# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Nils Metzler-Nolte' _publ_contact_author_email NILS.METZLER-NOLTE@RUB.DE _publ_section_title ; Chemoselective Synthesis of the First Hetero-Triorganometallic PNA Monomer-Like Derivative ; loop_ _publ_author_name 'Nils Metzler-Nolte' 'Dmytro Bobukhov' 'Gilles Gasser' 'Klaus Merz' 'Malay Patra' 'Alexander Shtemenko' data_090911 _database_code_depnum_ccdc_archive 'CCDC 755697' #TrackingRef '090911.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 F6 N3 O3 P Re' _chemical_formula_weight 652.51 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' F F 0.0171 0.0103 '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 orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 7.852(4) _cell_length_b 10.081(5) _cell_length_c 26.274(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2079.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 5.999 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3800 _exptl_absorpt_correction_T_max 0.5853 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10532 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1922 _reflns_number_gt 1693 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+11.2100P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0090(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1922 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1196 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.90747(4) 0.2500 0.104479(15) 0.0208(3) Uani 1 2 d S . . O2 O 1.1901(11) 0.2500 0.1853(4) 0.052(2) Uani 1 2 d S . . N1 N 0.7384(7) 0.1139(6) 0.1445(2) 0.0238(13) Uani 1 1 d . . . C1 C 0.7595(10) 0.0711(8) 0.1919(3) 0.0337(18) Uani 1 1 d . . . H1A H 0.8589 0.0949 0.2096 0.040 Uiso 1 1 calc R . . P1 P 0.0291(5) 0.7500 0.14871(16) 0.0467(9) Uani 1 2 d S . . F1 F 0.142(5) 0.7500 0.1916(12) 0.297(15) Uani 1 2 d S . . O1 O 1.1221(8) 0.0483(7) 0.0454(3) 0.0486(17) Uani 1 1 d . . . N2 N 0.6780(10) 0.2500 0.0544(3) 0.0223(18) Uani 1 2 d S . . C2 C 0.6412(12) -0.0066(9) 0.2158(3) 0.042(2) Uani 1 1 d . . . H2A H 0.6592 -0.0352 0.2494 0.050 Uiso 1 1 calc R . . F2 F 0.0515(14) 0.5932(8) 0.1561(5) 0.126(4) Uani 1 1 d . . . C3 C 0.4963(11) -0.0423(9) 0.1903(4) 0.044(2) Uani 1 1 d . . . H3A H 0.4150 -0.0974 0.2058 0.053 Uiso 1 1 calc R . . F3 F -0.030(7) 0.7500 0.0964(12) 0.297(15) Uani 1 2 d S . . C4 C 0.4717(11) 0.0030(8) 0.1421(3) 0.0372(19) Uani 1 1 d . . . H4A H 0.3719 -0.0193 0.1243 0.045 Uiso 1 1 calc R . . F4 F -0.120(3) 0.7500 0.1806(14) 0.27(2) Uani 1 2 d S . . C5 C 0.5936(9) 0.0820(8) 0.1193(4) 0.0283(17) Uani 1 1 d . . . C6 C 0.5819(10) 0.1264(10) 0.0654(4) 0.040(2) Uani 1 1 d . . . H6A H 0.6250 0.0554 0.0433 0.048 Uiso 1 1 calc R . . H6B H 0.4618 0.1406 0.0568 0.048 Uiso 1 1 calc R . . F5 F 0.188(2) 0.7500 0.1153(8) 