# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_xxx #TrackingRef '16936_web_deposit_cif_file_0_MichaelSeitz_1358418685.Dalton_Gueden-Silber_X-ray_4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 F6 N2 O2' _chemical_formula_weight 352.24 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-x+1/2, y+1/2, -z+1/4' '-y, -x, -z+1/2' _cell_length_a 11.873(5) _cell_length_b 11.873(5) _cell_length_c 9.961(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1404.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _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 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9677 _exptl_absorpt_correction_T_max 0.9837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'XtaLAB mini' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12062 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1235 _reflns_number_gt 983 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1993)' _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^)+(0.0589P)^2^+0.5206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1235 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F1 F 0.3028(2) 0.0406(3) -0.0204(3) 0.0922(10) Uani 1 1 d . . . F2 F 0.3621(2) 0.1987(2) 0.0477(3) 0.0890(10) Uani 1 1 d . . . F3 F 0.40368(18) 0.0514(2) 0.1533(3) 0.0783(8) Uani 1 1 d . . . O1 O -0.0610(2) 0.1490(2) 0.4033(3) 0.0628(8) Uani 1 1 d . . . C2 C 0.2069(3) 0.2053(3) 0.2583(4) 0.0471(9) Uani 1 1 d . . . H2A H 0.2651 0.2575 0.2644 0.056 Uiso 1 1 calc R . . C4 C 0.1332(3) 0.0361(3) 0.1658(4) 0.0415(8) Uani 1 1 d . . . H4A H 0.1397 -0.0253 0.1082 0.050 Uiso 1 1 calc R . . C5 C 0.0397(3) 0.0483(3) 0.2459(4) 0.0417(8) Uani 1 1 d . . . N1 N 0.0282(2) 0.1391(2) 0.3303(3) 0.0449(7) Uani 1 1 d . . . C3 C 0.2171(3) 0.1159(3) 0.1721(4) 0.0431(8) Uani 1 1 d . . . C6 C 0.0929(4) 0.3145(3) 0.4297(4) 0.0668(12) Uani 1 1 d . . . H6A H 0.1562 0.3648 0.4269 0.100 Uiso 1 1 calc R . . H6B H 0.0840 0.2859 0.5192 0.100 Uiso 1 1 calc R . . H6C H 0.0260 0.3543 0.4037 0.100 Uiso 1 1 calc R . . C1 C 0.1124(3) 0.2190(3) 0.3355(4) 0.0467(9) Uani 1 1 d . . . C7 C 0.3206(3) 0.1011(3) 0.0886(4) 0.0523(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0625(16) 0.133(3) 0.0814(18) -0.032(2) 0.0196(14) -0.0101(17) F2 0.0718(17) 0.0685(17) 0.127(2) 0.0392(17) 0.0470(17) 0.0040(13) F3 0.0446(13) 0.091(2) 0.0991(18) 0.0349(17) 0.0063(13) 0.0163(13) O1 0.0543(17) 0.0495(16) 0.0846(19) -0.0037(14) 0.0305(17) 0.0015(12) C2 0.0422(19) 0.044(2) 0.055(2) 0.0081(19) -0.006(2) -0.0103(15) C4 0.0359(18) 0.0367(19) 0.0518(19) 0.0024(16) 0.0045(17) 0.0038(14) C5 0.0381(19) 0.0302(18) 0.057(2) 0.0023(18) -0.0004(17) -0.0004(14) N1 0.0411(17) 0.0377(16) 0.0559(17) 0.0038(15) 0.0054(14) 0.0002(13) C3 0.0330(18) 0.043(2) 0.053(2) 0.0054(18) -0.0007(17) -0.0007(15) C6 