# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title 'Activation of a 1,10-phenanthroline ligand on a rhenium tricarbonyl complex.' _audit_creation_method SHELXL _publ_contact_author ; JULIO PEREZ Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; _publ_contact_author_phone +34-85-102985 _publ_contact_author_fax +34-85-103446 _publ_contact_author_email japm@sauron.quimica.uniovi.es loop_ _publ_author_name _publ_author_address 'Luciano Cuesta' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Eva Hevia' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Dolores Morales' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Julio Perez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Victor Riera' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; 'Elena Rodriguez' ; Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Química Universidad de Oviedo-CSIC C/ Julian Claveria s/n 33006 Oviedo (ASTURIAS) SPAIN ; ; D.Miguel ; ; Quimica Inorganica Facultad de Ciencias Universidad de Valladolid 47071 Valladolid SPAIN ; _publ_contact_author_name 'JULIO PEREZ' #-------------------------- data section of block --------------------------- data_Compound_2_(LC21cm) _database_code_depnum_ccdc_archive 'CCDC 246293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H22 N2 O5 P Re' _chemical_formula_weight 719.68 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.844(3) _cell_length_b 11.300(4) _cell_length_c 13.009(5) _cell_angle_alpha 86.592(7) _cell_angle_beta 71.976(6) _cell_angle_gamma 82.823(7) _cell_volume 1365.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour DEEP_RED _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 4.554 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.690997 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6131 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 23.32 _reflns_number_total 3917 _reflns_number_gt 3507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0550P)^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 3917 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 Re1 Re 0.36232(2) 0.21948(2) 0.218946(17) 0.03543(11) Uani 1 1 d . . . P1 P 0.38766(16) 0.31829(13) 0.37519(11) 0.0332(3) Uani 1 1 d . . . N1 N 0.5323(5) 0.3313(4) 0.1517(4) 0.0337(11) Uani 1 1 d . . . N2 N 0.5567(5) 0.1024(4) 0.2116(4) 0.0369(11) Uani 1 1 d . . . C1 C 0.3559(6) 0.1547(6) 0.0833(5) 0.0425(15) Uani 1 1 d . . . O1 O 0.3475(6) 0.1157(6) 0.0097(5) 0.0846(18) Uani 1 1 d . . . C3 C 0.2034(7) 0.3348(6) 0.2146(5) 0.0433(15) Uani 1 1 d . . . O3 O 0.1096(6) 0.4044(5) 0.2058(4) 0.0668(14) Uani 1 1 d . . . C2 C 0.2283(6) 0.1082(5) 0.2949(5) 0.0390(14) Uani 1 1 d . . . O2 O 0.1523(5) 0.0408(5) 0.3395(5) 0.0686(14) Uani 1 1 d . . . C4 C 0.3940(7) 0.4769(5) 0.3428(5) 0.0424(15) Uani 1 1 d . . . H4 H 0.3651 0.5284 0.4007 0.051 Uiso 1 1 calc R . . C5 C 0.4365(6) 