Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof. Mike Ward' _publ_contact_author_address ; Prof. Mike Ward Department of Chemistry University of Sheffield SHEFFIELD S3 7HF ; _publ_contact_author_fax '0114 2229346' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Luminescent complexes of Re(I) and Ru(II) with appended macrocycle groups derived from 5,6-dihydroxyphenanthroline: cation and anion binding ; _publ_contact_letter ; This CIF file contains details of the 4 crystal structure in the paper 'Luminescent complexes of Re(I) and Ru(II) with appended macrocycle groups..' by T. Lazarides et al, submitted to Dalton Trans for publication. ; loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'John C. Jeffery' 'Theodore Lazarides' 'Thomas A. Miller' 'Tanya K. Ronson' #======================================================== data_gingerm _database_code_depnum_ccdc_archive 'CCDC 253589' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H27 Cl N2 O9.50 Re' _chemical_formula_weight 729.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.0812(17) _cell_length_b 16.5695(11) _cell_length_c 12.9281(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.9390(10) _cell_angle_gamma 90.00 _cell_volume 5360.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 4.691 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.30 _exptl_absorpt_correction_T_max 0.61 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27774 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6176 _reflns_number_gt 4380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0333P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6176 _refine_ls_number_parameters 375 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 1.138449(7) 0.132432(10) -0.002595(13) 0.03139(6) Uani 1 1 d D . . Cl Cl 1.12103(9) 0.09147(12) 0.17488(15) 0.0341(4) Uani 0.82 1 d PDU A 1 C31 C 1.1478(7) 0.1655(9) -0.1413(10) 0.041(3) Uani 0.82 1 d PDU A 1 O31 O 1.1522(2) 0.1858(4) -0.2266(4) 0.0575(17) Uani 0.82 1 d PDU A 1 ClA Cl 1.1420(8) 0.1825(10) -0.1745(10) 0.042(3) Uani 0.18 1 d PDU A 2 C31A C 1.127(2) 0.089(2) 0.1317(17) 0.056(11) Uani 0.18 1 d PDU A 2 O31A O 1.1268(9) 0.0645(14) 0.2155(11) 0.040(6) Uani 0.18 1 d PDU A 2 C30 C 1.15420(19) 0.0238(3) -0.0412(4) 0.0383(11) Uani 1 1 d . A . O30 O 1.16300(14) -0.0428(2) -0.0595(3) 0.0511(9) Uani 1 1 d . . . C32 C 1.2132(2) 0.1490(3) 0.0316(4) 0.0399(11) Uani 1 1 d . A . O32 O 1.25808(15) 0.1598(2) 0.0495(3) 0.0542(10) Uani 1 1 d . . . N1 N 1.05244(14) 0.1280(2) -0.0360(2) 0.0297(8) Uani 1 1 d . A . N2 N 1.11059(14) 0.2480(2) 0.0526(2) 0.0298(8) Uani 1 1 d . A . C1 C 1.14018(18) 0.3079(2) 0.0959(3) 0.0310(10) Uani 1 1 d . . . H1 H 1.1772 0.3034 0.0988 0.037 Uiso 1 1 calc R A . C2 C 1.11751(19) 0.3773(3) 0.1370(3) 0.0354(10) Uani 1 1 d . A . H2 H 1.1394 0.4178 0.1661 0.042 Uiso 1 1 calc R . . C3 C 1.06326(19) 0.3853(2) 0.1341(3) 0.0333(10) Uani 1 1 d . . . H3 H 1.0479 0.4310 0.1611 0.040 Uiso 1 1 calc R A . C4 C 1.03088(18) 0.3231(2) 0.0896(3) 0.0297(10) Uani 1 1 d . A . C5 C 1.05646(16) 0.2557(2) 0.0499(3) 0.0273(9) Uani 1 1 d . . . C6 C 1.02538(17) 0.1927(2) 0.0009(3) 0.0273(9) Uani 1 1 d . A . C7 C 0.96915(17) 0.1978(2) -0.0080(3) 0.0303(10) Uani 1 1 d . . . C8 C 0.94084(18) 0.1364(3) -0.0632(3) 0.0340(9) Uani 1 1 d . A . H8 H 0.9037 0.1383 -0.0718 0.041 Uiso 1 1 calc R . . C9 C 0.96813(19) 0.0741(3) -0.1043(4) 0.0376(11) Uani 1 1 d . . . H9 H 0.9500 0.0340 -0.1428 0.045 Uiso 1 1 calc R A . C10 C 1.02353(19) 0.0716(3) -0.0874(3) 0.0350(10) Uani 1 1 d . A . H10 H 1.0415 0.0279 -0.1138 0.042 Uiso 1 1 calc R . . C11 C 0.97371(18) 0.3267(3) 0.0824(3) 0.0305(10) Uani 1 1 d . . . C12 C 0.94389(18) 0.2663(3) 0.0373(3) 0.0324(10) Uani 1 1 d . A . O13 O 0.88936(12) 0.26869(19) 0.0301(2) 0.0368(7) Uani 1 1 d . . . C14 C 0.86738(18) 0.2446(3) 0.1265(3) 0.0378(11) Uani 1 1 d . A . H14B H 0.8876 0.2696 0.1846 0.045 Uiso 1 1 calc R . . H14A H 0.8700 0.1865 0.1346 0.045 Uiso 1 1 calc R . . C15 C 0.81018(18) 0.2701(3) 0.1254(4) 0.0434(12) Uani 1 1 d . . . H15B H 0.7919 0.2564 0.0592 0.052 Uiso 1 1 calc R A . H15A H 0.7927 0.2419 0.1794 0.052 Uiso 1 1 calc R . . O16 O 0.80752(13) 0.35390(19) 0.1418(3) 0.0499(9) Uani 1 1 d . A . C17 C 0.7544(2) 0.3827(3) 0.1495(5) 0.0590(15) Uani 1 1 d . . . H17B H 0.7357 0.3472 0.1943 0.071 Uiso 1 1 calc R A . H17A H 0.7356 0.3820 0.0814 0.071 Uiso 1 1 calc R . . C18 C 0.7544(3) 0.4651(5) 0.1914(6) 0.103(3) Uani 1 1 d . A . H18B H 0.7687 0.5007 0.1404 0.123 Uiso 1 1 calc R . . H18A H 0.7176 0.4808 0.1979 0.123 Uiso 1 1 calc R . . O19 O 0.78024(17) 0.4784(3) 0.2784(4) 0.0891(15) Uani 1 1 d . . . C20 C 0.7794(2) 0.5548(3) 0.3259(5) 0.0566(14) Uani 1 1 d . A . H20B H 0.7839 0.5472 0.4004 0.068 Uiso 1 1 calc R . . H20A H 0.7445 0.5785 0.3103 0.068 Uiso 1 1 calc R . . C21 C 0.8203(2) 0.6131(3) 0.2956(4) 0.0525(14) Uani 1 1 d . . . H21B H 0.8152 0.6245 0.2220 0.063 Uiso 1 1 calc R A . H21A H 0.8167 0.6633 0.3332 0.063 Uiso 1 1 calc R . . O22 O 0.87213(13) 0.57965(18) 0.3191(2) 0.0389(8) Uani 1 1 d . A . C23 C 0.9151(2) 0.6319(3) 0.2968(3) 0.0418(11) Uani 1 1 d . . . H23B H 0.9476 0.6119 0.3328 0.050 Uiso 1 1 calc R A . H23A H 0.9081 0.6850 0.3243 0.050 Uiso 1 1 calc R . . C24 C 0.9243(2) 0.6401(3) 0.1830(3) 0.0423(11) Uani 1 1 d . A . H24B H 0.8912 0.6565 0.1458 0.051 Uiso 1 1 calc R . . H24A H 0.9504 0.6823 0.1745 0.051 Uiso 1 1 calc R . . O25 O 0.94259(13) 0.56715(18) 0.1385(2) 0.0410(8) Uani 1 1 d . . . C26 C 0.89991(18) 0.5141(3) 0.1071(3) 0.0362(10) Uani 1 1 d . A . H26B H 0.8736 0.5425 0.0622 0.043 Uiso 1 1 calc R . . H26A H 0.8826 0.4953 0.1674 0.043 Uiso 1 1 calc R . . C27 C 0.92137(19) 0.4441(3) 0.0508(3) 0.0359(11) Uani 1 1 d . . . H27B H 0.8923 0.4139 0.0161 0.043 Uiso 1 1 calc R A . H27A H 0.9446 0.4629 -0.0011 0.043 Uiso 1 1 calc R . . O28 O 0.95111(13) 0.39295(18) 0.1256(2) 0.0357(7) Uani 1 1 d . A . O40 O 0.0000 0.0879(6) 0.2500 0.164(4) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.03358(10) 0.03021(9) 0.03076(9) -0.00117(9) 0.00498(6) -0.00007(9) Cl 0.0412(10) 0.0332(9) 0.0278(13) 0.0021(9) 0.0007(11) -0.0039(7) C31 0.042(5) 0.038(7) 0.044(7) 0.003(4) 0.009(5) 0.012(4) O31 0.073(4) 0.062(3) 0.040(3) 0.017(3) 0.025(3) 0.021(3) ClA 0.052(7) 0.029(6) 0.048(10) 0.004(6) 0.017(8) 0.008(5) C31A 0.08(3) 0.07(2) 0.014(14) -0.008(15) -0.020(18) 0.013(19) O31A 0.044(12) 0.059(16) 0.019(11) -0.006(10) 0.000(10) 0.005(11) C30 0.035(3) 0.045(3) 0.036(2) -0.002(2) 0.008(2) 0.001(2) O30 0.056(2) 0.039(2) 0.059(2) -0.0074(17) 0.0085(18) 0.0111(17) C32 0.047(3) 0.036(3) 0.036(2) 0.006(2) 0.006(2) 0.001(2) O32 0.037(2) 0.058(2) 0.067(2) 0.0187(19) 0.0018(19) -0.0041(17) N1 0.034(2) 0.0282(18) 0.0266(16) -0.0009(16) 0.0026(14) -0.0005(17) N2 0.034(2) 0.0319(19) 0.0231(17) 0.0003(15) 0.0007(15) -0.0043(16) C1 0.036(3) 0.030(2) 0.027(2) 0.0023(18) 0.0040(19) -0.0078(19) C2 0.044(3) 0.030(2) 0.032(2) 0.0024(19) -0.0003(19) -0.012(2) C3 0.050(3) 0.030(2) 0.0203(19) 0.0015(17) 0.0024(19) -0.0029(19) C4 0.042(3) 0.028(2) 0.0186(19) 0.0009(18) 0.0006(18) -0.002(2) C5 0.031(2) 0.026(2) 0.024(2) 0.0041(17) 0.0005(18) -0.0028(18) C6 0.033(2) 0.025(2) 0.024(2) 0.0030(17) 0.0009(18) -0.0002(18) C7 0.038(3) 0.030(2) 0.022(2) 0.0022(18) -0.0002(18) -0.0005(19) C8 0.035(2) 0.033(2) 0.035(2) 0.002(2) -0.0015(18) -0.004(2) C9 0.043(3) 0.029(2) 