0.084(3) 0.046(2) 0.070(3) -0.015(2) 0.003(3) -0.003(2) C1 0.050(2) 0.0327(18) 0.058(2) 0.0024(18) -0.0063(19) -0.0032(16) C7 0.041(2) 0.050(2) 0.066(2) 0.011(2) 0.004(2) -0.0027(17) _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 F1 C7 1.319(5) . ? F2 C7 1.323(4) . ? F3 C7 1.317(4) . ? O1 N1 1.290(4) . ? C2 C3 1.370(5) . ? C2 C1 1.371(5) . ? C2 H2A 0.9300 . ? C4 C5 1.375(5) . ? C4 C3 1.377(5) . ? C4 H4A 0.9300 . ? C5 N1 1.375(4) . ? C5 C5 1.479(6) 8 ? N1 C1 1.379(4) . ? C3 C7 1.494(5) . ? C6 C1 1.490(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 C2 C1 121.1(3) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C5 C4 C3 119.0(4) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C5 116.7(3) . 8 ? C4 C5 C5 121.9(3) . 8 ? O1 N1 C5 119.8(3) . . ? O1 N1 C1 120.8(3) . . ? C5 N1 C1 119.4(3) . . ? C2 C3 C4 119.9(3) . . ? C2 C3 C7 120.8(3) . . ? C4 C3 C7 119.3(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C1 N1 119.4(3) . . ? C2 C1 C6 124.8(3) . . ? N1 C1 C6 115.8(3) . . ? F3 C7 F1 106.2(3) . . ? F3 C7 F2 105.3(3) . . ? F1 C7 F2 106.4(3) . . ? F3 C7 C3 113.4(3) . . ? F1 C7 C3 112.9(3) . . ? F2 C7 C3 112.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 C4 C5 N1 0.8(5) . . . . ? C3 C4 C5 C5 -173.9(3) . . . 8 ? C4 C5 N1 O1 179.3(3) . . . . ? C5 C5 N1 O1 -5.7(5) 8 . . . ? C4 C5 N1 C1 -0.5(5) . . . . ? C5 C5 N1 C1 174.4(3) 8 . . . ? C1 C2 C3 C4 -2.3(6) . . . . ? C1 C2 C3 C7 -179.7(3) . . . . ? C5 C4 C3 C2 0.6(5) . . . . ? C5 C4 C3 C7 178.0(3) . . . . ? C3 C2 C1 N1 2.6(6) . . . . ? C3 C2 C1 C6 -178.7(3) . . . . ? O1 N1 C1 C2 179.0(3) . . . . ? C5 N1 C1 C2 -1.2(5) . . . . ? O1 N1 C1 C6 0.1(5) . . . . ? C5 N1 C1 C6 -180.0(3) . . . . ? C2 C3 C7 F3 83.0(4) . . . . ? C4 C3 C7 F3 -94.4(4) . . . . ? C2 C3 C7 F1 -156.2(4) . . . . ? C4 C3 C7 F1 26.4(5) . . . . ? C2 C3 C7 F2 -36.1(5) . . . . ? C4 C3 C7 F2 146.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.164 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.043 _database_code_depnum_ccdc_archive 'CCDC 920406' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ttt #TrackingRef '16937_web_deposit_cif_file_1_MichaelSeitz_1358418685.Dalton_Gueden-Silber_X-ray_Tb-7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H24 F12 N5 O8 Tb' _chemical_formula_weight 1017.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1720 4.1540 '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 10.181(12) _cell_length_b 11.591(12) _cell_length_c 16.455(18) _cell_angle_alpha 78.15(3) _cell_angle_beta 85.49(3) _cell_angle_gamma 84.13(3) _cell_volume 1887(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'XtaLAB mini' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19245 _diffrn_reflns_av_R_equivalents 0.0542 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8479 _reflns_number_gt 