# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2016 data_global _publ_contact_author_name 'Dr \Isabel Santos' _publ_contact_author_address ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; _publ_contact_author_phone '00351 21 994 60 00' _publ_contact_author_fax '00351 21 994 14 55' _publ_contact_author_email 'isantos@itn1.itn.pt' _publ_requested_journal 'J. Chem. Soc., Dalton Trans' _publ_section_title ; Novel six-co-ordinate oxorhenium complexes with ligands containing PN~2~ and PNO donor atom sets: syntheses and characterization ; loop_ _publ_author_name _publ_author_address 'Correia, Jo\~ao D. G. ' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Domingos, \^Angela' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Paulo, Antonio' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; 'Santos, Isabel' ; Departamento de Quimica Instituto Tecnologico e Nuclear Estrada Nacional 10 2686-953 Sacavem Portugal ; data_re2lnh2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [ReO(k3-PN2)(OMe)Cl].CH3OH _chemical_formula_analytical ? _chemical_formula_sum 'C23 H27 Cl N2 O4 P Re' _chemical_formula_weight 648.09 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1698(10) _cell_length_b 24.026(3) _cell_length_c 10.8833(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.519(9) _cell_angle_gamma 90.00 _cell_volume 2377.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 12.9 _exptl_crystal_description 'irregular-prismatic' _exptl_crystal_colour purple _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method ? _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 5.324 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.7499 _exptl_absorpt_correction_T_max 0.9994 _exptl_special_details ; Crystals obtained by slow evaporation of a methanolic solution of the compound ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2.1 _diffrn_reflns_number 4911 _diffrn_reflns_av_R_equivalents 0.1210 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4665 _reflns_number_observed 3244 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 535 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+13.7023P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4130 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_obs 0.0500 _refine_ls_wR_factor_all 0.1128 _refine_ls_wR_factor_obs 0.0830 _refine_ls_goodness_of_fit_all 1.119 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.278 _refine_ls_restrained_S_obs 1.137 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.17005(4) 0.16700(2) 0.16220(3) 0.02817(11) Uani 1 d . . Cl1 Cl 0.0141(3) 0.12856(13) -0.0182(2) 0.0490(7) Uani 1 d . . P1 P 0.1085(3) 0.09421(10) 0.2969(2) 0.0277(5) Uani 1 d . . O1 O 0.0217(7) 0.2065(3) 0.1976(6) 0.044(2) Uani 1 d . . O2 O 0.3193(7) 0.1240(3) 0.1059(6) 0.033(2) Uani 1 d . . O3 O 0.4969(8) 0.1945(3) 0.4578(6) 0.055(2) Uani 1 d . . N1 N 0.3196(8) 0.2011(3) 0.2945(7) 0.031(2) Uani 1 d . . N2 N 0.2420(9) 0.2351(3) 0.0525(7) 0.038(2) Uani 1 d . . H2A H 0.3019(9) 0.2225(3) -0.0004(7) 0.045 Uiso 1 calc R . H2B H 0.1641(9) 0.2519(3) 0.0087(7) 0.045 Uiso 1 calc R . C1 C 0.4157(12) 0.2428(4) 0.2418(10) 0.046(3) Uani 1 d . . H1A H 0.4945(12) 0.2240(4) 0.2070(10) 0.055 Uiso 1 calc R . H1B H 0.4589(12) 0.2679(4) 0.3062(10) 0.055 Uiso 1 calc R . C2 C 0.3213(13) 0.2745(4) 0.1427(10) 0.049(3) Uani 1 d . . H2A H 0.2510(13) 0.2971(4) 0.1798(10) 0.059 Uiso 1 calc R . H2B H 0.3822(13) 0.2991(4) 0.1003(10) 0.059 Uiso 1 calc R . C3 C 0.3704(11) 0.1833(4) 0.4104(9) 0.037(2) Uani 1 d . . C20 C 0.3621(13) 0.0949(5) 0.0043(10) 0.055(3) Uani 1 d . . H20A H 0.4577(13) 0.0789(5) 0.0274(10) 0.083 Uiso 1 calc R . H20B H 0.3655(13) 0.1201(5) -0.0637(10) 0.083 Uiso 1 calc R . H20C H 0.2924(13) 0.0658(5) -0.0200(10) 0.083 Uiso 1 calc R . C100 C 0.1498(11) 0.1187(4) 0.4540(8) 0.033(2) Uani 1 d . . C101 C 0.2696(11) 0.1551(4) 0.4882(8) 0.035(2) Uani 1 d . . C102 C 0.2948(12) 0.1713(5) 0.6142(9) 0.050(3) Uani 1 d . . H102 H 0.3728(12) 0.1951(5) 0.6399(9) 0.060 Uiso 1 calc R . C103 C 0.2083(14) 0.1533(5) 0.6993(10) 0.060(4) Uani 1 d . . H103 H 0.2281(14) 0.1653(5) 0.7810(10) 0.072 Uiso 1 calc R . C104 C 0.0933(14) 0.1178(5) 0.6664(10) 0.051(3) Uani 1 d . . H104 H 0.0349(14) 0.1055(5) 0.7247(10) 0.061 Uiso 1 calc R . C105 C 0.0657(12) 0.1004(5) 0.5432(9) 0.046(3) Uani 1 d . . H105 H -0.0113(12) 0.0758(5) 0.5201(9) 0.055 Uiso 1 calc R . C200 C -0.0865(10) 0.0753(4) 0.2810(9) 0.032(2) Uani 1 d . . C201 C -0.1356(11) 0.0229(5) 0.2559(12) 0.054(3) Uani 1 d . . H201 H -0.0693(11) -0.0054(5) 0.2453(12) 0.065 Uiso 1 calc R . C202 C -0.2851(12) 0.0116(5) 0.2460(13) 0.068(4) Uani 1 d . . H202 H -0.3173(12) -0.0248(5) 0.2317(13) 0.082 Uiso 1 calc R . C203 C -0.3827(12) 0.0510(5) 0.2564(11) 0.054(3) Uani 1 d . . H203 H -0.4826(12) 0.0428(5) 0.2465(11) 0.065 Uiso 1 calc R . C204 C -0.3349(14) 0.1041(6) 0.2817(14) 0.073(4) Uani 1 d . . H204 H -0.4031(14) 0.1319(6) 0.2912(14) 0.087 Uiso 1 calc R . C205 C -0.1891(13) 0.1169(5) 0.2934(14) 0.074(5) Uani 1 d . . H205 H -0.1582(13) 0.1534(5) 0.3095(14) 0.089 Uiso 1 calc R . C300 C 0.2058(10) 0.0292(4) 0.2884(10) 0.036(2) Uani 1 d . . C301 C 0.2043(10) 0.0034(4) 0.1747(10) 0.042(3) Uani 1 d . . H301 H 0.1551(10) 0.0198(4) 0.1037(10) 0.050 Uiso 1 calc R . C302 C 0.2759(12) -0.0467(5) 0.1668(12) 0.056(3) Uani 1 d . . H302 H 0.2731(12) -0.0638(5) 0.0899(12) 0.067 Uiso 1 calc R . C303 C 0.3509(13) -0.0718(5) 0.2686(13) 0.061(4) Uani 1 d . . H303 H 0.4006(13) -0.1051(5) 0.2606(13) 0.073 Uiso 1 calc R . C304 C 0.3522(12) -0.0470(5) 0.3843(11) 0.053(3) Uani 1 d . . H304 H 0.4010(12) -0.0639(5) 0.4549(11) 0.064 Uiso 1 calc R . C305 C 0.2799(10) 0.0032(5) 0.3930(10) 0.044(3) Uani 1 d . . H305 H 0.2809(10) 0.0200(5) 0.4701(10) 0.052 Uiso 1 calc R . O1S O 0.5062(12) 0.2213(5) 0.9091(10) 0.095(3) Uani 1 d . . H1S H 0.4183(12) 0.2360(5) 0.8703(10) 0.114 Uiso 1 calc R . C1S C 0.6380(19) 0.1992(6) 0.9673(14) 0.087(5) Uani 1 d . . H1S1 H 0.6836(19) 0.1774(6) 0.9089(14) 0.131 Uiso 1 calc R . H1S2 H 0.6185(19) 0.1759(6) 1.0351(14) 0.131 Uiso 1 calc R . H1S3 H 0.7026(19) 0.2289(6) 0.9980(14) 0.131 Uiso 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 0.0242(2) 0.0345(2) 0.0252(2) 0.0015(2) 0.00106(12) -0.0048(2) Cl1 0.0403(14) 0.074(2) 0.0309(13) -0.0053(14) -0.0022(11) -0.0133(14) P1 0.0261(12) 0.0295(13) 0.0275(13) -0.0003(10) 0.0038(10) -0.0019(10) O1 0.033(4) 0.047(4) 0.052(4) 0.002(4) 0.012(3) 0.008(3) O2 0.029(3) 0.036(4) 0.036(4) -0.003(3) 0.014(3) 0.005(3) O3 0.039(4) 0.084(6) 0.037(4) -0.007(4) -0.016(4) -0.011(4) N1 0.033(4) 0.032(5) 0.024(4) -0.002(3) -0.005(4) -0.005(4) N2 0.030(4) 0.054(6) 0.029(4) 0.007(4) -0.001(4) 0.001(4) C1 