Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Neckers, D. C.' 'Gu, Haiyan' 'Kaafarani, Bilal R.' 'Pinkerton, A. Alan' _publ_contact_author_name 'Dr D C Neckers' _publ_contact_author_address ; Center for Photochemical Science Bowling Green State University Bowling Green OHIO 43403 USA ; _publ_contact_author_email ? _publ_section_title ; The Crystal and Molecular Structures of 1-Naphthylphenyliodonium Tetrafluoroborate and 1-Naphthylphenyliodonium Tetrakis(pentafluorophenyl)gallate1 ; data_hg _database_code_CSD 178309 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '1-Naphthylphenyliodonium Tetrafluoroborate' _chemical_melting_point 186 _chemical_formula_moiety ? _chemical_formula_sum 'C16 H12 B F4 I' _chemical_formula_weight 417.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0015 0.0009 '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' 0.0004 0.0004 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0096 0.0061 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.8919 1.1868 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8914(11) _cell_length_b 8.8699(9) _cell_length_c 14.4445(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.944(4) _cell_angle_gamma 90.00 _cell_volume 1523.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 30.24 _exptl_crystal_description cubic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.138 _exptl_absorpt_correction_type 'SADABS (Blessing 1995)' _exptl_absorpt_correction_T_min 1.0 _exptl_absorpt_correction_T_max 0.901078 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.56086 _diffrn_radiation_type AgK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24408 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0736 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 30.24 _reflns_number_total 8286 _reflns_number_gt 4017 _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^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap, geom H(6), H(12), H(14), H(15)' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8286 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I I 0.333971(13) 0.49766(2) 0.179476(11) 0.03111(6) Uani 1 1 d . . . B B 0.3721(3) -0.1574(4) 0.3043(2) 0.0356(7) Uani 1 1 d . . . F1 F 0.27732(15) -0.1931(3) 0.25457(19) 0.0877(9) Uani 1 1 d . . . F2 F 0.46446(17) -0.2081(3) 0.25776(15) 0.0876(9) Uani 1 1 d . . . F3 F 0.3818(4) -0.0091(2) 0.3152(2) 0.0958(13) Uani 1 1 d . . . F4 F 0.3699(2) -0.2186(3) 0.39347(18) 0.0816(8) Uani 1 1 d . . . C1 C 0.1576(2) 0.5223(3) 0.17344(19) 0.0283(5) Uani 1 1 d . . . C2 C 0.0982(3) 0.4507(4) 0.2411(2) 0.0364(6) Uani 1 1 d . . . H2 H 0.129(3) 0.401(4) 0.280(2) 0.038(9) Uiso 1 1 d . . . C3 C -0.0190(3) 0.4635(4) 0.2412(2) 0.0429(7) Uani 1 1 d . . . H3 H -0.061(2) 0.399(3) 0.2921(18) 0.030(7) Uiso 1 1 d . . . C4 C -0.0736(3) 0.5452(4) 0.1753(2) 0.0404(7) Uani 1 1 d . . . H4 H -0.140(3) 0.554(4) 0.1710(19) 0.035(8) Uiso 1 1 d . . . C5 C -0.0136(2) 0.6230(3) 0.10471(19) 0.0311(5) Uani 1 1 d . . . C6 C -0.0701(3) 0.7118(3) 