N12 C111 60.9(15) . . . . ? N31 Ni1 N12 C110 76.9(19) . . . . ? O3 Ni1 N12 C110 -24.8(19) . . . . ? N11 Ni1 N12 C110 170(2) . . . . ? O1W Ni1 N12 C110 -105.3(19) . . . . ? C112 N11 C11 C113 -174(2) . . . . ? Ni1 N11 C11 C113 21(3) . . . . ? C112 N11 C11 C12 4(3) . . . . ? Ni1 N11 C11 C12 -161.1(19) . . . . ? N11 C11 C12 C13 -2(4) . . . . ? C113 C11 C12 C13 176(3) . . . . ? C11 C12 C13 C14 1(5) . . . . ? C12 C13 C14 C15 -175(3) . . . . ? C12 C13 C14 C112 -3(4) . . . . ? C13 C14 C15 C16 173(3) . . . . ? C112 C14 C15 C16 0(4) . . . . ? C14 C15 C16 C17 -3(5) . . . . ? C15 C16 C17 C111 5(4) . . . . ? C15 C16 C17 C18 -174(3) . . . . ? C111 C17 C18 C19 -3(4) . . . . ? C16 C17 C18 C19 176(3) . . . . ? C17 C18 C19 C110 0(4) . . . . ? C111 N12 C110 C19 -5(3) . . . . ? Ni1 N12 C110 C19 160.2(17) . . . . ? C111 N12 C110 C114 174(2) . . . . ? Ni1 N12 C110 C114 -20(3) . . . . ? C18 C19 C110 N12 3(4) . . . . ? C18 C19 C110 C114 -176(2) . . . . ? C110 N12 C111 C17 3(3) . . . . ? Ni1 N12 C111 C17 -165.4(19) . . . . ? C110 N12 C111 C112 -170.2(19) . . . . ? Ni1 N12 C111 C112 22(2) . . . . ? C18 C17 C111 N12 1(4) . . . . ? C16 C17 C111 N12 -178(2) . . . . ? C18 C17 C111 C112 174(2) . . . . ? C16 C17 C111 C112 -5(3) . . . . ? C11 N11 C112 C111 174.4(19) . . . . ? Ni1 N11 C112 C111 -18(2) . . . . ? C11 N11 C112 C14 -5(3) . . . . ? Ni1 N11 C112 C14 162.9(14) . . . . ? N12 C111 C112 N11 -3(3) . . . . ? C17 C111 C112 N11 -176.1(19) . . . . ? N12 C111 C112 C14 176.5(18) . . . . ? C17 C111 C112 C14 3(3) . . . . ? C15 C14 C112 N11 178.9(19) . . . . ? C13 C14 C112 N11 5(3) . . . . ? C15 C14 C112 C111 -1(3) . . . . ? C13 C14 C112 C111 -175(2) . . . . ? N31 Ni1 N21 C21 -92(5) . . . . ? data_cmp5 _database_code_depnum_ccdc_archive 'CCDC 651350' _audit_creation_date 2004-06-30T15:14:31-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------- # CHEMICAL INFORMATION #-------------------------------------------- _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C17 H18 Cl4 Mn1 N2 O6 Re1, C14 H12 N2, C2 H3 N, H2 O' _chemical_formula_sum 'C33 H35 Cl4 Mn1 N5 O7 Re1' _chemical_formula_weight 996.6 _chemical_compound_source 'synthesis as described' #---------------------------------- # UNIT CELL INFORMATION #----------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.389(2) _cell_length_b 26.676(10) _cell_length_c 20.655(7) _cell_angle_alpha 90 _cell_angle_beta 97.74(3) _cell_angle_gamma 90 _cell_volume 4034(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.05 _cell_measurement_theta_max 13.15 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------- # CRYSTAL INFORMATION #----------------------------------------------------- _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_special_details ; ? ; #---------------------------------------------- # ABSORPTION CORRECTION #--------------------------------------------- _exptl_absorpt_coefficient_mu 3.625 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; MSC/AFC Diffractometer Software, 1997 ; _exptl_absorpt_correction_T_min 0.3180 _exptl_absorpt_correction_T_max 0.8686 #------------------------------------------------- # DATA COLLECTION #---------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_unetI/netI 0.0869 _diffrn_measurement_device_type 'Rigaku AFC-7S' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 40 _diffrn_reflns_number 9281 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7091 _reflns_number_gt 5021 _reflns_threshold_expression >2sigma(I) #--------------------------------------- # COMPUTER PROGRAMS USED #------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Software, 1997' _computing_cell_refinement 'MSC/AFC Diffractometer Software, 1997' _computing_data_reduction 'MSC/AFC Diffractometer Software, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #-------------------------------------------------- # REFINEMENT INFORMATION #------------------------------------------------ _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.20P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7091 _refine_ls_number_parameters 451 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.1091 _refine_ls_wR_factor_ref 0.2766 _refine_ls_wR_factor_gt 0.2523 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 4.371 _refine_diff_density_min -9.804 _refine_diff_density_rms 0.394 #-------------------------------------------- # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #--------------------------------------- loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.231 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.17804(6) 0.865653(17) 0.22621(3) 0.0335(3) Uani 1 1 d . . . Mn1 Mn 0.7112(2) 0.71857(7) 0.24457(10) 0.0309(5) Uani 1 1 d . . . Cl3 Cl 0.1913(6) 0.88661(17) 0.1171(2) 0.0605(11) Uani 1 1 d . . . Cl4 Cl 0.1623(6) 0.83868(17) 0.3340(2) 0.0613(10) Uani 1 1 d . . . Cl1 Cl 0.4271(5) 0.91611(15) 0.2609(2) 0.0615(11) Uani 1 1 d . . . Cl2 Cl -0.0434(6) 0.92571(15) 0.2353(3) 0.0643(12) Uani 1 1 d . . . O4 O 0.4494(12) 0.7336(3) 0.1870(5) 0.042(2) Uani 1 1 d . . . O1W O 0.9997(12) 0.7161(3) 0.2947(5) 0.040(2) Uani 1 1 d . . . O3 O -0.1393(12) 0.7422(4) 0.1632(5) 0.042(2) Uani 1 1 d . . . O1 O -0.0201(12) 0.8147(3) 0.1975(5) 0.039(2) Uani 1 1 d . . . O2 O 0.3542(12) 0.8072(3) 0.2192(5) 0.043(2) Uani 1 1 d . . . O2W O 0.7142(12) 0.7966(3) 0.2812(5) 0.043(2) Uani 1 1 d . . . N12 N 0.7029(14) 0.6356(4) 0.2161(6) 0.036(3) Uani 1 1 d . . . N11 N 0.6360(14) 0.6760(4) 0.3344(6) 0.038(3) Uani 1 1 d . . . C15 C 0.806(2) 0.5493(6) 0.3860(10) 0.057(5) Uani 1 1 d . . . H15 H 0.8387 0.5312 0.4242 0.068 Uiso 1 1 calc R . . C110 C 0.7115(19) 0.6140(5) 0.1592(7) 0.041(3) Uani 1 1 d . . . C111 C 0.7367(17) 0.6065(5) 0.2723(6) 