0.045(6) 0.049(7) 0.044(6) -0.001(5) 0.003(5) -0.025(5) C2 0.058(7) 0.034(6) 0.053(7) 0.006(5) 0.004(6) -0.008(5) C3 0.038(6) 0.036(6) 0.035(6) -0.009(4) -0.003(5) -0.003(4) C20 0.062(8) 0.058(8) 0.049(7) -0.007(6) 0.021(6) 0.014(6) C100 0.036(5) 0.037(6) 0.024(5) 0.006(4) 0.000(4) 0.003(5) C101 0.043(6) 0.033(6) 0.027(5) 0.002(4) 0.000(4) 0.009(4) C102 0.054(6) 0.062(7) 0.030(5) -0.004(6) -0.006(5) -0.013(6) C103 0.076(9) 0.074(10) 0.029(6) 0.005(6) 0.005(6) 0.002(7) C104 0.075(8) 0.046(7) 0.036(6) 0.005(5) 0.026(6) 0.005(6) C105 0.051(7) 0.051(7) 0.036(6) -0.003(5) 0.006(5) -0.002(5) C200 0.022(5) 0.041(6) 0.035(5) 0.007(5) 0.011(4) -0.004(4) C201 0.026(5) 0.041(7) 0.096(10) -0.010(6) 0.008(6) 0.000(5) C202 0.038(7) 0.050(8) 0.114(12) -0.019(8) 0.004(7) -0.006(6) C203 0.023(5) 0.072(9) 0.068(8) 0.017(7) 0.008(5) -0.001(6) C204 0.043(7) 0.062(9) 0.120(13) 0.016(8) 0.036(8) 0.017(6) C205 0.037(7) 0.048(7) 0.144(15) -0.007(8) 0.033(8) 0.000(6) C300 0.026(5) 0.034(6) 0.048(6) 0.004(5) 0.008(5) -0.005(4) C301 0.027(6) 0.038(6) 0.059(7) 0.011(6) -0.001(5) 0.003(4) C302 0.042(7) 0.048(7) 0.079(9) -0.013(7) 0.019(6) -0.003(6) C303 0.042(7) 0.037(7) 0.102(11) -0.005(7) 0.007(7) 0.006(5) C304 0.049(7) 0.058(8) 0.053(7) 0.022(6) 0.005(6) 0.013(6) C305 0.035(6) 0.045(6) 0.054(7) 0.004(6) 0.020(5) -0.002(5) O1S 0.082(7) 0.110(9) 0.098(8) 0.039(7) 0.033(7) 0.003(7) C1S 0.112(14) 0.067(10) 0.091(12) -0.009(9) 0.042(11) -0.020(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.742(6) . ? Re1 O2 1.881(6) . ? Re1 N1 2.027(7) . ? Re1 N2 2.178(8) . ? Re1 P1 2.397(2) . ? Re1 Cl1 2.453(3) . ? P1 C100 1.801(9) . ? P1 C300 1.808(10) . ? P1 C200 1.830(9) . ? O2 C20 1.406(11) . ? O3 C3 1.236(11) . ? N1 C3 1.355(12) . ? N1 C1 1.497(12) . ? N2 C2 1.483(12) . ? C1 C2 1.500(14) . ? C3 C101 1.496(13) . ? C100 C105 1.388(14) . ? C100 C101 1.414(13) . ? C101 C102 1.415(13) . ? C102 C103 1.367(15) . ? C103 C104 1.37(2) . ? C104 C105 1.396(14) . ? C200 C201 1.352(14) . ? C200 C205 1.392(14) . ? C201 C202 1.388(14) . ? C202 C203 1.32(2) . ? C203 C204 1.36(2) . ? C204 C205 1.36(2) . ? C300 C301 1.382(14) . ? C300 C305 1.394(14) . ? C301 C302 1.379(14) . ? C302 C303 1.37(2) . ? C303 C304 1.39(2) . ? C304 C305 1.386(15) . ? O1S C1S 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 O2 173.6(3) . . ? O1 Re1 N1 95.6(3) . . ? O2 Re1 N1 90.0(3) . . ? O1 Re1 N2 90.7(3) . . ? O2 Re1 N2 87.1(3) . . ? N1 Re1 N2 82.0(3) . . ? O1 Re1 P1 90.5(2) . . ? O2 Re1 P1 92.2(2) . . ? N1 Re1 P1 93.0(2) . . ? N2 Re1 P1 174.9(2) . . ? O1 Re1 Cl1 89.5(2) . . ? O2 Re1 Cl1 84.5(2) . . ? N1 Re1 Cl1 171.9(2) . . ? N2 Re1 Cl1 91.8(2) . . ? P1 Re1 Cl1 93.18(9) . . ? C100 P1 C300 106.7(5) . . ? C100 P1 C200 104.7(4) . . ? C300 P1 C200 105.2(4) . . ? C100 P1 Re1 107.8(3) . . ? C300 P1 Re1 116.2(3) . . ? C200 P1 Re1 115.4(3) . . ? C20 O2 Re1 145.0(7) . . ? C3 N1 C1 114.8(8) . . ? C3 N1 Re1 130.7(6) . . ? C1 N1 Re1 112.1(6) . . ? C2 N2 Re1 105.9(6) . . ? N1 C1 C2 107.6(8) . . ? N2 C2 C1 109.7(8) . . ? O3 C3 N1 120.7(9) . . ? O3 C3 C101 118.6(9) . . ? N1 C3 C101 120.5(9) . . ? C105 C100 C101 119.7(9) . . ? C105 C100 P1 119.5(8) . . ? C101 C100 P1 120.7(7) . . ? C100 C101 C102 116.6(9) . . ? C100 C101 C3 130.4(8) . . ? C102 C101 C3 112.8(9) . . ? C103 C102 C101 122.2(11) . . ? C102 C103 C104 121.1(11) . . ? C103 C104 C105 118.4(11) . . ? C100 C105 C104 122.0(11) . . ? C201 C200 C205 118.5(9) . . ? C201 C200 P1 123.1(8) . . ? C205 C200 P1 118.5(8) . . ? C200 C201 C202 119.8(10) . . ? C203 C202 C201 121.9(12) . . ? C202 C203 C204 119.0(11) . . ? C205 C204 C203 121.1(12) . . ? C204 C205 C200 119.7(12) . . ? C301 C300 C305 118.5(10) . . ? C301 C300 P1 119.1(8) . . ? C305 C300 P1 122.4(8) . . ? C302 C301 C300 119.8(10) . . ? C303 C302 C301 121.9(12) . . ? C302 C303 C304 119.3(11) . . ? C305 C304 C303 119.1(10) . . ? C304 C305 C300 121.4(11) . . ? _refine_diff_density_max 1.072 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.173 data_lrenop _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [ReO(k3-PNO)(k2-DPPBA)].CH3OH _chemical_formula_analytical ? _chemical_formula_sum 'C41 H36 N O6 P2 Re' _chemical_formula_weight 886.85 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' '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 9.496(1) _cell_length_b 13.118(2) _cell_length_c 15.706(2) _cell_angle_alpha 83.860(10) _cell_angle_beta 83.550(10) _cell_angle_gamma 69.170(10) _cell_volume 1812.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15.1 _exptl_crystal_description irregular _exptl_crystal_colour 'brownish-red' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method ? _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 3.490 _exptl_absorpt_correction_type 'empirical via \y-scan North et al(1968)' _exptl_absorpt_correction_T_min 0.7437 _exptl_absorpt_correction_T_max 0.9990 _exptl_special_details ; Crystals obtained by slow evaporation of a solution of the compound in CH2Cl2/MeOH ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 7007 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.03 _reflns_number_total 6551 _reflns_number_observed 5456 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MolEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+3.6906P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6549 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_obs 0.0399 _refine_ls_wR_factor_all 0.0869 _refine_ls_wR_factor_obs 0.0758 _refine_ls_goodness_of_fit_all 1.116 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.24803(3) 0.06278(2) 0.16386(2) 0.03031(9) Uani 1 d . . P1 P 0.1570(2) 0.25411(12) 0.10469(10) 0.0290(3) Uani 1 d . . P2 P 0.3401(2) 0.06254(13) 0.30491(10) 0.0300(3) Uani 1 d . . O1 O 0.4204(5) 0.0453(3) 0.1163(3) 0.0416(11) Uani 1 d . . O3 O 0.1330(5) 0.0465(3) 0.0740(3) 0.0417(11) Uani 1 d . . O2 O 0.0437(5) 0.1284(3) 0.2388(3) 0.0366(10) Uani 1 d . . O100 O 0.2830(6) -0.2531(4) 0.2731(3) 0.0523(13) Uani 1 d . . O200 O -0.1788(6) 0.2280(5) 0.2965(3) 0.070(2) Uani 1 d . . N1 N 0.2468(6) -0.0897(4) 0.2001(3) 0.0368(13) Uani 1 d . . C1 C 0.2585(7) -0.1533(5) 0.2746(4) 0.0325(14) Uani 1 d . . C2 C -0.0900(8) 0.2026(5) 0.2338(5) 0.040(2) Uani 1 d . . C3 C 0.1393(11) -0.0613(6) 0.0657(5) 0.066(2) Uani 1 d . . H3A H 0.1706(11) -0.0790(6) 0.0066(5) 0.079 Uiso 1 calc R . H3B H 0.0388(11) -0.0649(6) 0.0790(5) 0.079 Uiso 1 calc R . C4 C 0.2437(10) -0.1432(5) 0.1220(4) 0.052(2) Uani 1 d . . H4A H 0.3441(10) -0.1700(5) 0.0928(4) 0.063 Uiso 1 calc R . H4B H 0.2095(10) -0.2047(5) 0.1376(4) 0.063 Uiso 1 calc R . C10 C -0.0380(7) 0.2837(4) 0.0837(4) 0.0312(14) Uani 1 d . . C11 C 0.2503(7) 0.2763(5) 0.0006(4) 0.0335(14) Uani 1 d . . C12 C 0.1558(7) 