0.0383(2) 0.0402(7) Uani 1 1 d . . . H6 H -0.1479 0.7204 0.0399 0.048 Uiso 1 1 calc R . . C7 C -0.0110(3) 0.7865(4) -0.0292(3) 0.0437(7) Uani 1 1 d . . . H7 H -0.050(3) 0.847(4) -0.075(2) 0.059(10) Uiso 1 1 d . . . C8 C 0.1066(3) 0.7710(4) -0.0318(2) 0.0422(8) Uani 1 1 d . . . H8 H 0.130(3) 0.810(4) -0.061(2) 0.053(13) Uiso 1 1 d . . . C9 C 0.1642(2) 0.6879(3) 0.03103(19) 0.0333(6) Uani 1 1 d . . . H9 H 0.2395(19) 0.676(3) 0.0244(14) 0.008(5) Uiso 1 1 d . . . C10 C 0.1056(2) 0.6114(3) 0.10297(16) 0.0265(5) Uani 1 1 d . . . C11 C 0.3450(2) 0.3117(3) 0.08949(17) 0.0271(5) Uani 1 1 d . . . C12 C 0.3798(2) 0.3389(3) -0.00040(18) 0.0329(6) Uani 1 1 d . . . H12 H 0.3949 0.4361 -0.0208 0.039 Uiso 1 1 calc R . . C13 C 0.3911(3) 0.2163(4) -0.0582(2) 0.0448(8) Uani 1 1 d . . . H13 H 0.414(3) 0.235(4) -0.111(2) 0.052(11) Uiso 1 1 d . . . C14 C 0.3674(3) 0.0731(4) -0.0275(2) 0.0508(9) Uani 1 1 d . . . H14 H 0.3748 -0.0084 -0.0674 0.061 Uiso 1 1 calc R . . C15 C 0.3324(4) 0.0496(4) 0.0626(3) 0.0531(9) Uani 1 1 d . . . H15 H 0.3159 -0.0477 0.0823 0.064 Uiso 1 1 calc R . . C16 C 0.3216(3) 0.1700(3) 0.1238(2) 0.0384(6) Uani 1 1 d . . . H16 H 0.293(2) 0.155(3) 0.189(2) 0.037(8) Uiso 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 I 0.02711(9) 0.03492(11) 0.03111(9) -0.00774(7) -0.00505(6) 0.00360(7) B 0.0315(15) 0.0355(18) 0.0397(17) -0.0066(13) 0.0031(12) -0.0066(13) F1 0.0267(10) 0.120(2) 0.116(2) -0.0767(17) -0.0073(11) 0.0038(12) F2 0.0288(9) 0.165(3) 0.0694(15) -0.0427(15) 0.0076(9) -0.0030(13) F3 0.191(4) 0.0383(14) 0.0568(16) -0.0030(9) -0.020(2) -0.0318(14) F4 0.0677(15) 0.0862(18) 0.0917(18) 0.0510(14) 0.0288(13) 0.0122(13) C1 0.0239(11) 0.0290(15) 0.0321(12) -0.0048(9) 0.0037(9) -0.0001(9) C2 0.0416(17) 0.0349(14) 0.0330(15) 0.0031(12) 0.0088(12) -0.0015(13) C3 0.0407(17) 0.0416(17) 0.0470(18) -0.0005(13) 0.0179(14) -0.0070(13) C4 0.0322(15) 0.0437(17) 0.0455(17) -0.0072(14) 0.0095(13) -0.0024(13) C5 0.0280(12) 0.0261(13) 0.0392(14) -0.0068(10) -0.0021(10) -0.0010(10) C6 0.0320(14) 0.0385(17) 0.0497(17) -0.0106(13) -0.0095(12) 0.0064(13) C7 0.0461(18) 0.0422(19) 0.0426(15) -0.0003(15) -0.0076(13) 0.0061(14) C8 0.0493(19) 0.0384(18) 0.0388(17) 0.0076(14) 0.0007(14) -0.0038(15) C9 0.0312(13) 0.0312(15) 0.0376(14) -0.0005(11) 0.0001(11) -0.0042(11) C10 0.0277(12) 0.0233(12) 0.0285(12) -0.0052(9) 0.0034(9) -0.0012(9) C11 0.0232(11) 0.0284(13) 0.0296(12) -0.0035(10) -0.0017(9) 0.0027(10) C12 0.0289(13) 0.0357(15) 0.0341(13) -0.0014(11) 0.0021(10) -0.0005(11) C13 0.0392(16) 0.058(2) 0.0375(17) -0.0119(15) 0.0021(13) 0.0046(15) C14 0.051(2) 0.043(2) 0.058(2) -0.0231(16) -0.0122(15) 0.0149(16) C15 0.073(3) 0.0256(14) 0.060(2) -0.0010(16) -0.0126(18) 0.0075(17) C16 0.0477(17) 0.0333(16) 0.0340(14) 0.0004(12) -0.0047(12) -0.0007(13) _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 I C11 2.106(2) . ? I C1 2.109(3) . ? B F3 1.330(4) . ? B F1 1.364(4) . ? B F2 1.372(4) . ? B F4 1.398(4) . ? C1 C2 1.371(4) . ? C1 C10 1.422(4) . ? C2 C3 1.398(5) . ? C2 H2 0.80(3) . ? C3 C4 1.354(5) . ? C3 H3 1.06(3) . ? C4 C5 1.432(4) . ? C4 H4 0.80(3) . ? C5 C6 1.403(4) . ? C5 C10 1.422(3) . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.407(5) . ? C7 H7 0.96(3) . ? C8 C9 1.347(4) . ? C8 H8 0.62(3) . ? C9 C10 1.432(4) . ? C9 H9 0.91(2) . ? C11 C16 1.381(4) . ? C11 C12 1.390(4) . ? C12 C13 1.379(4) . ? C12 H12 0.9300 . ? C13 C14 1.375(5) . ? C13 H13 0.83(4) . ? C14 C15 1.389(5) . ? C14 H14 0.9300 . ? C15 C16 1.394(4) . ? C15 H15 0.9300 . ? C16 H16 1.02(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 C11 I C1 97.35(9) . . ? F3 B F1 111.1(3) . . ? F3 B F2 108.2(3) . . ? F1 B F2 109.1(2) . . ? F3 B F4 106.2(3) . . ? F1 B F4 111.5(3) . . ? F2 B F4 110.6(3) . . ? C2 C1 C10 123.1(3) . . ? C2 C1 I 116.4(2) . . ? C10 C1 I 120.49(18) . . ? C1 C2 C3 119.2(3) . . ? C1 C2 H2 121(2) . . ? C3 C2 H2 119(2) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 123.1(15) . . ? C2 C3 H3 116.1(15) . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 125(2) . . ? C5 C4 H4 114(2) . . ? C6 C5 C10 119.6(3) . . ? C6 C5 C4 121.3(3) . . ? C10 C5 C4 119.1(3) . . ? C7 C6 C5 120.6(3) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.3(3) . . ? C6 C7 H7 121(2) . . ? C8 C7 H7 120(2) . . ? C9 C8 C7 122.0(3) . . ? C9 C8 H8 123(4) . . ? C7 C8 H8 115(4) . . ? C8 C9 C10 120.0(3) . . ? C8 C9 H9 118.9(14) . . ? C10 C9 H9 120.9(14) . . ? C1 C10 C5 116.7(2) . . ? C1 C10 C9 124.9(2) . . ? C5 C10 C9 118.4(2) . . ? C16 C11 C12 123.9(2) . . ? C16 C11 I 118.42(19) . . ? C12 C11 I 117.59(19) . . ? C13 C12 C11 117.5(3) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13 123(3) . . ? C12 C13 H13 116(3) . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.8(3) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C11 C16 C15 116.6(3) . . ? C11 C16 H16 121.6(18) . . ? C15 C16 H16 121.6(18) . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 30.24 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 2.004 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.154 data_sad2 _database_code_CSD 178310 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; 1-Naphthylphenyliodonium Tetrakis(pentafluorophenyl)gallate ; _chemical_melting_point 117-118 _chemical_formula_moiety ? _chemical_formula_sum 'C40 H12 F20 Ga I' _chemical_formula_weight 1069.12 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' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.003(5) _cell_length_b 18.287(6) _cell_length_c 14.738(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.436(13) _cell_angle_gamma 90.00 _cell_volume 3651(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.07 _cell_measurement_theta_max 27.73 _exptl_crystal_description cubic _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.945 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type 'SADABS (Blessing 1995)' _exptl_absorpt_correction_T_min 1.0 _exptl_absorpt_correction_T_max 0.694997 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34816 