7024 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.1054P)^2^+6.7265P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8479 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0718 _refine_ls_wR_factor_ref 0.2072 _refine_ls_wR_factor_gt 0.1886 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 Tb1 Tb 0.49245(4) 0.61550(3) 0.231646(19) 0.04414(15) Uani 1 1 d . . . N102 N 0.4854(6) 0.7029(6) 0.0795(4) 0.0389(12) Uani 1 1 d . . . N101 N 0.3362(6) 0.5351(6) 0.1517(4) 0.0409(13) Uani 1 1 d . . . O204 O 0.3240(6) 0.7656(5) 0.2412(3) 0.0524(14) Uani 1 1 d . . . N201 N 0.6646(7) 0.5223(6) 0.3331(4) 0.0488(15) Uani 1 1 d . . . N202 N 0.4860(6) 0.6909(6) 0.3642(4) 0.0448(14) Uani 1 1 d . . . F101 F -0.0140(5) 0.3673(6) 0.0339(5) 0.090(2) Uani 1 1 d . . . C208 C 0.5693(8) 0.6447(8) 0.4261(4) 0.0469(18) Uani 1 1 d . . . C110 C 0.4857(7) 0.8119(7) -0.0869(4) 0.0438(16) Uani 1 1 d . . . F203 F 1.0479(6) 0.3640(8) 0.4995(5) 0.108(3) Uani 1 1 d . . . C109 C 0.4128(7) 0.7151(7) -0.0569(4) 0.0415(15) Uani 1 1 d . . . H109 H 0.3645 0.6856 -0.0926 0.050 Uiso 1 1 calc R . . O104 O 0.6314(6) 0.7658(5) 0.1867(3) 0.0500(13) Uani 1 1 d . . . C207 C 0.6660(8) 0.5460(8) 0.4099(5) 0.0464(17) Uani 1 1 d . . . O201 O 0.6411(7) 0.4762(6) 0.1836(3) 0.0567(15) Uani 1 1 d . . . O203 O 0.2197(6) 0.9049(6) 0.3035(4) 0.0594(15) Uani 1 1 d . . . F206 F 0.3891(13) 0.9413(9) 0.5743(5) 0.142(4) Uani 1 1 d . . . C107 C 0.3350(7) 0.5619(7) 0.0680(4) 0.0394(15) Uani 1 1 d . . . F102 F 0.1358(7) 0.2248(5) 0.0554(5) 0.092(2) Uani 1 1 d . . . F103 F 0.1494(7) 0.3536(7) -0.0540(4) 0.089(2) Uani 1 1 d . . . F204 F 0.5771(11) 0.8733(8) 0.5952(5) 0.128(4) Uani 1 1 d . . . C214 C 0.3059(8) 0.8232(7) 0.2988(5) 0.0464(17) Uani 1 1 d . . . F202 F 0.8887(7) 0.3197(10) 0.5818(4) 0.127(4) Uani 1 1 d . . . C202 C 0.7506(8) 0.4379(8) 0.3098(5) 0.0504(18) Uani 1 1 d . . . O102 O 0.1947(10) 0.3624(7) 0.3333(5) 0.091(3) Uani 1 1 d . . . O103 O 0.7016(7) 0.9195(6) 0.0903(4) 0.0607(16) Uani 1 1 d . . . C108 C 0.4132(7) 0.6638(7) 0.0264(4) 0.0386(14) Uani 1 1 d . . . O202 O 0.8218(9) 0.3477(8) 0.1944(5) 0.085(2) Uani 1 1 d . . . C201 C 0.7399(10) 0.4168(9) 0.2214(5) 0.060(2) Uani 1 1 d . . . C106 C 0.2659(7) 0.4995(7) 0.0243(5) 0.0409(15) Uani 1 1 d . . . H106 H 0.2689 0.5163 -0.0335 0.049 Uiso 1 1 calc R . . C212 C 0.3875(9) 0.8352(8) 0.4397(5) 0.053(2) Uani 1 1 d . . . H212 H 0.3261 0.8993 0.4437 0.063 Uiso 1 1 calc R . . C210 C 0.4743(10) 0.7884(8) 0.5030(5) 0.059(2) Uani 1 1 d . . . C105 C 0.1146(8) 0.3410(8) 0.0254(6) 0.0512(19) Uani 1 1 d . . . C213 C 0.3969(8) 0.7822(7) 0.3710(5) 0.0461(17) Uani 1 1 d . . . C102 C 0.2611(8) 0.4509(7) 0.1949(5) 0.0463(17) Uani 1 1 d . . . C104 C 0.1929(8) 0.4124(7) 0.0695(5) 0.0458(17) Uani 1 1 d . . . O101 O 0.3565(7) 0.4849(6) 0.3150(3) 0.0603(16) Uani 