0.040(3) -0.005(2) -0.005(2) -0.004(2) C10 0.045(3) 0.027(2) 0.033(2) -0.0044(19) 0.001(2) 0.001(2) C11 0.038(3) 0.030(2) 0.023(2) 0.0011(19) 0.0020(19) 0.007(2) C12 0.033(3) 0.036(2) 0.028(2) 0.0040(19) 0.0002(19) 0.003(2) O13 0.0340(18) 0.0475(19) 0.0290(16) 0.0003(14) 0.0019(13) 0.0007(15) C14 0.043(3) 0.032(2) 0.038(3) 0.003(2) 0.008(2) 0.001(2) C15 0.039(3) 0.042(3) 0.051(3) -0.007(2) 0.012(2) -0.006(2) O16 0.0371(19) 0.041(2) 0.071(2) -0.0103(17) 0.0036(17) 0.0069(15) C17 0.031(3) 0.066(4) 0.080(4) -0.011(3) 0.006(3) 0.006(3) C18 0.063(5) 0.117(7) 0.123(7) -0.051(5) -0.030(5) 0.052(4) O19 0.056(3) 0.078(3) 0.130(4) -0.044(3) -0.017(3) 0.028(2) C20 0.053(3) 0.052(3) 0.066(4) -0.004(3) 0.012(3) 0.019(3) C21 0.054(3) 0.048(3) 0.057(3) 0.006(3) 0.009(3) 0.017(3) O22 0.048(2) 0.0375(18) 0.0316(16) -0.0001(14) 0.0045(14) 0.0080(15) C23 0.055(3) 0.038(2) 0.033(2) -0.001(2) 0.006(2) 0.002(3) C24 0.062(3) 0.032(2) 0.033(2) 0.000(2) 0.007(2) -0.002(2) O25 0.050(2) 0.0341(17) 0.0399(18) -0.0063(14) 0.0113(15) 0.0008(15) C26 0.042(3) 0.032(2) 0.035(2) -0.002(2) 0.002(2) 0.004(2) C27 0.045(3) 0.037(3) 0.026(2) 0.0017(19) 0.003(2) 0.006(2) O28 0.048(2) 0.0327(16) 0.0262(15) -0.0035(13) 0.0003(14) 0.0097(14) O40 0.131(8) 0.135(8) 0.237(11) 0.000 0.094(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re C31 1.905(12) . ? Re C30 1.916(5) . ? Re C32 1.916(5) . ? Re C31A 1.918(19) . ? Re N1 2.172(3) . ? Re N2 2.176(3) . ? Re ClA 2.379(11) . ? Re Cl 2.4604(19) . ? C31 O31 1.165(12) . ? C31A O31A 1.158(18) . ? C30 O30 1.154(5) . ? C32 O32 1.147(6) . ? N1 C10 1.332(5) . ? N1 C6 1.372(5) . ? N2 C1 1.339(5) . ? N2 C5 1.362(5) . ? C1 C2 1.403(6) . ? C2 C3 1.365(6) . ? C3 C4 1.410(6) . ? C4 C5 1.403(6) . ? C4 C11 1.432(6) . ? C5 C6 1.425(5) . ? C6 C7 1.409(6) . ? C7 C8 1.406(6) . ? C7 C12 1.444(6) . ? C8 C9 1.366(6) . ? C9 C10 1.392(6) . ? C11 C12 1.356(6) . ? C11 O28 1.372(5) . ? C12 O13 1.365(5) . ? O13 C14 1.453(5) . ? C14 C15 1.495(6) . ? C15 O16 1.407(5) . ? O16 C17 1.424(6) . ? C17 C18 1.469(8) . ? C18 O19 1.278(7) . ? O19 C20 1.407(6) . ? C20 C21 1.480(7) . ? C21 O22 1.427(6) . ? O22 C23 1.427(5) . ? C23 C24 1.510(6) . ? C24 O25 1.428(5) . ? O25 C26 1.422(5) . ? C26 C27 1.489(6) . ? C27 O28 1.453(5) . ? 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 C31 Re C30 89.1(5) . . ? C31 Re C32 89.7(5) . . ? C30 Re C32 88.78(19) . . ? C31 Re C31A 174.4(14) . . ? C30 Re C31A 85.9(13) . . ? C32 Re C31A 92.7(15) . . ? C31 Re N1 90.4(5) . . ? C30 Re N1 97.83(17) . . ? C32 Re N1 173.39(16) . . ? C31A Re N1 87.8(15) . . ? C31 Re N2 96.8(4) . . ? C30 Re N2 171.43(16) . . ? C32 Re N2 97.43(16) . . ? C31A Re N2 87.9(13) . . ? N1 Re N2 75.99(13) . . ? C31 Re ClA 6.0(8) . . ? C30 Re ClA 93.6(4) . . ? C32 Re ClA 93.8(5) . . ? C31A Re ClA 173.5(16) . . ? N1 Re ClA 85.8(5) . . ? N2 Re ClA 91.9(4) . . ? C31 Re Cl 176.8(5) . . ? C30 Re Cl 92.10(14) . . ? C32 Re Cl 93.33(14) . . ? C31A Re Cl 6.2(13) . . ? N1 Re Cl 86.47(10) . . ? N2 Re Cl 81.69(10) . . ? ClA Re Cl 171.0(4) . . ? O31 C31 Re 178.3(15) . . ? O31A C31A Re 172(4) . . ? O30 C30 Re 176.5(4) . . ? O32 C32 Re 178.2(4) . . ? C10 N1 C6 117.1(4) . . ? C10 N1 Re 128.5(3) . . ? C6 N1 Re 114.4(3) . . ? C1 N2 C5 117.7(4) . . ? C1 N2 Re 127.5(3) . . ? C5 N2 Re 114.6(3) . . ? N2 C1 C2 122.6(4) . . ? C3 C2 C1 119.9(4) . . ? C2 C3 C4 119.1(4) . . ? C5 C4 C3 117.8(4) . . ? C5 C4 C11 119.4(4) . . ? C3 C4 C11 122.9(4) . . ? N2 C5 C4 123.0(4) . . ? N2 C5 C6 117.2(4) . . ? C4 C5 C6 119.7(4) . . ? N1 C6 C7 122.3(4) . . ? N1 C6 C5 117.3(4) . . ? C7 C6 C5 120.4(4) . . ? C8 C7 C6 117.8(4) . . ? C8 C7 C12 123.6(4) . . ? C6 C7 C12 118.6(4) . . ? C9 C8 C7 119.6(4) . . ? C8 C9 C10 118.9(4) . . ? N1 C10 C9 124.1(4) . . ? C12 C11 O28 122.3(4) . . ? C12 C11 C4 121.2(4) . . ? O28 C11 C4 116.5(4) . . ? C11 C12 O13 121.9(4) . . ? C11 C12 C7 120.7(4) . . ? O13 C12 C7 117.4(4) . . ? C12 O13 C14 111.8(3) . . ? O13 C14 C15 109.6(4) . . ? O16 C15 C14 109.4(4) . . ? C15 O16 C17 113.3(4) . . ? O16 C17 C18 111.1(5) . . ? O19 C18 C17 118.2(6) . . ? C18 O19 C20 121.2(6) . . ? O19 C20 C21 116.2(5) . . ? O22 C21 C20 109.1(4) . . ? C23 O22 C21 114.3(4) . . ? O22 C23 C24 114.8(4) . . ? O25 C24 C23 113.0(4) . . ? C26 O25 C24 112.4(4) . . ? O25 C26 C27 109.3(4) . . ? O28 C27 C26 108.4(3) . . ? C11 O28 C27 113.8(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.071 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.110 #=END data_ted _database_code_depnum_ccdc_archive 'CCDC 253590' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H34 Cl N2 O11 Re' _chemical_formula_weight 856.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -5.2083 5.8923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.4640(7) _cell_length_b 13.3917(4) _cell_length_c 11.4092(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.565(2) _cell_angle_gamma 90.00 _cell_volume 3250.91(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 8.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.02 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16284 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 67.83 _reflns_number_total 5068 _reflns_number_gt 5010 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+70.0064P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5068 _refine_ls_number_parameters 428 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.349 _refine_ls_restrained_S_all 1.349 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.37431(2) 0.63072(4) 0.21791(4) 0.01901(17) Uani 1 1 d D . . C41 C 0.3165(5) 0.6513(8) 0.0721(10) 0.023(2) Uani 1 1 d . A . O41 O 0.2870(4) 0.6669(7) -0.0148(7) 0.033(2) Uani 1 1 d . . . C42 C 0.3048(5) 0.6298(9) 0.3109(10) 0.023(2) Uani 1 1 d . A . O42 O 0.2643(4) 0.6215(6) 0.3651(7) 0.0299(19) Uani 1 1 d . . . C43 C 0.3638(9) 0.4854(14) 0.2004(16) 0.025 Uiso 0.766(13) 1 d PDU A 1 C43A C 0.390(3) 0.776(2) 0.224(7) 0.025 Uiso 0.234(13) 1 d PDU A 2 O43 O 0.3575(5) 0.3995(8) 0.1942(8) 0.024(2) Uiso 0.766(13) 1 d PDU A 1 O43A O 0.3862(17) 0.861(2) 0.240(3) 0.025 Uiso 0.234(13) 1 d PDU A 2 Cl Cl 0.38746(17) 0.8098(3) 0.2378(3) 0.0147(12) Uani 0.766(13) 1 d PDU A 1 ClA Cl 0.3726(6) 0.4583(7) 0.2017(11) 0.016(4) Uiso 0.234(13) 1 d PDU A 2 N1 N 0.4508(4) 0.6232(6) 0.3646(7) 0.0134(17) Uani 1 1 d . A . C2 C 0.4462(5) 0.6215(7) 0.4791(8) 0.014(2) Uani 1 1 d . . . H12 H 0.4056 0.6211 0.5037 0.017 Uiso 1 1 calc R A . C3 C 0.4989(5) 0.6201(7) 0.5651(8) 0.014(2) Uani 1 1 d . A . H11 H 0.4936 0.6201 0.6465 0.017 Uiso 1 1 calc R . . C4 C 0.5578(5) 0.6188(7) 0.5328(9) 0.017(2) Uani 1 1 d . . . H24 H 0.5937 0.6169 0.5912 0.020 Uiso 1 1 calc R A . C5 C 0.5649(5) 0.6204(7) 0.4121(9) 0.015(2) Uani 1 1 d . A . C6 C 0.5101(5) 0.6247(6) 0.3311(8) 0.011(2) Uani 1 1 d . . . C7 C 0.5143(5) 0.6267(7) 0.2077(9) 0.014(2) Uani 1 1 d . A . N8 N 0.4594(4) 0.6306(6) 0.1318(7) 0.0149(18) Uani 1 1 d . A . C9 C 0.4624(5) 0.6311(7) 0.0161(9) 0.018(2) Uani 1 1 d . . . H16 H 0.4245 0.6337 -0.0372 0.022 Uiso 1 1 calc R A . C10 C 0.5198(5) 0.6280(7) -0.0292(9) 0.018(2) Uani 1 1 d . A . H19 H 0.5202 0.6266 -0.1123 0.021 Uiso 1 1 calc R . . C11 C 0.5753(5) 0.6269(7) 0.0447(9) 0.017(2) Uani 1 1 d . . . H25 H 0.6144 0.6266 0.0141 0.021 Uiso 1 1 calc R A . C12 C 0.5729(5) 0.6264(7) 0.1678(9) 0.014(2) Uani 1 1 d . A . C13 C 0.6288(5) 0.6300(8) 0.2515(10) 0.024(2) Uiso 1 1 d . . . C14 C 