0.3652(5) 0.1648(4) 0.0325(14) Uani 1 d . . C20 C 0.2608(7) -0.0192(5) 0.3833(4) 0.0320(14) Uani 1 d . . C21 C 0.5433(7) -0.0116(5) 0.3020(4) 0.0340(14) Uani 1 d . . C22 C 0.3103(7) 0.1846(5) 0.3595(4) 0.0355(15) Uani 1 d . . C101 C -0.1369(7) 0.2570(5) 0.1476(4) 0.0318(14) Uani 1 d . . C102 C -0.2859(7) 0.2833(6) 0.1315(5) 0.044(2) Uani 1 d . . H102 H -0.3531(7) 0.2689(6) 0.1748(5) 0.053 Uiso 1 calc R . C103 C -0.3380(8) 0.3303(6) 0.0531(5) 0.047(2) Uani 1 d . . H103 H -0.4381(8) 0.3447(6) 0.0430(5) 0.056 Uiso 1 calc R . C104 C -0.2427(8) 0.3554(5) -0.0090(4) 0.044(2) Uani 1 d . . H104 H -0.2778(8) 0.3881(5) -0.0617(4) 0.053 Uiso 1 calc R . C105 C -0.0931(7) 0.3329(5) 0.0054(4) 0.0342(14) Uani 1 d . . H105 H -0.0286(7) 0.3509(5) -0.0378(4) 0.041 Uiso 1 calc R . C111 C 0.2902(8) 0.1971(5) -0.0577(4) 0.044(2) Uani 1 d . . H111 H 0.2756(8) 0.1309(5) -0.0421(4) 0.053 Uiso 1 calc R . C112 C 0.3509(9) 0.2158(6) -0.1383(5) 0.056(2) Uani 1 d . . H112 H 0.3754(9) 0.1627(6) -0.1776(5) 0.067 Uiso 1 calc R . C113 C 0.3764(8) 0.3126(6) -0.1623(5) 0.054(2) Uani 1 d . . H113 H 0.4189(8) 0.3243(6) -0.2171(5) 0.065 Uiso 1 calc R . C114 C 0.3385(8) 0.3909(6) -0.1048(5) 0.048(2) Uani 1 d . . H114 H 0.3555(8) 0.4563(6) -0.1203(5) 0.058 Uiso 1 calc R . C115 C 0.2749(7) 0.3732(5) -0.0238(4) 0.041(2) Uani 1 d . . H115 H 0.2484(7) 0.4272(5) 0.0149(4) 0.049 Uiso 1 calc R . C121 C 0.2920(8) 0.3627(6) 0.1903(4) 0.042(2) Uani 1 d . . H121 H 0.3788(8) 0.3022(6) 0.1805(4) 0.051 Uiso 1 calc R . C122 C 0.3001(9) 0.4480(7) 0.2298(5) 0.054(2) Uani 1 d . . H122 H 0.3925(9) 0.4456(7) 0.2460(5) 0.065 Uiso 1 calc R . C123 C 0.1725(11) 0.5374(7) 0.2457(5) 0.063(2) Uani 1 d . . H123 H 0.1784(11) 0.5955(7) 0.2726(5) 0.076 Uiso 1 calc R . C124 C 0.0359(10) 0.5405(6) 0.2215(5) 0.061(2) Uani 1 d . . H124 H -0.0510(10) 0.6004(6) 0.2325(5) 0.074 Uiso 1 calc R . C125 C 0.0282(8) 0.4548(5) 0.1810(4) 0.043(2) Uani 1 d . . H125 H -0.0641(8) 0.4574(5) 0.1644(4) 0.052 Uiso 1 calc R . C201 C 0.2394(8) 0.0048(5) 0.4686(4) 0.041(2) Uani 1 d . . H201 H 0.2610(8) 0.0639(5) 0.4839(4) 0.049 Uiso 1 calc R . C202 C 0.1869(8) -0.0573(6) 0.5305(4) 0.052(2) Uani 1 d . . H202 H 0.1738(8) -0.0403(6) 0.5875(4) 0.063 Uiso 1 calc R . C203 C 0.1534(8) -0.1438(7) 0.5095(5) 0.053(2) Uani 1 d . . H203 H 0.1162(8) -0.1852(7) 0.5517(5) 0.064 Uiso 1 calc R . C204 C 0.1756(8) -0.1689(6) 0.4252(4) 0.046(2) Uani 1 d . . H204 H 0.1510(8) -0.2273(6) 0.4112(4) 0.055 Uiso 1 calc R . C205 C 0.2331(7) -0.1110(5) 0.3603(4) 0.0310(14) Uani 1 d . . C211 C 0.6053(8) -0.1069(6) 0.3525(4) 0.046(2) Uani 1 d . . H211 H 0.5433(8) -0.1331(6) 0.3919(4) 0.055 Uiso 1 calc R . C212 C 0.7591(8) -0.1635(7) 0.3446(5) 0.060(2) Uani 1 d . . H212 H 0.7997(8) -0.2284(7) 0.3780(5) 0.071 Uiso 1 calc R . C213 C 0.8521(9) -0.1251(8) 0.2884(6) 0.064(2) Uani 1 d . . H213 H 0.9556(9) -0.1637(8) 0.2834(6) 0.077 Uiso 1 calc R . C214 C 0.7918(9) -0.0288(8) 0.2390(6) 0.067(2) Uani 1 d . . H214 H 0.8546(9) -0.0017(8) 0.2010(6) 0.080 Uiso 1 calc R . C215 C 0.6387(8) 0.0270(6) 0.2462(5) 0.047(2) Uani 1 d . . H215 H 0.5987(8) 0.0921(6) 0.2129(5) 0.057 Uiso 1 calc R . C221 C 0.4244(9) 0.2059(6) 0.3924(5) 0.051(2) Uani 1 d . . H221 H 0.5238(9) 0.1588(6) 0.3837(5) 0.061 Uiso 1 calc R . C222 C 0.3922(11) 0.2969(7) 0.4383(5) 0.070(3) Uani 1 d . . H222 H 0.4701(11) 0.3111(7) 0.4600(5) 0.084 Uiso 1 calc R . C223 C 0.2480(12) 0.3654(7) 0.4516(6) 0.068(2) Uani 1 d . . H223 H 0.2270(12) 0.4260(7) 0.4832(6) 0.082 Uiso 1 calc R . C224 C 0.1330(10) 0.3463(6) 0.4192(5) 0.056(2) Uani 1 d . . H224 H 0.0340(10) 0.3939(6) 0.4282(5) 0.067 Uiso 1 calc R . C225 C 0.1643(8) 0.2565(5) 0.3733(4) 0.043(2) Uani 1 d . . H225 H 0.0857(8) 0.2438(5) 0.3512(4) 0.052 Uiso 1 calc R . O1S O 0.6980(14) 0.4198(10) 0.4204(9) 0.188(5) Uiso 1 d . . C1S C 0.7088(40) 0.4770(30) 0.3429(24) 0.375(19) Uiso 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 0.03566(15) 0.02518(13) 0.03084(13) -0.00126(9) -0.01208(10) -0.00894(10) P1 0.0298(9) 0.0262(8) 0.0316(8) -0.0016(6) -0.0069(7) -0.0093(7) P2 0.0327(9) 0.0293(8) 0.0306(8) -0.0026(6) -0.0084(7) -0.0122(7) O1 0.048(3) 0.036(2) 0.032(2) -0.006(2) -0.001(2) -0.004(2) O3 0.056(3) 0.032(2) 0.039(2) -0.003(2) -0.021(2) -0.011(2) O2 0.036(3) 0.042(3) 0.034(2) 0.001(2) -0.006(2) -0.016(2) O100 0.075(4) 0.035(3) 0.052(3) -0.003(2) -0.004(3) -0.026(3) O200 0.047(3) 0.091(4) 0.047(3) 0.009(3) 0.008(3) 0.000(3) N1 0.054(4) 0.026(3) 0.034(3) -0.004(2) -0.014(3) -0.014(3) C1 0.034(4) 0.026(3) 0.040(4) 0.001(3) -0.009(3) -0.013(3) C2 0.033(4) 0.036(4) 0.051(4) 0.003(3) -0.008(3) -0.012(3) C3 0.102(7) 0.040(4) 0.061(5) -0.008(4) -0.043(5) -0.020(4) C4 0.086(6) 0.032(4) 0.043(4) -0.003(3) -0.029(4) -0.018(4) C10 0.033(3) 0.020(3) 0.039(3) -0.003(2) -0.008(3) -0.006(3) C11 0.034(4) 0.035(3) 0.028(3) -0.007(3) -0.004(3) -0.006(3) C12 0.042(4) 0.027(3) 0.032(3) 0.001(3) -0.010(3) -0.015(3) C20 0.030(3) 0.032(3) 0.034(3) 0.003(3) -0.010(3) -0.010(3) C21 0.034(4) 0.035(3) 0.037(3) -0.006(3) -0.009(3) -0.014(3) C22 0.046(4) 0.033(3) 0.034(3) 0.000(3) -0.009(3) -0.019(3) C101 0.032(3) 0.022(3) 0.042(4) 0.000(3) -0.014(3) -0.007(3) C102 0.030(4) 0.046(4) 0.060(5) 0.005(3) -0.007(3) -0.019(3) C103 0.034(4) 0.046(4) 0.061(5) 0.002(4) -0.022(4) -0.011(3) C104 0.056(5) 0.042(4) 0.038(4) 0.002(3) -0.022(3) -0.017(4) C105 0.038(4) 0.032(3) 0.033(3) -0.001(3) -0.011(3) -0.011(3) C111 0.053(5) 0.033(4) 0.044(4) -0.001(3) -0.006(3) -0.013(3) C112 0.063(5) 0.055(5) 0.038(4) -0.013(4) 0.002(4) -0.006(4) C113 0.048(5) 0.063(5) 0.041(4) 0.002(4) 0.006(4) -0.011(4) C114 0.039(4) 0.052(4) 0.054(5) 0.009(4) -0.003(3) -0.019(4) C115 0.044(4) 0.034(4) 0.044(4) -0.004(3) -0.001(3) -0.013(3) C121 0.035(4) 0.045(4) 0.052(4) 0.002(3) -0.008(3) -0.019(3) C122 0.063(5) 0.062(5) 0.055(5) -0.001(4) -0.018(4) -0.039(5) C123 0.092(7) 0.051(5) 0.063(5) -0.003(4) -0.030(5) -0.038(5) C124 0.073(6) 0.032(4) 0.075(6) -0.017(4) -0.016(5) -0.008(4) C125 0.043(4) 0.037(4) 0.048(4) -0.007(3) -0.011(3) -0.009(3) C201 0.048(4) 0.040(4) 0.036(4) 0.000(3) -0.010(3) -0.016(3) C202 0.057(5) 0.064(5) 0.033(4) -0.005(4) -0.001(3) -0.018(4) C203 0.050(5) 0.066(5) 0.042(4) 0.016(4) -0.006(4) -0.023(4) C204 0.044(4) 0.058(5) 0.046(4) 0.002(3) -0.007(3) -0.029(4) C205 0.025(3) 0.033(3) 0.034(3) 0.002(3) -0.005(3) -0.010(3) C211 0.038(4) 0.052(4) 0.042(4) -0.003(3) -0.008(3) -0.008(3) C212 0.040(5) 0.068(5) 0.058(5) -0.003(4) -0.020(4) 0.002(4) C213 0.032(4) 0.088(7) 0.068(6) -0.029(5) -0.005(4) -0.007(4) C214 0.042(5) 0.082(6) 0.087(6) -0.017(5) 0.004(4) -0.034(5) C215 0.040(4) 0.043(4) 0.064(5) 0.002(3) -0.009(4) -0.021(3) C221 0.051(5) 0.046(4) 0.058(5) -0.007(4) -0.022(4) -0.014(4) C222 