0.5266(5) 0.2432(5) 0.0390(14) Uani 1 1 d . . . C6 C 0.4055(7) 0.6594(6) 0.2350(5) 0.0449(15) Uani 1 1 d . . . O6 O 0.4213(7) 0.7297(4) 0.2933(4) 0.0757(16) Uani 1 1 d . . . O7 O 0.3511(6) 0.6901(4) 0.1532(4) 0.0593(13) Uani 1 1 d . . . C7 C 0.3064(9) 0.8165(6) 0.1402(7) 0.068(2) Uani 1 1 d . . . H7A H 0.2507 0.8484 0.2092 0.103 Uiso 1 1 calc R . . H7B H 0.2493 0.8263 0.0917 0.103 Uiso 1 1 calc R . . H7C H 0.3899 0.8580 0.1111 0.103 Uiso 1 1 calc R . . C11 C 0.5082(7) 0.4613(5) 0.1370(5) 0.0401(14) Uani 1 1 d . . . H11 H 0.4425 0.4767 0.0933 0.048 Uiso 1 1 calc R . . C12 C 0.6454(8) 0.5153(6) 0.0753(5) 0.0505(17) Uani 1 1 d . . . H12 H 0.6379 0.5948 0.0526 0.061 Uiso 1 1 calc R . . C13 C 0.7745(8) 0.4548(6) 0.0525(5) 0.0536(18) Uani 1 1 d . . . H13 H 0.8543 0.4933 0.0157 0.064 Uiso 1 1 calc R . . C14 C 0.7954(7) 0.3306(6) 0.0830(5) 0.0462(16) Uani 1 1 d . . . C15 C 0.6680(7) 0.2760(6) 0.1322(5) 0.0398(14) Uani 1 1 d . . . C16 C 0.6847(6) 0.1529(6) 0.1624(5) 0.0391(14) Uani 1 1 d . . . C17 C 0.8206(7) 0.0858(7) 0.1486(5) 0.0510(17) Uani 1 1 d . . . C18 C 0.8225(8) -0.0310(7) 0.1848(6) 0.064(2) Uani 1 1 d . . . H18 H 0.9102 -0.0771 0.1766 0.077 Uiso 1 1 calc R . . C19 C 0.6986(8) -0.0802(6) 0.2323(6) 0.0572(18) Uani 1 1 d . . . H19 H 0.7011 -0.1594 0.2563 0.069 Uiso 1 1 calc R . . C20 C 0.5679(7) -0.0106(6) 0.2447(5) 0.0453(15) Uani 1 1 d . . . H20 H 0.4838 -0.0451 0.2781 0.054 Uiso 1 1 calc R . . C21 C 0.9290(7) 0.2610(7) 0.0657(6) 0.061(2) Uani 1 1 d . . . H21 H 1.0119 0.2967 0.0309 0.074 Uiso 1 1 calc R . . C22 C 0.9439(8) 0.1436(8) 0.0972(7) 0.068(2) Uani 1 1 d . . . H22 H 1.0350 0.1020 0.0847 0.081 Uiso 1 1 calc R . . C31 C 0.2474(6) 0.3237(5) 0.5070(5) 0.0380(14) Uani 1 1 d . . . C32 C 0.2706(7) 0.3627(6) 0.5985(5) 0.0502(16) Uani 1 1 d . . . H32 H 0.3609 0.3828 0.5945 0.060 Uiso 1 1 calc R . . C33 C 0.1618(8) 0.3722(6) 0.6952(5) 0.0555(18) Uani 1 1 d . . . H33 H 0.1793 0.3975 0.7562 0.067 Uiso 1 1 calc R . . C34 C 0.0278(9) 0.3444(7) 0.7018(6) 0.066(2) Uani 1 1 d . . . H34 H -0.0464 0.3528 0.7666 0.079 Uiso 1 1 calc R . . C35 C 0.0037(8) 0.3046(9) 0.6131(7) 0.082(3) Uani 1 1 d . . . H35 H -0.0866 0.2836 0.6181 0.099 Uiso 1 1 calc R . . C36 C 0.1130(8) 0.2949(8) 0.5144(6) 0.067(2) Uani 1 1 d . . . H36 H 0.0950 0.2690 0.4538 0.081 Uiso 1 1 calc R . . C41 C 0.5521(6) 0.2666(5) 0.4090(4) 0.0365(14) Uani 1 1 d . . . C42 C 0.6714(7) 0.3271(7) 0.3739(5) 0.0517(17) Uani 1 1 d . . . H42 H 0.6662 0.4006 0.3382 0.062 Uiso 1 1 calc R . . C43 C 0.8015(7) 0.2786(8) 0.3914(6) 0.064(2) Uani 1 1 d . . . H43 H 0.8822 0.3196 0.3676 0.077 Uiso 1 1 calc R . . C44 C 0.8078(8) 0.1688(8) 0.4447(6) 0.064(2) Uani 1 1 d . . . H44 H 0.8928 0.1362 0.4575 0.077 Uiso 1 1 calc R . . C45 C 0.6878(8) 0.1079(7) 0.4786(6) 0.0584(19) Uani 1 1 d . . . H45 H 0.6926 0.0338 0.5132 0.070 Uiso 1 1 calc R . . C46 C 0.5613(7) 