0.6255(5) 0.6185(8) 0.3716(9) 0.020(2) Uani 1 1 d . A . O15 O 0.6757(3) 0.6060(6) 0.4540(6) 0.0224(16) Uani 1 1 d . . . C16 C 0.7200(5) 0.6898(9) 0.4707(10) 0.026(3) Uani 1 1 d . A . H10A H 0.7023 0.7443 0.5149 0.031 Uiso 1 1 calc R . . H10B H 0.7282 0.7162 0.3932 0.031 Uiso 1 1 calc R . . C17 C 0.7790(5) 0.6520(9) 0.5383(10) 0.028(3) Uani 1 1 d . . . H26A H 0.8053 0.7090 0.5706 0.034 Uiso 1 1 calc R A . H26B H 0.7691 0.6107 0.6053 0.034 Uiso 1 1 calc R . . O18 O 0.8131(3) 0.5931(6) 0.4622(6) 0.0273(18) Uani 1 1 d . A . C19 C 0.8709(5) 0.5557(9) 0.5214(10) 0.027(3) Uani 1 1 d . . . H40A H 0.8629 0.5190 0.5934 0.033 Uiso 1 1 calc R A . H40B H 0.8994 0.6121 0.5460 0.033 Uiso 1 1 calc R . . C20 C 0.9012(6) 0.4874(8) 0.4422(10) 0.028(3) Uani 1 1 d . A . H39A H 0.9364 0.4514 0.4889 0.034 Uiso 1 1 calc R . . H39B H 0.8703 0.4374 0.4072 0.034 Uiso 1 1 calc R . . O21 O 0.9244(4) 0.5426(5) 0.3503(7) 0.0254(17) Uani 1 1 d . . . C22 C 0.9594(5) 0.4794(8) 0.2815(10) 0.026(3) Uani 1 1 d . A . H41A H 0.9337 0.4207 0.2531 0.031 Uiso 1 1 calc R . . H41B H 0.9978 0.4552 0.3309 0.031 Uiso 1 1 calc R . . C23 C 0.9775(6) 0.5379(9) 0.1762(10) 0.029(3) Uani 1 1 d . . . H38A H 0.9988 0.4932 0.1249 0.035 Uiso 1 1 calc R A . H38B H 0.9392 0.5650 0.1289 0.035 Uiso 1 1 calc R . . O24 O 1.0181(4) 0.6169(6) 0.2179(7) 0.0317(19) Uani 1 1 d . A . C25 C 1.0576(6) 0.6533(7) 0.1433(9) 0.022(2) Uani 1 1 d . . . C26 C 1.1196(5) 0.6645(8) 0.1872(10) 0.025(3) Uani 1 1 d . A . H102 H 1.1335 0.6415 0.2650 0.030 Uiso 1 1 calc R . . C27 C 1.1628(5) 0.7077(8) 0.1233(10) 0.025(3) Uani 1 1 d . . . H43 H 1.2053 0.7169 0.1568 0.030 Uiso 1 1 calc R A . C28 C 1.1418(6) 0.7373(9) 0.0080(10) 0.028(3) Uani 1 1 d . A . H35 H 1.1710 0.7645 -0.0391 0.033 Uiso 1 1 calc R . . C29 C 1.0799(5) 0.7280(8) -0.0393(10) 0.024(2) Uani 1 1 d . . . H37 H 1.0667 0.7502 -0.1177 0.029 Uiso 1 1 calc R A . C30 C 1.0363(6) 0.6862(8) 0.0270(10) 0.025(2) Uani 1 1 d . A . O31 O 0.9733(4) 0.6781(6) -0.0128(7) 0.0258(17) Uani 1 1 d . . . C32 C 0.9529(6) 0.7166(9) -0.1282(10) 0.030(3) Uani 1 1 d . A . H42A H 0.9735 0.6795 -0.1876 0.035 Uiso 1 1 calc R . . H42B H 0.9646 0.7879 -0.1321 0.035 Uiso 1 1 calc R . . C33 C 0.8839(5) 0.7055(8) -0.1535(12) 0.032(3) Uani 1 1 d . . . H8A H 0.8642 0.7315 -0.0860 0.038 Uiso 1 1 calc R A . H8B H 0.8681 0.7452 -0.2243 0.038 Uiso 1 1 calc R . . O34 O 0.8666(4) 0.6019(6) -0.1735(7) 0.0321(19) Uani 1 1 d . A . C35 C 0.8082(5) 0.5766(8) -0.1363(9) 0.022(2) Uani 1 1 d . . . H32A H 0.7903 0.5167 -0.1789 0.027 Uiso 1 1 calc R A . H32B H 0.7780 0.6324 -0.1521 0.027 Uiso 1 1 calc R . . C36 C 0.8215(7) 0.5559(10) -0.0032(11) 0.040(3) Uani 1 1 d . A . H34A H 0.8426 0.4905 0.0105 0.048 Uiso 1 1 calc R . . H34B H 0.8497 0.6081 0.0356 0.048 Uiso 1 1 calc R . . O37 O 0.7660(4) 0.5556(8) 0.0440(7) 0.045(2) Uani 1 1 d . . . C38 C 0.7776(6) 0.5325(11) 0.1682(10) 0.038(3) Uani 1 1 d . A . H33A H 0.8033 0.5858 0.2110 0.046 Uiso 1 1 calc R . . H33B H 0.8007 0.4686 0.1806 0.046 Uiso 1 1 calc R . . C39 C 0.7158(5) 0.5251(10) 0.2126(10) 0.029(3) Uani 1 1 d . . . H10C H 0.6885 0.4778 0.1628 0.035 Uiso 1 1 calc R A . H10D H 0.7218 0.4992 0.2946 0.035 Uiso 1 1 calc R . . O40 O 0.6858(3) 0.6229(6) 0.2100(6) 0.0229(16) Uani 1 1 d . A . 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 Re 0.0210(3) 0.0256(3) 0.0106(3) -0.0005(2) 0.00314(18) 0.0063(2) C41 0.031(6) 0.022(6) 0.017(6) 0.000(5) 0.011(5) 0.005(5) O41 0.039(5) 0.044(5) 0.015(4) -0.001(4) -0.004(4) 0.013(4) C42 0.017(6) 0.029(6) 0.026(6) -0.004(5) 0.010(5) 0.005(5) O42 0.024(4) 0.037(5) 0.030(4) -0.004(4) 0.010(4) 0.004(4) Cl 0.0174(17) 0.017(2) 0.0099(17) -0.0026(16) 0.0027(12) 0.0007(18) N1 0.021(5) 0.009(4) 0.009(4) 0.001(3) -0.002(3) -0.004(3) C2 0.018(5) 0.009(5) 0.016(5) -0.007(4) 0.007(4) -0.005(4) C3 0.027(6) 0.006(4) 0.009(5) -0.001(4) 0.000(4) -0.006(4) C4 0.028(6) 0.009(5) 0.014(5) -0.001(4) 0.004(4) -0.004(4) C5 0.023(5) 0.002(4) 0.019(5) -0.004(4) 0.001(4) -0.004(4) C6 0.024(5) 0.003(4) 0.005(5) -0.001(3) 0.000(4) -0.004(4) C7 0.019(5) 0.003(4) 0.020(5) -0.004(4) 0.005(4) -0.005(4) N8 0.014(4) 0.014(4) 0.019(5) -0.007(3) 0.012(3) 0.000(3) C9 0.029(6) 0.009(5) 0.016(5) -0.004(4) 0.001(4) -0.011(4) C10 0.027(6) 0.015(5) 0.012(5) 0.001(4) 0.007(4) -0.002(4) C11 0.030(6) 0.010(5) 0.013(5) 0.003(4) 0.009(4) 0.001(4) C12 0.022(5) 0.005(4) 0.017(5) -0.004(4) 0.004(4) -0.002(4) C14 0.027(6) 0.016(5) 0.019(6) -0.002(4) 0.006(5) -0.005(4) O15 0.024(4) 0.028(4) 0.015(4) 0.002(3) -0.001(3) 0.000(3) C16 0.029(6) 0.024(6) 0.025(6) -0.006(5) 0.005(5) 0.000(5) C17 0.028(6) 0.038(7) 0.019(6) -0.005(5) 0.004(5) -0.010(5) O18 0.023(4) 0.040(5) 0.019(4) 0.003(4) 0.003(3) 0.001(4) C19 0.032(6) 0.024(6) 0.025(6) 0.009(5) 0.002(5) -0.001(5) C20 0.038(7) 0.011(5) 0.036(7) 0.010(5) 0.007(5) 0.000(5) O21 0.034(5) 0.009(3) 0.035(5) 0.004(3) 0.013(4) -0.002(3) C22 0.037(7) 0.007(5) 0.030(7) 0.000(5) -0.008(5) -0.002(5) C23 0.038(7) 0.024(6) 0.024(6) 0.000(5) 0.001(5) 0.004(5) O24 0.033(5) 0.031(5) 0.033(5) -0.004(4) 0.012(4) -0.002(4) C25 0.040(7) 0.009(5) 0.022(6) -0.005(4) 0.015(5) 0.001(5) C26 0.025(6) 0.028(6) 0.023(6) 0.011(5) 0.009(5) 0.012(5) C27 0.027(6) 0.014(5) 0.034(7) 0.000(5) 0.006(5) 0.003(5) C28 0.033(7) 0.024(6) 0.029(7) -0.004(5) 0.015(5) 0.001(5) C29 0.033(6) 0.013(5) 0.026(6) 0.004(5) 0.007(5) -0.002(5) C30 0.035(7) 0.012(5) 0.026(6) -0.003(5) 0.002(5) -0.001(5) O31 0.031(4) 0.021(4) 0.026(4) 0.005(3) 0.006(3) -0.002(3) C32 0.036(7) 0.022(6) 0.029(7) 0.001(5) 0.000(5) 0.008(5) C33 0.024(6) 0.018(6) 0.049(8) -0.008(5) -0.009(5) -0.005(5) O34 0.030(5) 0.029(4) 0.038(5) -0.013(4) 0.007(4) -0.005(4) C35 0.032(6) 0.018(5) 0.018(6) 0.000(4) 0.006(5) -0.002(5) C36 0.056(9) 0.037(7) 0.030(7) 0.001(6) 0.018(6) 0.014(7) O37 0.044(5) 0.067(7) 0.029(5) 0.013(5) 0.017(4) 0.022(5) C38 0.042(8) 0.058(9) 0.018(6) 0.016(6) 0.013(5) 0.017(7) C39 0.023(6) 0.043(7) 0.022(6) 0.000(5) 0.009(5) 0.009(5) O40 0.021(4) 0.030(4) 0.020(4) -0.004(3) 0.010(3) -0.001(3) _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 Re C42 1.941(11) . ? Re C41 1.959(12) . ? Re C43 1.967(19) . ? Re C43A 1.97(3) . ? Re N8 2.185(8) . ? Re N1 2.187(8) . ? Re ClA 2.316(10) . ? Re Cl 2.421(4) . ? C41 O41 1.124(13) . ? C42 O42 1.137(13) . ? C43 O43 1.16(2) . ? C43A O43A 1.16(3) . ? N1 C2 1.324(12) . ? N1 C6 1.376(13) . ? C2 C3 1.396(14) . ? C3 C4 1.364(15) . ? C4 C5 1.405(14) . ? C5 C6 1.398(14) . ? C5 C14 1.437(15) . ? C6 C7 1.422(13) . ? C7 N8 1.368(13) . ? C7 C12 1.394(14) . ? N8 C9 1.330(13) . ? C9 C10 1.398(15) . ? C10 C11 1.366(15) . ? C11 C12 1.412(14) . ? C12 C13 1.433(15) . ? C13 O40 1.373(13) . ? C13 C14 1.390(15) . ? C14 O15 1.344(13) . ? O15 C16 1.467(13) . ? C16 C17 1.483(16) . ? C17 O18 1.442(14) . ? O18 C19 1.422(13) . ? C19 C20 1.494(16) . ? C20 O21 1.424(13) . ? O21 C22 1.434(13) . ? C22 C23 1.526(16) . ? C23 O24 1.413(14) . ? O24 C25 1.369(13) . ? C25 C26 1.365(16) . ? C25 C30 1.416(16) . ? C26 C27 1.380(16) . ? C27 C28 1.391(17) . ? C28 C29 1.371(16) . ? C29 C30 1.397(16) . ? C30 O31 1.373(13) . ? O31 C32 1.427(14) . ? C32 C33 1.479(16) . ? C33 O34 1.446(13) . ? O34 C35 1.416(13) . ? C35 C36 1.533(16) . ? C36 O37 1.370(16) . ? O37 C38 1.440(14) . ? C38 C39 1.484(16) . ? C39 O40 1.457(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C42 Re C41 91.1(5) . . ? C42 Re C43 87.9(7) . . ? C41 