0.087(7) 0.066(6) 0.073(6) -0.023(5) -0.029(5) -0.035(5) C223 0.099(8) 0.044(5) 0.070(6) -0.021(4) -0.010(5) -0.030(5) C224 0.071(6) 0.039(4) 0.050(4) -0.008(3) -0.001(4) -0.010(4) C225 0.051(4) 0.037(4) 0.043(4) -0.004(3) -0.012(3) -0.013(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 O1 1.668(4) . ? Re1 O3 1.951(4) . ? Re1 N1 2.025(5) . ? Re1 O2 2.100(4) . ? Re1 P1 2.459(2) . ? Re1 P2 2.471(2) . ? P1 C10 1.813(6) . ? P1 C12 1.815(6) . ? P1 C11 1.817(6) . ? P2 C22 1.816(6) . ? P2 C20 1.821(6) . ? P2 C21 1.824(6) . ? O3 C3 1.413(8) . ? O2 C2 1.301(7) . ? O100 C1 1.249(7) . ? O200 C2 1.214(8) . ? N1 C1 1.352(7) . ? N1 C4 1.485(8) . ? C1 C205 1.473(8) . ? C2 C101 1.498(9) . ? C3 C4 1.468(9) . ? C10 C105 1.392(8) . ? C10 C101 1.400(8) . ? C11 C115 1.379(8) . ? C11 C111 1.381(9) . ? C12 C125 1.377(9) . ? C12 C121 1.385(8) . ? C20 C201 1.384(9) . ? C20 C205 1.411(8) . ? C21 C215 1.378(9) . ? C21 C211 1.381(9) . ? C22 C221 1.375(9) . ? C22 C225 1.380(9) . ? C101 C102 1.377(8) . ? C102 C103 1.379(9) . ? C103 C104 1.350(9) . ? C104 C105 1.384(9) . ? C111 C112 1.366(9) . ? C112 C113 1.382(10) . ? C113 C114 1.364(10) . ? C114 C115 1.379(9) . ? C121 C122 1.365(10) . ? C122 C123 1.376(11) . ? C123 C124 1.378(11) . ? C124 C125 1.378(9) . ? C201 C202 1.367(9) . ? C202 C203 1.363(10) . ? C203 C204 1.374(10) . ? C204 C205 1.386(9) . ? C211 C212 1.381(10) . ? C212 C213 1.363(11) . ? C213 C214 1.379(12) . ? C214 C215 1.373(10) . ? C221 C222 1.384(10) . ? C222 C223 1.352(12) . ? C223 C224 1.364(11) . ? C224 C225 1.371(9) . ? O1S C1S 1.37(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 O1 Re1 O3 104.9(2) . . ? O1 Re1 N1 105.4(2) . . ? O3 Re1 N1 80.7(2) . . ? O1 Re1 O2 161.0(2) . . ? O3 Re1 O2 88.7(2) . . ? N1 Re1 O2 89.7(2) . . ? O1 Re1 P1 90.58(15) . . ? O3 Re1 P1 81.58(13) . . ? N1 Re1 P1 158.7(2) . . ? O2 Re1 P1 78.08(12) . . ? O1 Re1 P2 90.23(15) . . ? O3 Re1 P2 162.85(14) . . ? N1 Re1 P2 87.54(14) . . ? O2 Re1 P2 78.70(12) . . ? P1 Re1 P2 106.76(5) . . ? C10 P1 C12 105.8(3) . . ? C10 P1 C11 104.6(3) . . ? C12 P1 C11 104.0(3) . . ? C10 P1 Re1 105.7(2) . . ? C12 P1 Re1 121.8(2) . . ? C11 P1 Re1 113.5(2) . . ? C22 P2 C20 103.4(3) . . ? C22 P2 C21 105.0(3) . . ? C20 P2 C21 103.8(3) . . ? C22 P2 Re1 124.5(2) . . ? C20 P2 Re1 108.4(2) . . ? C21 P2 Re1 109.8(2) . . ? C3 O3 Re1 115.5(4) . . ? C2 O2 Re1 140.6(4) . . ? C1 N1 C4 115.6(5) . . ? C1 N1 Re1 135.8(4) . . ? C4 N1 Re1 108.4(4) . . ? O100 C1 N1 119.8(6) . . ? O100 C1 C205 116.2(5) . . ? N1 C1 C205 123.9(5) . . ? O200 C2 O2 122.2(6) . . ? O200 C2 C101 119.0(6) . . ? O2 C2 C101 118.9(6) . . ? O3 C3 C4 113.1(6) . . ? C3 C4 N1 107.6(5) . . ? C105 C10 C101 118.6(6) . . ? C105 C10 P1 121.8(5) . . ? C101 C10 P1 119.6(4) . . ? C115 C11 C111 118.9(6) . . ? C115 C11 P1 121.6(5) . . ? C111 C11 P1 119.4(5) . . ? C125 C12 C121 118.8(6) . . ? C125 C12 P1 123.0(5) . . ? C121 C12 P1 118.1(5) . . ? C201 C20 C205 119.8(6) . . ? C201 C20 P2 118.5(5) . . ? C205 C20 P2 121.5(5) . . ? C215 C21 C211 118.5(6) . . ? C215 C21 P2 119.1(5) . . ? C211 C21 P2 122.3(5) . . ? C221 C22 C225 118.2(6) . . ? C221 C22 P2 123.4(5) . . ? C225 C22 P2 118.3(5) . . ? C102 C101 C10 118.9(6) . . ? C102 C101 C2 117.8(6) . . ? C10 C101 C2 123.4(5) . . ? C101 C102 C103 121.7(7) . . ? C104 C103 C102 119.6(6) . . ? C103 C104 C105 120.4(6) . . ? C104 C105 C10 120.8(6) . . ? C112 C111 C11 120.0(7) . . ? C111 C112 C113 120.9(7) . . ? C114 C113 C112 119.3(7) . . ? C113 C114 C115 120.0(7) . . ? C11 C115 C114 120.8(6) . . ? C122 C121 C12 120.7(7) . . ? C121 C122 C123 120.4(7) . . ? C122 C123 C124 119.5(7) . . ? C125 C124 C123 120.0(7) . . ? C124 C125 C12 120.6(7) . . ? C202 C201 C20 120.8(6) . . ? C203 C202 C201 120.7(7) . . ? C202 C203 C204 119.0(7) . . ? C203 C204 C205 122.8(7) . . ? C204 C205 C20 116.9(6) . . ? C204 C205 C1 115.6(6) . . ? C20 C205 C1 127.5(5) . . ? C21 C211 C212 120.3(7) . . ? C213 C212 C211 120.6(8) . . ? C212 C213 C214 119.6(7) . . ? C215 C214 C213 119.8(8) . . ? C214 C215 C21 121.2(7) . . ? C22 C221 C222 120.3(7) . . ? C223 C222 C221 120.2(8) . . ? C222 C223 C224 120.4(7) . . ? C223 C224 C225 119.6(8) . . ? C224 C225 C22 121.1(7) . . ? _refine_diff_density_max 1.307 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.122 # data_repno _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [ReO(k3-PNO)(k2-PNO)]Cl _chemical_formula_analytical ? _chemical_formula_sum 'C42 H38 Cl N2 O5 P2 Re' _chemical_formula_weight 934.33 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'H' 'H' 0.0000 0.0000 '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' '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' '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' _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 14.300(3) _cell_length_b 16.977(2) _cell_length_c 18.752(4) _cell_angle_alpha 92.570(14) _cell_angle_beta 109.78(2) _cell_angle_gamma 96.122(13) _cell_volume 4243.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.4 _cell_measurement_theta_max 14.8 _exptl_crystal_description irregular _exptl_crystal_colour purple _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method ? _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 3.045 _exptl_absorpt_correction_type 'empirical via \y-scan North et al (1968)' _exptl_absorpt_correction_T_min 0.596 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; Crystals were obtained by recrystallisation from an ethanol-ethyl acetate solution ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4-Enraf-Nonius' _diffrn_measurement_method '\w/2\qscans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% none _diffrn_reflns_number 13799 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 24.01 _reflns_number_total 13286 _reflns_number_observed 8367 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 software(Enraf-Nonius,1989)' _computing_cell_refinement 'CAD4 software(Enraf-Nonius,1989)' _computing_data_reduction 'process-MOLEN(Fair,1990)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP(Johnson,1976)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1901 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1133P)^2^+43.9673P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11385 _refine_ls_number_parameters 972 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_obs 0.0750 _refine_ls_wR_factor_all 0.2657 _refine_ls_wR_factor_obs 0.1853 _refine_ls_goodness_of_fit_all 1.063 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.251 _refine_ls_restrained_S_obs 1.110 _refine_ls_shift/esd_max 0.068 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Re1 Re 0.07947(5) 0.01518(4) 0.35708(4) 0.0312(2) Uani 1 d . . Re2 Re 0.25121(5) 