1 1 d . . . F201 F 0.9475(13) 0.2103(8) 0.4993(7) 0.160(5) Uani 1 1 d . . . C113 C 0.5557(7) 0.7967(7) 0.0510(4) 0.0407(15) Uani 1 1 d . . . C205 C 0.9342(11) 0.3178(11) 0.5039(6) 0.074(3) Uani 1 1 d . . . C203 C 0.8425(9) 0.3707(8) 0.3639(6) 0.057(2) Uani 1 1 d . . . H203 H 0.9031 0.3136 0.3467 0.068 Uiso 1 1 calc R . . C204 C 0.8399(9) 0.3923(9) 0.4430(5) 0.057(2) Uani 1 1 d . . . C114 C 0.6360(8) 0.8313(8) 0.1140(5) 0.0473(17) Uani 1 1 d . . . F205 F 0.4228(13) 0.7662(8) 0.6457(4) 0.158(5) Uani 1 1 d . . . C206 C 0.7511(9) 0.4804(8) 0.4674(5) 0.055(2) Uani 1 1 d . . . H206 H 0.7490 0.4949 0.5210 0.066 Uiso 1 1 calc R . . C209 C 0.5633(10) 0.6935(9) 0.4969(5) 0.056(2) Uani 1 1 d . . . H209 H 0.6192 0.6620 0.5395 0.068 Uiso 1 1 calc R . . C112 C 0.5574(8) 0.8538(7) -0.0325(5) 0.0451(16) Uani 1 1 d . . . H112 H 0.6058 0.9190 -0.0513 0.054 Uiso 1 1 calc R . . C101 C 0.2678(11) 0.4286(8) 0.2896(5) 0.059(2) Uani 1 1 d . . . C211 C 0.4655(14) 0.8401(10) 0.5796(6) 0.077(3) Uani 1 1 d . . . F104 F 0.3764(6) 0.8778(5) -0.2102(3) 0.0707(15) Uani 1 1 d . . . F106 F 0.5349(8) 0.9756(6) -0.1926(4) 0.086(2) Uani 1 1 d . . . F105 F 0.5766(9) 0.8007(7) -0.2186(4) 0.118(3) Uani 1 1 d . . . C111 C 0.4954(9) 0.8664(8) -0.1780(5) 0.0528(19) Uani 1 1 d . . . C103 C 0.1868(8) 0.3879(7) 0.1564(5) 0.0494(18) Uani 1 1 d . . . H103 H 0.1345 0.3310 0.1870 0.059 Uiso 1 1 calc R . . N1T N 0.0040(11) 0.8840(9) 0.2087(7) 0.086(3) Uani 1 1 d . . . HN1T H 0.0795 0.8822 0.2352 0.103 Uiso 1 1 calc R . . C3T C -0.062(2) 1.0041(16) 0.1990(15) 0.158(10) Uani 1 1 d . . . H3TB H -0.1469 1.0065 0.1751 0.189 Uiso 1 1 calc R . . H3TA H -0.0087 1.0588 0.1613 0.189 Uiso 1 1 calc R . . C6T C -0.008(2) 0.6677(15) 0.2488(16) 0.160(10) Uani 1 1 d . . . H6TA H -0.0661 0.6127 0.2807 0.240 Uiso 1 1 calc R . . H6TB H 0.0772 0.6539 0.2719 0.240 Uiso 1 1 calc R . . H6TC H 0.0010 0.6571 0.1922 0.240 Uiso 1 1 calc R . . C1T C 0.042(2) 0.860(3) 0.1221(11) 0.194(13) Uani 1 1 d . . . H1TA H 0.0598 0.7754 0.1271 0.232 Uiso 1 1 calc R . . H1TB H -0.0342 0.8847 0.0891 0.232 Uiso 1 1 calc R . . C2T C 0.158(2) 0.9167(16) 0.0735(11) 0.133(7) Uani 1 1 d . . . H2TB H 0.1716 0.8915 0.0211 0.200 Uiso 1 1 calc R . . H2TA H 0.2358 0.8934 0.1044 0.200 Uiso 1 1 calc R . . H2TC H 0.1406 1.0012 0.0638 0.200 Uiso 1 1 calc R . . C5T C -0.067(2) 0.797(2) 0.251(2) 0.31(3) Uani 1 1 d . . . H5TB H -0.1542 0.8077 0.2300 0.375 Uiso 1 1 calc R . . H5TA H -0.0774 0.8048 0.3091 0.375 Uiso 1 1 calc R . . C4T C -0.085(3) 1.044(3) 0.286(2) 0.34(3) Uani 1 1 d . . . H4TA H -0.1271 1.1225 0.2788 0.509 Uiso 1 1 calc R . . H4TC H -0.0009 1.0413 0.3099 0.509 Uiso 1 1 calc R . . H4TB H -0.1397 0.9905 0.3232 0.509 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 Tb1 0.0497(2) 0.0652(3) 0.01964(19) -0.01205(15) -0.00815(14) -0.00311(16) N102 