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.07 _diffrn_reflns_theta_max 27.73 _reflns_number_total 8063 _reflns_number_gt 7767 _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^)+(0.0228P)^2^+3.4453P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8063 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0250 _refine_ls_R_factor_gt 0.0237 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.003 _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 I I 0.069807(9) 0.667078(7) 0.804418(9) 0.02426(4) Uani 1 1 d . . . Ga Ga 0.242805(14) 0.319970(11) 0.015960(14) 0.01733(5) Uani 1 1 d . . . F1 F 0.12334(8) 0.33406(6) 0.14168(8) 0.0243(2) Uani 1 1 d . . . C2 C 0.22921(18) 0.63667(13) 0.74147(18) 0.0351(5) Uani 1 1 d . . . H2 H 0.188(2) 0.5975(16) 0.714(2) 0.044(8) Uiso 1 1 d . . . F2 F 0.16552(9) 0.38876(7) 0.32435(9) 0.0303(3) Uani 1 1 d . . . C3 C 0.3186(2) 0.64665(15) 0.7329(2) 0.0437(6) Uani 1 1 d . . . H3 H 0.336(2) 0.6120(16) 0.700(2) 0.046(8) Uiso 1 1 d . . . F3 F 0.34197(11) 0.45575(7) 0.43233(9) 0.0358(3) Uani 1 1 d . . . C4 C 0.37648(18) 0.70562(14) 0.77562(19) 0.0368(5) Uani 1 1 d . . . H4 H 0.436(2) 0.7129(17) 0.770(2) 0.053(8) Uiso 1 1 d . . . F4 F 0.47778(10) 0.46447(7) 0.35563(9) 0.0365(3) Uani 1 1 d . . . C5 C 0.35050(14) 0.75806(11) 0.83117(15) 0.0263(4) Uani 1 1 d . . . F5 F 0.43969(8) 0.40586(7) 0.17665(9) 0.0293(3) Uani 1 1 d . . . C6 C 0.41085(16) 0.81958(12) 0.87565(17) 0.0305(4) Uani 1 1 d . . . H6 H 0.465(2) 0.8241(14) 0.865(2) 0.036(7) Uiso 1 1 d . . . F6 F 0.33256(9) 0.45901(6) -0.02861(9) 0.0309(3) Uani 1 1 d . . . C7 C 0.38611(16) 0.86918(13) 0.92974(16) 0.0319(5) Uani 1 1 d . . . H7 H 0.4264(19) 0.9080(14) 0.9570(19) 0.033(6) Uiso 1 1 d . . . F7 F 0.46027(11) 0.48223(7) -0.10964(10) 0.0399(3) Uani 1 1 d . . . C8 C 0.29827(16) 0.86021(12) 0.94178(16) 0.0301(4) Uani 1 1 d . . . H8 H 0.2790(17) 0.8938(13) 0.9759(18) 0.026(6) Uiso 1 1 d . . . F8 F 0.54315(10) 0.36601(9) -0.16141(10) 0.0417(3) Uani 1 1 d . . . C9 C 0.23758(15) 0.80169(11) 0.89975(15) 0.0250(4) Uani 1 1 d . . . H9 H 0.1775(18) 0.7959(13) 0.9059(18) 0.029(6) Uiso 1 1 d . . . F9 F 0.49752(9) 0.22759(8) -0.13033(10) 0.0362(3) Uani 1 1 d . . . C10 C 0.26134(14) 0.74896(11) 0.84301(14) 0.0219(4) Uani 1 1 d . . . F10 F 0.37233(9) 0.20382(6) -0.04692(9) 0.0262(2) Uani 1 1 d . . . C11 C 0.13310(14) 0.64286(11) 0.95941(14) 0.0225(4) Uani 1 1 d . . . F11 F 0.09227(8) 0.45561(6) -0.00147(8) 0.0248(2) Uani 1 1 d . . . C12 C 0.09317(15) 0.67664(11) 1.01741(16) 0.0260(4) Uani 1 1 d . . . H12 H 0.039(2) 0.7106(15) 0.986(2) 0.040(7) Uiso 1 1 d . . . F12 F -0.04773(9) 0.51924(6) -0.16341(9) 0.0294(3) Uani 1 1 d . . . C1 C 0.20392(15) 0.68699(11) 0.79501(15) 0.0248(4) Uani 1 1 d . . . C13 C 0.13338(16) 0.65844(13) 1.11870(16) 0.0308(4) Uani 1 1 d . . . H13 H 0.1090(19) 0.6811(13) 1.1612(19) 0.031(6) Uiso 1 1 d . . . F13 F -0.09567(9) 0.46394(7) -0.35004(9) 0.0322(3) Uani 1 1 d . . . C14 C 0.21047(16) 0.60900(13) 1.15825(16) 0.0330(5) Uani 1 1 d . . . H14 H 0.2376(19) 