0.1564(6) 0.4614(5) 0.0448(15) Uani 1 1 d . . . H46 H 0.4809 0.1151 0.4852 0.054 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 0.03727(16) 0.03836(17) 0.03396(16) -0.00356(10) -0.01198(11) -0.01247(10) P1 0.0360(8) 0.0371(8) 0.0287(8) -0.0025(6) -0.0100(6) -0.0117(6) N1 0.036(3) 0.030(3) 0.035(3) -0.001(2) -0.007(2) -0.012(2) N2 0.040(3) 0.040(3) 0.030(3) -0.002(2) -0.008(2) -0.010(2) C1 0.037(3) 0.057(4) 0.034(3) -0.006(3) -0.007(3) -0.011(3) O1 0.086(4) 0.118(5) 0.061(4) -0.033(3) -0.029(3) -0.022(4) C3 0.052(4) 0.041(4) 0.038(3) -0.005(3) -0.009(3) -0.020(3) O3 0.057(3) 0.064(3) 0.081(4) 0.003(3) -0.027(3) 0.004(3) C2 0.037(3) 0.036(3) 0.042(3) -0.002(3) -0.007(3) -0.007(3) O2 0.056(3) 0.056(3) 0.088(4) 0.011(3) -0.010(3) -0.024(3) C4 0.052(4) 0.046(4) 0.036(3) -0.005(3) -0.017(3) -0.017(3) C5 0.045(4) 0.041(3) 0.037(3) -0.001(3) -0.016(3) -0.015(3) C6 0.055(4) 0.042(4) 0.038(4) 0.003(3) -0.010(3) -0.018(3) O6 0.130(5) 0.044(3) 0.068(3) -0.006(3) -0.046(4) -0.023(3) O7 0.087(4) 0.042(3) 0.057(3) -0.003(2) -0.033(3) -0.007(2) C7 0.093(6) 0.044(4) 0.071(5) 0.004(4) -0.028(5) -0.012(4) C11 0.049(4) 0.041(3) 0.033(3) 0.001(3) -0.014(3) -0.014(3) C12 0.066(5) 0.044(4) 0.043(4) 0.002(3) -0.012(3) -0.025(3) C13 0.052(4) 0.065(5) 0.043(4) -0.002(3) -0.005(3) -0.032(4) C14 0.038(4) 0.064(4) 0.037(3) -0.004(3) -0.008(3) -0.015(3) C15 0.042(4) 0.048(4) 0.033(3) -0.003(3) -0.012(3) -0.019(3) C16 0.036(3) 0.049(4) 0.034(3) -0.006(3) -0.010(3) -0.009(3) C17 0.054(4) 0.070(5) 0.030(3) -0.006(3) -0.014(3) -0.009(3) C18 0.057(5) 0.061(5) 0.074(5) -0.008(4) -0.025(4) 0.014(4) C19 0.059(5) 0.048(4) 0.062(5) -0.003(3) -0.018(4) 0.000(3) C20 0.049(4) 0.044(4) 0.043(4) -0.008(3) -0.013(3) -0.005(3) C21 0.037(4) 0.082(6) 0.058(5) -0.013(4) 0.003(3) -0.019(4) C22 0.038(4) 0.085(6) 0.075(5) -0.007(5) -0.010(4) -0.003(4) C31 0.041(3) 0.039(3) 0.032(3) -0.001(3) -0.006(3) -0.009(3) C32 0.052(4) 0.061(4) 0.039(4) -0.011(3) -0.008(3) -0.018(3) C33 0.067(5) 0.057(4) 0.039(4) -0.011(3) -0.008(3) -0.009(4) C34 0.068(5) 0.066(5) 0.047(4) -0.010(4) 0.007(4) -0.007(4) C35 0.044(5) 0.128(8) 0.068(5) -0.026(5) 0.003(4) -0.026(5) C36 0.046(4) 0.111(7) 0.049(4) -0.018(4) -0.013(3) -0.017(4) C41 0.038(3) 0.045(4) 0.028(3) -0.006(3) -0.008(3) -0.014(3) C42 0.051(4) 0.063(5) 0.048(4) 0.003(3) -0.019(3) -0.028(3) C43 0.041(4) 0.090(6) 0.068(5) 0.007(4) -0.020(4) -0.031(4) C44 0.042(4) 0.088(6) 0.067(5) -0.008(4) -0.026(4) 0.001(4) C45 0.063(5) 0.060(5) 0.060(5) 0.007(4) -0.031(4) -0.009(4) C46 0.039(4) 0.054(4) 0.045(4) 0.003(3) -0.014(3) -0.014(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 Re1 C3 1.920(7) . ? Re1 C2 1.939(6) . ? Re1 C1 1.972(6) . ? Re1 N1 2.157(4) . ? Re1 N2 2.166(5) . ? Re1 P1 2.4685(16) . ? P1 C4 1.821(6) . ? P1 C41 1.824(6) . ? P1 C31 1.838(6) . ? N1 C15 1.356(8) . ? N1 C11 1.469(8) . ? N2 C20 