0.039(3) 0.057(3) 0.024(3) -0.016(2) -0.006(2) -0.002(2) N101 0.041(3) 0.060(4) 0.024(3) -0.014(2) -0.003(2) -0.002(3) O204 0.050(3) 0.076(4) 0.036(3) -0.021(3) -0.014(2) 0.003(3) N201 0.056(4) 0.070(4) 0.019(3) -0.002(3) -0.010(3) -0.008(3) N202 0.044(3) 0.069(4) 0.024(3) -0.013(3) -0.004(2) -0.010(3) F101 0.036(3) 0.106(5) 0.149(7) -0.071(5) -0.008(3) -0.001(3) C208 0.055(4) 0.071(5) 0.018(3) -0.003(3) -0.008(3) -0.028(4) C110 0.044(4) 0.059(4) 0.025(3) -0.010(3) -0.001(3) 0.010(3) F203 0.046(3) 0.150(7) 0.103(6) 0.045(5) -0.018(3) -0.026(4) C109 0.043(4) 0.058(4) 0.024(3) -0.014(3) -0.008(3) 0.007(3) O104 0.052(3) 0.072(3) 0.029(3) -0.014(2) -0.013(2) -0.005(3) C207 0.047(4) 0.068(5) 0.025(3) -0.007(3) -0.006(3) -0.013(3) O201 0.072(4) 0.071(4) 0.028(3) -0.017(2) -0.010(3) 0.009(3) O203 0.056(4) 0.081(4) 0.046(3) -0.025(3) 0.001(3) -0.002(3) F206 0.244(13) 0.132(7) 0.061(5) -0.061(5) -0.012(6) 0.016(7) C107 0.039(3) 0.056(4) 0.022(3) -0.009(3) -0.003(3) 0.003(3) F102 0.105(5) 0.060(3) 0.119(6) -0.033(4) -0.038(4) 0.001(3) F103 0.094(5) 0.129(6) 0.063(4) -0.049(4) 0.003(3) -0.046(4) F204 0.208(10) 0.128(6) 0.076(5) -0.042(5) -0.039(6) -0.081(7) C214 0.043(4) 0.062(4) 0.039(4) -0.018(3) 0.002(3) -0.013(3) F202 0.067(4) 0.236(10) 0.048(4) 0.049(5) -0.018(3) -0.013(5) C202 0.053(4) 0.069(5) 0.028(4) -0.006(3) -0.008(3) -0.002(4) O102 0.144(8) 0.088(5) 0.046(4) -0.015(4) 0.024(5) -0.052(5) O103 0.065(4) 0.073(4) 0.049(4) -0.014(3) -0.006(3) -0.023(3) C108 0.036(3) 0.057(4) 0.026(3) -0.017(3) -0.008(3) 0.004(3) O202 0.098(6) 0.107(6) 0.045(4) -0.026(4) -0.010(4) 0.042(5) C201 0.067(6) 0.086(6) 0.024(4) -0.009(4) -0.002(4) 0.007(5) C106 0.037(3) 0.055(4) 0.034(4) -0.019(3) -0.006(3) 0.005(3) C212 0.069(5) 0.061(5) 0.033(4) -0.016(3) 0.007(4) -0.022(4) C210 0.087(7) 0.069(5) 0.031(4) -0.019(4) -0.004(4) -0.036(5) C105 0.043(4) 0.060(5) 0.056(5) -0.024(4) -0.001(3) -0.006(3) C213 0.052(4) 0.067(5) 0.026(3) -0.015(3) 0.001(3) -0.025(4) C102 0.058(5) 0.053(4) 0.029(4) -0.014(3) 0.003(3) -0.004(3) C104 0.042(4) 0.058(4) 0.043(4) -0.023(3) -0.006(3) 0.000(3) O101 0.086(5) 0.075(4) 0.021(3) -0.009(2) 0.001(3) -0.018(3) F201 0.228(12) 0.102(6) 0.155(10) -0.012(6) -0.137(9) 0.035(7) C113 0.041(4) 0.054(4) 0.027(3) -0.008(3) -0.010(3) 0.003(3) C205 0.065(6) 0.103(8) 0.047(6) 0.014(5) -0.027(5) -0.017(6) C203 0.051(5) 0.067(5) 0.047(5) 0.004(4) -0.012(4) -0.002(4) C204 0.048(4) 0.079(6) 0.038(4) 0.009(4) -0.015(3) -0.014(4) C114 0.042(4) 0.065(5) 0.040(4) -0.020(4) -0.006(3) -0.008(3) F205 0.310(14) 0.145(7) 0.046(4) -0.051(4) 0.058(6) -0.137(9) C206 0.057(5) 0.080(6) 0.027(4) 0.006(4) -0.015(3) -0.028(4) C209 0.074(6) 0.080(6) 0.019(3) -0.007(3) -0.006(3) -0.030(5) C112 0.050(4) 0.052(4) 0.034(4) -0.009(3) -0.008(3) 0.000(3) C101 