0.31800(4) 0.72347(4) 0.0286(2) Uani 1 d . . P1A P 0.0314(3) -0.0436(3) 0.2246(2) 0.0326(9) Uani 1 d . . P2A P 0.2545(3) -0.0086(2) 0.4133(2) 0.0318(9) Uani 1 d . . P1B P 0.3484(3) 0.4063(2) 0.8380(2) 0.0321(9) Uani 1 d . . P2B P 0.1485(3) 0.4043(2) 0.6359(2) 0.0289(9) Uani 1 d . . O1A O 0.0314(8) -0.0681(7) 0.3826(7) 0.043(3) Uani 1 d . . O2A O -0.1319(11) 0.1520(8) 0.2308(8) 0.070(4) Uani 1 d . . O3A O 0.1213(8) 0.0923(7) 0.4451(6) 0.038(3) Uani 1 d . . O4A O 0.1639(8) 0.1012(6) 0.3129(6) 0.040(3) Uani 1 d . . O1B O 0.1636(8) 0.2954(6) 0.7622(6) 0.035(3) Uani 1 d . . O2B O 0.4693(9) 0.1791(8) 0.8437(7) 0.051(3) Uani 1 d . . O3B O 0.2154(8) 0.2496(6) 0.6303(6) 0.038(3) Uani 1 d . . O4B O 0.3625(8) 0.3826(7) 0.6855(6) 0.038(3) Uani 1 d . . N1A N -0.0288(10) 0.0869(8) 0.3197(8) 0.038(3) Uani 1 d . . N2A N 0.2479(13) 0.2110(9) 0.2962(9) 0.062(5) Uani 1 d . . H2A H 0.3008(13) 0.2451(9) 0.3145(9) 0.074 Uiso 1 calc R . N1B N 0.3476(10) 0.2393(8) 0.7590(8) 0.038(3) Uani 1 d . . N2B N 0.4520(10) 0.4551(9) 0.6314(8) 0.047(4) Uani 1 d . . H2B H 0.4538(10) 0.4808(9) 0.5933(8) 0.057 Uiso 1 calc R . C1A C -0.0989(12) 0.0909(10) 0.2501(10) 0.041(4) Uani 1 d . . C2A C -0.0079(16) 0.1617(11) 0.3675(11) 0.061(6) Uani 1 d . . H2A1 H -0.0698(16) 0.1825(11) 0.3638(11) 0.073 Uiso 1 calc R . H2A2 H 0.0340(16) 0.2009(11) 0.3518(11) 0.073 Uiso 1 calc R . C3A C 0.0467(14) 0.1421(11) 0.4492(12) 0.057(6) Uani 1 d . . H3A1 H 0.0785(14) 0.1905(11) 0.4817(12) 0.069 Uiso 1 calc R . H3A2 H -0.0001(14) 0.1142(11) 0.4696(12) 0.069 Uiso 1 calc R . C4A C 0.2363(15) 0.1542(10) 0.3384(11) 0.046(5) Uani 1 d . . O5A1 O 0.2299(25) 0.3552(19) 0.2244(18) 0.138(14) Uani 0.75(4) d PU 1 H5A1 H 0.2715(25) 0.3525(19) 0.2667(18) 0.207 Uiso 0.75(4) calc PR 1 O5A2 O 0.0983(54) 0.3149(45) 0.1355(42) 0.099(30) Uani 0.25(4) d PU 2 H5A2 H 0.0786(54) 0.3587(45) 0.1324(42) 0.148 Uiso 0.25(4) calc PR 2 C6A C 0.1432(29) 0.3013(21) 0.2146(23) 0.129(12) Uani 1 d U . H6A1 H 0.0930(29) 0.3035(21) 0.1650(23) 0.155 Uiso 1 calc R 1 H6A2 H 0.1147(29) 0.3129(21) 0.2535(23) 0.155 Uiso 1 calc R 1 C5A C 0.1797(23) 0.2214(15) 0.2218(13) 0.096(9) Uani 1 d . . H5A1 H 0.1223(23) 0.1807(15) 0.2090(13) 0.115 Uiso 1 calc R . H5A2 H 0.2129(23) 0.2137(15) 0.1851(13) 0.115 Uiso 1 calc R . C11A C -0.1052(12) -0.0490(11) 0.1858(9) 0.039(4) Uani 1 d . . C12A C -0.1469(13) 0.0147(10) 0.2022(10) 0.042(4) Uani 1 d . . C13A C -0.2537(15) 0.0112(12) 0.1667(11) 0.058(5) Uani 1 d . . H13A H -0.2858(15) 0.0531(12) 0.1766(11) 0.069 Uiso 1 calc R . C14A C -0.3100(14) -0.0545(13) 0.1173(11) 0.060(6) Uani 1 d . . H14A H -0.3788(14) -0.0560(13) 0.0939(11) 0.072 Uiso 1 calc R . C15A C -0.2616(17) -0.1183(14) 0.1034(14) 0.071(6) Uani 1 d . . H15A H -0.2982(17) -0.1630(14) 0.0720(14) 0.086 Uiso 1 calc R . C16A C -0.1604(13) -0.1134(11) 0.1369(10) 0.047(5) Uani 1 d . . H16A H -0.1277(13) -0.1546(11) 0.1264(10) 0.057 Uiso 1 calc R . C21A C 0.0554(12) -0.1435(9) 0.2065(9) 0.035(4) Uani 1 d . . C22A C 0.0490(12) -0.1985(10) 0.2543(11) 0.045(5) Uani 1 d . . H22A H 0.0353(12) -0.1841(10) 0.2978(11) 0.054 Uiso 1 calc R . C23A C 0.0629(15) -0.2795(11) 0.2397(13) 0.057(5) Uani 1 d . . H23A H 0.0571(15) -0.3172(11) 0.2729(13) 0.068 Uiso 1 calc R . C24A C 0.0843(16) -0.2998(12) 0.1781(12) 0.059(6) Uani 1 d . . H24A H 0.0930(16) -0.3522(12) 0.1681(12) 0.071 Uiso 1 calc R . C25A C 0.0941(17) -0.2420(11) 0.1271(13) 0.066(6) Uani 1 d . . H25A H 0.1110(17) -0.2555(11) 0.0848(13) 0.079 Uiso 1 calc R . C26A C 0.0778(15) -0.1658(12) 0.1428(10) 0.056(5) Uani 1 d . . H26A H 0.0820(15) -0.1278(12) 0.1094(10) 0.067 Uiso 1 calc R . C31A C 0.0728(14) 0.0149(9) 0.1589(9) 0.040(4) Uani 1 d . . C32A C 0.1722(15) 0.0136(11) 0.1626(12) 0.052(5) Uani 1 d . . H32A H 0.2154(15) -0.0148(11) 0.1977(12) 0.062 Uiso 1 calc R . C33A C 0.2041(23) 0.0570(18) 0.1111(17) 0.096(9) Uani 1 d . . H33A H 0.2705(23) 0.0595(18) 0.1138(17) 0.115 Uiso 1 calc R . C34A C 0.1405(30) 0.0948(17) 0.0581(14) 0.099(12) Uani 1 d . . H34A H 0.1613(30) 0.1194(17) 0.0217(14) 0.119 Uiso 1 calc R . C35A C 0.0450(26) 0.0971(15) 0.0577(12) 0.093(10) Uani 1 d . . H35A H 0.0035(26) 0.1283(15) 0.0245(12) 0.111 Uiso 1 calc R . C36A C 0.0102(17) 0.0551(11) 0.1044(10) 0.056(5) Uani 1 d . . H36A H -0.0569(17) 0.0531(11) 0.0997(10) 0.068 Uiso 1 calc R . C41A C 0.3273(12) 0.0865(10) 0.4532(9) 0.034(4) Uani 1 d . . C42A C 0.3118(11) 0.1569(9) 0.4155(9) 0.033(4) Uani 1 d . . C43A C 0.3710(13) 0.2273(10) 0.4510(10) 0.049(5) Uani 1 d . . H43A H 0.3607(13) 0.2736(10) 0.4263(10) 0.059 Uiso 1 calc R . C44A C 0.4450(14) 0.2313(12) 0.5220(11) 0.053(5) Uani 1 d . . H44A H 0.4843(14) 0.2790(12) 0.5449(11) 0.063 Uiso 1 calc R . C45A C 0.4578(14) 0.1632(11) 0.5567(11) 0.050(5) Uani 1 d . . H45A H 0.5072(14) 0.1646(11) 0.6043(11) 0.060 Uiso 1 calc R . C46A C 0.4014(11) 0.0928(10) 0.5249(9) 0.035(4) Uani 1 d . . H46A H 0.4125(11) 0.0478(10) 0.5514(9) 0.041 Uiso 1 calc R . C51A C 0.2764(11) -0.0649(10) 0.4950(9) 0.034(4) Uani 1 d . . C52A C 0.3483(13) -0.1178(10) 0.5144(11) 0.045(5) Uani 1 d . . H52A H 0.3826(13) -0.1294(10) 0.4818(11) 0.054 Uiso 1 calc R . C53A C 0.3676(15) -0.1524(12) 0.5820(13) 0.065(6) Uani 1 d . . H53A H 0.4136(15) -0.1888(12) 0.5948(13) 0.078 Uiso 1 calc R . C54A C 0.3160(18) -0.1320(14) 0.6332(13) 0.072(7) Uani 1 d . . H54A H 0.3294(18) -0.1536(14) 0.6797(13) 0.087 Uiso 1 calc R . C55A C 0.2497(16) -0.0820(13) 0.6121(12) 0.064(6) Uani 1 d . . H55A H 0.2148(16) -0.0707(13) 0.6443(12) 0.076 Uiso 1 calc R . C56A C 0.2286(14) -0.0458(11) 0.5464(10) 0.048(5) Uani 1 d . . H56A H 0.1832(14) -0.0090(11) 0.5356(10) 0.058 Uiso 1 calc R . C61A C 0.3181(11) -0.0470(10) 0.3546(10) 0.036(4) Uani 1 d . . C62A C 0.2889(14) -0.1277(11) 0.3240(12) 0.056(5) Uani 1 d . . H62A H 0.2431(14) -0.1598(11) 0.3387(12) 0.067 Uiso 1 calc R . C63A C 0.3279(15) -0.1585(13) 0.2727(11) 0.062(6) Uani 1 d . . H63A H 0.3098(15) -0.2113(13) 0.2527(11) 0.074 Uiso 1 calc R . C64A C 0.3976(16) -0.1063(15) 0.2511(13) 0.067(6) Uani 1 d . . H64A H 0.4231(16) -0.1255(15) 0.2151(13) 0.081 Uiso 1 calc R . C65A C 0.4256(19) -0.0346(16) 0.2796(13) 0.073(7) Uani 1 d . . H65A H 0.4728(19) -0.0028(16) 0.2658(13) 0.088 Uiso 1 calc R . C66A C 0.3840(14) -0.0027(11) 0.3334(11) 0.051(5) Uani 1 d . . H66A H 0.4039(14) 0.0500(11) 0.3533(11) 0.061 Uiso 1 calc R . C1B C 0.4398(12) 0.2412(10) 0.8189(9) 0.037(4) Uani 1 d . . C2B C 0.3037(15) 0.1603(10) 0.7176(11) 0.052(5) Uani 1 d . . H2B1 H 0.2528(15) 0.1357(10) 0.7360(11) 0.062 Uiso 1 calc R . H2B2 H 0.3552(15) 0.1256(10) 0.7243(11) 0.062 Uiso 1 calc R . C3B C 0.2582(16) 0.1754(13) 0.6350(11) 0.060(6) Uani 1 d . . H3B1 H 0.3092(16) 0.1785(13) 0.6115(11) 0.072 Uiso 1 calc R . H3B2 