1.325(8) . ? N2 C16 1.400(7) . ? C1 O1 1.107(7) . ? C3 O3 1.165(8) . ? C2 O2 1.139(7) . ? C4 C5 1.344(8) . ? C5 C6 1.498(9) . ? C5 C11 1.530(9) . ? C6 O6 1.186(8) . ? C6 O7 1.342(8) . ? O7 C7 1.457(8) . ? C11 C12 1.522(9) . ? C12 C13 1.321(10) . ? C13 C14 1.442(10) . ? C14 C21 1.407(10) . ? C14 C15 1.419(8) . ? C15 C16 1.426(9) . ? C16 C17 1.418(9) . ? C17 C18 1.375(10) . ? C17 C22 1.410(10) . ? C18 C19 1.356(10) . ? C19 C20 1.391(9) . ? C21 C22 1.368(11) . ? C31 C36 1.375(9) . ? C31 C32 1.385(9) . ? C32 C33 1.377(9) . ? C33 C34 1.370(10) . ? C34 C35 1.360(11) . ? C35 C36 1.396(10) . ? C41 C42 1.373(8) . ? C41 C46 1.391(8) . ? C42 C43 1.408(10) . ? C43 C44 1.389(11) . ? C44 C45 1.382(10) . ? C45 C46 1.373(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Re1 C2 89.6(2) . . ? C3 Re1 C1 88.5(3) . . ? C2 Re1 C1 87.3(3) . . ? C3 Re1 N1 98.0(2) . . ? C2 Re1 N1 170.4(2) . . ? C1 Re1 N1 98.7(2) . . ? C3 Re1 N2 173.7(2) . . ? C2 Re1 N2 96.6(2) . . ? C1 Re1 N2 90.7(2) . . ? N1 Re1 N2 75.94(18) . . ? C3 Re1 P1 90.76(18) . . ? C2 Re1 P1 99.48(18) . . ? C1 Re1 P1 173.19(18) . . ? N1 Re1 P1 74.72(13) . . ? N2 Re1 P1 89.34(13) . . ? C4 P1 C41 106.0(3) . . ? C4 P1 C31 100.6(3) . . ? C41 P1 C31 103.6(3) . . ? C4 P1 Re1 108.42(19) . . ? C41 P1 Re1 114.44(19) . . ? C31 P1 Re1 122.0(2) . . ? C15 N1 C11 120.1(5) . . ? C15 N1 Re1 115.7(4) . . ? C11 N1 Re1 124.0(4) . . ? C20 N2 C16 117.3(5) . . ? C20 N2 Re1 127.8(4) . . ? C16 N2 Re1 114.9(4) . . ? O1 C1 Re1 177.0(6) . . ? O3 C3 Re1 176.2(6) . . ? O2 C2 Re1 178.4(6) . . ? C5 C4 P1 126.2(5) . . ? C4 C5 C6 116.6(6) . . ? C4 C5 C11 126.8(6) . . ? C6 C5 C11 116.6(5) . . ? O6 C6 O7 123.3(6) . . ? O6 C6 C5 126.1(6) . . ? O7 C6 C5 110.5(5) . . ? C6 O7 C7 116.6(5) . . ? N1 C11 C12 112.6(5) . . ? N1 C11 C5 113.3(5) . . ? C12 C11 C5 109.4(5) . . ? C13 C12 C11 123.2(6) . . ? C12 C13 C14 122.0(6) . . ? C21 C14 C15 118.7(6) . . ? C21 C14 C13 125.6(6) . . ? C15 C14 C13 115.6(6) . . ? N1 C15 C14 125.1(6) . . ? N1 C15 C16 117.8(5) . . ? C14 C15 C16 117.1(6) . . ? N2 C16 C17 121.3(6) . . ? N2 C16 C15 115.5(5) . . ? C17 C16 C15 123.2(6) . . ? C18 C17 C22 124.9(7) . . ? C18 C17 C16 117.7(6) . . ? C22 C17 C16 117.4(7) . . ? C19 C18 C17 121.1(7) . . ? C18 C19 C20 119.1(7) . . ? N2 C20 C19 123.5(6) . . ? C22 C21 C14 123.6(6) . . ? C21 C22 C17 119.8(7) . . ? C36 C31 C32 118.7(6) . . ? C36 C31 P1 119.4(5) . . ? C32 C31 P1 121.7(5) . . ? C33 C32 C31 120.9(6) . . ? C34 C33 C32 120.1(7) . . ? C35 C34 C33 119.7(7) . . ? C34 C35 C36 120.7(7) . . ? C31 C36 C35 119.8(7) . . ? C42 C41 C46 119.3(6) . . ? C42 C41 P1 121.8(5) . . ? C46 C41 P1 118.6(4) . . ? C41 C42 C43 120.4(7) . . ? C44 C43 C42 119.2(6) . . ? C45 C44 C43 119.9(7) . . ? C46 C45 C44 120.3(7) . . ? C45 C46 C41 120.8(6) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.484 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.127 #===END data_Compound_3_(dm417bm) _database_code_depnum_ccdc_archive 'CCDC 246294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.25 H24.50 Cl0.50 N2 O5 P Re' _chemical_formula_weight 742.92 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 25.629(6) _cell_length_b 9.692(2) _cell_length_c 24.818(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.334(4) _cell_angle_gamma 90.00 _cell_volume 6165(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description BLOCK _exptl_crystal_colour RED _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2916 _exptl_absorpt_coefficient_mu 4.078 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.780198 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13470 _diffrn_reflns_av_R_equivalents 0.0747 _diffrn_reflns_av_sigmaI/netI 0.0904 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 23.34 _reflns_number_total 4450 _reflns_number_gt 2947 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0252P)^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 4450 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.0930 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.881297(16) 0.03185(5) 0.793981(16) 0.03501(14) Uani 1 1 d . . . P1 P 0.88329(10) 0.2120(3) 0.86463(11) 0.0368(7) Uani 1 1 d . . . N1 N 0.8525(3) -0.0803(8) 0.8620(3) 0.036(2) Uani 1 1 d . . . N2 N 0.7972(3) 0.0384(9) 0.7828(3) 0.036(2) Uani 1 1 d . . . C1 C 0.8847(4) -0.1169(13) 0.7423(5) 0.044(3) Uani 1 1 d . . . O1 O 0.8906(3) -0.2023(10) 0.7107(4) 0.074(3) Uani 1 1 d . . . C2 C 0.8993(4) 0.1535(13) 0.7383(5) 0.047(3) Uani 1 1 d . . . O2 O 0.9103(3) 0.2327(9) 0.7038(3) 0.069(3) Uani 1 1 d . . . C3 C 0.9546(4) 0.0004(10) 0.8073(4) 0.038(3) Uani 1 1 d . . . O3 O 0.9977(3) -0.0246(9) 0.8140(3) 0.058(2) Uani 1 1 d . . . C4 C 0.9162(4) 0.1349(11) 0.9230(4) 0.042(3) Uani 1 1 d . . . H4A H 0.9505 0.1038 0.9120 0.051 Uiso 1 1 calc R . . H4B H 0.9211 0.2055 0.9502 0.051 Uiso 1 1 calc R . . C5 C 0.8868(4) 0.0123(11) 0.9483(3) 0.039(3) Uani 1 1 d . . . H5 H 0.8519 0.0434 0.9585 0.047 Uiso 1 1 d R . . C6 C 0.9162(4) -0.0292(15) 0.9989(4) 0.055(3) Uani 1 1 d . . . O6 O 0.9532(4) -0.1002(10) 1.0002(3) 0.089(3) Uani 1 1 d . . . C7 C 0.9271(7) 0.011(3) 1.0905(5) 0.289(19) Uani 1 1 d . . . H7A H 0.9177 -0.0754 1.1068 0.433 Uiso 1 1 calc R . . H7B H 0.9196 0.0850 1.1149 0.433 Uiso 1 1 calc R . . H7C H 0.9637 0.0107 1.0824 0.433 Uiso 1 1 calc R . . O7 O 0.8971(3) 0.0297(15) 1.0407(3) 0.149(6) Uani 1 1 d . . . C11 C 0.8813(4) -0.1140(11) 0.9108(4) 0.041(3) Uani 1 1 d . . . H11 H 0.9163 -0.1444 0.9006 0.049 Uiso 1 1 calc R . . C12 C 0.8547(5) -0.2321(12) 0.9417(4) 0.057(3) Uani 1 1 d . . . H12 H 0.8751 -0.2920 0.9623 0.068 Uiso 1 1 calc R . . C13 C 0.8042(5) -0.2502(13) 0.9397(4) 0.057(3) Uani 1 1 d . . . H13 H 0.7888 -0.3155 0.9621 0.068 Uiso 1 1 calc R . . C14 C 0.7726(5) -0.1722(13) 0.9042(5) 