0.084(6) 0.060(5) 0.036(4) -0.017(4) 0.006(4) -0.012(4) C211 0.128(10) 0.078(7) 0.034(5) -0.022(4) -0.002(5) -0.031(7) F104 0.088(4) 0.085(4) 0.035(3) 0.000(2) -0.025(3) 0.000(3) F106 0.120(6) 0.081(4) 0.049(3) 0.015(3) 0.001(3) -0.031(4) F105 0.167(8) 0.132(6) 0.028(3) -0.006(3) 0.010(4) 0.083(6) C111 0.057(5) 0.073(5) 0.025(4) -0.006(3) -0.002(3) 0.001(4) C103 0.049(4) 0.054(4) 0.049(5) -0.018(4) 0.002(3) -0.006(3) N1T 0.087(7) 0.090(7) 0.084(7) -0.019(5) -0.026(6) -0.006(5) C3T 0.148(17) 0.132(14) 0.22(2) -0.094(15) -0.112(17) 0.045(12) C6T 0.164(19) 0.094(11) 0.24(3) -0.033(14) -0.096(18) -0.017(11) C1T 0.118(16) 0.39(4) 0.063(10) -0.003(17) -0.014(10) -0.05(2) C2T 0.172(18) 0.130(13) 0.086(11) 0.015(10) 0.006(11) -0.044(13) C5T 0.143(18) 0.17(2) 0.57(6) 0.18(3) -0.23(3) -0.093(17) C4T 0.30(4) 0.44(5) 0.35(4) -0.33(4) -0.20(3) 0.28(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Tb1 O201 2.315(6) . ? Tb1 O101 2.317(6) . ? Tb1 O104 2.322(6) . ? Tb1 O204 2.335(6) . ? Tb1 N101 2.502(6) . ? Tb1 N102 2.504(6) . ? Tb1 N202 2.504(7) . ? Tb1 N201 2.522(7) . ? N102 C113 1.345(10) . ? N102 C108 1.357(8) . ? N101 C107 1.350(9) . ? N101 C102 1.351(10) . ? O204 C214 1.260(9) . ? N201 C202 1.341(11) . ? N201 C207 1.348(10) . ? N202 C213 1.339(11) . ? N202 C208 1.364(10) . ? F101 C105 1.317(10) . ? C208 C209 1.390(11) . ? C208 C207 1.484(13) . ? C110 C112 1.388(11) . ? C110 C109 1.392(11) . ? C110 C111 1.503(10) . ? F203 C205 1.315(12) . ? C109 C108 1.379(10) . ? C109 H109 0.9300 . ? O104 C114 1.278(10) . ? C207 C206 1.386(11) . ? O201 C201 1.286(11) . ? O203 C214 1.233(10) . ? F206 C211 1.330(16) . ? C107 C106 1.389(10) . ? C107 C108 1.507(11) . ? F102 C105 1.338(11) . ? F103 C105 1.309(11) . ? F204 C211 1.296(15) . ? C214 C213 1.533(11) . ? F202 C205 1.332(14) . ? C202 C203 1.404(11) . ? C202 C201 1.539(11) . ? O102 C101 1.211(12) . ? O103 C114 1.256(10) . ? O202 C201 1.218(11) . ? C106 C104 1.372(11) . ? C106 H106 0.9300 . ? C212 C213 1.385(11) . ? C212 C210 1.406(13) . ? C212 H212 0.9300 . ? C210 C209 1.367(15) . ? C210 C211 1.495(12) . ? C105 C104 1.523(11) . ? C102 C103 1.373(11) . ? C102 C101 1.531(11) . ? C104 C103 1.397(12) . ? O101 C101 1.307(11) . ? F201 C205 1.256(15) . ? C113 C112 1.398(10) . ? C113 C114 1.509(10) . ? C205 C204 1.516(12) . ? C203 C204 1.373(14) . ? C203 H203 0.9300 . ? C204 C206 1.394(14) . ? F205 C211 1.314(13) . ? C206 H206 0.9300 . ? C209 H209 0.9300 . ? C112 H112 0.9300 . ? F104 C111 1.344(10) . ? F106 C111 1.335(11) . ? F105 C111 1.305(10) . ? C103 H103 0.9300 . ? N1T C5T 1.35(2) . ? N1T C3T 1.467(19) . ? N1T C1T 1.52(2) . ? N1T HN1T 0.9100 . ? C3T C4T 1.59(3) . ? C3T H3TB 0.9700 . ? C3T H3TA 0.9700 . ? C6T C5T 1.56(3) . ? C6T H6TA 0.9600 . ? C6T H6TB 0.9600 . ? C6T H6TC 0.9600 . ? C1T C2T 1.50(2) . ? C1T