0.5993(15) 1.226(2) 0.038(7) Uiso 1 1 d . . . F14 F 0.00158(9) 0.34418(7) -0.37266(8) 0.0307(3) Uani 1 1 d . . . C15 C 0.24934(16) 0.57726(12) 1.09789(17) 0.0333(5) Uani 1 1 d . . . H15 H 0.304(2) 0.5454(15) 1.125(2) 0.038(7) Uiso 1 1 d . . . F15 F 0.14529(9) 0.28151(7) -0.21022(9) 0.0287(2) Uani 1 1 d . . . C16 C 0.21052(16) 0.59366(11) 0.99612(17) 0.0288(4) Uani 1 1 d . . . H16 H 0.2367(18) 0.5712(14) 0.9563(19) 0.032(6) Uiso 1 1 d . . . F16 F 0.04237(8) 0.21796(6) -0.08310(8) 0.0252(2) Uani 1 1 d . . . C17 C 0.27866(13) 0.36840(10) 0.14951(13) 0.0194(3) Uani 1 1 d . . . F17 F 0.01548(9) 0.07751(7) -0.05569(9) 0.0320(3) Uani 1 1 d . . . F18 F 0.16900(10) -0.00595(7) 0.07410(10) 0.0385(3) Uani 1 1 d . . . C18 C 0.21288(13) 0.36636(10) 0.19277(13) 0.0199(3) Uani 1 1 d . . . F19 F 0.34916(10) 0.05568(7) 0.17726(10) 0.0395(3) Uani 1 1 d . . . C19 C 0.23202(15) 0.39479(10) 0.28568(14) 0.0227(4) Uani 1 1 d . . . F20 F 0.37712(8) 0.19917(7) 0.15398(9) 0.0284(2) Uani 1 1 d . . . C20 C 0.32105(16) 0.42900(10) 0.34051(14) 0.0255(4) Uani 1 1 d . . . C21 C 0.38994(15) 0.43268(11) 0.30178(14) 0.0253(4) Uani 1 1 d . . . C22 C 0.36769(14) 0.40191(10) 0.20857(14) 0.0218(4) Uani 1 1 d . . . C23 C 0.34906(14) 0.33058(10) -0.03199(14) 0.0207(4) Uani 1 1 d . . . C24 C 0.37437(14) 0.39989(11) -0.05048(15) 0.0241(4) Uani 1 1 d . . . C25 C 0.43926(15) 0.41356(12) -0.09251(15) 0.0279(4) Uani 1 1 d . . . C26 C 0.48105(15) 0.35518(13) -0.11895(15) 0.0296(4) Uani 1 1 d . . . C27 C 0.45795(14) 0.28460(12) -0.10300(14) 0.0261(4) Uani 1 1 d . . . C28 C 0.39299(13) 0.27432(11) -0.06006(14) 0.0217(4) Uani 1 1 d . . . C29 C 0.12654(13) 0.36667(10) -0.09850(13) 0.0194(3) Uani 1 1 d . . . C30 C 0.07443(13) 0.42705(10) -0.09203(13) 0.0201(4) Uani 1 1 d . . . C31 C 0.00130(14) 0.46084(10) -0.17454(15) 0.0222(4) Uani 1 1 d . . . C32 C -0.02346(14) 0.43311(11) -0.26960(14) 0.0239(4) Uani 1 1 d . . . C33 C 0.02599(14) 0.37225(11) -0.27996(14) 0.0237(4) Uani 1 1 d . . . C34 C 0.09922(14) 0.34135(10) -0.19542(14) 0.0222(4) Uani 1 1 d . . . C35 C 0.21203(13) 0.21485(10) 0.03359(13) 0.0185(3) Uani 1 1 d . . . C36 C 0.12204(14) 0.18034(10) -0.01578(14) 0.0199(4) Uani 1 1 d . . . C37 C 0.10552(14) 0.10730(11) -0.00349(14) 0.0227(4) Uani 1 1 d . . . C38 C 0.18224(16) 0.06535(11) 0.06167(15) 0.0260(4) Uani 1 1 d . . . C39 C 0.27403(15) 0.09713(11) 0.11454(15) 0.0262(4) Uani 1 1 d . . . C40 C 0.28584(14) 0.17033(10) 0.10001(14) 0.0214(4) 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 I 0.02247(7) 0.02861(7) 0.02057(7) 0.00053(5) 0.00817(5) -0.00319(5) Ga 0.01687(10) 0.01818(10) 0.01749(10) -0.00070(7) 0.00789(8) -0.00092(7) F1 0.0191(5) 0.0298(6) 0.0247(6) 0.0002(4) 0.0100(5) -0.0037(4) C2 0.0415(13) 0.0315(11) 0.0383(12) -0.0098(10) 0.0227(10) -0.0046(10) F2 0.0380(7) 0.0349(6) 0.0267(6) 0.0047(5) 0.0222(5) 0.0051(5) C3 0.0524(15) 0.0413(13) 0.0519(15) -0.0111(12) 0.0363(13) 0.0041(11) F3 0.0557(8) 0.0309(6) 0.0188(6) -0.0061(5) 0.0140(6) -0.0053(6) C4 0.0338(12) 0.0442(13) 