Re C43 90.1(6) . . ? C42 Re C43A 97(2) . . ? C41 Re C43A 89(2) . . ? C43 Re C43A 175(2) . . ? C42 Re N8 173.7(4) . . ? C41 Re N8 95.2(4) . . ? C43 Re N8 92.6(6) . . ? C43A Re N8 83(2) . . ? C42 Re N1 97.8(4) . . ? C41 Re N1 169.7(4) . . ? C43 Re N1 95.6(6) . . ? C43A Re N1 85(2) . . ? N8 Re N1 75.9(3) . . ? C42 Re ClA 91.9(5) . . ? C41 Re ClA 94.1(4) . . ? C43 Re ClA 5.7(7) . . ? C43A Re ClA 171(2) . . ? N8 Re ClA 88.2(4) . . ? N1 Re ClA 91.0(4) . . ? C42 Re Cl 92.5(3) . . ? C41 Re Cl 89.6(3) . . ? C43 Re Cl 179.5(6) . . ? C43A Re Cl 5(2) . . ? N8 Re Cl 87.1(2) . . ? N1 Re Cl 84.7(2) . . ? ClA Re Cl 174.2(3) . . ? O41 C41 Re 174.8(10) . . ? O42 C42 Re 174.7(10) . . ? O43 C43 Re 177.7(15) . . ? O43A C43A Re 164(6) . . ? C2 N1 C6 117.8(8) . . ? C2 N1 Re 127.6(7) . . ? C6 N1 Re 114.5(6) . . ? N1 C2 C3 122.3(9) . . ? C4 C3 C2 120.3(9) . . ? C3 C4 C5 119.2(9) . . ? C6 C5 C4 117.3(9) . . ? C6 C5 C14 120.4(9) . . ? C4 C5 C14 122.3(9) . . ? N1 C6 C5 123.0(8) . . ? N1 C6 C7 117.2(8) . . ? C5 C6 C7 119.8(9) . . ? N8 C7 C12 122.1(9) . . ? N8 C7 C6 117.8(9) . . ? C12 C7 C6 120.1(9) . . ? C9 N8 C7 118.7(9) . . ? C9 N8 Re 126.7(7) . . ? C7 N8 Re 114.6(6) . . ? N8 C9 C10 121.8(9) . . ? C11 C10 C9 120.8(9) . . ? C10 C11 C12 118.1(10) . . ? C7 C12 C11 118.6(9) . . ? C7 C12 C13 119.6(9) . . ? C11 C12 C13 121.8(10) . . ? O40 C13 C14 119.8(10) . . ? O40 C13 C12 118.3(9) . . ? C14 C13 C12 120.4(10) . . ? O15 C14 C13 124.3(10) . . ? O15 C14 C5 117.0(9) . . ? C13 C14 C5 118.8(10) . . ? C14 O15 C16 116.2(8) . . ? O15 C16 C17 107.6(9) . . ? O18 C17 C16 109.9(9) . . ? C19 O18 C17 112.8(8) . . ? O18 C19 C20 110.5(9) . . ? O21 C20 C19 110.5(9) . . ? C20 O21 C22 110.8(8) . . ? O21 C22 C23 109.5(8) . . ? O24 C23 C22 109.2(9) . . ? C25 O24 C23 117.6(9) . . ? C26 C25 O24 117.7(10) . . ? C26 C25 C30 119.3(10) . . ? O24 C25 C30 122.9(11) . . ? C25 C26 C27 122.8(10) . . ? C26 C27 C28 117.5(11) . . ? C29 C28 C27 121.5(11) . . ? C28 C29 C30 120.4(11) . . ? O31 C30 C29 123.7(10) . . ? O31 C30 C25 117.9(10) . . ? C29 C30 C25 118.4(11) . . ? C30 O31 C32 116.4(8) . . ? O31 C32 C33 108.7(10) . . ? O34 C33 C32 110.9(9) . . ? C35 O34 C33 113.7(9) . . ? O34 C35 C36 106.5(10) . . ? O37 C36 C35 109.4(11) . . ? C36 O37 C38 109.9(10) . . ? O37 C38 C39 107.7(10) . . ? O40 C39 C38 110.2(10) . . ? C13 O40 C39 117.8(8) . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 67.83 _diffrn_measured_fraction_theta_full 0.859 _refine_diff_density_max 1.761 _refine_diff_density_min -2.142 _refine_diff_density_rms 0.172 #=END data_aristotm _database_code_depnum_ccdc_archive 'CCDC 253591' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H38 Cl F6 K0 N2 Na O13 P Re' _chemical_formula_weight 1060.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.908(4) _cell_length_b 17.748(4) _cell_length_c 27.982(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.70(3) _cell_angle_gamma 90.00 _cell_volume 8849(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 2.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50139 _diffrn_reflns_av_R_equivalents 0.1465 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10159 _reflns_number_gt 5418 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1417P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10159 _refine_ls_number_parameters 578 _refine_ls_number_restraints 330 _refine_ls_R_factor_all 0.1384 _refine_ls_R_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.2398 _refine_ls_wR_factor_gt 0.2118 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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 0.24152(2) 0.76344(3) 0.636158(14) 0.05784(19) Uani 1 1 d . . . N1 N 0.3041(5) 0.8177(5) 0.6963(3) 0.066(2) Uani 1 1 d . . . C2 C 0.3518(7) 0.8739(6) 0.6949(4) 0.072(3) Uani 1 1 d . . . H2 H 0.3592 0.8946 0.6644 0.086 Uiso 1 1 calc R . . C3 C 0.3930(7) 0.9055(8) 0.7361(5) 0.091(4) Uani 1 1 d . . . H3 H 0.4256 0.9472 0.7334 0.109 Uiso 1 1 calc R . . C4 C 0.3838(10) 0.8727(11) 0.7816(5) 0.133(7) Uani 1 1 d . . . H4 H 0.4028 0.8968 0.8106 0.160 Uiso 1 1 calc R . . C5 C 0.3444(9) 0.8016(10) 0.7821(5) 0.103(5) Uani 1 1 d . . . C6 C 0.2983(9) 0.7852(10) 0.7395(5) 0.113(6) Uani 1 1 d . . . C7 C 0.2499(7) 0.7223(8) 0.7415(5) 0.079(4) Uani 1 1 d . . . N8 N 0.2056(6) 0.7075(7) 0.6986(3) 0.087(3) Uani 1 1 d . . . C9 C 0.1532(8) 0.6533(8) 0.6999(4) 0.092(4) Uani 1 1 d . . . H9 H 0.1245 0.6403 0.6707 0.110 Uiso 1 1 calc R . . C10 C 0.1389(10) 0.6160(10) 0.7406(5) 0.121(7) Uani 1 1 d . . . H10 H 0.0978 0.5819 0.7399 0.145 Uiso 1 1 calc R . . C11 C 0.1820(8) 0.6272(8) 0.7807(5) 0.096(4) Uani 1 1 d . . . H11 H 0.1746 0.5979 0.8083 0.115 Uiso 1 1 calc R . . C12 C 0.2402(7) 0.6832(9) 0.7834(4) 0.086(4) Uani 1 1 d . . . C13 C 0.2909(10) 0.7026(11) 0.8271(5) 0.112(6) Uani 1 1 d . A . C14 C 0.3358(9) 0.7593(9) 0.8253(5) 0.096(5) Uani 1 1 d . . . O15 O 0.3848(6) 0.7784(7) 0.8685(3) 0.112(4) Uani 1 1 d . . . C16 C 0.4585(10) 0.7620(11) 0.8696(6) 0.141(7) Uani 1 1 d DU . . H16A H 0.4800 0.7855 0.8419 0.169 Uiso 1 1 calc R . . H16B H 0.4659 0.7069 0.8681 0.169 Uiso 1 1 calc R . . C17 C 0.4957(8) 0.7933(12) 0.9162(5) 0.136(6) Uani 1 1 d DU . . H17A H 0.5511 0.7915 0.9169 0.163 Uiso 1 1 calc R . . H17B H 0.4799 0.8459 0.9212 0.163 Uiso 1 1 calc R . . O18 O 0.4693(6) 0.7431(7) 0.9525(4) 0.129(4) Uani 1 1 d DU . . C19 C 0.5016(10) 0.7650(12) 0.9962(6) 0.145(7) Uani 1 1 d DU . . H19A H 0.4893 0.8185 1.0015 0.174 Uiso 1 1 calc R . . H19B H 0.5569 0.7608 0.9968 0.174 Uiso 1 1 calc R . . C20 C 0.4748(9) 0.7168(13) 1.0370(6) 0.174(8) Uani 1 1 d DU . . H20A H 0.4884 0.6635 1.0317 0.209 Uiso 1 1 calc R . . H20B H 0.5018 0.7331 1.0678 0.209 Uiso 1 1 calc R . . O21 O 0.3975(6) 0.7211(5) 1.0406(3) 0.087(3) Uani 1 1 d D . . C22 C 0.3782(9) 0.7803(7) 1.0722(4) 0.125(7) Uani 1 1 d DU . . H22C H 0.3242 0.7927 1.0669 0.150 Uiso 1 1 calc R . . H22D H 0.4080 0.8263 1.0678 0.150 Uiso 1 1 calc R . . C23 C 0.3984(13) 0.7456(11) 1.1225(5) 0.143(8) Uani 1 1 d D . . H23C H 0.4484 0.7212 1.1244 0.171 Uiso 1 1 calc R . . H23D H 0.3994 0.7851 1.1476 0.171 Uiso 1 1 calc R . . O24 O 0.3440(5) 0.6936(6) 1.1288(3) 0.092(3) Uani 1 1 d D . . C25 C 0.3454(10) 0.6567(10) 1.1693(5) 0.112(5) Uani 1 1 d . A . C26 C 0.3896(10) 0.6717(10) 1.2075(5) 0.113(5) Uani 1 1 d . . . H26 H 0.4225 0.7136 1.2072 0.136 Uiso 1 1 calc R . . C27 C 0.3905(10) 0.6253(14) 1.2518(6) 0.134(7) Uani 1 1 d . . . H27 H 0.4230 0.6378 1.2795 0.161 Uiso 1 1 calc R . . C28 C 0.3445(12) 0.5654(16) 1.2520(7) 0.156(9) Uani 1 1 d . . . H28 H 0.3447 0.5336 1.2793 0.187 Uiso 1 1 calc R . . C29 C 0.2941(10) 0.5511(12) 1.2083(5) 0.129(6) Uani 1 1 d . A . H29 H 0.2588 0.5110 1.2076 0.154 Uiso 1 1 calc R . . C30 C 0.2981(9) 0.5952(10) 1.1689(5) 0.107(5) Uani 1 1 d . . . O31A O 0.2462(15) 0.5893(13) 1.1281(6) 0.100(8) Uani 0.67(4) 1 d PDU A 2 O31B O 0.262(2) 0.560(3) 1.1334(15) 0.090(12) Uani 0.33(4) 1 d PDU A 1 C32 C 0.2146(11) 0.5121(11) 1.1205(7) 0.138(7) Uani 1 1 d D . . H32A H 0.1660 0.5277 1.1313 0.166 Uiso 0.33(4) 1 calc PR A 1 H32B H 0.2290 0.4636 1.1362 0.166 Uiso 0.33(4) 1 calc PR A 1 H32C H 0.2551 0.4753 1.1165 0.166 Uiso 0.67(4) 1 d PR A 2 H32D H 0.1859 0.4953 1.1470 0.166 Uiso 0.67(4) 1 d PR A 2 C33A C 0.205(4) 0.501(3) 1.0663(9) 0.098(14) Uani 0.33(4) 1 d PDU A 1 H33A H 0.2095 0.4452 1.0638 0.118 Uiso 0.33(4) 1 calc PR A 1 H33B H 0.1508 0.5108 