H 0.2064(16) 0.1320(13) 0.6082(11) 0.072 Uiso 1 calc R . C4B C 0.3687(12) 0.4153(10) 0.6270(9) 0.035(4) Uani 1 d . . C5B C 0.5441(13) 0.4596(14) 0.6973(12) 0.063(6) Uani 1 d . . H5B1 H 0.5370(13) 0.4194(14) 0.7309(12) 0.075 Uiso 1 calc R . H5B2 H 0.5580(13) 0.5114(14) 0.7254(12) 0.075 Uiso 1 calc R . O5B O 0.6344(19) 0.3897(18) 0.6363(16) 0.157(10) Uani 1 d U . H5B H 0.4933(299) 0.3046(235) 0.5458(226) 0.236 Uiso 1 d . . C6B C 0.6287(34) 0.4462(28) 0.6694(27) 0.170(18) Uani 1 d U . H6B1 H 0.6337(34) 0.4893(28) 0.6380(27) 0.204 Uiso 1 calc R . H6B2 H 0.6891(34) 0.4548(28) 0.7140(27) 0.204 Uiso 1 calc R . C11B C 0.4789(12) 0.3911(10) 0.8612(10) 0.038(4) Uani 1 d . . C12B C 0.5066(11) 0.3166(9) 0.8494(9) 0.031(4) Uani 1 d . . C13B C 0.6067(13) 0.3111(13) 0.8680(10) 0.051(5) Uani 1 d . . H13B H 0.6264(13) 0.2616(13) 0.8614(10) 0.061 Uiso 1 calc R . C14B C 0.6782(14) 0.3742(15) 0.8955(13) 0.065(6) Uani 1 d . . H14B H 0.7452(14) 0.3668(15) 0.9086(13) 0.078 Uiso 1 calc R . C15B C 0.6556(14) 0.4446(15) 0.9040(11) 0.064(6) Uani 1 d . . H15B H 0.7060(14) 0.4877(15) 0.9197(11) 0.077 Uiso 1 calc R . C16B C 0.5542(13) 0.4571(11) 0.8896(10) 0.048(5) Uani 1 d . . H16B H 0.5379(13) 0.5073(11) 0.8986(10) 0.058 Uiso 1 calc R . C21B C 0.3513(12) 0.5145(10) 0.8459(10) 0.040(4) Uani 1 d . . C22B C 0.3779(12) 0.5577(10) 0.7916(11) 0.045(5) Uani 1 d . . H22B H 0.3909(12) 0.5319(10) 0.7518(11) 0.054 Uiso 1 calc R . C23B C 0.3838(14) 0.6356(13) 0.7992(14) 0.064(6) Uani 1 d . . H23B H 0.4007(14) 0.6650(13) 0.7637(14) 0.077 Uiso 1 calc R . C24B C 0.3650(17) 0.6765(13) 0.8600(16) 0.076(7) Uani 1 d . . H24B H 0.3703(17) 0.7317(13) 0.8647(16) 0.091 Uiso 1 calc R . C25B C 0.3398(15) 0.6337(13) 0.9097(12) 0.060(6) Uani 1 d . . H25B H 0.3270(15) 0.6597(13) 0.9494(12) 0.072 Uiso 1 calc R . C26B C 0.3318(14) 0.5521(10) 0.9042(10) 0.046(5) Uani 1 d . . H26B H 0.3136(14) 0.5231(10) 0.9395(10) 0.055 Uiso 1 calc R . C31B C 0.3159(13) 0.3722(10) 0.9173(10) 0.041(4) Uani 1 d . . C32B C 0.2159(16) 0.3712(13) 0.9167(12) 0.062(6) Uani 1 d . . H32B H 0.1658(16) 0.3874(13) 0.8759(12) 0.074 Uiso 1 calc R . C33B C 0.1972(19) 0.3448(15) 0.9797(15) 0.081(8) Uani 1 d . . H33B H 0.1329(19) 0.3456(15) 0.9811(15) 0.097 Uiso 1 calc R . C34B C 0.2647(20) 0.3184(15) 1.0386(13) 0.076(7) Uani 1 d . . H34B H 0.2473(20) 0.3017(15) 1.0796(13) 0.091 Uiso 1 calc R . C35B C 0.3567(21) 0.3161(15) 1.0384(11) 0.075(7) Uani 1 d . . H35B H 0.4028(21) 0.2953(15) 1.0786(11) 0.089 Uiso 1 calc R . C36B C 0.3866(15) 0.3442(11) 0.9791(11) 0.055(5) Uani 1 d . . H36B H 0.4524(15) 0.3442(11) 0.9810(11) 0.066 Uiso 1 calc R . C41B C 0.1822(12) 0.4014(9) 0.5505(9) 0.036(4) Uani 1 d . . C42B C 0.2834(11) 0.4092(9) 0.5542(9) 0.033(4) Uani 1 d . . C43B C 0.3057(13) 0.4087(10) 0.4877(10) 0.042(4) Uani 1 d . . H43B H 0.3720(13) 0.4165(10) 0.4897(10) 0.051 Uiso 1 calc R . C44B C 0.2269(13) 0.3963(10) 0.4171(10) 0.042(4) Uani 1 d . . H44B H 0.2413(13) 0.3938(10) 0.3723(10) 0.050 Uiso 1 calc R . C45B C 0.1317(14) 0.3881(10) 0.4138(10) 0.043(4) Uani 1 d . . H45B H 0.0808(14) 0.3802(10) 0.3666(10) 0.051 Uiso 1 calc R . C46B C 0.1069(13) 0.3911(10) 0.4791(10) 0.042(4) Uani 1 d . . H46B H 0.0399(13) 0.3862(10) 0.4753(10) 0.051 Uiso 1 calc R . C51B C 0.0164(10) 0.3672(8) 0.6032(9) 0.026(3) Uani 1 d . . C52B C -0.0564(11) 0.4160(10) 0.5942(10) 0.037(4) Uani 1 d . . H52B H -0.0370(11) 0.4704(10) 0.6064(10) 0.045 Uiso 1 calc R . C53B C -0.1579(12) 0.3876(12) 0.5676(10) 0.048(5) Uani 1 d . . H53B H -0.2060(12) 0.4217(12) 0.5631(10) 0.057 Uiso 1 calc R . C54B C -0.1855(13) 0.3051(12) 0.5477(11) 0.053(5) Uani 1 d . . H54B H -0.2529(13) 0.2843(12) 0.5288(11) 0.064 Uiso 1 calc R . C55B C -0.1144(14) 0.2559(10) 0.5560(12) 0.051(5) Uani 1 d . . H55B H -0.1338(14) 0.2015(10) 0.5438(12) 0.062 Uiso 1 calc R . C56B C -0.0149(12) 0.2848(10) 0.5821(9) 0.038(4) Uani 1 d . . H56B H 0.0326(12) 0.2503(10) 0.5859(9) 0.046 Uiso 1 calc R . C61B C 0.1533(11) 0.5088(9) 0.6634(9) 0.035(4) Uani 1 d . . C62B C 0.1264(12) 0.5272(10) 0.7243(11) 0.044(5) Uani 1 d . . H62B H 0.1086(12) 0.4875(10) 0.7516(11) 0.053 Uiso 1 calc R . C63B C 0.1263(13) 0.6087(13) 0.7453(12) 0.059(6) Uani 1 d . . H63B H 0.1098(13) 0.6220(13) 0.7878(12) 0.070 Uiso 1 calc R . C64B C 0.1494(18) 0.6678(12) 0.7052(13) 0.070(7) Uani 1 d . . H64B H 0.1496(18) 0.7208(12) 0.7203(13) 0.084 Uiso 1 calc R . C65B C 0.1723(17) 0.6479(13) 0.6421(15) 0.074(7) Uani 1 d . . H65B H 0.1863(17) 0.6875(13) 0.6131(15) 0.088 Uiso 1 calc R . C66B C 0.1748(14) 0.5673(10) 0.6206(11) 0.047(5) Uani 1 d . . H66B H 0.1909(14) 0.5539(10) 0.5779(11) 0.057 Uiso 1 calc R . Cl1 Cl 0.9798(4) 0.4453(4) 0.0671(3) 0.081(2) Uani 1 d . . Cl2 Cl 0.5583(5) 0.3996(4) 0.4656(4) 0.099(2) Uani 1 d . . O1S O 0.4435(13) 0.3116(11) 0.3110(10) 0.094(5) Uiso 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 0.0295(4) 0.0342(4) 0.0289(4) -0.0007(3) 0.0082(3) 0.0075(3) Re2 0.0296(4) 0.0280(4) 0.0279(4) 0.0018(3) 0.0085(3) 0.0066(3) P1A 0.035(2) 0.036(2) 0.026(2) 0.003(2) 0.009(2) 0.004(2) P2A 0.027(2) 0.031(2) 0.037(2) 0.000(2) 0.010(2) 0.006(2) P1B 0.036(2) 0.035(2) 0.028(2) 0.001(2) 0.013(2) 0.009(2) P2B 0.029(2) 0.029(2) 0.029(2) 0.002(2) 0.009(2) 0.007(2) O1A 0.034(6) 0.040(7) 0.052(8) 0.005(6) 0.014(6) 0.000(5) O2A 0.089(11) 0.049(8) 0.054(9) 0.002(7) -0.007(8) 0.036(8) O3A 0.031(6) 0.051(7) 0.030(6) -0.013(5) 0.007(5) 0.011(5) O4A 0.045(7) 0.035(6) 0.033(7) -0.006(5) 0.010(5) -0.008(6) O1B 0.035(6) 0.032(6) 0.035(6) 0.004(5) 0.008(5) 0.004(5) O2B 0.042(7) 0.054(8) 0.053(8) 0.017(7) 0.007(6) 0.018(6) O3B 0.043(7) 0.042(7) 0.024(6) 0.002(5) 0.004(5) 0.012(5) O4B 0.037(6) 0.046(7) 0.032(7) 0.006(5) 0.015(5) 0.003(5) N1A 0.041(8) 0.034(8) 0.031(8) -0.010(6) 0.003(7) 0.011(6) N2A 0.079(12) 0.039(9) 0.048(10) -0.002(8) 0.004(9) -0.017(8) N1B 0.048(9) 0.036(8) 0.031(8) 0.008(6) 0.014(7) 0.012(7) N2B 0.040(9) 0.068(11) 0.036(9) 0.011(8) 0.019(7) -0.003(8) C1A 0.032(9) 0.043(10) 0.049(11) 0.005(9) 0.014(8) 0.020(8) C2A 0.072(14) 0.048(12) 0.053(13) -0.021(10) 0.008(11) 0.025(10) C3A 0.052(11) 0.049(11) 0.067(14) -0.024(10) 0.015(10) 0.027(9) C4A 0.063(12) 0.037(10) 0.048(11) 0.015(9) 0.029(10) 0.010(9) O5A1 0.152(21) 0.134(19) 0.122(19) 0.040(14) 0.036(15) 0.021(15) O5A2 0.097(34) 0.105(34) 0.092(35) 0.010(19) 0.028(20) 0.019(19) C6A 0.129(14) 0.122(14) 0.124(15) 0.018(10) 0.028(10) 0.013(10) C5A 0.143(25) 0.068(16) 0.046(14) 0.004(12) 0.002(15) -0.018(16) C11A 0.026(8) 0.062(12) 0.026(9) 0.014(8) 0.005(7) 0.008(8) C12A 0.043(10) 0.043(10) 0.043(11) -0.001(8) 0.015(8) 0.016(8) C13A 0.068(13) 0.063(13) 0.039(11) 0.002(10) 0.008(10) 0.029(11) C14A 0.037(11) 0.085(16) 0.039(12) 0.004(11) -0.009(9) 0.000(11) C15A 