0.033(3) Uani 1 1 d U . . C12 C 0.617(2) 0.6680(7) 0.4466(8) 0.055(4) Uani 1 1 d . . . H12 H 0.5844 0.682 0.4846 0.066 Uiso 1 1 calc R . . C14 C 0.7364(18) 0.5987(6) 0.3904(8) 0.048(4) Uani 1 1 d . . . C11 C 0.5891(19) 0.6940(6) 0.3887(8) 0.048(4) Uani 1 1 d . . . C13 C 0.693(2) 0.6222(7) 0.4480(8) 0.057(5) Uani 1 1 d . . . H13 H 0.7178 0.6054 0.4877 0.068 Uiso 1 1 calc R . . C112 C 0.7044(17) 0.6286(5) 0.3335(7) 0.038(3) Uani 1 1 d . . . C17 C 0.7871(17) 0.5558(5) 0.2689(8) 0.047(4) Uani 1 1 d . . . C19 C 0.755(2) 0.5635(6) 0.1542(9) 0.055(4) Uani 1 1 d . . . H19 H 0.7542 0.5489 0.1133 0.067 Uiso 1 1 calc R . . C1 C -0.0137(16) 0.7731(5) 0.1688(6) 0.034(3) Uani 1 1 d . . . C16 C 0.826(2) 0.5278(6) 0.3282(9) 0.054(4) Uani 1 1 d . . . H16 H 0.8657 0.4947 0.3269 0.064 Uiso 1 1 calc R . . C114 C 0.671(3) 0.6463(6) 0.0976(8) 0.057(4) Uani 1 1 d . . . H11A H 0.6429 0.6799 0.1096 0.086 Uiso 1 1 calc R . . H11B H 0.5683 0.6325 0.0697 0.086 Uiso 1 1 calc R . . H11C H 0.7757 0.6466 0.0747 0.086 Uiso 1 1 calc R . . C113 C 0.497(2) 0.7450(7) 0.3861(9) 0.064(5) Uani 1 1 d . . . H11D H 0.4869 0.7579 0.3424 0.097 Uiso 1 1 calc R . . H11E H 0.5691 0.7676 0.4153 0.097 Uiso 1 1 calc R . . H11F H 0.3778 0.7418 0.399 0.097 Uiso 1 1 calc R . . C3 C 0.3302(16) 0.7676(4) 0.1845(6) 0.029(3) Uani 1 1 d U . . C18 C 0.799(2) 0.5353(7) 0.2102(10) 0.061(5) Uani 1 1 d . . . H18 H 0.8378 0.5023 0.2073 0.073 Uiso 1 1 calc R . . C2 C 0.1557(17) 0.7600(6) 0.1376(7) 0.041(3) Uani 1 1 d . . . H2A H 0.1482 0.7253 0.1234 0.05 Uiso 1 1 calc R . . H2B H 0.1594 0.7808 0.0993 0.05 Uiso 1 1 calc R . . N22 N 1.1889(15) 0.6276(4) 0.3255(6) 0.037(2) Uani 1 1 d U . . C212 C 1.1723(18) 0.6358(5) 0.4404(7) 0.036(3) Uani 1 1 d . . . N21 N 1.1123(14) 0.6831(4) 0.4303(6) 0.037(2) Uani 1 1 d . . . C211 C 1.2138(18) 0.6063(5) 0.3856(7) 0.038(3) Uani 1 1 d U . . C210 C 1.2319(17) 0.6008(5) 0.2745(8) 0.044(3) Uani 1 1 d . . . C24 C 1.203(2) 0.6130(7) 0.5034(7) 0.053(4) Uani 1 1 d . . . C214 C 1.208(2) 0.6251(6) 0.2084(8) 0.053(4) Uani 1 1 d . . . H21A H 1.1645 0.6588 0.2121 0.08 Uiso 1 1 calc R . . H21B H 1.1203 0.6064 0.1793 0.08 Uiso 1 1 calc R . . H21C H 1.3225 0.6257 0.1916 0.08 Uiso 1 1 calc R . . C21 C 1.0753(19) 0.7102(6) 0.4807(7) 0.048(4) Uani 1 1 d . . . C27 C 1.2790(18) 0.5560(5) 0.3957(9) 0.049(4) Uani 1 1 d . . . C28 C 1.318(2) 0.5296(6) 0.3425(11) 0.063(5) Uani 1 1 d . . . H28 H 1.3604 0.4968 0.348 0.075 Uiso 1 1 calc R . . C29 C 1.295(2) 0.5505(7) 0.2815(10) 0.061(5) Uani 1 1 d . . . H29 H 1.3211 0.5323 0.2454 0.073 Uiso 1 1 calc R . . C23 C 1.176(3) 0.6431(8) 0.5552(9) 0.068(6) Uani 1 1 d . . . H23 H 1.2053 0.631 0.5976 0.082 Uiso 1 1 calc R . . C22 C 1.107(2) 0.6909(8) 0.5453(8) 0.065(5) Uani 1 1 d . . . H22 H 1.0822 0.7102 0.5805 0.078 Uiso 1 1 calc R . . C26 C 1.302(2) 0.5374(7) 0.4627(12) 0.071(6) Uani 1 1 d . . . H26 H 1.3429 