1.0587 0.118 Uiso 0.33(4) 1 calc PR A 1 C33B C 0.1638(12) 0.5197(13) 1.0740(5) 0.072(7) Uani 0.67(4) 1 d PDU A 2 H33C H 0.1363 0.5682 1.0721 0.086 Uiso 0.67(4) 1 calc PR A 2 H33D H 0.1277 0.4774 1.0692 0.086 Uiso 0.67(4) 1 calc PR A 2 O34 O 0.2243(7) 0.5165(6) 1.0383(4) 0.105(4) Uani 1 1 d . . . C35 C 0.1829(7) 0.5157(8) 0.9910(4) 0.087(4) Uani 1 1 d D A . H35A H 0.1488 0.5595 0.9868 0.104 Uiso 1 1 calc R . . H35B H 0.1530 0.4689 0.9861 0.104 Uiso 1 1 calc R . . C36 C 0.2423(9) 0.5195(9) 0.9563(5) 0.110(5) Uani 1 1 d D . . H36A H 0.2789 0.4780 0.9629 0.132 Uiso 1 1 calc R A . H36B H 0.2189 0.5142 0.9229 0.132 Uiso 1 1 calc R . . O37 O 0.2801(4) 0.5915(5) 0.9624(3) 0.081(2) Uani 1 1 d . A . C38 C 0.3415(10) 0.5958(11) 0.9333(5) 0.124(6) Uani 1 1 d D . . H38A H 0.3726 0.5499 0.9386 0.148 Uiso 1 1 calc R A . H38B H 0.3732 0.6396 0.9438 0.148 Uiso 1 1 calc R . . C39 C 0.3169(9) 0.6035(12) 0.8791(5) 0.122(6) Uani 1 1 d D A . H39A H 0.3614 0.6008 0.8608 0.146 Uiso 1 1 calc R . . H39B H 0.2826 0.5618 0.8683 0.146 Uiso 1 1 calc R . . O40 O 0.2823(6) 0.6693(6) 0.8710(3) 0.092(3) Uani 1 1 d . . . C41 C 0.1594(9) 0.8455(12) 0.6313(5) 0.092(6) Uani 1 1 d . . . O41 O 0.1235(7) 0.8770(8) 0.6276(4) 0.109(4) Uani 1 1 d . . . C42 C 0.1840(7) 0.7047(8) 0.5864(4) 0.074(3) Uani 1 1 d . . . O42 O 0.1501(5) 0.6711(5) 0.5575(3) 0.089(3) Uani 1 1 d . . . C43 C 0.2867(7) 0.8110(7) 0.5847(4) 0.072(3) Uani 1 1 d . . . O43 O 0.3141(5) 0.8413(6) 0.5548(3) 0.097(3) Uani 1 1 d . . . Cl1 Cl 0.34601(19) 0.6685(2) 0.64524(13) 0.0994(11) Uani 1 1 d . . . Na1 Na 0.3038(3) 0.6234(4) 1.04819(19) 0.1052(18) Uani 1 1 d . A . O100 O 0.4074(10) 0.5349(11) 1.0628(8) 0.248(9) Uani 1 1 d U . . P1 P 0.02335(15) 0.46795(17) 0.36472(9) 0.0630(7) Uani 1 1 d D . . F1A F 0.037(2) 0.3808(7) 0.3680(5) 0.170(16) Uani 0.40 1 d PDU B 1 F2A F -0.0635(7) 0.4529(19) 0.3627(5) 0.170(16) Uani 0.40 1 d PDU B 1 F4A F 0.0193(13) 0.5561(5) 0.3647(4) 0.059(5) Uani 0.40 1 d PDU B 1 F5A F 0.1108(6) 0.474(3) 0.3695(5) 0.155(17) Uani 0.40 1 d PDU B 1 F1B F -0.0035(9) 0.3837(6) 0.3665(5) 0.129(8) Uani 0.60 1 d PDU B 2 F2B F -0.0641(5) 0.4872(9) 0.3606(4) 0.085(5) Uani 0.60 1 d PDU B 2 F4B F 0.0471(15) 0.5527(7) 0.3666(5) 0.177(13) Uani 0.60 1 d PDU B 2 F5B F 0.1084(6) 0.4484(18) 0.3696(5) 0.170(13) Uani 0.60 1 d PDU B 2 F3 F 0.0251(5) 0.4695(5) 0.4219(2) 0.128(3) Uani 1 1 d DU B . F6 F 0.0198(4) 0.4652(5) 0.3089(2) 0.119(3) Uani 1 1 d DU B . O200 O 0.2015(4) 0.7031(5) 1.0428(3) 0.078(2) Uani 1 1 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 0.0602(3) 0.0652(3) 0.0473(2) 0.00509(19) 0.00103(17) -0.0038(2) N1 0.067(5) 0.076(7) 0.055(5) 0.007(4) 0.004(4) -0.028(5) C2 0.087(8) 0.063(7) 0.063(7) 0.000(5) 0.000(6) -0.015(6) C3 0.086(9) 0.088(10) 0.098(10) -0.001(8) 0.007(7) -0.028(7) C4 0.168(16) 0.162(17) 0.069(9) -0.023(9) 0.013(9) -0.104(14) C5 0.108(11) 0.135(14) 0.067(8) -0.019(8) 0.017(8) -0.040(10) C6 0.123(12) 0.154(14) 0.062(8) -0.009(8) 0.009(8) -0.096(11) C7 0.073(8) 0.092(10) 0.073(8) -0.008(7) 0.008(6) -0.025(7) N8 0.088(7) 0.131(9) 0.039(5) -0.008(5) -0.003(5) -0.045(7) C9 0.111(10) 0.116(11) 0.050(6) -0.011(6) 0.011(6) -0.067(9) C10 0.152(14) 0.146(15) 0.061(8) -0.006(8) -0.012(9) -0.089(12) C11 0.105(10) 0.090(10) 0.093(10) 0.020(8) 0.007(8) -0.031(8) C12 0.081(8) 0.119(12) 0.057(7) -0.001(7) 0.008(6) -0.012(8) C13 0.134(13) 0.146(14) 0.057(8) -0.032(8) 0.016(8) -0.068(12) C14 0.106(11) 0.120(12) 0.062(8) -0.021(7) 0.008(7) -0.038(9) O15 0.113(8) 0.158(10) 0.066(6) -0.028(6) 0.018(5) -0.045(7) C16 0.093(12) 0.24(2) 0.090(8) 0.030(10) -0.005(9) 0.064(11) C17 0.052(7) 0.232(17) 0.121(9) 0.044(10) -0.004(7) -0.032(9) O18 0.073(6) 0.225(13) 0.086(6) 0.029(6) -0.004(5) -0.021(6) C19 0.079(9) 0.254(19) 0.102(8) -0.006(10) 0.005(8) -0.066(11) C20 0.123(14) 0.30(2) 0.104(10) 0.075(14) 0.005(11) 0.040(15) O21 0.103(7) 0.098(7) 0.062(5) -0.015(4) 0.015(5) -0.029(5) C22 0.162(16) 0.135(15) 0.075(9) -0.007(9) -0.009(10) -0.083(13) C23 0.17(2) 0.19(2) 0.069(10) -0.030(10) 0.012(12) -0.062(15) O24 0.106(7) 0.104(7) 0.064(5) 0.017(5) 0.000(5) -0.030(6) C25 0.130(13) 0.124(14) 0.072(9) 0.022(9) -0.028(9) -0.035(11) C26 0.138(14) 0.122(14) 0.080(10) 0.010(9) 0.020(10) 0.002(11) C27 0.108(13) 0.21(2) 0.086(11) -0.013(12) 0.006(9) -0.037(14) C28 0.150(18) 0.23(3) 0.085(12) -0.030(14) 0.005(12) -0.036(18) C29 0.148(15) 0.163(18) 0.079(10) 0.022(11) 0.031(10) 0.030(13) C30 0.116(12) 0.135(14) 0.067(9) 0.022(9) -0.013(8) -0.015(11) O31A 0.125(15) 0.092(14) 0.073(9) 0.051(9) -0.043(9) -0.037(12) O31B 0.098(19) 0.10(3) 0.07(2) -0.018(19) -0.029(15) 0.050(18) C32 0.156(16) 0.112(15) 0.143(16) 0.057(13) -0.008(13) -0.052(13) C33A 0.09(3) 0.05(2) 0.15(3) -0.01(2) 0.03(3) -0.04(2) C33B 0.076(14) 0.090(14) 0.054(10) -0.017(8) 0.030(9) -0.035(11) O34 0.129(9) 0.084(7) 0.105(8) 0.044(6) 0.016(7) -0.001(6) C35 0.101(10) 0.081(9) 0.077(8) -0.015(7) -0.001(7) -0.020(7) C36 0.138(14) 0.105(12) 0.090(10) -0.030(9) 0.019(10) 0.008(10) O37 0.069(5) 0.112(7) 0.065(5) -0.006(4) 0.015(4) -0.029(5) C38 0.151(15) 0.135(15) 0.083(10) 0.011(10) 0.003(10) 0.014(12) C39 0.103(12) 0.18(2) 0.077(10) 0.017(11) -0.003(8) 0.009(12) O40 0.118(7) 0.096(7) 0.063(5) 0.013(5) 0.020(5) 0.008(6) C41 0.069(10) 0.17(2) 0.044(7) -0.012(10) 0.008(7) -0.028(10) O41 0.128(11) 0.119(9) 0.079(7) -0.017(6) 0.008(7) 0.039(8) C42 0.090(9) 0.076(8) 0.055(7) 0.001(6) 0.009(6) 0.005(7) O42 0.110(7) 0.092(7) 0.063(5) -0.012(5) -0.008(5) -0.012(5) C43 0.071(7) 0.088(9) 0.056(6) 0.010(6) 0.003(6) 0.014(6) O43 0.087(6) 0.113(8) 0.093(6) 0.042(6) 0.021(5) -0.007(5) Cl1 0.085(2) 0.128(3) 0.085(2) 0.024(2) 0.0023(17) 0.002(2) Na1 0.122(4) 0.111(5) 0.082(3) -0.012(3) 0.001(3) -0.020(4) O100 0.191(15) 0.197(18) 0.36(3) -0.062(19) 0.040(17) -0.001(14) P1 0.0595(17) 0.075(2) 0.0540(15) -0.0034(13) 0.0016(12) 0.0164(14) F1A 0.28(4) 0.11(2) 0.12(2) -0.050(16) 0.01(2) 0.10(2) F2A 0.15(2) 0.18(3) 0.20(3) -0.14(2) 0.118(19) -0.116(19) F4A 0.087(13) 0.035(9) 0.054(9) 0.001(7) -0.004(8) 0.020(8) F5A 0.06(2) 0.27(4) 0.13(2) -0.09(2) -0.014(17) 0.06(2) F1B 0.101(12) 0.088(11) 0.182(17) 0.044(11) -0.071(10) -0.005(9) F2B 0.067(8) 0.095(13) 0.090(9) -0.008(7) -0.010(7) 0.002(7) F4B 0.21(3) 0.16(2) 0.18(2) -0.027(16) 0.072(16) -0.095(18) F5B 0.051(13) 0.25(3) 0.21(2) -0.136(19) -0.021(13) 0.017(13) F3 0.175(8) 0.146(8) 0.059(4) 0.009(5) 0.003(5) 0.020(7) F6 0.156(7) 0.147(8) 0.056(4) -0.016(4) 0.023(4) -0.023(6) O200 0.081(5) 0.092(6) 0.058(4) -0.013(4) -0.006(4) -0.003(5) _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 C43 1.916(12) . ? Re1 C42 1.949(14) . ? Re1 C41 2.06(2) . ? Re1 N1 2.156(8) . ? Re1 N8 2.162(9) . ? Re1 Cl1 2.513(4) . ? N1 C2 1.317(13) . ? N1 C6 1.353(15) . ? C2 C3 1.420(16) . ? C3 C4 1.425(18) . ? C4 C5 1.45(2) . ? C5 C6 1.411(18) . ? C5 C14 1.44(2) . ? C6 C7 1.418(17) . ? C7 N8 1.396(15) . ? C7 C12 1.389(17) . ? N8 C9 1.348(14) . ? C9 C10 1.363(17) . ? C10 C11 1.312(18) . ? C11 C12 1.437(18) . ? C12 C13 1.489(18) . ? C13 C14 1.292(19) . ? C13 O40 1.385(16) . ? C14 O15 1.462(17) . ? O15 C16 1.348(19) . ? C16 C17 1.511(15) . ? C17 O18 1.465(14) . ? O18 C19 1.36(2) . ? C19 C20 1.541(15) . ? C20 O21 1.402(13) . ? O21 C22 1.437(13) . ? O21 Na1 2.436(10) . ? C22 C23 1.547(15) . ? C22 Na1 3.131(14) . ? C23 O24 1.37(2) . ? O24 C25 1.308(16) . ? O24 Na1 2.614(10) . ? C25 C26 1.292(19) . ? C25 C30 1.38(2) . ? C26 C27 1.49(2) . ? C27 C28 1.35(3) . ? C28 C29 1.47(2) . ? C29 C30 1.36(2) . ? C30 O31B 1.29(3) . ? C30 O31A 1.403(19) . ? O31A C32 1.49(2) . ? O31A Na1 2.62(2) . ? O31B C32 1.23(4) . ? O31B Na1 2.81(6) . ? C32 C33B 1.519(16) . ? C32 C33A 1.523(17) . ? C33A O34 0.93(3) . ? C33A Na1 2.88(4) . ? C33B O34 1.55(2) . ? O34 C35 1.450(15) . ? O34 Na1 2.372(12) . ? C35 C36 1.511(13) . ? C36 O37 1.449(16) . ? O37 C38 1.434(18) . ? O37 Na1 2.462(9) . ? C38 C39 1.542(13) . ? C39 O40 1.33(2) . ? C41 O41 0.850(18) . ? C42 O42 1.131(14) . ? C43 O43 1.145(13) . ? Na1 O200 2.308(10) . ? Na1 O100 2.43(2) . ? P1 F5B 1.554(10) . ? P1 F6 1.557(6) . ? P1 F5A 1.561(11) . ? P1 F4B 1.562(10) . ? P1 F4A 1.566(10) . ? P1 F1A 1.569(11) . ? P1 F1B 1.572(10) . ? P1 F2A 1.573(11) . ? P1 F2B 1.595(9) . ? P1 F3 1.598(7) . ? 