H1TA 0.9700 . ? C1T H1TB 0.9700 . ? C2T H2TB 0.9600 . ? C2T H2TA 0.9600 . ? C2T H2TC 0.9600 . ? C5T H5TB 0.9700 . ? C5T H5TA 0.9700 . ? C4T H4TA 0.9600 . ? C4T H4TC 0.9600 . ? C4T H4TB 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O201 Tb1 O101 97.5(3) . . ? O201 Tb1 O104 92.8(2) . . ? O101 Tb1 O104 162.2(2) . . ? O201 Tb1 O204 163.6(2) . . ? O101 Tb1 O204 87.7(3) . . ? O104 Tb1 O204 86.4(2) . . ? O201 Tb1 N101 82.2(2) . . ? O101 Tb1 N101 66.6(2) . . ? O104 Tb1 N101 129.6(2) . . ? O204 Tb1 N101 85.7(2) . . ? O201 Tb1 N102 82.3(2) . . ? O101 Tb1 N102 129.3(2) . . ? O104 Tb1 N102 66.43(19) . . ? O204 Tb1 N102 82.3(2) . . ? N101 Tb1 N102 63.2(2) . . ? O201 Tb1 N202 129.5(2) . . ? O101 Tb1 N202 80.4(2) . . ? O104 Tb1 N202 81.9(2) . . ? O204 Tb1 N202 66.6(2) . . ? N101 Tb1 N202 137.7(2) . . ? N102 Tb1 N202 136.9(2) . . ? O201 Tb1 N201 66.5(2) . . ? O101 Tb1 N201 84.4(2) . . ? O104 Tb1 N201 86.4(2) . . ? O204 Tb1 N201 129.7(2) . . ? N101 Tb1 N201 134.0(2) . . ? N102 Tb1 N201 137.6(2) . . ? N202 Tb1 N201 63.1(2) . . ? C113 N102 C108 119.5(6) . . ? C113 N102 Tb1 116.3(4) . . ? C108 N102 Tb1 124.2(5) . . ? C107 N101 C102 119.3(6) . . ? C107 N101 Tb1 123.2(5) . . ? C102 N101 Tb1 117.1(5) . . ? C214 O204 Tb1 125.5(5) . . ? C202 N201 C207 120.1(7) . . ? C202 N201 Tb1 116.1(5) . . ? C207 N201 Tb1 123.5(6) . . ? C213 N202 C208 120.8(7) . . ? C213 N202 Tb1 116.2(5) . . ? C208 N202 Tb1 123.0(6) . . ? N202 C208 C209 120.0(9) . . ? N202 C208 C207 115.6(7) . . ? C209 C208 C207 124.4(7) . . ? C112 C110 C109 119.4(7) . . ? C112 C110 C111 119.4(8) . . ? C109 C110 C111 121.1(7) . . ? C108 C109 C110 118.9(7) . . ? C108 C109 H109 120.5 . . ? C110 C109 H109 120.5 . . ? C114 O104 Tb1 125.2(5) . . ? N201 C207 C206 121.1(8) . . ? N201 C207 C208 114.4(7) . . ? C206 C207 C208 124.6(7) . . ? C201 O201 Tb1 126.9(5) . . ? N101 C107 C106 121.8(7) . . ? N101 C107 C108 115.0(6) . . ? C106 C107 C108 123.2(6) . . ? O203 C214 O204 126.2(8) . . ? O203 C214 C213 118.2(7) . . ? O204 C214 C213 115.6(7) . . ? N201 C202 C203 121.8(8) . . ? N201 C202 C201 116.1(7) . . ? C203 C202 C201 122.1(8) . . ? N102 C108 C109 121.9(7) . . ? N102 C108 C107 113.4(6) . . ? C109 C108 C107 124.7(6) . . ? O202 C201 O201 126.9(8) . . ? O202 C201 C202 119.0(8) . . ? O201 C201 C202 114.1(8) . . ? C104 C106 C107 117.7(7) . . ? C104 C106 H106 121.2 . . ? C107 C106 H106 121.2 . . ? C213 C212 C210 117.4(9) . . ? C213 C212 H212 121.3 . . ? C210 C212 H212 121.3 . . ? C209 C210 C212 120.9(7) . . ? C209 C210 C211 119.6(9) . . ? C212 C210 C211 119.5(10) . . ? F103 C105 F101 108.7(8) . . ? F103 C105 F102 104.6(8) . . ? F101 C105 F102 106.3(8) . . ? F103 C105 C104 112.6(7) . . ? F101 C105 C104 112.6(7) . . ? F102 C105 C104 111.6(7) . . ? N202 C213 C212 121.8(8) . . ? N202 C213 C214 115.9(6) . . ? C212 C213 