0.5047 0.4701 0.085 Uiso 1 1 calc R . . C25 C 1.268(3) 0.5636(7) 0.5126(11) 0.071(6) Uani 1 1 d . . . H25 H 1.2867 0.5498 0.5543 0.085 Uiso 1 1 calc R . . C213 C 1.008(3) 0.7633(7) 0.4668(9) 0.070(5) Uani 1 1 d . . . H21D H 0.9949 0.7694 0.4206 0.104 Uiso 1 1 calc R . . H21E H 1.0947 0.7865 0.4888 0.104 Uiso 1 1 calc R . . H21F H 0.8922 0.7676 0.4822 0.104 Uiso 1 1 calc R . . C31 C 0.656(8) 0.8670(19) 0.479(2) 0.206(12) Uani 1 1 d D . . N31 N 0.633(7) 0.8491(17) 0.5272(18) 0.206(12) Uani 1 1 d D . . C32 C 0.713(7) 0.8886(18) 0.4202(19) 0.206(12) Uani 1 1 d D . . H32A H 0.7505 0.9228 0.4285 0.309 Uiso 1 1 calc R . . H32B H 0.6133 0.8876 0.3854 0.309 Uiso 1 1 calc R . . H32C H 0.814 0.8697 0.4079 0.309 Uiso 1 1 calc R . . O3W O 0.264(16) 0.977(4) 0.452(5) 0.25(3) Uani 0.5 1 d P . . O4W O 0.247(16) 0.984(4) 0.400(5) 0.25(3) Uani 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0172(3) 0.0336(4) 0.0513(4) 0.0050(2) 0.0108(2) 0.00246(18) Mn1 0.0114(8) 0.0352(10) 0.0465(11) 0.0034(8) 0.0054(7) 0.0017(7) Cl3 0.063(3) 0.063(2) 0.058(2) 0.0172(19) 0.020(2) 0.004(2) Cl4 0.062(3) 0.068(3) 0.056(2) 0.0052(19) 0.0142(19) 0.002(2) Cl1 0.038(2) 0.057(2) 0.091(3) -0.014(2) 0.011(2) -0.0163(17) Cl2 0.045(2) 0.049(2) 0.103(3) 0.005(2) 0.027(2) 0.0159(18) O4 0.019(4) 0.042(5) 0.065(6) -0.003(4) 0.008(4) 0.001(4) O1W 0.020(4) 0.049(5) 0.050(6) 0.010(4) -0.005(4) -0.003(4) O3 0.017(4) 0.061(6) 0.049(5) 0.005(4) 0.007(4) -0.013(4) O1 0.021(4) 0.040(5) 0.056(6) 0.001(4) 0.009(4) -0.004(4) O2 0.018(4) 0.046(5) 0.062(6) 0.004(5) -0.003(4) 0.004(4) O2W 0.020(5) 0.045(5) 0.067(7) -0.007(5) 0.012(4) 0.001(4) N12 0.014(5) 0.036(6) 0.057(7) 0.005(5) 0.001(5) 0.003(4) N11 0.016(5) 0.045(6) 0.052(7) 0.010(5) 0.002(5) -0.006(5) C15 0.034(8) 0.041(8) 0.088(13) 0.021(8) -0.021(8) -0.018(7) C110 0.029(7) 0.050(8) 0.043(8) -0.013(6) 0.006(6) -0.008(6) C111 0.023(4) 0.036(4) 0.040(4) 0.002(4) 0.003(4) -0.006(4) C12 0.042(9) 0.073(11) 0.051(9) 0.001(8) 0.011(7) -0.021(8) C14 0.021(7) 0.057(9) 0.064(10) 0.012(7) -0.007(6) -0.018(6) C11 0.027(7) 0.059(9) 0.060(9) -0.012(7) 0.015(6) -0.018(6) C13 0.032(8) 0.087(12) 0.050(9) 0.021(8) -0.002(7) -0.030(8) C112 0.013(6) 0.049(8) 0.051(8) 0.011(6) -0.003(5) -0.008(5) C17 0.016(6) 0.027(6) 0.093(13) 0.015(7) -0.009(7) 0.001(5) C19 0.045(9) 0.051(9) 0.069(11) -0.012(8) 0.006(8) -0.007(7) C1 0.015(6) 0.043(7) 0.043(7) 0.015(6) 0.003(5) 0.007(5) C16 0.024(7) 0.045(8) 0.089(13) 0.009(8) -0.003(8) -0.008(6) C114 0.070(12) 0.060(9) 0.041(8) 0.004(7) 0.005(8) -0.002(9) C113 0.040(9) 0.086(12) 0.072(11) -0.016(10) 0.025(8) -0.002(9) C3 0.021(4) 0.031(4) 0.037(4) 0.005(4) 0.007(4) 0.004(4) C18 0.041(9) 0.055(9) 0.095(14) -0.006(9) 0.035(9) 0.003(7) C2 0.017(6) 0.056(8) 0.051(8) 0.012(6) 0.002(6) 0.003(6) N22 0.025(4) 0.040(4) 0.045(4) -0.003(4) 0.005(3) -0.005(3) C212 0.019(6) 0.043(7) 0.044(8) 