0.056(3) Uani 1 1 d . . . C15 C 0.7178(5) -0.1792(14) 0.9006(5) 0.069(4) Uani 1 1 d . . . H15 H 0.6999 -0.2300 0.9263 0.083 Uiso 1 1 calc R . . C16 C 0.6889(5) -0.1136(14) 0.8602(6) 0.070(4) Uani 1 1 d . . . H16 H 0.6527 -0.1204 0.8602 0.084 Uiso 1 1 calc R . . C17 C 0.7139(4) -0.0367(13) 0.8190(4) 0.052(3) Uani 1 1 d . . . C18 C 0.6888(4) 0.0297(14) 0.7758(5) 0.064(3) Uani 1 1 d . . . H18 H 0.6526 0.0272 0.7732 0.077 Uiso 1 1 calc R . . C19 C 0.7165(5) 0.0972(13) 0.7379(5) 0.063(4) Uani 1 1 d . . . H19 H 0.6997 0.1407 0.7092 0.076 Uiso 1 1 calc R . . C20 C 0.7715(4) 0.1006(12) 0.7426(4) 0.051(3) Uani 1 1 d . . . H20 H 0.7905 0.1479 0.7167 0.061 Uiso 1 1 calc R . . C21 C 0.7995(4) -0.0907(11) 0.8643(4) 0.042(3) Uani 1 1 d . . . C22 C 0.7694(3) -0.0296(12) 0.8216(4) 0.040(3) Uani 1 1 d . . . C31 C 0.9216(4) 0.3647(11) 0.8499(4) 0.034(3) Uani 1 1 d . . . C32 C 0.9002(4) 0.4952(11) 0.8469(4) 0.045(3) Uani 1 1 d . . . H32 H 0.8652 0.5067 0.8554 0.054 Uiso 1 1 calc R . . C33 C 0.9286(5) 0.6090(13) 0.8316(4) 0.057(3) Uani 1 1 d . . . H33 H 0.9126 0.6950 0.8291 0.069 Uiso 1 1 calc R . . C34 C 0.9811(5) 0.5948(16) 0.8200(5) 0.069(4) Uani 1 1 d . . . H34 H 1.0011 0.6718 0.8114 0.083 Uiso 1 1 calc R . . C35 C 1.0032(5) 0.4665(18) 0.8212(6) 0.088(4) Uani 1 1 d . . . H35 H 1.0381 0.4549 0.8122 0.105 Uiso 1 1 calc R . . C36 C 0.9734(5) 0.3539(13) 0.8360(5) 0.070(4) Uani 1 1 d . . . H36 H 0.9890 0.2673 0.8367 0.084 Uiso 1 1 calc R . . C41 C 0.8236(4) 0.2852(11) 0.8922(5) 0.045(3) Uani 1 1 d . . . C42 C 0.8203(5) 0.3271(13) 0.9455(5) 0.059(4) Uani 1 1 d . . . H42 H 0.8488 0.3158 0.9684 0.071 Uiso 1 1 calc R . . C43 C 0.7751(6) 0.3852(14) 0.9648(6) 0.083(5) Uani 1 1 d . . . H43 H 0.7736 0.4119 1.0008 0.100 Uiso 1 1 calc R . . C44 C 0.7325(6) 0.4048(15) 0.9326(7) 0.088(5) Uani 1 1 d . . . H44 H 0.7021 0.4438 0.9462 0.106 Uiso 1 1 calc R . . C45 C 0.7354(5) 0.3662(15) 0.8808(7) 0.080(4) Uani 1 1 d . . . H45 H 0.7065 0.3782 0.8585 0.096 Uiso 1 1 calc R . . C46 C 0.7815(4) 0.3078(12) 0.8592(5) 0.062(4) Uani 1 1 d . . . H46 H 0.7830 0.2849 0.8228 0.074 Uiso 1 1 calc R . . Cl91 Cl 1.0343(8) 0.463(3) 0.4958(10) 0.184(10) Uiso 0.25 1 d PG . . Cl92 Cl 0.9380(11) 0.553(4) 0.5393(14) 0.284(18) Uiso 0.25 1 d PG . . C90 C 1.0027(13) 0.604(4) 0.527(3) 0.17(3) Uiso 0.25 1 d PG . . H90A H 1.0156 0.6574 0.5566 0.100 Uiso 0.25 1 d PG . . H90B H 1.0036 0.6598 0.4946 0.100 Uiso 0.25 1 d PG . . 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 0.0349(2) 0.0356(3) 0.0345(2) 0.0012(3) 0.00062(16) -0.0007(3) P1 0.0372(16) 0.035(2) 0.0382(17) -0.0006(13) 0.0006(13) 0.0019(14) N1 0.040(5) 0.030(6) 0.038(5) 0.001(4) -0.004(4) -0.003(4) N2 0.026(4) 0.040(6) 0.042(5) -0.012(5) -0.003(4) -0.005(5) C1 0.032(6) 0.055(10) 0.044(8) 0.014(6) 0.002(6) 0.001(6) O1 0.089(7) 0.061(8) 0.074(7) -0.026(5) 0.010(5) -0.016(5) C2 0.025(6) 0.068(11) 