C214 122.4(8) . . ? N101 C102 C103 122.2(7) . . ? N101 C102 C101 115.2(7) . . ? C103 C102 C101 122.6(8) . . ? C106 C104 C103 121.3(7) . . ? C106 C104 C105 120.3(7) . . ? C103 C104 C105 118.3(8) . . ? C101 O101 Tb1 126.2(5) . . ? N102 C113 C112 121.4(7) . . ? N102 C113 C114 115.6(6) . . ? C112 C113 C114 123.0(7) . . ? F201 C205 F203 112.9(12) . . ? F201 C205 F202 105.2(11) . . ? F203 C205 F202 102.5(9) . . ? F201 C205 C204 113.5(9) . . ? F203 C205 C204 111.7(8) . . ? F202 C205 C204 110.3(10) . . ? C204 C203 C202 117.7(9) . . ? C204 C203 H203 121.2 . . ? C202 C203 H203 121.2 . . ? C203 C204 C206 120.7(8) . . ? C203 C204 C205 118.9(10) . . ? C206 C204 C205 120.4(9) . . ? O103 C114 O104 126.5(7) . . ? O103 C114 C113 117.7(7) . . ? O104 C114 C113 115.8(7) . . ? C207 C206 C204 118.5(8) . . ? C207 C206 H206 120.7 . . ? C204 C206 H206 120.7 . . ? C210 C209 C208 119.2(8) . . ? C210 C209 H209 120.4 . . ? C208 C209 H209 120.4 . . ? C110 C112 C113 118.9(7) . . ? C110 C112 H112 120.5 . . ? C113 C112 H112 120.5 . . ? O102 C101 O101 126.2(9) . . ? O102 C101 C102 119.4(9) . . ? O101 C101 C102 114.4(8) . . ? F204 C211 F205 108.2(11) . . ? F204 C211 F206 100.6(10) . . ? F205 C211 F206 107.7(12) . . ? F204 C211 C210 113.1(11) . . ? F205 C211 C210 112.1(8) . . ? F206 C211 C210 114.4(10) . . ? F105 C111 F106 109.0(8) . . ? F105 C111 F104 108.2(8) . . ? F106 C111 F104 105.6(7) . . ? F105 C111 C110 110.7(7) . . ? F106 C111 C110 112.5(7) . . ? F104 C111 C110 110.6(7) . . ? C102 C103 C104 117.5(8) . . ? C102 C103 H103 121.3 . . ? C104 C103 H103 121.3 . . ? C5T N1T C3T 115.9(19) . . ? C5T N1T C1T 109(2) . . ? C3T N1T C1T 107.5(16) . . ? C5T N1T HN1T 108.1 . . ? C3T N1T HN1T 108.1 . . ? C1T N1T HN1T 108.1 . . ? N1T C3T C4T 110.6(19) . . ? N1T C3T H3TB 109.5 . . ? C4T C3T H3TB 109.5 . . ? N1T C3T H3TA 109.5 . . ? C4T C3T H3TA 109.5 . . ? H3TB C3T H3TA 108.1 . . ? C5T C6T H6TA 109.5 . . ? C5T C6T H6TB 109.5 . . ? H6TA C6T H6TB 109.5 . . ? C5T C6T H6TC 109.5 . . ? H6TA C6T H6TC 109.5 . . ? H6TB C6T H6TC 109.5 . . ? C2T C1T N1T 119(2) . . ? C2T C1T H1TA 107.5 . . ? N1T C1T H1TA 107.5 . . ? C2T C1T H1TB 107.5 . . ? N1T C1T H1TB 107.5 . . ? H1TA C1T H1TB 107.0 . . ? C1T C2T H2TB 109.5 . . ? C1T C2T H2TA 109.5 . . ? H2TB C2T H2TA 109.5 . . ? C1T C2T H2TC 109.5 . . ? H2TB C2T H2TC 109.5 . . ? H2TA C2T H2TC 109.5 . . ? N1T C5T C6T 116(3) . . ? N1T C5T H5TB 108.2 . . ? C6T C5T H5TB 108.2 . . ? N1T C5T H5TA 108.2 . . ? C6T C5T H5TA 108.2 . . ? H5TB C5T H5TA 107.4 . . ? C3T C4T H4TA 109.5 . . ? C3T C4T H4TC 109.5 . . ? H4TA C4T H4TC 109.5 . . ? C3T C4T H4TB 109.5 . . ? H4TA C4T H4TB 109.5 . . ? H4TC C4T H4TB 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.367 _refine_diff_density_min -1.847 _refine_diff_density_rms 0.237 _database_code_depnum_ccdc_archive 'CCDC 920407'