0.008(6) -0.005(5) -0.006(5) N21 0.019(5) 0.046(6) 0.045(6) -0.004(5) 0.002(4) -0.009(5) C211 0.028(4) 0.040(5) 0.045(5) 0.000(4) 0.004(4) -0.005(4) C210 0.012(6) 0.043(7) 0.076(10) -0.002(7) 0.006(6) -0.004(5) C24 0.037(8) 0.077(11) 0.040(8) 0.015(8) -0.013(7) -0.020(8) C214 0.040(9) 0.063(9) 0.062(10) -0.011(8) 0.025(8) -0.002(7) C21 0.027(7) 0.068(9) 0.051(8) -0.022(7) 0.011(6) -0.020(7) C27 0.020(6) 0.033(7) 0.089(12) 0.010(7) -0.012(7) 0.002(5) C28 0.038(9) 0.031(7) 0.120(16) -0.015(9) 0.011(9) -0.002(6) C29 0.029(8) 0.064(10) 0.091(14) -0.018(10) 0.008(8) 0.000(7) C23 0.050(11) 0.105(15) 0.044(10) 0.030(10) -0.012(8) -0.017(10) C22 0.038(9) 0.106(15) 0.050(10) -0.017(10) 0.005(7) -0.025(9) C26 0.047(10) 0.051(10) 0.107(16) 0.037(11) -0.018(11) -0.002(8) C25 0.053(11) 0.065(11) 0.087(14) 0.030(11) -0.021(11) -0.022(9) C213 0.059(11) 0.079(12) 0.073(12) -0.021(10) 0.013(9) 0.002(10) C31 0.21(3) 0.27(3) 0.14(2) 0.00(3) 0.04(2) 0.03(2) N31 0.21(3) 0.27(3) 0.14(2) 0.00(3) 0.04(2) 0.03(2) C32 0.21(3) 0.27(3) 0.14(2) 0.00(3) 0.04(2) 0.03(2) O3W 0.25(5) 0.24(5) 0.27(10) 0.11(7) 0.08(8) 0.04(4) O4W 0.25(5) 0.24(5) 0.27(10) 0.11(7) 0.08(8) 0.04(4) #------------------------------------------- # MOLECULAR GEOMETRY #----------------------------------------- _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 2.028(9) . ? Re1 O2 2.048(9) . ? Re1 Cl1 2.314(4) . ? Re1 Cl2 2.315(4) . ? Re1 Cl3 2.337(4) . ? Re1 Cl4 2.357(4) . ? Mn1 O4 2.167(9) . ? Mn1 O2W 2.214(10) . ? Mn1 O3 2.224(9) 1_655 ? Mn1 O1W 2.242(9) . ? Mn1 N12 2.289(10) . ? Mn1 N11 2.306(11) . ? O4 C3 1.260(14) . ? O3 C1 1.235(15) . ? O3 Mn1 2.224(9) 1_455 ? O1 C1 1.261(16) . ? O2 C3 1.275(15) . ? N12 C110 1.317(18) . ? N12 C111 1.391(17) . ? N11 C11 1.309(19) . ? N11 C112 1.363(18) . ? C15 C16 1.35(3) . ? C15 C14 1.42(2) . ? C15 H15 0.93 . ? C110 C19 1.39(2) . ? C110 C114 1.53(2) . ? C111 C17 1.407(18) . ? C111 C112 1.44(2) . ? C12 C13 1.34(3) . ? C12 C11 1.37(2) . ? C12 H12 0.93 . ? C14 C112 1.41(2) . ? C14 C13 1.42(2) . ? C11 C113 1.52(2) . ? C13 H13 0.93 . ? C17 C18 1.34(2) . ? C17 C16 1.43(2) . ? C19 C18 1.38(3) . ? C19 H19 0.93 . ? C1 C2 1.525(18) . ? C16 H16 0.93 . ? C114 H11A 0.96 . ? C114 H11B 0.96 . ? C114 H11C 0.96 . ? C113 H11D 0.96 . ? C113 H11E 0.96 . ? C113 H11F 0.96 . ? C3 C2 1.519(17) . ? C18 H18 0.93 . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? N22 C210 1.346(19) . ? N22 C211 1.354(18) . ? C212 N21 1.344(16) . ? C212 C24 1.43(2) . ? C212 C211 1.45(2) . ? N21 C21 1.324(18) . ? C211 C27 1.430(18) . ? C210 C29 1.42(2) . ? C210 C214 1.50(2) . ? C24 C23 1.37(3) . ? C24 C25 1.41(3) . ? C214 H21A 0.96 . ? C214 H21B 0.96 . ? C214 H21C 0.96 . ? C21 C22 1.42(2) . ? C21 C213 1.52(2) . ? C27 C28 1.37(3) . ? C27 C26 1.46(3) . ? C28 C29 1.37(3) . ? C28 H28 0.93 . ? C29 H29 0.93 . ? C23 C22 1.38(3) . ? C23 H23 0.93 . ? C22 H22 0.93 . ? C26 C25 1.30(3) . ? C26 H26 0.93 . ? C25 H25 0.93 . ? C213 H21D 0.96 . ? C213 H21E 0.96 . ? C213 H21F 0.96 . ? C31 N31 1.14(6) . ? C31 C32 1.46(6) . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 84.8(4) . . ? O1 Re1 Cl1 173.4(3) . . ? O2 Re1 Cl1 88.7(3) . . ? O1 Re1 Cl2 89.9(3) . . ? O2 Re1 Cl2 174.2(3) . . ? Cl1 Re1 Cl2 96.52(16) . . ? O1 Re1 Cl3 90.0(3) . . ? O2 Re1 Cl3 90.2(3) . . ? Cl1 Re1 Cl3 91.40(18) . . ? Cl2 Re1 Cl3 91.98(17) . . ? O1 Re1 Cl4 86.9(3) . . ? O2 Re1 Cl4 87.0(3) . . ? Cl1 Re1 Cl4 91.37(17) . . ? Cl2 Re1 Cl4 90.54(17) . . ? Cl3 Re1 Cl4 176.03(15) . . ? O4 Mn1 O2W 88.9(3) . . ? O4 Mn1 O3 91.7(4) . 1_655 ? O2W Mn1 O3 90.5(4) . 1_655 ? O4 Mn1 O1W 169.0(4) . . ? O2W Mn1 O1W 84.5(4) . . ? O3 Mn1 O1W 79.6(3) 1_655 . ? O4 Mn1 N12 92.7(4) . . ? O2W Mn1 N12 174.7(4) . . ? O3 Mn1 N12 94.5(4) 1_655 . ? O1W Mn1 N12 94.6(4) . . ? O4 Mn1 N11 103.8(4) . . ? O2W Mn1 N11 100.3(4) . . ? O3 Mn1 N11 161.1(4) 1_655 . ? O1W Mn1 N11 86.0(4) . . ? N12 Mn1 N11 74.4(4) . . ? C3 O4 Mn1 136.3(9) . . ? C1 O3 Mn1 124.1(9) . 1_455 ? C1 O1 Re1 131.0(8) . . ? C3 O2 Re1 129.0(8) . . ? C110 N12 C111 118.4(12) . . ? C110 N12 Mn1 130.5(10) . . ? C111 N12 Mn1 109.2(9) . . ? C11 N11 C112 119.6(13) . . ? C11 N11 Mn1 129.0(10) . . ? C112 N11 Mn1 108.4(9) . . ? C16 C15 C14 122.4(15) . . ? C16 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N12 C110 C19 122.0(15) . . ? N12 C110 C114 117.8(13) . . ? C19 C110 C114 120.2(14) . . ? N12 C111 C17 120.8(13) . . ? N12 C111 C112 118.1(12) . . ? C17 C111 C112 120.9(13) . . ? C13 C12 C11 119.5(16) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C112 C14 C13 114.6(15) . . ? C112 C14 C15 119.4(16) . . ? C13 C14 C15 126.0(16) . . ? N11 C11 C12 122.3(15) . . ? N11 C11 C113 117.8(15) . . ? C12 C11 C113 119.9(15) . . ? C12 C13 C14 121.7(15) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? N11 C112 C14 122.2(14) . . ? N11 C112 C111 119.8(12) . . ? C14 C112 C111 117.9(13) . . ? C18 C17 C111 119.2(15) . . ? C18 C17 C16 121.9(15) . . ? C111 C17 C16 118.9(16) . . ? C18 C19 C110 119.7(16) . . ? C18 C19 H19 120.1 . . ? C110 C19 H19 120.1 . . ? O3 C1 O1 123.8(12) . . ? O3 C1 C2 117.2(12) . . ? O1 C1 C2 119.0(11) . . ? C15 C16 C17 120.0(15) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C110 C114 H11A 109.5 . . ? C110 C114 H11B 109.5 . . ? H11A C114 H11B 109.5 . . ? C110 C114 H11C 109.5 . . ? H11A C114 H11C 109.5 . . ? H11B C114 H11C 109.5 . . ? C11 C113 H11D 109.5 . . ? C11 C113 H11E 109.5 . . ? H11D C113 H11E 109.5 . . ? C11 C113 H11F 109.5 . . ? H11D C113 H11F 109.5 . . ? H11E C113 H11F 109.5 . . ? O4 C3 O2 122.0(11) . . ? O4 C3 C2 117.2(11) . . ? O2 C3 C2 120.8(11) . . ? C17 C18 C19 119.7(15) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C3 C2 C1 111.9(12) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C210 N22 C211 118.5(12) . . ? N21 