0.0427(13) 0.0015(10) 0.0263(10) 0.0042(10) F4 0.0335(7) 0.0382(7) 0.0265(6) -0.0056(5) 0.0021(5) -0.0146(6) C5 0.0224(9) 0.0301(10) 0.0258(9) 0.0056(8) 0.0098(8) 0.0044(8) F5 0.0200(5) 0.0386(7) 0.0300(6) -0.0024(5) 0.0115(5) -0.0065(5) C6 0.0199(10) 0.0370(12) 0.0308(10) 0.0083(9) 0.0072(8) 0.0009(8) F6 0.0380(7) 0.0212(6) 0.0370(7) 0.0002(5) 0.0193(6) 0.0001(5) C7 0.0268(10) 0.0315(11) 0.0275(10) 0.0024(9) 0.0022(8) -0.0044(9) F7 0.0499(8) 0.0368(7) 0.0371(7) -0.0006(6) 0.0225(6) -0.0210(6) C8 0.0307(11) 0.0286(10) 0.0257(10) -0.0038(8) 0.0071(8) 0.0023(8) F8 0.0316(7) 0.0657(10) 0.0377(7) -0.0024(7) 0.0244(6) -0.0126(6) C9 0.0238(10) 0.0278(10) 0.0238(9) -0.0001(8) 0.0107(8) 0.0018(8) F9 0.0331(7) 0.0466(8) 0.0361(7) -0.0041(6) 0.0216(6) 0.0083(6) C10 0.0216(9) 0.0242(9) 0.0190(8) 0.0034(7) 0.0080(7) 0.0034(7) F10 0.0286(6) 0.0225(5) 0.0296(6) -0.0031(5) 0.0143(5) -0.0006(5) C11 0.0209(9) 0.0234(9) 0.0212(9) 0.0016(7) 0.0073(7) -0.0036(7) F11 0.0285(6) 0.0256(6) 0.0198(5) -0.0030(4) 0.0098(5) 0.0025(5) C12 0.0225(9) 0.0291(10) 0.0253(10) -0.0020(8) 0.0094(8) -0.0033(8) F12 0.0301(6) 0.0260(6) 0.0311(6) 0.0042(5) 0.0123(5) 0.0088(5) C1 0.0252(10) 0.0278(10) 0.0236(9) 0.0016(8) 0.0126(8) 0.0004(8) C13 0.0301(11) 0.0381(12) 0.0227(10) -0.0063(9) 0.0100(8) -0.0114(9) F13 0.0307(6) 0.0357(7) 0.0225(6) 0.0087(5) 0.0040(5) 0.0039(5) C14 0.0323(11) 0.0364(12) 0.0215(10) 0.0027(9) 0.0032(9) -0.0144(9) F14 0.0350(7) 0.0396(7) 0.0173(5) -0.0038(5) 0.0110(5) -0.0041(5) C15 0.0272(11) 0.0261(10) 0.0363(12) 0.0087(9) 0.0038(9) -0.0022(8) F15 0.0307(6) 0.0287(6) 0.0272(6) -0.0066(5) 0.0130(5) 0.0038(5) C16 0.0281(10) 0.0239(10) 0.0345(11) 0.0012(8) 0.0135(9) -0.0007(8) F16 0.0185(5) 0.0257(6) 0.0270(6) 0.0000(5) 0.0056(4) 0.0000(4) C17 0.0199(8) 0.0189(8) 0.0181(8) 0.0009(7) 0.0069(7) 0.0010(7) F17 0.0273(6) 0.0320(6) 0.0342(6) -0.0038(5) 0.0108(5) -0.0125(5) F18 0.0498(8) 0.0226(6) 0.0383(7) 0.0075(5) 0.0142(6) -0.0076(6) C18 0.0199(8) 0.0192(8) 0.0193(8) 0.0014(7) 0.0074(7) -0.0001(7) F19 0.0391(7) 0.0301(7) 0.0359(7) 0.0112(6) 0.0034(6) 0.0061(6) C19 0.0285(10) 0.0222(9) 0.0205(9) 0.0052(7) 0.0134(8) 0.0051(7) F20 0.0197(5) 0.0312(6) 0.0281(6) 0.0020(5) 0.0044(5) -0.0019(5) C20 0.0381(11) 0.0202(9) 0.0159(8) 0.0009(7) 0.0094(8) 0.0021(8) C21 0.0267(10) 0.0208(9) 0.0203(9) 0.0014(7) 0.0024(8) -0.0040(7) C22 0.0206(9) 0.0216(9) 0.0226(9) 0.0031(7) 0.0089(7) 0.0000(7) C23 0.0187(9) 0.0252(9) 0.0177(8) -0.0007(7) 0.0074(7) -0.0027(7) C24 0.0246(9) 0.0241(9) 0.0241(9) -0.0021(7) 0.0109(8) -0.0022(7) C25 0.0292(10) 0.0314(10) 0.0218(9) -0.0005(8) 0.0098(8) -0.0127(8) C26 0.0208(9) 0.0481(13) 0.0228(9) -0.0021(9) 0.0122(8) -0.0087(9) C27 0.0199(9) 0.0377(11) 0.0215(9) -0.0041(8) 0.0096(7) 0.0013(8) C28 0.0182(9) 0.0259(9) 0.0191(8) -0.0011(7) 0.0062(7) -0.0023(7) C29 0.0185(8) 0.0202(8) 0.0199(8) 0.0012(7) 0.0087(7) -0.0021(7) C30 0.0208(9) 0.0220(9) 0.0183(8) -0.0014(7) 0.0092(7) -0.0039(7) C31 0.0225(9) 0.0191(9) 0.0263(9) 0.0029(7) 0.0118(8) 0.0013(7) C32 