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 C43 Re1 C42 86.1(5) . . ? C43 Re1 C41 89.5(6) . . ? C42 Re1 C41 90.4(6) . . ? C43 Re1 N1 99.5(4) . . ? C42 Re1 N1 173.6(4) . . ? C41 Re1 N1 92.8(5) . . ? C43 Re1 N8 172.3(4) . . ? C42 Re1 N8 98.8(4) . . ? C41 Re1 N8 96.3(6) . . ? N1 Re1 N8 75.4(3) . . ? C43 Re1 Cl1 90.3(3) . . ? C42 Re1 Cl1 92.8(4) . . ? C41 Re1 Cl1 176.8(5) . . ? N1 Re1 Cl1 84.1(3) . . ? N8 Re1 Cl1 83.6(4) . . ? C2 N1 C6 117.3(10) . . ? C2 N1 Re1 127.1(7) . . ? C6 N1 Re1 115.3(7) . . ? N1 C2 C3 124.0(11) . . ? C4 C3 C2 117.9(12) . . ? C3 C4 C5 117.7(12) . . ? C6 C5 C14 119.8(13) . . ? C6 C5 C4 114.6(14) . . ? C14 C5 C4 123.8(12) . . ? N1 C6 C5 125.2(11) . . ? N1 C6 C7 118.2(11) . . ? C5 C6 C7 116.1(13) . . ? N8 C7 C12 121.6(11) . . ? N8 C7 C6 114.4(11) . . ? C12 C7 C6 123.7(12) . . ? C9 N8 C7 116.6(10) . . ? C9 N8 Re1 127.9(7) . . ? C7 N8 Re1 114.8(7) . . ? N8 C9 C10 124.0(11) . . ? C11 C10 C9 119.8(13) . . ? C10 C11 C12 120.8(13) . . ? C7 C12 C11 116.9(11) . . ? C7 C12 C13 117.5(12) . . ? C11 C12 C13 125.7(12) . . ? C14 C13 O40 119.4(12) . . ? C14 C13 C12 118.6(14) . . ? O40 C13 C12 121.2(12) . . ? C13 C14 C5 123.8(13) . . ? C13 C14 O15 118.2(13) . . ? C5 C14 O15 117.8(12) . . ? C16 O15 C14 118.2(12) . . ? O15 C16 C17 106.7(13) . . ? O18 C17 C16 103.3(14) . . ? C19 O18 C17 108.1(13) . . ? O18 C19 C20 111.8(14) . . ? O21 C20 C19 114.0(13) . . ? C20 O21 C22 112.5(12) . . ? C20 O21 Na1 131.4(12) . . ? C22 O21 Na1 104.9(7) . . ? O21 C22 C23 102.8(12) . . ? O21 C22 Na1 48.7(6) . . ? C23 C22 Na1 84.1(8) . . ? O24 C23 C22 106.2(13) . . ? C25 O24 C23 119.8(12) . . ? C25 O24 Na1 119.3(10) . . ? C23 O24 Na1 110.6(8) . . ? C26 C25 O24 124.8(16) . . ? C26 C25 C30 119.6(15) . . ? O24 C25 C30 115.5(13) . . ? C25 C26 C27 122.0(17) . . ? C28 C27 C26 119.0(18) . . ? C27 C28 C29 117(2) . . ? C30 C29 C28 120(2) . . ? O31B C30 C29 106(3) . . ? O31B C30 C25 131(3) . . ? C29 C30 C25 122.0(16) . . ? O31B C30 O31A 25.9(16) . . ? C29 C30 O31A 122.2(17) . . ? C25 C30 O31A 114.9(14) . . ? C30 O31A C32 113.3(17) . . ? C30 O31A Na1 113.0(15) . . ? C32 O31A Na1 105.4(14) . . ? C32 O31B C30 147(5) . . ? C32 O31B Na1 105(2) . . ? C30 O31B Na1 108(3) . . ? O31B C32 O31A 23.6(16) . . ? O31B C32 C33B 122(3) . . ? O31A C32 C33B 103.1(14) . . ? O31B C32 C33A 113(3) . . ? O31A C32 C33A 105.6(15) . . ? C33B C32 C33A 33(2) . . ? O34 C33A C32 142(3) . . ? O34 C33A Na1 48.6(18) . . ? C32 C33A Na1 93.6(14) . . ? C32 C33B O34 98.7(15) . . ? C33A O34 C35 125(3) . . ? C33A O34 C33B 29(5) . . ? C35 O34 C33B 105.3(11) . . ? C33A O34 Na1 114.3(19) . . ? C35 O34 Na1 111.2(7) . . ? C33B O34 Na1 110.2(10) . . ? O34 C35 C36 104.9(11) . . ? O37 C36 C35 108.3(10) . . ? C38 O37 C36 110.8(11) . . ? C38 O37 Na1 118.3(8) . . ? C36 O37 Na1 110.5(7) . . ? O37 C38 C39 113.8(13) . . ? O40 C39 C38 109.1(15) . . ? C39 O40 C13 115.7(12) . . ? O41 C41 Re1 175(2) . . ? O42 C42 Re1 179.3(13) . . ? O43 C43 Re1 178.0(12) . . ? O200 Na1 O34 91.1(4) . . ? O200 Na1 O21 96.1(4) . . ? O34 Na1 O21 165.8(4) . . ? O200 Na1 O100 173.4(6) . . ? O34 Na1 O100 86.7(6) . . ? O21 Na1 O100 87.4(6) . . ? O200 Na1 O37 91.1(3) . . ? O34 Na1 O37 70.1(4) . . ? O21 Na1 O37 97.6(3) . . ? O100 Na1 O37 94.0(6) . . ? O200 Na1 O24 85.0(3) . . ? O34 Na1 O24 126.4(4) . . ? O21 Na1 O24 66.6(3) . . ? O100 Na1 O24 91.3(6) . . ? O37 Na1 O24 163.1(4) . . ? O200 Na1 O31A 79.6(7) . . ? O34 Na1 O31A 68.5(5) . . ? O21 Na1 O31A 124.8(5) . . ? O100 Na1 O31A 93.8(9) . . ? O37 Na1 O31A 137.2(5) . . ? O24 Na1 O31A 58.2(4) . . ? O200 Na1 O31B 91.5(8) . . ? O34 Na1 O31B 64.5(7) . . ? O21 Na1 O31B 127.2(7) . . ? O100 Na1 O31B 81.9(9) . . ? O37 Na1 O31B 134.5(7) . . ? O24 Na1 O31B 62.2(7) . . ? O31A Na1 O31B 12.4(8) . . ? O200 Na1 C33A 88.7(16) . . ? O34 Na1 C33A 17.1(5) . . ? O21 Na1 C33A 173.2(12) . . ? O100 Na1 C33A 87.4(16) . . ? O37 Na1 C33A 87.1(5) . . ? O24 Na1 C33A 109.3(5) . . ? O31A Na1 C33A 51.4(5) . . ? O31B Na1 C33A 47.6(7) . . ? O200 Na1 C22 77.7(4) . . ? O34 Na1 C22 167.0(5) . . ? O21 Na1 C22 26.3(3) . . ? O100 Na1 C22 103.7(6) . . ? O37 Na1 C22 116.2(4) . . ? O24 Na1 C22 46.8(3) . . ? O31A Na1 C22 102.5(5) . . ? O31B Na1 C22 108.7(7) . . ? C33A Na1 C22 152.9(8) . . ? F5B P1 F6 91.3(5) . . ? F5B P1 F5A 17(3) . . ? F6 P1 F5A 91.6(6) . . ? F5B P1 F4B 87.2(11) . . ? F6 P1 F4B 92.8(6) . . ? F5A P1 F4B 71(2) . . ? F5B P1 F4A 105.5(16) . . ? F6 P1 F4A 91.9(5) . . ? F5A P1 F4A 89.0(16) . . ? F4B P1 F4A 18.3(16) . . ? F5B P1 F1A 68.0(16) . . ? F6 P1 F1A 91.0(6) . . ? F5A P1 F1A 85(3) . . ? F4B P1 F1A 155.0(16) . . ? F4A P1 F1A 173.0(15) . . ? F5B P1 F1B 94.9(14) . . ? F6 P1 F1B 91.1(5) . . ? F5A P1 F1B 111.4(18) . . ? F4B P1 F1B 175.6(9) . . ? F4A P1 F1B 159.3(11) . . ? F1A P1 F1B 26.9(14) . . ? F5B P1 F2A 157.1(19) . . ? F6 P1 F2A 90.9(6) . . ? F5A P1 F2A 173.3(17) . . ? F4B P1 F2A 115.4(16) . . ? F4A P1 F2A 97.1(16) . . ? F1A P1 F2A 89.2(15) . . ? F1B P1 F2A 62.3(13) . . ? F5B P1 F2B 179.0(10) . . ? F6 P1 F2B 89.5(5) . . ? F5A P1 F2B 164(2) . . ? F4B P1 F2B 93.3(12) . . ? F4A P1 F2B 75.0(11) . . ? F1A P1 F2B 111.4(15) . . ? F1B P1 F2B 84.5(8) . . ? F2A P1 F2B 22.2(14) . . ? F5B P1 F3 89.7(5) . . ? F6 P1 F3 178.5(4) . . ? F5A P1 F3 89.6(6) . . ? F4B P1 F3 88.4(5) . . ? F4A P1 F3 88.8(5) . . ? F1A P1 F3 88.4(5) . . ? F1B P1 F3 87.7(5) . . ? F2A P1 F3 87.7(6) . . ? F2B P1 F3 89.5(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.534 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.220 #=END data_imw96m _database_code_depnum_ccdc_archive 'CCDC 253592' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 Cl2 N8 O12 Ru' _chemical_formula_weight 1032.