C212 C24 123.4(14) . . ? N21 C212 C211 119.5(12) . . ? C24 C212 C211 117.1(13) . . ? C21 N21 C212 119.2(13) . . ? N22 C211 C27 121.9(13) . . ? N22 C211 C212 118.1(12) . . ? C27 C211 C212 120.0(13) . . ? N22 C210 C29 122.0(15) . . ? N22 C210 C214 118.1(13) . . ? C29 C210 C214 119.8(15) . . ? C23 C24 C25 121.6(16) . . ? C23 C24 C212 116.1(16) . . ? C25 C24 C212 122.2(18) . . ? C210 C214 H21A 109.5 . . ? C210 C214 H21B 109.5 . . ? H21A C214 H21B 109.5 . . ? C210 C214 H21C 109.5 . . ? H21A C214 H21C 109.5 . . ? H21B C214 H21C 109.5 . . ? N21 C21 C22 121.0(16) . . ? N21 C21 C213 117.2(15) . . ? C22 C21 C213 121.7(15) . . ? C28 C27 C211 118.0(15) . . ? C28 C27 C26 125.1(15) . . ? C211 C27 C26 116.8(16) . . ? C27 C28 C29 121.1(15) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C28 C29 C210 118.4(17) . . ? C28 C29 H29 120.8 . . ? C210 C29 H29 120.8 . . ? C24 C23 C22 121.0(15) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C22 C21 119.1(17) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C25 C26 C27 124.0(16) . . ? C25 C26 H26 118 . . ? C27 C26 H26 118 . . ? C26 C25 C24 119.8(18) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C21 C213 H21D 109.5 . . ? C21 C213 H21E 109.5 . . ? H21D C213 H21E 109.5 . . ? C21 C213 H21F 109.5 . . ? H21D C213 H21F 109.5 . . ? H21E C213 H21F 109.5 . . ? N31 C31 C32 172(7) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2W Mn1 O4 C3 -12.8(12) . . . . ? O3 Mn1 O4 C3 -103.3(12) 1_655 . . . ? O1W Mn1 O4 C3 -66(3) . . . . ? N12 Mn1 O4 C3 162.1(12) . . . . ? N11 Mn1 O4 C3 87.5(12) . . . . ? O2 Re1 O1 C1 -19.7(11) . . . . ? Cl2 Re1 O1 C1 162.5(11) . . . . ? Cl3 Re1 O1 C1 70.5(11) . . . . ? Cl4 Re1 O1 C1 -106.9(11) . . . . ? O1 Re1 O2 C3 24.7(11) . . . . ? Cl1 Re1 O2 C3 -156.7(11) . . . . ? Cl3 Re1 O2 C3 -65.3(11) . . . . ? Cl4 Re1 O2 C3 111.9(11) . . . . ? O4 Mn1 N12 C110 67.4(12) . . . . ? O3 Mn1 N12 C110 -24.6(12) 1_655 . . . ? O1W Mn1 N12 C110 -104.4(12) . . . . ? N11 Mn1 N12 C110 171.0(12) . . . . ? O4 Mn1 N12 C111 -128.9(8) . . . . ? O3 Mn1 N12 C111 139.1(8) 1_655 . . . ? O1W Mn1 N12 C111 59.3(9) . . . . ? N11 Mn1 N12 C111 -25.3(8) . . . . ? O4 Mn1 N11 C11 -84.8(12) . . . . ? O2W Mn1 N11 C11 6.6(12) . . . . ? O3 Mn1 N11 C11 130.7(14) 1_655 . . . ? O1W Mn1 N11 C11 90.3(12) . . . . ? N12 Mn1 N11 C11 -173.8(12) . . . . ? O4 Mn1 N11 C112 115.3(8) . . . . ? O2W Mn1 N11 C112 -153.3(8) . . . . ? O3 Mn1 N11 C112 -29.2(16) 1_655 . . . ? O1W Mn1 N11 C112 -69.6(8) . . . . ? N12 Mn1 N11 C112 26.4(8) . . . . ? C111 N12 C110 C19 -1(2) . . . . ? Mn1 N12 C110 C19 161.7(11) . . . . ? C111 N12 C110 C114 179.0(12) . . . . ? Mn1 N12 C110 C114 -18.5(19) . . . . ? C110 N12 C111 C17 2.9(18) . . . . ? Mn1 N12 C111 C17 -163.1(10) . . . . ? C110 N12 C111 C112 -172.2(11) . . . . ? Mn1 N12 C111 C112 21.8(13) . . . . ? C16 C15 C14 C112 -7(2) . . . . ? C16 C15 C14 C13 