0.146(8) Uani 1 2 d S . . C7 C 0.7129(14) 0.2500 -0.0010(4) 0.032(2) Uani 1 2 d S . . H7A H 0.7806 0.3286 -0.0095 0.039 Uiso 0.50 1 calc PR . . H7B H 0.7806 0.1714 -0.0095 0.039 Uiso 0.50 1 calc PR . . C8 C 0.5573(17) 0.2500 -0.0316(5) 0.039(3) Uani 1 2 d S . . C9 C 0.4276(18) 0.2500 -0.0543(7) 0.055(4) Uani 1 2 d S . . H9 H 0.3243 0.2500 -0.0724 0.066 Uiso 1 2 calc SR . . C10 C 1.0364(9) 0.1206(7) 0.0679(3) 0.0244(15) Uani 1 1 d . . . C11 C 1.0843(13) 0.2500 0.1548(5) 0.030(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0180(3) 0.0211(3) 0.0235(4) 0.000 -0.00121(13) 0.000 O2 0.036(5) 0.069(6) 0.051(6) 0.000 -0.022(4) 0.000 N1 0.029(3) 0.021(3) 0.021(3) -0.001(2) 0.000(2) 0.002(2) C1 0.029(4) 0.043(4) 0.029(5) 0.010(4) -0.004(3) 0.002(3) P1 0.0434(19) 0.0434(19) 0.053(2) 0.000 0.0141(17) 0.000 F1 0.44(4) 0.28(3) 0.17(2) 0.000 -0.20(2) 0.000 O1 0.046(4) 0.051(4) 0.049(4) -0.011(3) 0.004(3) 0.016(3) N2 0.020(4) 0.026(4) 0.021(5) 0.000 0.000(3) 0.000 C2 0.048(5) 0.050(5) 0.028(5) 0.017(4) 0.008(4) 0.008(4) F2 0.142(8) 0.050(5) 0.187(11) -0.030(6) 0.084(8) -0.028(5) C3 0.036(5) 0.045(5) 0.051(6) 0.013(4) 0.013(4) 0.000(4) F3 0.44(4) 0.28(3) 0.17(2) 0.000 -0.20(2) 0.000 C4 0.035(4) 0.039(5) 0.038(5) 0.007(4) 0.006(4) -0.006(4) F4 0.20(2) 0.103(12) 0.52(5) 0.000 0.28(3) 0.000 C5 0.029(4) 0.025(4) 0.030(5) -0.005(4) -0.003(3) -0.002(3) C6 0.041(5) 0.049(6) 0.030(5) 0.007(4) -0.007(3) -0.023(4) F5 0.124(13) 0.093(10) 0.22(2) 0.000 0.112(14) 0.000 C7 0.032(5) 0.039(6) 0.025(6) 0.000 0.003(5) 0.000 C8 0.047(7) 0.048(7) 0.021(7) 0.000 -0.004(5) 0.000 C9 0.054(9) 0.065(10) 0.046(10) 0.000 -0.014(7) 0.000 C10 0.022(3) 0.032(4) 0.019(4) 0.003(3) -0.003(3) 0.000(3) C11 0.033(6) 0.027(6) 0.031(7) 0.000 0.005(5) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C10 1.911(8) . ? Re1 C10 1.911(8) 8_565 ? Re1 C11 1.917(12) . ? Re1 N1 2.179(6) 8_565 ? Re1 N1 2.179(6) . ? Re1 N2 2.231(8) . ? O2 C11 1.153(15) . ? N1 C1 1.329(10) . ? N1 C5 1.354(10) . ? C1 C2 1.368(12) . ? C1 H1A 0.9400 . ? P1 F1 1.44(2) . ? P1 F4 1.441(14) . ? P1 F3 1.45(2) . ? P1 F5 1.524(13) . ? P1 F2 1.602(9) 8_575 ? P1 F2 1.602(9) . ? O1 C10 1.155(10) . ? N2 C7 1.479(14) . ? N2 C6 1.486(9) 8_565 ? N2 C6 1.486(9) . ? C2 C3 1.369(14) . ? C2 H2A 0.9400 . ? C3 C4 1.360(13) . ? C3 H3A 0.9400 . ? F3 F5 1.78(5) . ? C4 C5 1.380(11) . ? C4 H4A 0.9400 . ? C5 C6 1.490(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.464(17) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.180(19) . ? C9 H9 0.9400 . ? 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 C10 Re1 C10 86.1(4) . 8_565 ? C10 Re1 C11 87.9(3) . . ? C10 Re1 C11 87.9(3) 8_565 . ? C10 Re1 N1 174.4(3) . 8_565 ? C10 Re1 N1 97.8(3) 8_565 8_565 ? C11 Re1 N1 96.2(3) . 