0.065(15) 0.068(15) 0.080(17) 0.013(13) 0.023(13) 0.010(12) C16A 0.043(11) 0.041(10) 0.048(12) 0.004(9) 0.001(9) 0.013(8) C21A 0.041(9) 0.035(9) 0.025(9) 0.006(7) 0.006(7) 0.002(7) C22A 0.037(10) 0.044(10) 0.058(12) -0.011(9) 0.027(9) 0.001(8) C23A 0.072(14) 0.032(10) 0.076(15) -0.002(10) 0.040(12) 0.006(9) C24A 0.077(15) 0.038(11) 0.054(13) 0.003(10) 0.008(11) 0.015(10) C25A 0.099(17) 0.041(11) 0.067(15) -0.015(10) 0.042(13) 0.019(11) C26A 0.074(14) 0.061(13) 0.032(11) 0.000(9) 0.022(10) -0.005(11) C31A 0.059(11) 0.031(9) 0.030(9) -0.010(7) 0.020(9) -0.009(8) C32A 0.065(13) 0.048(11) 0.056(13) 0.001(9) 0.040(11) 0.001(10) C33A 0.099(22) 0.114(24) 0.083(21) -0.001(18) 0.051(18) -0.008(18) C34A 0.168(32) 0.085(19) 0.039(15) -0.009(13) 0.051(19) -0.053(21) C35A 0.146(27) 0.083(18) 0.020(11) 0.012(11) 0.002(14) -0.029(19) C36A 0.081(15) 0.052(12) 0.027(10) 0.015(9) 0.005(10) 0.006(11) C41A 0.033(9) 0.040(9) 0.028(9) 0.000(7) 0.010(7) 0.004(7) C42A 0.024(8) 0.029(8) 0.043(10) 0.013(7) 0.008(7) 0.002(7) C43A 0.050(11) 0.035(10) 0.045(11) -0.011(8) -0.003(9) 0.002(8) C44A 0.055(12) 0.045(11) 0.052(12) -0.019(10) 0.019(10) -0.010(9) C45A 0.051(11) 0.051(12) 0.042(11) 0.005(9) 0.009(9) -0.004(9) C46A 0.029(9) 0.047(10) 0.035(10) 0.006(8) 0.019(8) 0.013(8) C51A 0.030(8) 0.039(9) 0.029(9) -0.003(7) 0.006(7) 0.005(7) C52A 0.043(10) 0.031(9) 0.063(13) 0.020(9) 0.017(9) 0.008(8) C53A 0.045(12) 0.051(12) 0.086(17) 0.031(12) -0.001(11) 0.016(10) C54A 0.072(15) 0.084(17) 0.059(15) 0.028(13) 0.021(13) -0.006(13) C55A 0.065(14) 0.079(15) 0.059(14) 0.014(12) 0.029(12) 0.029(12) C56A 0.056(12) 0.054(11) 0.024(9) -0.006(8) 0.003(8) 0.004(9) C61A 0.024(8) 0.045(10) 0.043(10) 0.005(8) 0.012(7) 0.020(7) C62A 0.044(11) 0.037(10) 0.083(16) 0.005(10) 0.012(10) 0.026(9) C63A 0.047(12) 0.073(14) 0.049(12) -0.029(11) -0.005(10) 0.025(11) C64A 0.060(14) 0.086(17) 0.059(14) -0.011(13) 0.020(11) 0.032(13) C65A 0.091(17) 0.094(18) 0.064(15) 0.010(14) 0.057(14) 0.038(15) C66A 0.062(12) 0.045(11) 0.062(13) 0.020(10) 0.039(11) 0.015(9) C1B 0.040(10) 0.047(10) 0.032(9) 0.004(8) 0.022(8) 0.018(8) C2B 0.065(12) 0.032(10) 0.055(12) 0.009(9) 0.009(10) 0.026(9) C3B 0.067(13) 0.069(14) 0.042(12) 0.007(10) 0.009(10) 0.029(11) C4B 0.038(9) 0.041(9) 0.025(9) -0.004(7) 0.012(7) -0.004(8) C5B 0.039(11) 0.092(17) 0.053(13) -0.013(12) 0.018(10) -0.013(11) O5B 0.136(15) 0.168(17) 0.162(17) 0.005(14) 0.027(13) 0.077(14) C6B 0.161(19) 0.170(20) 0.173(20) 0.000(10) 0.049(11) 0.030(10) C11B 0.030(9) 0.038(10) 0.046(11) 0.012(8) 0.006(8) 0.018(7) C12B 0.028(8) 0.036(9) 0.027(9) -0.009(7) 0.008(7) 0.008(7) C13B 0.044(11) 0.073(14) 0.038(11) 0.009(10) 0.010(9) 0.028(10) C14B 0.029(10) 0.092(17) 0.070(15) -0.018(13) 0.014(10) 0.013(11) C15B 0.037(11) 0.104(19) 0.037(11) -0.019(12) 0.004(9) -0.016(12) C16B 0.046(11) 0.053(11) 0.043(11) -0.008(9) 0.015(9) 0.004(9) C21B 0.029(9) 0.039(10) 0.046(11) 0.005(8) 0.005(8) 0.013(7) C22B 0.028(9) 0.037(10) 0.060(12) -0.005(9) 0.010(8) -0.010(8) C23B 0.045(12) 0.056(14) 0.082(17) 0.025(12) 0.008(11) 0.006(10) C24B 0.069(15) 0.034(11) 0.104(21) -0.022(13) 0.007(14) 0.000(11) C25B 0.053(12) 0.062(14) 0.052(13) -0.004(11) -0.001(10) 0.017(11) C26B 0.066(12) 0.039(10) 0.026(9) -0.002(8) 0.005(9) 0.016(9) C31B 0.045(10) 0.044(10) 0.032(10) -0.003(8) 0.013(8) -0.003(8) C32B 0.058(13) 0.083(15) 0.045(12) -0.012(11) 0.021(10) 0.006(11) C33B 0.071(16) 0.108(20) 0.080(18) -0.009(15) 0.061(15) -0.027(15) C34B 0.083(18) 0.094(19) 0.045(14) 0.015(13) 0.020(13) -0.009(15) C35B 0.098(19) 0.096(18) 0.025(11) 0.017(11) 0.017(12) -0.003(15) C36B 0.054(12) 0.046(11) 0.055(13) -0.009(10) 0.010(10) -0.008(9) C41B 0.039(9) 0.034(9) 0.036(10) 0.005(7) 0.013(8) 0.008(7) C42B 0.025(8) 0.029(8) 0.041(10) 0.013(7) 0.004(7) 0.004(7) C43B 0.038(10) 0.044(10) 0.053(12) 0.021(9) 0.022(9) 0.010(8) C44B 0.046(11) 0.045(10) 0.047(11) 0.009(9) 0.031(9) 0.011(8) C45B 0.054(11) 0.041(10) 0.036(10) 0.002(8) 0.016(9) 0.020(9) C46B 0.041(10) 0.035(9) 0.039(11) -0.006(8) 0.000(8) 0.007(8) C51B 0.019(7) 0.028(8) 0.034(9) 0.003(7) 0.010(7) 0.010(6) C52B 0.030(9) 0.033(9) 0.043(10) 0.002(8) 0.005(8) 0.003(7) C53B 0.028(9) 0.064(13) 0.049(12) 0.005(10) 0.007(8) 0.020(9) C54B 0.031(10) 0.067(14) 0.062(13) 0.014(11) 0.015(9) 0.005(9) C55B 0.046(11) 0.030(9) 0.080(15) 0.005(9) 0.027(10) -0.007(8) C56B 0.032(9) 0.047(10) 0.030(9) 0.005(8) 0.003(7) 0.003(8) C61B 0.030(8) 0.028(8) 0.038(10) -0.005(7) 0.001(7) 0.010(7) C62B 0.031(9) 0.038(10) 0.057(12) -0.012(9) 0.007(8) 0.012(8) C63B 0.042(11) 0.071(14) 0.047(12) -0.018(11) -0.009(9) 0.029(10) C64B 0.100(18) 0.035(11) 0.061(15) 0.004(11) 0.001(13) 0.035(12) C65B 0.071(15) 0.046(13) 0.081(18) 0.024(12) -0.007(13) 0.014(11) C66B 0.063(12) 0.029(9) 0.042(11) 0.002(8) 0.008(9) 0.006(9) Cl1 0.070(4) 0.128(5) 0.049(3) -0.004(3) 0.012(3) 0.066(4) Cl2 0.086(5) 0.096(5) 0.107(6) 0.028(4) 0.026(4) -0.014(4) _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 O1A 1.666(11) . ? Re1 O3A 1.941(10) . ? Re1 N1A 2.028(13) . ? Re1 O4A 2.165(11) . ? Re1 P2A 2.451(4) . ? Re1 P1A 2.473(4) . ? Re2 O1B 1.668(11) . ? Re2 O3B 1.936(11) . ? Re2 N1B 1.995(13) . ? Re2 O4B 2.170(10) . ? Re2 P1B 2.457(4) . ? Re2 P2B 2.458(4) . ? P1A C21A 1.81(2) . ? P1A C11A 1.83(2) . ? P1A C31A 1.83(2) . ? P2A C61A 1.79(2) . ? P2A C51A 1.80(2) . ? P2A C41A 1.80(2) . ? P1B C31B 1.80(2) . ? P1B C11B 1.82(2) . ? P1B C21B 1.83(2) . ? P2B C51B 1.808(14) . ? P2B C61B 1.81(2) . ? P2B C41B 1.82(2) . ? O2A C1A 1.20(2) . ? O3A C3A 1.45(2) . ? O4A C4A 1.24(2) . ? O2B C1B 1.23(2) . ? O3B C3B 1.45(2) . ? O4B C4B 1.28(2) . ? N1A C1A 1.36(2) . ? N1A C2A 1.46(2) . ? N2A C4A 1.31(2) . ? N2A C5A 1.44(3) . ? N1B C1B 1.41(2) . ? N1B C2B 1.48(2) . ? N2B C4B 1.28(2) . ? N2B C5B 1.46(2) . ? C1A C12A 1.50(2) . ? C2A C3A 1.54(3) . ? C4A C42A 1.48(2) . ? O5A1 C6A 1.41(4) . ? O5A2 C6A 1.44(7) . ? C6A C5A 1.50(4) . ? C11A C12A 1.36(2) . ? C11A C16A 1.38(2) . ? C12A C13A 1.44(3) . ? C13A C14A 1.40(3) . ? C14A C15A 1.40(3) . ? C15A C16A 1.36(3) . ? C21A C22A 1.34(2) . ? C21A C26A 1.39(2) . ? C22A C23A 1.44(2) . ? C23A C24A 1.33(3) . ? C24A C25A 1.43(3) . ? C25A C26A 1.38(3) . ? C31A C36A 1.37(3) . ? C31A C32A 1.40(3) . ? C32A C33A 1.40(3) . ? C33A C34A 1.34(4) . ? C34A C35A 1.37(4) . ? C35A C36A 1.34(3) . ? C41A C46A 1.39(2) . ? C41A C42A 1.41(2) . ? C42A C43A 1.39(2) . ? C43A C44A 1.39(3) . ? C44A C45A 1.35(3) . ? C45A C46A 1.36(2) . ? C51A C56A 1.40(2) . ? C51A C52A 1.40(2) . ? C52A C53A 1.38(3) . ? C53A C54A 1.44(3) . ? C54A C55A 1.31(3) . ? C55A C56A 1.36(3) . ? C61A C66A 1.32(2) . ? C61A C62A 1.42(2) . ? C62A C63A 1.37(3) . ? C63A C64A 1.43(3) . ? C64A C65A 1.27(3) . ? C65A C66A 1.45(3) . ? C1B