0.0214(9) 0.0268(9) 0.0207(9) 0.0074(7) 0.0064(7) -0.0018(7) C33 0.0253(9) 0.0293(10) 0.0177(8) -0.0015(7) 0.0103(7) -0.0057(8) C34 0.0220(9) 0.0226(9) 0.0237(9) -0.0011(7) 0.0113(8) -0.0022(7) C35 0.0211(9) 0.0205(8) 0.0173(8) -0.0006(7) 0.0113(7) 0.0004(7) C36 0.0196(9) 0.0236(9) 0.0179(8) 0.0007(7) 0.0093(7) 0.0020(7) C37 0.0235(9) 0.0257(9) 0.0211(9) -0.0032(7) 0.0115(7) -0.0069(7) C38 0.0370(11) 0.0205(9) 0.0239(9) 0.0017(7) 0.0162(8) -0.0041(8) C39 0.0291(10) 0.0256(10) 0.0216(9) 0.0053(8) 0.0086(8) 0.0035(8) C40 0.0190(9) 0.0249(9) 0.0192(9) -0.0008(7) 0.0071(7) -0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I C1 2.107(2) . ? I C11 2.110(2) . ? Ga C17 2.0095(19) . ? Ga C23 2.0115(19) . ? Ga C35 2.0197(19) . ? Ga C29 2.0223(19) . ? F1 C18 1.361(2) . ? C2 C1 1.368(3) . ? C2 C3 1.412(3) . ? C2 H2 0.92(3) . ? F2 C19 1.349(2) . ? C3 C4 1.358(4) . ? C3 H3 0.90(3) . ? F3 C20 1.343(2) . ? C4 C5 1.420(3) . ? C4 H4 0.93(3) . ? F4 C21 1.344(2) . ? C5 C6 1.416(3) . ? C5 C10 1.431(3) . ? F5 C22 1.353(2) . ? C6 C7 1.360(3) . ? C6 H6 0.89(3) . ? F6 C24 1.357(2) . ? C7 C8 1.413(3) . ? C7 H7 0.91(3) . ? F7 C25 1.345(2) . ? C8 C9 1.369(3) . ? C8 H8 0.91(2) . ? F8 C26 1.341(2) . ? C9 C10 1.418(3) . ? C9 H9 0.95(3) . ? F9 C27 1.344(2) . ? C10 C1 1.415(3) . ? F10 C28 1.359(2) . ? C11 C12 1.382(3) . ? C11 C16 1.383(3) . ? F11 C30 1.349(2) . ? C12 C13 1.389(3) . ? C12 H12 0.97(3) . ? F12 C31 1.346(2) . ? C13 C14 1.384(3) . ? C13 H13 0.95(3) . ? F13 C32 1.339(2) . ? C14 C15 1.383(4) . ? C14 H14 0.92(3) . ? F14 C33 1.354(2) . ? C15 C16 1.389(3) . ? C15 H15 0.94(3) . ? F15 C34 1.361(2) . ? C16 H16 0.93(3) . ? F16 C36 1.367(2) . ? C17 C22 1.385(3) . ? C17 C18 1.386(3) . ? F17 C37 1.349(2) . ? F18 C38 1.343(2) . ? C18 C19 1.375(3) . ? F19 C39 1.343(2) . ? C19 C20 1.379(3) . ? F20 C40 1.360(2) . ? C20 C21 1.380(3) . ? C21 C22 1.386(3) . ? C23 C28 1.378(3) . ? C23 C24 1.383(3) . ? C24 C25 1.383(3) . ? C25 C26 1.376(3) . ? C26 C27 1.383(3) . ? C27 C28 1.384(3) . ? C29 C30 1.380(3) . ? C29 C34 1.385(3) . ? C30 C31 1.385(3) . ? C31 C32 1.382(3) . ? C32 C33 1.382(3) . ? C33 C34 1.379(3) . ? C35 C36 1.381(3) . ? C35 C40 1.384(3) . ? C36 C37 1.385(3) . ? C37 C38 1.373(3) . ? C38 C39 1.385(3) . ? C39 C40 1.379(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 C1 I C11 96.26(8) . . ? C17 Ga C23 112.49(8) . . ? C17 Ga C35 105.86(7) . . ? C23 Ga C35 113.36(7) . . ? C17 Ga C29 113.77(8) . . ? C23 Ga C29 101.30(8) . . ? C35 Ga C29 110.26(7) . . ? C1 C2 C3 118.3(2) . . ? C1 C2 H2 118.9(18) . . ? C3 C2 H2 122.8(18) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 122.5(18) . . ? C2 C3 H3 117.2(18) . . ? C3 C4 C5 121.6(2) . . ? C3 C4 H4 121.1(19) . . ? C5 C4 H4 117.3(19) . . ? C6 C5 C4 121.6(2) . . ? C6 C5 C10 118.76(19) . . ? C4 C5 C10 119.6(2) . . ? C7 C6 C5 121.3(2) . . ? C7 C6 H6 122.6(17) . . ? C5 C6 H6 116.0(17) . . ? C6 C7 C8 120.0(2) . . ? C6 C7 H7 119.0(16) . . ? C8 C7 H7 121.0(16) . . ? C9 C8 C7 120.6(2) . . ? C9 C8 H8 117.8(15) . . ? C7 C8 H8 