8_565 ? C10 Re1 N1 97.8(3) . . ? C10 Re1 N1 174.4(3) 8_565 . ? C11 Re1 N1 96.2(3) . . ? N1 Re1 N1 78.1(3) 8_565 . ? C10 Re1 N2 97.5(3) . . ? C10 Re1 N2 97.5(3) 8_565 . ? C11 Re1 N2 172.5(4) . . ? N1 Re1 N2 78.0(2) 8_565 . ? N1 Re1 N2 78.0(2) . . ? C1 N1 C5 119.0(7) . . ? C1 N1 Re1 125.5(5) . . ? C5 N1 Re1 115.3(6) . . ? N1 C1 C2 122.1(8) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? F1 P1 F4 93(2) . . ? F1 P1 F3 160(3) . . ? F4 P1 F3 107(3) . . ? F1 P1 F5 87(2) . . ? F4 P1 F5 179.6(19) . . ? F3 P1 F5 73(2) . . ? F1 P1 F2 80.6(5) . 8_575 ? F4 P1 F2 91.1(4) . 8_575 ? F3 P1 F2 98.6(6) . 8_575 ? F5 P1 F2 88.8(4) . 8_575 ? F1 P1 F2 80.6(5) . . ? F4 P1 F2 91.1(4) . . ? F3 P1 F2 98.6(6) . . ? F5 P1 F2 88.8(4) . . ? F2 P1 F2 161.2(11) 8_575 . ? C7 N2 C6 106.6(6) . 8_565 ? C7 N2 C6 106.6(6) . . ? C6 N2 C6 114.1(9) 8_565 . ? C7 N2 Re1 115.5(6) . . ? C6 N2 Re1 107.2(5) 8_565 . ? C6 N2 Re1 107.2(5) . . ? C3 C2 C1 119.3(8) . . ? C3 C2 H2A 120.3 . . ? C1 C2 H2A 120.3 . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? P1 F3 F5 55.2(13) . . ? C3 C4 C5 119.9(8) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 C4 120.6(9) . . ? N1 C5 C6 116.4(7) . . ? C4 C5 C6 122.8(7) . . ? N2 C6 C5 113.9(7) . . ? N2 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? P1 F5 F3 51.3(15) . . ? C8 C7 N2 112.7(9) . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7B 109.0 . . ? N2 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 176.9(16) . . ? C8 C9 H9 180.0 . . ? O1 C10 Re1 175.7(7) . . ? O2 C11 Re1 179.7(11) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.908 _refine_diff_density_min -1.140 _refine_diff_density_rms 0.272 # Attachment '090914t.cif' data_090914t _database_code_depnum_ccdc_archive 'CCDC 755698' #TrackingRef '090914t.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H35 B N3 O3 Re' _chemical_formula_weight 826.75 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.135(4) _cell_length_b 12.789(6) _cell_length_c 19.230(9) _cell_angle_alpha 108.477(9) _cell_angle_beta 91.253(10) _cell_angle_gamma 101.914(9) _cell_volume 2075.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 164 _cell_measurement_theta_min 9.2 _cell_measurement_theta_max 43.7 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.965 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5886 _exptl_absorpt_correction_T_max 0.7559 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11212 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.98 _reflns_number_total 6947 _reflns_number_gt 6075 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6947 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.85632(2) 0.517537(18) 0.312668(13) 0.02754(14) Uani 1 1 d . . . O1 O 0.9521(8) 0.6895(6) 0.4686(3) 0.072(2) Uani 1 1 d . . . N1 N 0.7587(6) 0.6324(4) 0.2745(3) 0.0279(11) Uani 1 1 d . . . C1 C 0.8398(7) 0.7214(5) 0.2576(4) 0.0325(14) Uani 1 1 d . . . H1A H 0.9450 0.7320 0.2596 0.039 Uiso 1 1 calc R . . B1 B 0.2344(8) 0.9675(5) 0.1985(4) 0.0247(14) Uani 1 1 d . . . O2 O 1.1783(6) 0.5807(5) 0.2734(4) 0.0599(16) Uani 1 1 d . . . N2 N 0.6138(6) 0.4626(4) 0.3232(3) 0.0240(10) Uani 1 1 d . . . C2 C 0.7743(8) 0.7964(6) 0.2376(4) 0.0381(16) Uani 1 1 d . . . H2A H 0.8329 0.8575 0.2264 0.046 Uiso 1 1 calc R . . O3 O 0.9495(7) 0.3390(5) 0.3690(4) 0.0680(19) Uani 1 1 d . . . N3 N 0.7651(6) 0.3939(4) 0.2067(3) 0.0286(11) Uani 1 1 d . . . C3 C 0.6196(9) 0.7793(6) 0.2345(5) 0.0476(18) Uani 1 1 d . . . H3A H 0.5720 0.8297 0.2213 0.057 Uiso 1 1 calc R . . C4 C 0.5360(7) 0.6908(6) 0.2502(4) 0.0379(16) Uani 1 1 d . . . H4A H 0.4306 0.6777 0.2464 0.045 Uiso 1 1 calc R . . C5 C 0.6092(7) 0.6190(5) 0.2721(3) 0.0247(12) Uani 1 1 d . . . C6 C 0.5219(7) 0.5220(6) 0.2882(4) 0.0378(16) Uani 1 1 d . . . H6A H 0.4679 0.4674 0.2422 0.045 Uiso 1 1 calc R . . H6B H 0.4467 0.5472 0.3212 0.045 Uiso 1 1 calc R . . C7 C 0.5786(8) 0.4797(6) 0.4011(4) 0.0403(16) Uani 1 1 d . . . H7A H 0.6467 0.4478 0.4243 0.048 Uiso 1 1 calc R . . H7B H 0.5985 0.5611 0.4278 0.048 Uiso 1 1 calc R . . C8 C 0.4245(8) 0.4290(7) 0.4090(4) 0.0433(17) Uani 1 1 d . . . C9 C 0.3024(9) 0.3854(8) 0.4142(4) 0.059(2) Uani 1 1 d . . . H9 H 0.2036 0.3501 0.4184 0.071 Uiso 1 1 calc R . . C10 C 0.5755(7) 0.3388(5) 0.2802(3) 0.0272(13) Uani 1 1 d . . . H10A H 0.4663 0.3099 0.2746 0.033 Uiso 1 1 calc R . . H10B H 0.6216 0.2974 0.3062 0.033 Uiso 1 1 calc R . . C11 C 0.6330(7) 0.3219(5) 0.2060(3) 0.0295(13) Uani 1 1 d . . . C12 C 0.5631(9) 0.2384(6) 0.1433(4) 0.0461(18) Uani 1 1 d . . . H12A H 0.4704 0.1911 0.1447 0.055 Uiso 1 1 calc R . . C13 C 0.6279(10) 0.2240(8) 0.0794(4) 0.059(2) Uani 1 1 d . . . H13A H 0.5807 0.1657 0.0366 0.070 Uiso 1 1 calc R . . C14 C 0.7654(10) 0.2957(8) 0.0765(4) 0.052(2) Uani 1 1 d . . . H14A H 0.8119 0.2866 0.0326 0.063 Uiso 1 1 calc R . . C15 C 0.8296(9) 0.3810(6) 0.1422(4) 0.0407(17) Uani 1 1 d . . . H15A H 0.9203 0.4312 0.1417 0.049 Uiso 1 1 calc R . . C16 C 0.9156(9) 0.6276(7) 0.4097(5) 0.0487(19) Uani 1 1 d . . . C17 C 1.0579(7) 0.5567(6) 0.2880(4) 0.0366(16) Uani 1 1 d . . . C18 C 0.9155(8) 0.4070(6) 0.3475(5) 0.0424(18) Uani 1 1 d . . . C19 C 0.4179(7) 0.9842(5) 0.1940(3) 0.0255(13) Uani 1 1 d . . . C20 C 0.4811(8) 0.9424(6) 0.1269(4) 0.0394(16) Uani 1 1 d . . . H20A H 0.4163 0.8967 0.0848 0.047 Uiso 1 1 calc R . . C21 C 0.6332(9) 0.9659(7) 0.1206(5) 0.050(2) Uani 1 1 d . . . H21A H 0.6692 0.9343 0.0750 0.060 Uiso 1 1 calc R . . C22 C 0.7329(8) 1.0340(6) 0.1792(5) 0.0464(19) Uani 1 1 d . . . H22A H 0.8362 1.0524 0.1738 0.056 Uiso 1 1 calc R . . C23 C 0.6781(8) 1.0757(6) 0.2473(5) 0.0407(17) Uani 1 1 d . . . H23A H 0.7448 1.1194 0.2892 