0.049(8) -0.014(7) -0.010(6) 0.000(6) O2 0.074(6) 0.069(7) 0.064(6) 0.031(5) 0.004(5) -0.008(5) C3 0.061(7) 0.024(9) 0.029(6) -0.009(4) 0.007(5) -0.001(5) O3 0.028(4) 0.081(7) 0.065(5) -0.002(5) -0.002(4) 0.011(4) C4 0.036(6) 0.043(8) 0.049(7) 0.002(6) -0.002(5) 0.000(5) C5 0.037(6) 0.045(9) 0.036(6) -0.004(5) 0.003(5) 0.005(5) C6 0.040(7) 0.081(10) 0.044(7) 0.008(7) -0.001(6) 0.004(7) O6 0.092(7) 0.105(9) 0.071(6) 0.000(5) -0.024(5) 0.042(6) C7 0.137(16) 0.69(6) 0.039(9) 0.02(2) -0.033(10) 0.18(3) O7 0.095(8) 0.318(18) 0.034(5) -0.006(7) -0.005(5) 0.106(10) C11 0.046(7) 0.038(8) 0.038(7) 0.002(6) 0.001(5) 0.000(5) C12 0.081(10) 0.035(9) 0.055(8) 0.016(6) 0.002(7) 0.005(7) C13 0.064(9) 0.055(10) 0.051(8) 0.023(6) 0.002(7) -0.007(7) C14 0.055(8) 0.054(10) 0.060(8) -0.008(7) 0.022(7) -0.017(7) C15 0.063(10) 0.081(12) 0.064(9) -0.005(8) 0.019(8) -0.030(8) C16 0.050(8) 0.072(11) 0.089(11) -0.021(8) 0.024(8) -0.020(7) C17 0.039(6) 0.055(8) 0.063(7) -0.008(7) -0.003(6) -0.008(7) C18 0.033(6) 0.072(10) 0.087(9) -0.023(8) -0.011(7) 0.004(7) C19 0.050(8) 0.069(11) 0.070(9) 0.005(7) -0.014(7) -0.001(7) C20 0.048(8) 0.055(9) 0.050(7) 0.000(6) -0.014(6) -0.010(6) C21 0.054(7) 0.033(8) 0.037(7) -0.014(5) 0.006(6) -0.002(6) C22 0.028(5) 0.042(7) 0.051(6) -0.014(6) 0.005(5) -0.006(6) C31 0.037(6) 0.028(8) 0.036(6) -0.006(5) 0.006(5) 0.005(5) C32 0.046(7) 0.031(11) 0.057(7) -0.002(5) 0.000(5) 0.001(5) C33 0.081(10) 0.033(9) 0.059(8) -0.001(6) 0.003(7) -0.010(7) C34 0.073(10) 0.048(11) 0.086(10) -0.008(8) 0.029(8) -0.027(8) C35 0.069(9) 0.046(10) 0.148(13) 0.002(11) 0.042(9) -0.003(10) C36 0.050(8) 0.035(9) 0.125(12) 0.000(8) 0.024(8) 0.008(7) C41 0.046(7) 0.029(8) 0.061(8) 0.003(6) 0.012(6) 0.004(5) C42 0.052(8) 0.066(11) 0.059(9) 0.002(7) 0.021(7) 0.022(7) C43 0.109(13) 0.058(11) 0.083(11) 0.013(8) 0.043(10) 0.003(9) C44 0.079(12) 0.062(12) 0.123(15) 0.008(10) 0.041(11) 0.014(9) C45 0.036(8) 0.082(12) 0.122(14) -0.009(10) -0.002(9) 0.015(7) C46 0.055(8) 0.045(9) 0.085(10) -0.014(7) -0.011(8) 0.010(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C2 1.876(13) . ? Re1 C3 1.929(11) . ? Re1 C1 1.932(13) . ? Re1 N1 2.142(8) . ? Re1 N2 2.173(7) . ? Re1 P1 2.475(3) . ? P1 C31 1.814(11) . ? P1 C41 1.822(11) . ? P1 C4 1.831(9) . ? N1 C21 1.363(12) . ? N1 C11 1.452(11) . ? N2 C20 1.336(12) . ? N2 C22 1.369(12) . ? C1 O1 1.150(12) . ? C2 O2 1.186(13) . ? C3 O3 1.143(10) . ? C4 C5 1.543(13) . ? C5 C6 1.515(13) . ? C5 C11 1.543(13) . ? C6 O6 1.172(12) . ? C6 O7 1.285(13) . ? C7 O7 1.464(14) . ? C11 C12 1.540(14) . ? C12 C13 1.307(14) . ? C13 C14 1.412(15) . ? C14 C15 1.409(15) . ? C14 C21 1.446(14) . ? C15 C16 1.395(16) . ? C16 C17 1.421(15) . ? C17 C18 1.403(15) . ? C17 C22 1.425(12) . ? C18 C19 1.351(15) . ? C19 C20 1.415(14) . ? C21 C22 1.436(13) . ? C31 C36 1.379(14) . ? C31 C32 1.381(13) . ? C32 C33 