C12B 1.48(2) . ? C2B C3B 1.51(3) . ? C4B C42B 1.48(2) . ? C5B C6B 1.50(4) . ? O5B C6B 1.14(4) . ? C11B C12B 1.40(2) . ? C11B C16B 1.41(2) . ? C12B C13B 1.37(2) . ? C13B C14B 1.35(3) . ? C14B C15B 1.29(3) . ? C15B C16B 1.42(3) . ? C21B C26B 1.36(2) . ? C21B C22B 1.41(2) . ? C22B C23B 1.31(3) . ? C23B C24B 1.42(3) . ? C24B C25B 1.33(3) . ? C25B C26B 1.37(3) . ? C31B C36B 1.40(3) . ? C31B C32B 1.42(3) . ? C32B C33B 1.38(3) . ? C33B C34B 1.33(3) . ? C34B C35B 1.32(3) . ? C35B C36B 1.40(3) . ? C41B C46B 1.40(2) . ? C41B C42B 1.42(2) . ? C42B C43B 1.39(2) . ? C43B C44B 1.41(2) . ? C44B C45B 1.33(2) . ? C45B C46B 1.39(2) . ? C51B C52B 1.37(2) . ? C51B C56B 1.42(2) . ? C52B C53B 1.39(2) . ? C53B C54B 1.41(3) . ? C54B C55B 1.36(3) . ? C55B C56B 1.37(2) . ? C61B C62B 1.36(2) . ? C61B C66B 1.38(2) . ? C62B C63B 1.42(2) . ? C63B C64B 1.36(3) . ? C64B C65B 1.37(3) . ? C65B C66B 1.42(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 O1A Re1 O3A 106.6(5) . . ? O1A Re1 N1A 109.4(6) . . ? O3A Re1 N1A 81.1(5) . . ? O1A Re1 O4A 164.4(5) . . ? O3A Re1 O4A 84.0(4) . . ? N1A Re1 O4A 83.2(5) . . ? O1A Re1 P2A 95.4(4) . . ? O3A Re1 P2A 81.1(3) . . ? N1A Re1 P2A 152.8(4) . . ? O4A Re1 P2A 74.6(3) . . ? O1A Re1 P1A 91.2(4) . . ? O3A Re1 P1A 161.5(4) . . ? N1A Re1 P1A 88.2(4) . . ? O4A Re1 P1A 79.7(3) . . ? P2A Re1 P1A 102.85(14) . . ? O1B Re2 O3B 107.4(5) . . ? O1B Re2 N1B 104.9(5) . . ? O3B Re2 N1B 80.4(5) . . ? O1B Re2 O4B 163.0(5) . . ? O3B Re2 O4B 86.2(4) . . ? N1B Re2 O4B 87.1(5) . . ? O1B Re2 P1B 89.2(4) . . ? O3B Re2 P1B 162.1(3) . . ? N1B Re2 P1B 88.9(4) . . ? O4B Re2 P1B 78.9(3) . . ? O1B Re2 P2B 92.7(4) . . ? O3B Re2 P2B 81.6(3) . . ? N1B Re2 P2B 157.9(4) . . ? O4B Re2 P2B 79.0(3) . . ? P1B Re2 P2B 104.86(14) . . ? C21A P1A C11A 104.3(8) . . ? C21A P1A C31A 105.1(8) . . ? C11A P1A C31A 103.5(8) . . ? C21A P1A Re1 119.8(5) . . ? C11A P1A Re1 105.0(6) . . ? C31A P1A Re1 117.2(5) . . ? C61A P2A C51A 108.5(8) . . ? C61A P2A C41A 103.5(8) . . ? C51A P2A C41A 102.7(7) . . ? C61A P2A Re1 120.3(5) . . ? C51A P2A Re1 112.9(5) . . ? C41A P2A Re1 106.9(5) . . ? C31B P1B C11B 104.4(8) . . ? C31B P1B C21B 105.5(8) . . ? C11B P1B C21B 104.5(8) . . ? C31B P1B Re2 108.9(6) . . ? C11B P1B Re2 107.1(6) . . ? C21B P1B Re2 124.7(6) . . ? C51B P2B C61B 104.0(7) . . ? C51B P2B C41B 104.9(7) . . ? C61B P2B C41B 105.7(8) . . ? C51B P2B Re2 112.4(5) . . ? C61B P2B Re2 121.2(5) . . ? C41B P2B Re2 107.4(5) . . ? C3A O3A Re1 115.4(10) . . ? C4A O4A Re1 137.7(11) . . ? C3B O3B Re2 117.3(10) . . ? C4B O4B Re2 139.7(10) . . ? C1A N1A C2A 111.9(14) . . ? C1A N1A Re1 131.9(11) . . ? C2A N1A Re1 113.0(11) . . ? C4A N2A C5A 125.7(18) . . ? C1B N1B C2B 115.5(13) . . ? C1B N1B Re2 133.9(11) . . ? C2B N1B Re2 110.1(10) . . ? C4B N2B C5B 124.1(16) . . ? O2A C1A N1A 121.7(16) . . ? O2A C1A C12A 119.5(16) . . ? N1A C1A C12A 118.1(15) . . ? N1A C2A C3A 106.1(15) . . ? O3A C3A C2A 106.4(15) . . ? O4A C4A N2A 119.5(18) . . ? O4A C4A C42A 123.2(15) . . ? N2A C4A C42A 117.3(16) . . ? O5A1 C6A C5A 104.3(30) . . ? O5A2 C6A C5A 110.4(44) . . ? N2A C5A C6A 114.2(24) . . ? C12A C11A C16A 122.8(16) . . ? C12A C11A P1A 117.6(13) . . ? C16A C11A P1A 119.3(14) . . ? C11A C12A C13A 116.5(16) . . ? C11A C12A C1A 130.3(16) . . ? C13A C12A C1A 113.2(15) . . ? C14A C13A C12A 120.7(18) . . ? C13A C14A C15A 119.5(19) . . ? C16A C15A C14A 118.8(21) . . ? C15A C16A C11A 121.6(19) . . ? C22A C21A C26A 118.5(17) . . ? C22A C21A P1A 120.0(13) . . ? C26A C21A P1A 121.5(13) . . ? C21A C22A C23A 121.4(17) . . ? C24A C23A C22A 119.2(19) . . ? C23A C24A C25A 120.7(18) . . ? C26A C25A C24A 117.8(19) . . ? C25A C26A C21A 122.4(19) . . ? C36A C31A C32A 119.7(18) . . ? C36A C31A P1A 123.2(15) . . ? C32A C31A P1A 116.9(14) . . ? C33A C32A C31A 117.4(22) . . ? C34A C33A C32A 121.3(27) . . ? C33A C34A C35A 119.8(24) . . ? C36A C35A C34A 121.0(27) . . ? C35A C36A C31A 120.5(24) . . ? C46A C41A C42A 117.3(15) . . ? C46A C41A P2A 119.7(13) . . ? C42A C41A P2A 123.0(12) . . ? C43A C42A C41A 118.8(15) . . ? C43A C42A C4A 121.0(15) . . ? C41A C42A C4A 120.2(14) . . ? C42A C43A C44A 122.4(18) . . ? C45A C44A C43A 117.4(17) . . ? C44A C45A C46A 122.6(18) . . ? C45A C46A C41A 121.4(17) . . ? C56A C51A C52A 119.2(17) . . ? C56A C51A P2A 117.1(13) . . ? C52A C51A P2A 123.1(13) . . ? C53A C52A C51A 119.4(19) . . ? C52A C53A C54A 119.7(19) . . ? C55A C54A C53A 118.2(20) . . ? C54A C55A C56A 124.4(22) . . ? C55A C56A C51A 119.1(19) . . ? C66A C61A C62A 118.7(17) . . ? C66A C61A P2A 123.3(14) . . ? C62A C61A P2A 117.8(14) . . ? C63A C62A C61A 120.6(20) . . ? C62A C63A C64A 117.6(19) . . ? C65A C64A C63A 122.1(21) . . ? C64A C65A C66A 119.8(23) . . ? C61A C66A C65A 121.2(20) . . ? O2B C1B N1B 120.4(16) . . ? O2B C1B C12B 118.3(15) . . ? N1B C1B C12B 121.2(15) . . ? N1B C2B C3B 105.8(15) . . ? O3B C3B C2B 108.9(15) . . ? O4B C4B N2B 118.6(15) . . ? O4B C4B C42B 122.7(14) . . ? N2B C4B C42B 118.7(15) . . ? N2B C5B C6B 108.5(23) . . ? O5B C6B C5B 125.7(42) . . ? C12B C11B C16B 119.1(15) . . ? C12B C11B P1B 121.8(12) . . ? C16B C11B P1B 119.0(13) . . ? C13B C12B C11B 117.5(15) . . ? C13B C12B C1B 115.1(15) . . ? C11B C12B C1B 127.4(14) . . ? C14B C13B C12B 123.0(19) . . ? C15B C14B C13B 121.4(19) . . ? C14B C15B C16B 120.6(19) . . ? C11B C16B C15B 118.1(18) . . ? C26B C21B C22B 121.3(16) . . ? C26B C21B P1B 120.8(14) . . ? C22B C21B P1B 117.9(13) . . ? C23B C22B C21B 117.7(19) . . ? C22B C23B C24B 122.3(22) . . ? C25B C24B C23B 118.2(20) . . ? C24B C25B C26B 122.1(21) . . ? C25B C26B C21B 118.4(19) . . ? C36B C31B C32B 118.6(18) . . ? C36B C31B P1B 121.2(14) . . ? C32B C31B P1B 120.1(15) . . ? C33B C32B C31B 116.6(21) . . ? C34B C33B C32B 124.5(23) . . ? C35B C34B C33B 119.4(22) . . ? C34B C35B C36B 121.7(23) . . ? C31B C36B C35B 119.0(20) . . ? C46B C41B C42B 118.5(16) . . ? C46B C41B P2B 119.6(13) . . ? C42B C41B P2B 121.9(13) . . ? C43B C42B C41B 119.9(15) . . ? C43B C42B C4B 117.2(14) . . ? C41B C42B C4B 122.8(15) . . ? C42B C43B C44B 119.2(15) . . ? C45B C44B C43B 120.6(17) . . ? C44B C45B C46B 121.6(17) . . ? C45B C46B C41B 120.0(17) . . ? C52B C51B C56B 117.7(14) . . ? C52B C51B P2B 122.7(12) . . ? C56B C51B P2B 119.5(11) . . ? C51B C52B C53B 122.6(16) . . ? C52B C53B C54B 117.6(16) . . ? C55B C54B C53B 120.5(17) . . ? C54B C55B C56B 121.1(17) . . ? C55B C56B C51B 120.3(16) . . ? C62B C61B C66B 120.9(16) . . ? C62B C61B P2B 117.4(13) . . ? C66B C61B P2B 121.5(13) . . ? C61B C62B C63B 118.3(19) . . ? C64B C63B C62B 122.1(20) . . ? C65B C64B C63B 118.6(19) . . ? C64B C65B C66B 120.5(21) . . ? C61B C66B C65B 119.5(20) . . ? _refine_diff_density_max 3.292 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.219