0.049 Uiso 1 1 calc R . . C24 C 0.5219(7) 1.0519(5) 0.2530(4) 0.0305(14) Uani 1 1 d . . . H24A H 0.4865 1.0834 0.2988 0.037 Uiso 1 1 calc R . . C25 C 0.1927(6) 1.0698(5) 0.1730(3) 0.0258(13) Uani 1 1 d . . . C26 C 0.1706(8) 1.0585(5) 0.0971(4) 0.0333(14) Uani 1 1 d . . . H26A H 0.1727 0.9888 0.0616 0.040 Uiso 1 1 calc R . . C27 C 0.1464(9) 1.1448(6) 0.0738(4) 0.0445(18) Uani 1 1 d . . . H27A H 0.1288 1.1332 0.0232 0.053 Uiso 1 1 calc R . . C28 C 0.1482(9) 1.2520(6) 0.1267(5) 0.0477(19) Uani 1 1 d . . . H28A H 0.1344 1.3128 0.1117 0.057 Uiso 1 1 calc R . . C29 C 0.1706(8) 1.2654(6) 0.2004(5) 0.047(2) Uani 1 1 d . . . H29A H 0.1712 1.3356 0.2360 0.057 Uiso 1 1 calc R . . C30 C 0.1922(7) 1.1765(5) 0.2223(4) 0.0324(14) Uani 1 1 d . . . H30A H 0.2074 1.1884 0.2730 0.039 Uiso 1 1 calc R . . C31 C 0.1891(7) 0.9668(5) 0.2803(3) 0.0275(13) Uani 1 1 d . . . C32 C 0.2506(8) 0.9041(5) 0.3162(3) 0.0315(14) Uani 1 1 d . . . H32A H 0.3292 0.8710 0.2956 0.038 Uiso 1 1 calc R . . C33 C 0.2011(9) 0.8884(7) 0.3811(4) 0.0471(18) Uani 1 1 d . . . H33A H 0.2464 0.8453 0.4028 0.056 Uiso 1 1 calc R . . C34 C 0.0897(10) 0.9340(7) 0.4125(4) 0.056(2) Uani 1 1 d . . . H34A H 0.0547 0.9217 0.4555 0.067 Uiso 1 1 calc R . . C35 C 0.0273(10) 0.9994(8) 0.3809(4) 0.055(2) Uani 1 1 d . . . H35A H -0.0477 1.0349 0.4038 0.066 Uiso 1 1 calc R . . C36 C 0.0737(8) 1.0132(6) 0.3161(4) 0.0375(15) Uani 1 1 d . . . H36A H 0.0258 1.0556 0.2948 0.045 Uiso 1 1 calc R . . C37 C 0.1435(7) 0.8418(5) 0.1425(3) 0.0262(13) Uani 1 1 d . . . C38 C 0.1939(8) 0.7432(5) 0.1370(4) 0.0372(15) Uani 1 1 d . . . H38A H 0.2900 0.7501 0.1588 0.045 Uiso 1 1 calc R . . C39 C 0.1063(9) 0.6359(5) 0.1005(4) 0.0419(17) Uani 1 1 d . . . H39A H 0.1437 0.5722 0.0991 0.050 Uiso 1 1 calc R . . C40 C -0.0338(9) 0.6208(6) 0.0662(4) 0.0458(18) Uani 1 1 d . . . H40A H -0.0919 0.5478 0.0412 0.055 Uiso 1 1 calc R . . C41 C -0.0870(8) 0.7159(6) 0.0695(4) 0.0384(16) Uani 1 1 d . . . H41A H -0.1820 0.7082 0.0461 0.046 Uiso 1 1 calc R . . C42 C 0.0013(7) 0.8241(5) 0.1079(3) 0.0302(13) Uani 1 1 d . . . H42A H -0.0378 0.8875 0.1103 0.036 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 0.01549(18) 0.02983(18) 0.03857(19) 0.01537(12) -0.00225(10) 0.00181(10) O1 0.072(4) 0.077(4) 0.037(3) 0.001(3) -0.016(3) -0.018(3) N1 0.022(3) 0.024(2) 0.029(3) 0.001(2) -0.005(2) -0.002(2) C1 0.022(3) 0.036(3) 0.039(4) 0.015(3) 0.001(3) 0.001(3) B1 0.025(4) 0.021(3) 0.023(3) 0.003(3) -0.002(3) -0.001(3) O2 0.021(3) 0.068(4) 0.101(5) 0.043(4) 0.015(3) 0.005(2) N2 0.019(3) 0.029(3) 0.031(3) 0.018(2) 0.009(2) 0.006(2) C2 0.031(4) 0.035(4) 0.050(4) 0.020(3) 0.005(3) 0.004(3) O3 0.038(3) 0.068(4) 0.115(5) 0.059(4) -0.014(3) 0.007(3) N3 0.027(3) 0.030(3) 0.033(3) 0.016(2) 0.008(2) 0.006(2) C3 0.037(4) 0.045(4) 0.071(5) 