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.411(8) _cell_length_b 13.877(12) _cell_length_c 19.278(17) _cell_angle_alpha 85.394(16) _cell_angle_beta 83.010(15) _cell_angle_gamma 74.521(16) _cell_volume 2405(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1003 _cell_measurement_theta_min 4.263 _cell_measurement_theta_max 50.756 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13696 _diffrn_reflns_av_R_equivalents 0.2412 _diffrn_reflns_av_sigmaI/netI 0.4123 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6253 _reflns_number_gt 2323 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1626P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.27(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6253 _refine_ls_number_parameters 526 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2673 _refine_ls_R_factor_gt 0.1410 _refine_ls_wR_factor_ref 0.4107 _refine_ls_wR_factor_gt 0.3135 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ru01 Ru 0.52808(17) 0.53347(16) 0.27358(9) 0.0623(11) Uani 1 1 d . . . O1 O 0.3682(12) 0.6669(10) -0.0450(7) 0.048(4) Uani 1 1 d . . . O2 O 0.0785(12) 0.7357(10) 0.0344(7) 0.056(4) Uani 1 1 d . . . O3 O -0.1338(17) 1.0279(13) -0.1649(10) 0.098(6) Uani 1 1 d . . . O4 O -0.3448(13) 0.9160(12) -0.1340(8) 0.060(4) Uani 1 1 d . . . O5 O 0.2809(15) 0.8693(12) -0.0323(10) 0.076(5) Uani 1 1 d . . . O6 O -0.2321(15) 0.7931(11) 0.0853(8) 0.064(4) Uani 1 1 d . . . N5 N 0.3218(16) 0.6063(15) 0.2426(8) 0.065(6) Uani 1 1 d . . . N6 N 0.5798(15) 0.5444(11) 0.1673(8) 0.045(4) Uani 1 1 d . . . N7 N 0.1298(19) 0.8938(16) -0.1188(11) 0.079(6) Uani 1 1 d . . . H7 H 0.0872 0.8633 -0.1436 0.095 Uiso 1 1 calc R . . N8 N -0.2406(15) 0.7580(12) -0.0262(8) 0.051(5) Uani 1 1 d . . . H8 H -0.1920 0.7296 -0.0631 0.062 Uiso 1 1 calc R . . N1 N 0.5180(6) 0.3896(5) 0.2633(3) 0.052(5) Uani 1 1 d G . . C1 C 0.4026(7) 0.3639(6) 0.2371(4) 0.057(6) Uani 1 1 d G . . H1 H 0.3208 0.4137 0.2243 0.068 Uiso 1 1 calc R . . C2 C 0.4095(9) 0.2638(7) 0.2299(4) 0.081(8) Uani 1 1 d G . . H2 H 0.3322 0.2467 0.2123 0.097 Uiso 1 1 calc R . . C3 C 0.5318(10) 0.1895(6) 0.2489(5) 0.090(8) Uani 1 1 d G . . H3 H 0.5364 0.1225 0.2441 0.108 Uiso 1 1 calc R . . C4 C 0.6472(9) 0.2152(5) 0.2751(4) 0.075(7) Uani 1 1 d G . . H4 H 0.7290 0.1654 0.2878 0.090 Uiso 1 1 calc R . . C5 C 0.6404(7) 0.3152(5) 0.2823(3) 0.053(6) Uani 1 1 d G . . N2 N 0.7337(5) 0.4518(5) 0.2993(3) 0.063(6) Uani 1 1 d G . . C6 C 0.7603(6) 0.3483(5) 0.3005(3) 0.075(8) Uani 1 1 d G . . C7 C 0.8925(6) 0.2875(5) 0.3215(4) 0.093(9) Uani 1 1 d G . . H7' H 0.9103 0.2182 0.3223 0.112 Uiso 1 1 calc R . . C8 C 0.9982(5) 0.3302(6) 0.3414(4) 0.068(7) Uani 1 1 d G . . H8' H 1.0867 0.2896 0.3554 0.082 Uiso 1 1 calc R . . C9 C 0.9717(5) 0.4338(6) 0.3402(4) 0.067(7) Uani 1 1 d G . . H9 H 1.0424 0.4624 0.3535 0.080 Uiso 1 1 calc R . . C10 C 0.8394(5) 0.4946(5) 0.3192(3) 0.071(7) Uani 1 1 d G . . H10 H 0.8217 0.5638 0.3184 0.085 Uiso 1 1 calc R . . N3 N 0.4498(5) 0.5415(5) 0.3768(3) 0.066(5) Uani 1 1 d G . . C11 C 0.3861(6) 0.4719(6) 0.4153(3) 0.074(7) Uani 1 1 d G . . H11 H 0.3960 0.4097 0.3976 0.088 Uiso 1 1 calc R . . C12 C 0.3074(7) 0.4951(7) 0.4803(3) 0.075(8) Uani 1 1 d G . . H12 H 0.2647 0.4485 0.5061 0.090 Uiso 1 1 calc R . . C13 C 0.2925(8) 0.5880(8) 0.5067(4) 0.083(9) Uani 1 1 d G . . H13 H 0.2398 0.6036 0.5502 0.100 Uiso 1 1 calc R . . C14 C 0.3562(7) 0.6576(7) 0.4681(4) 0.084(8) Uani 1 1 d G . . H14 H 0.3463 0.7198 0.4858 0.101 Uiso 1 1 calc R . . C15 C 0.4349(6) 0.6344(5) 0.4032(3) 0.076(8) Uani 1 1 d G . . N4 N 0.5519(6) 0.6708(5) 0.2912(4) 0.060(5) Uani 1 1 d G . . C16 C 0.5004(7) 0.7006(5) 0.3589(4) 0.065(7) Uani 1 1 d G . . C17 C 0.5200(8) 0.7891(5) 0.3803(5) 0.081(8) Uani 1 1 d G . . H17 H 0.4855 0.8090 0.4255 0.097 Uiso 1 1 calc R . . C18 C 0.5911(10) 0.8477(5) 0.3341(6) 0.092(9) Uani 1 1 d G . . H18 H 0.6042 0.9069 0.3484 0.111 Uiso 1 1 calc R . . C19 C 0.6426(10) 0.8178(5) 0.2665(6) 0.065(7) Uani 1 1 d G . . H19 H 0.6902 0.8571 0.2356 0.078 Uiso 1 1 calc R . . C20 C 0.6230(8) 0.7294(5) 0.2450(4) 0.066(7) Uani 1 1 d G . . H20 H 0.6575 0.7094 0.1998 0.079 Uiso 1 1 calc R . . C21 C 0.196(2) 0.6313(17) 0.2804(12) 0.062(6) Uani 1 1 d . . . H21 H 0.1937 0.6152 0.3282 0.075 Uiso 1 1 calc R . . C22 C 0.060(2) 0.6826(18) 0.2527(12) 0.065(7) Uani 1 1 d . . . H22 H -0.0260 0.7037 0.2826 0.077 Uiso 1 1 calc R . . C23 C 0.0581(19) 0.7003(15) 0.1825(12) 0.055(6) Uani 1 1 d . . . H23 H -0.0295 0.7307 0.1628 0.066 Uiso 1 1 calc R . . C24 C 0.1957(18) 0.6704(15) 0.1404(11) 0.050(6) Uani 1 1 d . . . C25 C 0.3204(18) 0.6209(17) 0.1726(11) 0.054(6) Uani 1 1 d . . . C26 C 0.462(2) 0.5916(16) 0.1320(11) 0.055(6) Uani 1 1 d . . . C27 C 0.471(2) 0.6070(15) 0.0579(11) 0.052(6) Uani 1 1 d . . . C28 C 0.6154(17) 0.5753(15) 0.0232(10) 0.048(5) Uani 1 1 d . . . H28 H 0.6301 0.5853 -0.0252 0.057 Uiso 1 1 calc R . . C29 C 0.7326(19) 0.5307(15) 0.0591(11) 0.050(6) Uani 1 1 d . . . H29 H 0.8259 0.5064 0.0351 0.060 Uiso 1 1 calc R . . C30 C 0.7145(19) 0.5214(15) 0.1289(10) 0.047(5) Uani 1 1 d . . . H30 H 0.7985 0.4980 0.1525 0.056 Uiso 1 1 calc R . . C31 C 0.2089(18) 0.6853(14) 0.0655(11) 0.047(5) Uani 1 1 d . . . C32 C 0.3395(18) 0.6605(14) 0.0250(11) 0.043(5) Uani 1 1 d . . . C33 C 0.263(2) 0.730(2) -0.0883(12) 0.080(9) Uani 1 1 d . . . H33A H 0.1723 0.7089 -0.0810 0.096 Uiso 1 1 calc R . . H33B H 0.3023 0.7210 -0.1369 0.096 Uiso 1 1 calc R . . C34 C 0.226(2) 0.8402(18) -0.0757(12) 0.050(6) Uani 1 1 d . . . C35 C 0.097(3) 0.999(2) -0.1244(15) 0.090(9) Uani 1 1 d . . . H35A H 0.1554 1.0205 -0.0938 0.108 Uiso 1 1 calc R . . H35B H 0.1273 1.0191 -0.1720 0.108 Uiso 1 1 calc R . . C36 C -0.051(4) 1.048(2) -0.1080(18) 0.123(12) Uani 1 1 d . . . H36A H -0.0628 1.1197 -0.1063 0.147 Uiso 1 1 calc R . . H36B H -0.0888 1.0236 -0.0629 0.147 Uiso 1 1 calc R . . C37 C -0.282(3) 1.078(2) -0.1481(15) 0.098(9) Uiso 1 1 d . . . H37A H -0.3055 1.1432 -0.1730 0.118 Uiso 1 1 calc R . . H37B H -0.3024 1.0879 -0.0982 0.118 Uiso 1 1 calc R . . C38 C -0.373(3) 1.011(2) -0.1705(14) 0.085(8) Uani 1 1 d . . . H38A H -0.4779 1.0447 -0.1620 0.102 Uiso 1 1 calc R . . H38B H -0.3503 1.0021 -0.2203 0.102 Uiso 1 1 calc R . . C39 C -0.397(2) 0.9156(18) -0.0624(13) 0.065(7) Uani 1 1 d . . . H39A H -0.4995 0.9551 -0.0571 0.078 Uiso 1 1 calc R . . H39B H -0.3399 0.9479 -0.0379 0.078 Uiso 1 1 calc R . . C40 C -0.3896(18) 0.8160(18) -0.0293(11) 0.060(7) Uani 1 1 d . . . H40A H -0.4398 0.8228 0.0178 0.072 Uiso 1 1 calc R . . H40B H -0.4409 0.7813 -0.0554 0.072 Uiso 1 1 calc R . . C41 C -0.1737(19) 0.7463(16) 0.0329(11) 0.045(5) Uani 1 1 d . . . C42 C -0.0259(19) 0.6764(16) 0.0318(12) 0.063(6) Uani 1 1 d . . . H42A H -0.0217 0.6289 0.0718 0.076 Uiso 1 1 calc R . . H42B H -0.0028 0.6395 -0.0106 0.076 Uiso 1 1 calc R . . Cl1 Cl 0.2399(12) 0.8973(8) 0.5420(5) 0.166(5) Uani 1 1 d . . . Cl2 Cl 0.0974(5) 0.4168(4) 0.1329(3) 0.0626(18) Uani 1 1 d . . . O2W O 0.9463(15) 0.7971(11) 0.8147(8) 0.070(4) Uani 1 1 d . . . O3W O 0.921(3) 0.719(2) 0.4383(14) 0.053(5) Uiso 0.51(2) 1 d PU A 1 O3W' O 0.921(3) 0.655(3) 0.4189(14) 0.052(5) Uiso 0.49(2) 1 d PU A 2 O4W O 0.373(3) 0.223(3) 0.4244(14) 0.135(17) Uani 0.70(4) 1 d P B 1 O4W' O 0.438(8) 0.076(5) 0.425(4) 0.14(4) Uani 0.30(4) 1 d P B 2 O5W O 0.908(4) 0.089(3) 0.6935(16) 0.225(15) Uani 1 1 d . . . O6W O 0.800(4) 0.996(2) 0.3256(13) 0.195(13) Uani 1 1 d . . . O1W O 0.887(3) -0.022(3) 0.5971(18) 0.236(16) Uani 1 1 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 Ru01 0.0300(11) 0.101(2) 0.0546(15) 0.0045(10) -0.0067(7) -0.0164(9) O1 0.031(7) 0.062(10) 0.042(9) -0.008(7) 0.000(6) 0.003(6) O2 0.023(7) 0.064(10) 0.075(10) 0.001(7) -0.012(6) 0.001(6) O3 0.059(10) 0.085(14) 0.145(17) 0.028(11) -0.054(10) -0.003(9) O4 0.038(7) 0.091(13) 0.048(10) 0.008(9) -0.018(7) -0.008(7) O5 0.038(8) 0.077(13) 0.111(15) -0.005(10) -0.014(9) -0.009(8) O6 0.043(8) 0.074(12) 0.072(11) -0.006(9) -0.017(8) -0.007(8) N5 0.028(9) 0.143(19) 0.027(10) 0.011(10) 0.003(7) -0.034(10) N6 0.032(9) 0.042(11) 0.058(11) 0.013(8) -0.010(8) -0.008(7) N7 0.063(12) 0.070(16) 0.115(17) 0.017(12) -0.071(12) -0.016(11) N8 0.026(8) 0.081(14) 0.044(10) 0.001(9) -0.011(7) -0.006(8) N1 0.062(11) 0.063(13) 0.036(10) 