1.376(14) . ? C33 C34 1.386(16) . ? C34 C35 1.367(17) . ? C35 C36 1.383(17) . ? C41 C46 1.370(14) . ? C41 C42 1.387(14) . ? C42 C43 1.378(16) . ? C43 C44 1.362(18) . ? C44 C45 1.343(18) . ? C45 C46 1.417(15) . ? Cl91 Cl92 1.14(4) 5_766 ? Cl91 C90 1.28(5) 5_766 ? Cl91 C90 1.7700 . ? Cl91 Cl91 1.91(4) 5_766 ? Cl92 Cl91 1.14(4) 5_766 ? Cl92 C90 1.7612 . ? C90 Cl91 1.28(5) 5_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Re1 C3 89.0(4) . . ? C2 Re1 C1 88.2(5) . . ? C3 Re1 C1 87.0(4) . . ? C2 Re1 N1 170.6(4) . . ? C3 Re1 N1 97.1(3) . . ? C1 Re1 N1 99.3(4) . . ? C2 Re1 N2 97.8(4) . . ? C3 Re1 N2 172.1(4) . . ? C1 Re1 N2 89.2(4) . . ? N1 Re1 N2 76.6(3) . . ? C2 Re1 P1 94.2(4) . . ? C3 Re1 P1 88.5(3) . . ? C1 Re1 P1 174.9(3) . . ? N1 Re1 P1 78.8(2) . . ? N2 Re1 P1 94.9(2) . . ? C31 P1 C41 102.3(5) . . ? C31 P1 C4 104.2(4) . . ? C41 P1 C4 104.2(5) . . ? C31 P1 Re1 116.3(3) . . ? C41 P1 Re1 121.8(4) . . ? C4 P1 Re1 106.3(4) . . ? C21 N1 C11 116.7(8) . . ? C21 N1 Re1 114.8(6) . . ? C11 N1 Re1 126.6(6) . . ? C20 N2 C22 119.1(8) . . ? C20 N2 Re1 126.3(7) . . ? C22 N2 Re1 114.6(6) . . ? O1 C1 Re1 174.7(10) . . ? O2 C2 Re1 178.6(12) . . ? O3 C3 Re1 176.6(9) . . ? C5 C4 P1 114.4(6) . . ? C6 C5 C4 107.5(8) . . ? C6 C5 C11 109.5(9) . . ? C4 C5 C11 114.1(8) . . ? O6 C6 O7 123.5(11) . . ? O6 C6 C5 125.3(11) . . ? O7 C6 C5 111.2(10) . . ? C6 O7 C7 115.1(11) . . ? N1 C11 C12 111.0(8) . . ? N1 C11 C5 111.7(8) . . ? C12 C11 C5 109.2(8) . . ? C13 C12 C11 121.5(11) . . ? C12 C13 C14 121.0(11) . . ? C15 C14 C13 125.7(12) . . ? C15 C14 C21 117.5(12) . . ? C13 C14 C21 116.5(11) . . ? C16 C15 C14 123.3(12) . . ? C15 C16 C17 121.1(11) . . ? C18 C17 C16 125.7(11) . . ? C18 C17 C22 117.8(11) . . ? C16 C17 C22 116.5(11) . . ? C19 C18 C17 120.9(11) . . ? C18 C19 C20 118.8(11) . . ? N2 C20 C19 122.5(11) . . ? N1 C21 C22 118.0(9) . . ? N1 C21 C14 123.3(10) . . ? C22 C21 C14 118.3(10) . . ? N2 C22 C17 121.0(10) . . ? N2 C22 C21 115.9(8) . . ? C17 C22 C21 123.1(10) . . ? C36 C31 C32 116.0(10) . . ? C36 C31 P1 120.8(9) . . ? C32 C31 P1 123.0(8) . . ? C33 C32 C31 122.6(11) . . ? C32 C33 C34 119.6(12) . . ? C35 C34 C33 119.2(12) . . ? C34 C35 C36 119.6(12) . . ? C31 C36 C35 122.8(12) . . ? C46 C41 C42 118.1(10) . . ? C46 C41 P1 119.9(9) . . ? C42 C41 P1 121.9(9) . . ? C43 C42 C41 120.5(12) . . ? C44 C43 C42 121.8(14) . . ? C45 C44 C43 118.3(14) . . ? C44 C45 C46 121.7(13) . . ? C41 C46 C45 119.6(12) . . ? Cl92 Cl91 C90 94(4) 5_766 5_766 ? Cl92 Cl91 C90 137(5) 5_766 . ? C90 Cl91 C90 104(3) 5_766 . ? Cl92 Cl91 Cl91 135(4) 5_766 5_766 ? C90 Cl91 Cl91 64(3) 5_766 5_766 ? C90 Cl91 Cl91 40.4(16) . 5_766 ? Cl91 Cl92 C90 46(2) 5_766 . ? Cl91 C90 Cl92 40.1(17) 5_766 . ? Cl91 C90 Cl91 76(2) 5_766 . ? Cl92 C90 Cl91 106.9 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.135 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.145 #===END