173.1(14) . . . . ? C112 N11 C11 C12 4(2) . . . . ? Mn1 N11 C11 C12 -153.5(11) . . . . ? C112 N11 C11 C113 -174.4(12) . . . . ? Mn1 N11 C11 C113 27.7(18) . . . . ? C13 C12 C11 N11 -1(2) . . . . ? C13 C12 C11 C113 177.7(14) . . . . ? C11 C12 C13 C14 -3(2) . . . . ? C112 C14 C13 C12 4(2) . . . . ? C15 C14 C13 C12 -175.9(14) . . . . ? C11 N11 C112 C14 -3.5(18) . . . . ? Mn1 N11 C112 C14 158.5(10) . . . . ? C11 N11 C112 C111 173.0(12) . . . . ? Mn1 N11 C112 C111 -25.0(13) . . . . ? C13 C14 C112 N11 -0.5(18) . . . . ? C15 C14 C112 N11 179.3(12) . . . . ? C13 C14 C112 C111 -177.1(11) . . . . ? C15 C14 C112 C111 2.7(18) . . . . ? N12 C111 C112 N11 2.4(18) . . . . ? C17 C111 C112 N11 -172.6(11) . . . . ? N12 C111 C112 C14 179.1(11) . . . . ? C17 C111 C112 C14 4.0(18) . . . . ? N12 C111 C17 C18 -1(2) . . . . ? C112 C111 C17 C18 173.9(13) . . . . ? N12 C111 C17 C16 178.0(12) . . . . ? C112 C111 C17 C16 -7.1(19) . . . . ? N12 C110 C19 C18 -3(2) . . . . ? C114 C110 C19 C18 177.1(15) . . . . ? Mn1 O3 C1 O1 -46.8(16) 1_455 . . . ? Mn1 O3 C1 C2 134.8(10) 1_455 . . . ? Re1 O1 C1 O3 168.4(9) . . . . ? Re1 O1 C1 C2 -13.3(17) . . . . ? C14 C15 C16 C17 4(2) . . . . ? C18 C17 C16 C15 -177.7(15) . . . . ? C111 C17 C16 C15 3(2) . . . . ? Mn1 O4 C3 O2 5(2) . . . . ? Mn1 O4 C3 C2 -175.6(9) . . . . ? Re1 O2 C3 O4 -177.3(9) . . . . ? Re1 O2 C3 C2 3.6(18) . . . . ? C111 C17 C18 C19 -3(2) . . . . ? C16 C17 C18 C19 178.1(15) . . . . ? C110 C19 C18 C17 5(2) . . . . ? O4 C3 C2 C1 135.3(12) . . . . ? O2 C3 C2 C1 -45.5(17) . . . . ? O3 C1 C2 C3 -131.1(12) . . . . ? O1 C1 C2 C3 50.5(16) . . . . ? C24 C212 N21 C21 -1.4(19) . . . . ? C211 C212 N21 C21 -179.7(12) . . . . ? C210 N22 C211 C27 -1.8(19) . . . . ? C210 N22 C211 C212 178.2(11) . . . . ? N21 C212 C211 N22 -0.4(18) . . . . ? C24 C212 C211 N22 -178.8(12) . . . . ? N21 C212 C211 C27 179.6(12) . . . . ? C24 C212 C211 C27 1.2(19) . . . . ? C211 N22 C210 C29 2.5(19) . . . . ? C211 N22 C210 C214 -178.8(12) . . . . ? N21 C212 C24 C23 -3(2) . . . . ? C211 C212 C24 C23 175.0(13) . . . . ? N21 C212 C24 C25 -179.2(14) . . . . ? C211 C212 C24 C25 -1(2) . . . . ? C212 N21 C21 C22 3(2) . . . . ? C212 N21 C21 C213 180.0(13) . . . . ? N22 C211 C27 C28 1(2) . . . . ? C212 C211 C27 C28 -179.5(13) . . . . ? N22 C211 C27 C26 179.5(13) . . . . ? C212 C211 C27 C26 -0.5(19) . . . . ? C211 C27 C28 C29 0(2) . . . . ? C26 C27 C28 C29 -178.8(15) . . . . ? C27 C28 C29 C210 1(2) . . . . ? N22 C210 C29 C28 -2(2) . . . . ? C214 C210 C29 C28 179.4(14) . . . . ? C25 C24 C23 C22 -178.1(17) . . . . ? C212 C24 C23 C22 6(2) . . . . ? C24 C23 C22 C21 -4(3) . . . . ? N21 C21 C22 C23 -1(2) . . . . ? C213 C21 C22 C23 -177.1(16) . . . . ? C28 C27 C26 C25 178.3(17) . . . . ? C211 C27 C26 C25 -1(3) . . . . ? C27 C26 C25 C24 1(3) . . . . ? C23 C24 C25 C26 -175.9(18) . . . . ? C212 C24 C25 C26 0(3) . . . . ? #===END