121.5(15) . . ? C8 C9 C10 120.77(19) . . ? C8 C9 H9 121.2(15) . . ? C10 C9 H9 118.0(15) . . ? C1 C10 C9 125.86(18) . . ? C1 C10 C5 115.61(18) . . ? C9 C10 C5 118.53(18) . . ? C12 C11 C16 124.27(19) . . ? C12 C11 I 117.55(15) . . ? C16 C11 I 118.17(15) . . ? C11 C12 C13 117.0(2) . . ? C11 C12 H12 119.7(16) . . ? C13 C12 H12 123.3(16) . . ? C2 C1 C10 124.54(19) . . ? C2 C1 I 115.53(16) . . ? C10 C1 I 119.93(14) . . ? C14 C13 C12 120.5(2) . . ? C14 C13 H13 119.9(15) . . ? C12 C13 H13 119.6(15) . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 120.2(17) . . ? C13 C14 H14 119.0(17) . . ? C14 C15 C16 120.5(2) . . ? C14 C15 H15 121.1(16) . . ? C16 C15 H15 118.4(16) . . ? C11 C16 C15 117.1(2) . . ? C11 C16 H16 123.5(16) . . ? C15 C16 H16 119.4(16) . . ? C22 C17 C18 114.06(17) . . ? C22 C17 Ga 126.20(14) . . ? C18 C17 Ga 119.64(13) . . ? F1 C18 C19 116.72(16) . . ? F1 C18 C17 119.06(16) . . ? C19 C18 C17 124.22(17) . . ? F2 C19 C18 120.91(18) . . ? F2 C19 C20 119.70(17) . . ? C18 C19 C20 119.38(18) . . ? F3 C20 C19 120.26(19) . . ? F3 C20 C21 120.42(18) . . ? C19 C20 C21 119.26(18) . . ? F4 C21 C20 119.69(18) . . ? F4 C21 C22 121.24(19) . . ? C20 C21 C22 119.05(18) . . ? F5 C22 C17 120.24(17) . . ? F5 C22 C21 115.76(17) . . ? C17 C22 C21 124.00(18) . . ? C28 C23 C24 114.70(17) . . ? C28 C23 Ga 125.94(14) . . ? C24 C23 Ga 118.92(14) . . ? F6 C24 C25 116.66(18) . . ? F6 C24 C23 119.30(17) . . ? C25 C24 C23 124.03(19) . . ? F7 C25 C26 119.94(18) . . ? F7 C25 C24 121.3(2) . . ? C26 C25 C24 118.72(19) . . ? F8 C26 C25 120.6(2) . . ? F8 C26 C27 119.5(2) . . ? C25 C26 C27 119.88(18) . . ? F9 C27 C26 119.87(18) . . ? F9 C27 C28 121.34(19) . . ? C26 C27 C28 118.79(19) . . ? F10 C28 C23 119.85(16) . . ? F10 C28 C27 116.26(17) . . ? C23 C28 C27 123.89(18) . . ? C30 C29 C34 114.40(17) . . ? C30 C29 Ga 126.27(14) . . ? C34 C29 Ga 119.09(14) . . ? F11 C30 C29 120.06(16) . . ? F11 C30 C31 116.22(16) . . ? C29 C30 C31 123.71(17) . . ? F12 C31 C32 119.44(17) . . ? F12 C31 C30 121.01(17) . . ? C32 C31 C30 119.53(18) . . ? F13 C32 C33 120.65(18) . . ? F13 C32 C31 120.39(18) . . ? C33 C32 C31 118.95(17) . . ? F14 C33 C34 121.41(18) . . ? F14 C33 C32 119.42(17) . . ? C34 C33 C32 119.16(17) . . ? F15 C34 C33 116.54(17) . . ? F15 C34 C29 119.22(17) . . ? C33 C34 C29 124.23(18) . . ? C36 C35 C40 114.08(17) . . ? C36 C35 Ga 126.37(14) . . ? C40 C35 Ga 119.54(13) . . ? F16 C36 C35 120.32(16) . . ? F16 C36 C37 115.51(16) . . ? C35 C36 C37 124.16(17) . . ? F17 C37 C38 120.42(17) . . ? F17 C37 C36 120.44(17) . . ? C38 C37 C36 119.14(18) . . ? F18 C38 C37 120.59(18) . . ? F18 C38 C39 119.99(18) . . ? C37 C38 C39 119.41(18) . . ? F19 C39 C40 121.93(18) . . ? F19 C39 C38 119.20(18) . . ? C40 C39 C38 118.86(18) . . ? F20 C40 C39 116.73(17) . . ? F20 C40 C35 118.96(16) . . ? C39 C40 C35 124.30(18) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.73 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.350 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.072 #===END