0.028(4) 0.009(4) 0.016(3) C4 0.019(3) 0.035(3) 0.064(5) 0.024(3) 0.007(3) 0.003(3) C5 0.020(3) 0.019(3) 0.034(3) 0.007(2) 0.001(2) 0.004(2) C6 0.020(3) 0.034(3) 0.066(5) 0.027(3) -0.002(3) 0.004(3) C7 0.030(4) 0.049(4) 0.035(4) 0.007(3) 0.002(3) 0.005(3) C8 0.033(4) 0.061(5) 0.031(4) 0.013(3) 0.005(3) 0.001(3) C9 0.033(5) 0.086(6) 0.042(4) 0.009(4) 0.004(3) -0.001(4) C10 0.023(3) 0.021(3) 0.032(3) 0.005(2) -0.002(2) -0.002(2) C11 0.031(4) 0.027(3) 0.033(3) 0.014(3) 0.004(3) 0.005(3) C12 0.042(4) 0.049(4) 0.037(4) 0.007(3) -0.006(3) -0.002(3) C13 0.062(6) 0.062(5) 0.033(4) 0.001(4) -0.003(4) -0.004(4) C14 0.057(5) 0.075(6) 0.030(4) 0.023(4) 0.014(3) 0.015(4) C15 0.041(4) 0.049(4) 0.041(4) 0.027(3) 0.012(3) 0.011(3) C16 0.034(4) 0.055(5) 0.056(5) 0.024(4) -0.002(3) -0.003(3) C17 0.020(4) 0.036(4) 0.062(5) 0.026(3) 0.008(3) 0.007(3) C18 0.025(4) 0.049(4) 0.064(5) 0.038(4) -0.006(3) 0.001(3) C19 0.029(3) 0.027(3) 0.027(3) 0.014(2) 0.000(2) 0.011(2) C20 0.031(4) 0.050(4) 0.038(4) 0.014(3) 0.005(3) 0.008(3) C21 0.040(5) 0.069(5) 0.053(5) 0.028(4) 0.019(4) 0.027(4) C22 0.022(4) 0.052(4) 0.072(5) 0.024(4) 0.010(3) 0.016(3) C23 0.028(4) 0.035(4) 0.063(5) 0.023(3) -0.013(3) 0.005(3) C24 0.026(3) 0.022(3) 0.040(4) 0.006(3) -0.001(3) 0.003(2) C25 0.014(3) 0.027(3) 0.034(3) 0.012(3) 0.000(2) -0.001(2) C26 0.034(4) 0.028(3) 0.034(3) 0.009(3) -0.002(3) 0.001(3) C27 0.048(5) 0.045(4) 0.044(4) 0.025(3) -0.001(3) 0.002(3) C28 0.042(5) 0.040(4) 0.076(6) 0.035(4) 0.008(4) 0.016(3) C29 0.033(4) 0.025(3) 0.075(6) 0.004(4) 0.005(4) 0.007(3) C30 0.024(3) 0.029(3) 0.041(4) 0.008(3) 0.001(3) 0.003(3) C31 0.028(3) 0.028(3) 0.020(3) 0.002(2) -0.004(2) 0.002(2) C32 0.040(4) 0.027(3) 0.027(3) 0.010(3) 0.001(3) 0.005(3) C33 0.056(5) 0.048(4) 0.037(4) 0.016(3) -0.003(3) 0.008(4) C34 0.071(6) 0.060(5) 0.030(4) 0.010(4) 0.020(4) 0.005(4) C35 0.060(6) 0.065(5) 0.041(4) 0.016(4) 0.028(4) 0.017(4) C36 0.031(4) 0.044(4) 0.039(4) 0.015(3) 0.007(3) 0.012(3) C37 0.029(3) 0.022(3) 0.023(3) 0.006(2) 0.004(2) -0.003(2) C38 0.038(4) 0.032(3) 0.040(4) 0.011(3) -0.003(3) 0.010(3) C39 0.051(5) 0.022(3) 0.044(4) 0.001(3) 0.003(3) 0.005(3) C40 0.054(5) 0.030(4) 0.038(4) -0.001(3) -0.002(3) -0.006(3) C41 0.029(4) 0.034(4) 0.040(4) 0.004(3) -0.009(3) -0.005(3) C42 0.032(4) 0.029(3) 0.029(3) 0.011(3) -0.002(3) 0.005(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 C18 1.907(7) . ? Re1 C17 1.916(7) . ? Re1 C16 1.932(9) . ? Re1 N3 2.165(5) . ? Re1 N1 2.166(5) . ? Re1 N2 2.216(5) . ? O1 C16 1.153(10) . ? N1 C5 1.339(8) . ? N1 C1 1.358(9) . ? C1 C2 1.374(10) . ? C1 H1A 0.9400 . ? B1 C31 1.637(9) . ? B1 C25 1.644(9) . ? B1 C19 1.653(9) . ? B1 C37 1.657(8) . ? O2 C17 1.146(8) . ? N2 C7 1.496(9) . ? N2 C10 1.497(7) . ? N2 C6 1.516(8) . ? C2 C3 1.382(10) . ? C2 H2A 0.9400 . ? O3 C18 1.166(9) . ? N3 C11 1.356(8) . ? N3 C15 1.362(9) . ? C3 C4 1.351(10) . ? C3 H3A 0.9400 . ? C4 C5 1.398(9) . ? C4 H4A 0.9400 . ? C5 C6 1.454(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 C8 1.456(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C8 C9 1.161(11) . ? C9 H9 0.9400 . ? C10 C11 1.498(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.367(9) . ? C12 C13 1.351(11) . ? C12 H12A 0.9400 . ? C13 C14 1.407(12) . ? C13 H13A 0.9400 . ? C14 C15 1.399(11) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C19 C24 1.388(8) . ? C19 C20 1.417(9) . ? C20 C21 1.376(10) . ? C20 H20A 0.9400 . ? C21 C22 1.365(11) . ? C21 H21A 0.9400 . ? C22 C23 1.396(11) . ? C22 H22A 0.9400 . ? C23 C24 1.410(10) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 C30 1.394(9) . ? C25 C26 1.425(9) . ? C26 C27 1.372(10) . ? C26 H26A 0.9400 . ? C27 C28 1.422(11) . ? C27 H27A 0.9400 . ? C28 C29 1.379(12) . ? C28 H28A 0.9400 . ? C29 C30 1.379(10) . ? C29 H29A 0.9400 . ? C30 H30A 0.9400 . ? C31 C32 1.398(9) . ? C31 C36 1.403(9) . ? C32 C33 1.396(10) . ? C32 H32A 0.9400 . ? C33 C34 1.338(12) . ? C33 H33A 0.9400 . ? C34 C35 1.377(13) . ? C34 H34A 0.9400 . ? C35 C36 1.378(11) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C37 C42 1.388(9) . ? C37 C38 1.403(9) . ? C38 C39 1.389(9) . ? C38 H38A 0.9400 . ? C39 C40 1.375(11) . ? C39 H39A 0.9400 . ? C40 C41 1.385(11) . ? C40 H40A 0.9400 . ? C41 C42 1.406(9) . ? C41 H41A 0.9400 . ? C42 H42A 0.9400 . ? 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 C18 Re1 C17 88.2(3) . . ? C18 Re1 C16 89.0(4) . . ? C17 Re1 C16 88.9(3) . . ? C18 Re1 N3 92.6(3) . . ? C17 Re1 N3 97.1(3) . . ? C16 Re1 N3 173.8(3) . . ? C18 Re1 N1 172.4(2) . . ? C17 Re1 N1 99.2(2) . . ? C16 Re1 N1 92.6(3) . . ? N3 Re1 N1 85.03(19) . . ? C18 Re1 N2 95.0(3) . . ? C17 Re1 N2 171.5(2) . . ? C16 Re1 N2 99.1(3) . . ? N3 Re1 N2 74.87(19) . . ? N1 Re1 N2 77.41(19) . . ? C5 N1 C1 118.1(5) . . ? C5 N1 Re1 117.5(4) . . ? C1 N1 Re1 124.3(4) . . ? N1 C1 C2 122.6(6) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C31 B1 C25 115.5(5) . . ? C31 B1 C19 111.1(5) . . ? C25 B1 C19 104.2(5) . . ? C31 B1 C37 104.0(5) . . ? C25 B1 C37 111.1(5) . . ? C19 B1 C37 111.1(5) . . ? C7 N2 C10 109.5(5) . . ? C7 N2 C6 110.0(5) . . ? C10 N2 C6 108.8(5) . . ? C7 N2 Re1 113.2(4) . . ? C10 N2 Re1 104.4(3) . . ? C6 N2 Re1 110.7(4) . . ? C1 C2 C3 118.0(6) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C11 N3 C15 118.0(6) . . ? C11 N3 Re1 115.9(4) . . ? C15 N3 Re1 126.1(5) . . ? C4 C3 C2 120.6(7) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 118.8(6) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 118.1(5) . . ? C4 C5 C6 119.9(5) . . ? C5 C6 N2 114.6(5) . . ? C5 C6 H6A 108.6 . . ? N2 C6 H6A 108.6 . . ? C5 C6 H6B 108.6 . . ? N2 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 N2 114.5(6) . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7B 108.6 . . ? N2 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C9 C8 C7 178.0(9) . . ? C8 C9 H9 180.0 . . ? N2 C10 C11 108.8(5) . . ? N2 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N2 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? N3 C11 C12 122.5(6) . . ? N3 C11 C10 114.0(5) . . ? C12 C11 C10 123.5(6) . . ? C13 C12 C11 119.8(7) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C12 C13 C14 120.6(7) . . ? C12 C13 H13A 119.7 . . ? C14 C13 H13A 119.7 . . ? C15 C14 C13 116.9(7) . . ? C15 C14 H14A 121.6 . . ? C13 C14 H14A 121.6 . . ? N3 C15 C14 122.3(7) . . ? N3 C15 H15A 118.9 . . ? C14 C15 H15A 118.9 . . ? O1 C16 Re1 177.1(8) . . ? O2 C17 Re1 179.7(6) . . ? O3 C18 Re1 179.0(7) . . ? C24 C19 C20 114.6(6) . . ? C24 C19 B1 122.9(5) . . ? C20 C19 B1 122.1(5) . . ? C21 C20 C19 122.9(7) . . ? C21 C20 H20A 118.6 . . ? C19 C20 H20A 118.6 . . ? C22 C21 C20 121.4(7) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C21 C22 C23 118.5(7) . . ? C21 C22 H22A 120.8 . . ? C23 C22 H22A 120.8 . . ? C22 C23 C24 119.5(7) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C19 C24 C23 123.1(6) . . ? C19 C24 H24A 118.5 . . ? C23 C24 H24A 118.5 . . ? C30 C25 C26 115.2(6) . . ? C30 C25 B1 123.2(5) . . ? C26 C25 B1 121.2(5) . . ? C27 C26 C25 122.9(6) . . ? C27 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C26 C27 C28 119.4(7) . . ? C26 C27 H27A 120.3 . . ? C28 C27 H27A 120.3 . . ? C29 C28 C27 118.8(6) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? C28 C29 C30 120.5(7) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C29 C30 C25 123.2(7) . . ? C29 C30 H30A 118.4 . . ? C25 C30 H30A 118.4 . . ? C32 C31 C36 113.6(6) . . ? C32 C31 B1 121.0(6) . . ? C36 C31 B1 124.8(6) . . ? C33 C32 C31 123.2(7) . . ? C33 C32 H32A 118.4 . . ? C31 C32 H32A 118.4 . . ? C34 C33 C32 120.7(8) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C35 118.9(7) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C34 C35 C36 120.6(8) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C31 123.0(7) . . ? C35 C36 H36A 118.5 . . ? C31 C36 H36A 118.5 . . ? C42 C37 C38 115.2(5) . . ? C42 C37 B1 122.4(5) . . ? C38 C37 B1 121.6(6) . . ? C39 C38 C37 122.2(7) . . ? C39 C38 H38A 118.9 . . ? C37 C38 H38A 118.9 . . ? C40 C39 C38 121.5(7) . . ? C40 C39 H39A 119.3 . . ? C38 C39 H39A 119.3 . . ? C39 C40 C41 118.2(6) . . ? C39 C40 H40A 120.9 . . ? C41 C40 H40A 120.9 . . ? C40 C41 C42 119.8(6) . . ? C40 C41 H41A 120.1 . . ? C42 C41 H41A 120.1 . . ? C37 C42 C41 123.2(6) . . ? C37 C42 H42A 118.4 . . ? C41 C42 H42A 118.4 . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.244 _refine_diff_density_min -2.340 _refine_diff_density_rms 0.160