0.010(8) -0.010(8) -0.029(9) C1 0.045(12) 0.055(16) 0.076(17) -0.003(13) -0.016(11) -0.017(11) C2 0.042(13) 0.14(3) 0.062(16) 0.006(16) -0.020(11) -0.016(15) C3 0.064(16) 0.08(2) 0.13(2) -0.009(17) 0.004(15) -0.032(15) C4 0.070(16) 0.12(2) 0.044(14) -0.006(14) -0.007(11) -0.036(16) C5 0.043(12) 0.073(18) 0.045(13) 0.006(12) -0.013(9) -0.018(12) N2 0.031(9) 0.129(18) 0.038(10) -0.006(11) -0.016(7) -0.033(11) C6 0.052(14) 0.11(2) 0.057(16) 0.026(15) 0.002(11) -0.022(15) C7 0.041(14) 0.15(3) 0.065(17) -0.006(16) 0.005(12) 0.020(15) C8 0.015(9) 0.11(2) 0.070(16) 0.019(14) -0.012(9) -0.003(12) C9 0.025(11) 0.09(2) 0.069(16) 0.010(14) -0.017(10) 0.012(12) C10 0.060(15) 0.09(2) 0.061(16) -0.017(13) 0.000(12) -0.008(13) N3 0.084(14) 0.045(13) 0.059(13) 0.001(10) -0.030(10) 0.009(10) C11 0.054(14) 0.12(2) 0.051(16) 0.019(14) -0.009(11) -0.027(14) C12 0.049(13) 0.13(3) 0.035(14) 0.003(14) 0.001(11) -0.005(14) C13 0.034(12) 0.15(3) 0.049(16) 0.008(16) -0.003(11) -0.007(15) C14 0.033(12) 0.13(3) 0.067(18) 0.000(16) -0.007(11) 0.008(14) C15 0.036(12) 0.11(2) 0.068(18) 0.039(16) -0.011(11) -0.010(14) N4 0.029(9) 0.098(16) 0.047(11) 0.001(10) -0.007(8) -0.005(9) C16 0.031(11) 0.082(19) 0.080(18) -0.008(15) -0.016(11) -0.005(12) C17 0.074(17) 0.09(2) 0.08(2) 0.009(16) -0.023(13) -0.018(15) C18 0.10(2) 0.06(2) 0.12(2) -0.002(17) -0.040(19) -0.016(16) C19 0.042(12) 0.073(19) 0.078(18) -0.005(14) -0.018(12) -0.006(12) C20 0.034(11) 0.10(2) 0.054(15) 0.012(14) -0.021(10) 0.005(12) C21 0.031(11) 0.084(18) 0.066(15) 0.002(12) -0.009(10) -0.004(11) C22 0.026(10) 0.12(2) 0.051(15) -0.006(14) -0.009(9) -0.016(11) C23 0.021(10) 0.055(16) 0.091(19) -0.001(13) -0.013(10) -0.007(9) C24 0.019(10) 0.064(16) 0.060(15) 0.005(11) 0.009(9) -0.004(9) C25 0.020(10) 0.089(18) 0.056(15) -0.003(12) -0.002(9) -0.021(10) C26 0.041(12) 0.067(16) 0.063(16) 0.000(12) -0.015(11) -0.021(11) C27 0.049(12) 0.054(15) 0.054(15) 0.003(11) -0.004(10) -0.019(11) C28 0.017(9) 0.062(15) 0.059(14) 0.000(11) -0.002(9) -0.005(9) C29 0.028(10) 0.066(16) 0.053(15) 0.003(11) -0.009(9) -0.008(10) C30 0.028(10) 0.073(16) 0.039(13) 0.005(11) -0.004(9) -0.015(10) C31 0.022(10) 0.040(14) 0.071(16) 0.011(11) -0.015(9) 0.005(8) C32 0.026(10) 0.043(14) 0.052(14) 0.001(10) -0.018(9) 0.006(9) C33 0.029(11) 0.13(3) 0.081(18) 0.053(17) -0.020(11) -0.030(13) C34 0.047(13) 0.048(17) 0.053(15) 0.006(12) 0.001(11) -0.012(12) C35 0.076(18) 0.08(2) 0.13(2) 0.038(17) -0.069(17) -0.022(16) C36 0.11(3) 0.11(3) 0.16(3) -0.03(2) -0.05(2) -0.04(2) C38 0.085(18) 0.10(2) 0.083(19) -0.001(17) -0.044(15) -0.034(16) C39 0.040(12) 0.08(2) 0.075(19) -0.015(15) -0.031(12) 0.005(11) C40 0.018(10) 0.10(2) 0.060(15) -0.006(14) -0.016(9) 0.001(11) C41 0.028(10) 0.059(16) 0.048(14) -0.013(12) 0.001(10) -0.009(10) C42 0.028(11) 0.057(16) 0.099(18) -0.022(13) -0.017(11) 0.008(10) Cl1 0.164(9) 0.124(9) 0.159(9) 0.012(6) 0.033(7) 0.022(7) Cl2 0.035(3) 0.082(5) 0.068(4) -0.002(3) -0.011(2) -0.008(3) O2W 0.052(9) 0.079(12) 0.076(11) -0.024(8) 0.014(7) -0.015(8) O4W 0.12(3) 0.23(4) 0.07(2) 0.01(2) -0.034(16) -0.07(2) O4W' 0.11(6) 0.06(6) 0.23(9) -0.01(5) 0.00(5) -0.01(4) O5W 0.21(3) 0.30(4) 0.20(3) -0.04(3) 0.07(2) -0.15(3) O6W 0.21(3) 0.24(3) 0.12(2) 0.003(19) -0.065(19) -0.01(2) O1W 0.12(2) 0.35(5) 0.27(4) 0.05(3) 0.01(2) -0.13(3) _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 Ru01 N4 2.036(7) . ? Ru01 N3 2.037(6) . ? Ru01 N6 2.050(15) . ? Ru01 N1 2.050(7) . ? Ru01 N2 2.061(5) . ? Ru01 N5 2.070(15) . ? O1 C32 1.34(2) . ? O1 C33 1.44(2) . ? O2 C31 1.417(19) . ? O2 C42 1.45(2) . ? O3 C37 1.39(3) . ? O3 C36 1.50(3) . ? O4 C39 1.41(2) . ? O4 C38 1.42(3) . ? O5 C34 1.18(2) . ? O6 C41 1.24(2) . ? N5 C21 1.29(2) . ? N5 C25 1.35(2) . ? N6 C26 1.36(2) . ? N6 C30 1.36(2) . ? N7 C34 1.34(3) . ? N7 C35 1.40(3) . ? N8 C41 1.35(2) . ? N8 C40 1.42(2) . ? N1 C1 1.3900 . ? N1 C5 1.3900 . ? C1 C2 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.4161 . ? N2 C6 1.3900 . ? N2 C10 1.3901 . ? C6 C7 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? N3 C15 1.3899 . ? N3 C11 1.3899 . ? C11 C12 1.3902 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.4150 . ? N4 C16 1.3900 . ? N4 C20 1.3901 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C21 C22 1.43(3) . ? C22 C23 1.36(3) . ? C23 C24 1.42(3) . ? C24 C25 1.38(3) . ? C24 C31 1.44(3) . ? C25 C26 1.44(3) . ? C26 C27 1.42(3) . ? C27 C28 1.41(3) . ? C27 C32 1.46(2) . ? C28 C29 1.35(2) . ? C29 C30 1.34(2) . ? C31 C32 1.35(3) . ? C33 C34 1.50(3) . ? C35 C36 1.39(4) . ? C37 C38 1.54(3) . ? C39 C40 1.46(3) . ? C41 C42 1.47(3) . ? 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 N4 Ru01 N3 80.5(2) . . ? N4 Ru01 N6 95.3(5) . . ? N3 Ru01 N6 171.1(4) . . ? N4 Ru01 N1 174.3(2) . . ? N3 Ru01 N1 96.6(3) . . ? N6 Ru01 N1 88.2(5) . . ? N4 Ru01 N2 96.9(2) . . ? N3 Ru01 N2 90.50(18) . . ? N6 Ru01 N2 97.8(4) . . ? N1 Ru01 N2 78.2(2) . . ? N4 Ru01 N5 87.3(6) . . ? N3 Ru01 N5 92.2(5) . . ? N6 Ru01 N5 79.7(6) . . ? N1 Ru01 N5 97.8(6) . . ? N2 Ru01 N5 175.4(6) . . ? C32 O1 C33 121.5(15) . . ? C31 O2 C42 114.9(14) . . ? C37 O3 C36 106(2) . . ? C39 O4 C38 115.9(18) . . ? C21 N5 C25 117.2(16) . . ? C21 N5 Ru01 128.7(14) . . ? C25 N5 Ru01 113.8(11) . . ? C26 N6 C30 116.3(17) . . ? C26 N6 Ru01 113.6(13) . . ? C30 N6 Ru01 129.7(12) . . ? C34 N7 C35 121.5(19) . . ? C41 N8 C40 121.8(17) . . ? C1 N1 C5 120.0 . . ? C1 N1 Ru01 124.67(13) . . ? C5 N1 Ru01 115.29(13) . . ? C2 C1 N1 120.0 . . ? C1 C2 C3 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 C6 123.4 . . ? N1 C5 C6 116.2 . . ? C6 N2 C10 120.0 . . ? C6 N2 Ru01 116.2(2) . . ? C10 N2 Ru01 123.6(2) . . ? C7 C6 N2 120.0 . . ? C7 C6 C5 126.0 . . ? N2 C6 C5 113.9 . . ? C6 C7 C8 120.0 . . ? C7 C8 C9 120.0 . . ? C8 C9 C10 120.0 . . ? C9 C10 N2 120.0 . . ? C15 N3 C11 120.0 . . ? C15 N3 Ru01 113.6(2) . . ? C11 N3 Ru01 125.0(2) . . ? N3 C11 C12 120.0 . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? N3 C15 C14 120.0 . . ? N3 C15 C16 115.4 . . ? C14 C15 C16 124.6 . . ? C16 N4 C20 120.0 . . ? C16 N4 Ru01 113.49(15) . . ? C20 N4 Ru01 126.29(16) . . ? C17 C16 N4 120.0 . . ? C17 C16 C15 123.8 . . ? N4 C16 C15 116.2 . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 N4 120.0 . . ? N5 C21 C22 124(2) . . ? C23 C22 C21 119.6(19) . . ? C22 C23 C24 116.9(17) . . ? C25 C24 C23 118.6(19) . . ? C25 C24 C31 118.8(16) . . ? C23 C24 C31 122.5(17) . . ? N5 C25 C24 123.7(17) . . ? N5 C25 C26 115.8(16) . . ? C24 C25 C26 120.1(19) . . ? N6 C26 C27 123.5(18) . . ? N6 C26 C25 116.8(19) . . ? C27 C26 C25 119.6(17) . . ? C28 C27 C26 114.9(18) . . ? C28 C27 C32 125.5(19) . . ? C26 C27 C32 119.3(18) . . ? C29 C28 C27 121.1(19) . . ? C30 C29 C28 120.0(18) . . ? C29 C30 N6 123.6(17) . . ? C32 C31 O2 119.4(18) . . ? C32 C31 C24 123.3(15) . . ? O2 C31 C24 117.2(16) . . ? O1 C32 C31 129.9(15) . . ? O1 C32 C27 111.2(16) . . ? C31 C32 C27 118.4(18) . . ? O1 C33 C34 115(2) . . ? O5 C34 N7 128(2) . . ? O5 C34 C33 120(2) . . ? N7 C34 C33 111(2) . . ? C36 C35 N7 115(2) . . ? C35 C36 O3 106(2) . . ? O3 C37 C38 106(2) . . ? O4 C38 C37 112(2) . . ? O4 C39 C40 114.6(19) . . ? N8 C40 C39 112.0(17) . . ? O6 C41 N8 122.0(17) . . ? O6 C41 C42 121.2(18) . . ? N8 C41 C42 116.8(19) . . ? O2 C42 C41 106.9(16) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.402 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.205 #=END