# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Parkin, Gerard' _publ_contact_author_name 'Parkin, Gerard' _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_section_title ; Structural Characterization of TaMe3Cl2 and Ta(PMe3)2Me3Cl2, a Pair of Five and Seven-Coordinate d0 Tantalum Methyl Compounds ; # Attachment '- (PMe3)2TaMe3Cl2[TAP2S10].cif' data_tap2s10 _database_code_depnum_ccdc_archive 'CCDC 824223' #TrackingRef '- (PMe3)2TaMe3Cl2[TAP2S10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H27 Cl2 P2 Ta' _chemical_formula_weight 449.10 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.613(3) _cell_length_b 9.3349(9) _cell_length_c 13.9838(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.2670(10) _cell_angle_gamma 90.00 _cell_volume 3308.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 32.43 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 7.132 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.1416 _exptl_absorpt_correction_T_max 0.1416 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27366 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 31.51 _reflns_number_total 5509 _reflns_number_gt 4734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0116P)^2^+5.8725P] 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 0.00034(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5509 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0444 _refine_ls_wR_factor_gt 0.0422 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Ta Ta 0.111797(4) 0.702887(10) 0.587067(7) 0.01905(4) Uani 1 1 d . . . P1 P 0.10494(3) 0.95713(7) 0.67203(5) 0.02386(13) Uani 1 1 d . . . P2 P 0.17216(3) 0.52098(7) 0.50348(5) 0.02361(13) Uani 1 1 d . . . Cl1 Cl 0.15587(3) 0.87342(7) 0.49108(5) 0.02980(13) Uani 1 1 d . . . Cl2 Cl 0.18989(3) 0.70921(7) 0.71079(5) 0.02928(13) Uani 1 1 d . . . C1 C 0.10122(12) 0.4918(3) 0.6547(2) 0.0319(6) Uani 1 1 d . . . H1A H 0.0893 0.5062 0.7176 0.048 Uiso 1 1 calc R . . H1B H 0.1349 0.4400 0.6637 0.048 Uiso 1 1 calc R . . H1C H 0.0748 0.4359 0.6127 0.048 Uiso 1 1 calc R . . C2 C 0.02834(11) 0.7172(3) 0.6169(2) 0.0335(6) Uani 1 1 d . . . H2A H 0.0090 0.6313 0.5921 0.050 Uiso 1 1 calc R . . H2B H 0.0115 0.8022 0.5850 0.050 Uiso 1 1 calc R . . H2C H 0.0281 0.7243 0.6868 0.050 Uiso 1 1 calc R . . C3 C 0.06590(11) 0.6608(3) 0.44160(19) 0.0277(5) Uani 1 1 d . . . H3A H 0.0903 0.6483 0.3943 0.042 Uiso 1 1 calc R . . H3B H 0.0424 0.7419 0.4226 0.042 Uiso 1 1 calc R . . H3C H 0.0449 0.5735 0.4442 0.042 Uiso 1 1 calc R . . C11 C 0.08342(14) 0.9507(4) 0.7901(2) 0.0430(8) Uani 1 1 d . . . H11A H 0.0800 1.0485 0.8140 0.065 Uiso 1 1 calc R . . H11B H 0.1095 0.8982 0.8352 0.065 Uiso 1 1 calc R . . H11C H 0.0492 0.9020 0.7850 0.065 Uiso 1 1 calc R . . C12 C 0.05797(12) 1.0774(3) 0.6032(3) 0.0407(7) Uani 1 1 d . . . H12A H 0.0222 1.0388 0.6011 0.061 Uiso 1 1 calc R . . H12B H 0.0663 1.0863 0.5373 0.061 Uiso 1 1 calc R . . H12C H 0.0600 1.1718 0.6341 0.061 Uiso 1 1 calc R . . C13 C 0.16416(12) 1.0651(3) 0.6940(2) 0.0369(7) Uani 1 1 d . . . H13A H 0.1754 1.0911 0.6322 0.055 Uiso 1 1 calc R . . H13B H 0.1922 1.0104 0.7329 0.055 Uiso 1 1 calc R . . H13C H 0.1569 1.1523 0.7289 0.055 Uiso 1 1 calc R . . C21 C 0.13706(12) 0.3609(3) 0.4549(2) 0.0359(7) Uani 1 1 d . . . H21A H 0.1068 0.3889 0.4074 0.054 Uiso 1 1 calc R . . H21B H 0.1246 0.3075 0.5075 0.054 Uiso 1 1 calc R . . H21C H 0.1609 0.3004 0.4236 0.054 Uiso 1 1 calc R . . C22 C 0.22905(11) 0.4455(3) 0.5797(2) 0.0360(6) Uani 1 1 d . . . H22A H 0.2463 0.3752 0.5426 0.054 Uiso 1 1 calc R . . H22B H 0.2175 0.3985 0.6357 0.054 Uiso 1 1 calc R . . H22C H 0.2540 0.5222 0.6018 0.054 Uiso 1 1 calc R . . C23 C 0.20100(11) 0.5853(3) 0.4006(2) 0.0341(6) Uani 1 1 d . . . H23A H 0.2276 0.6585 0.4220 0.051 Uiso 1 1 calc R . . H23B H 0.1733 0.6271 0.3530 0.051 Uiso 1 1 calc R . . H23C H 0.2177 0.5054 0.3711 0.051 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 Ta 0.02051(5) 0.01699(5) 0.01990(5) -0.00077(4) 0.00373(3) -0.00227(4) P1 0.0251(3) 0.0186(3) 0.0270(3) -0.0024(2) 0.0006(3) -0.0007(2) P2 0.0249(3) 0.0235(3) 0.0228(3) -0.0027(2) 0.0049(2) -0.0006(2) Cl1 0.0351(3) 0.0280(3) 0.0270(3) 0.0067(2) 0.0066(3) -0.0058(3) Cl2 0.0333(3) 0.0286(3) 0.0237(3) 0.0002(2) -0.0035(2) 0.0018(3) C1 0.0387(15) 0.0239(13) 0.0358(15) 0.0020(11) 0.0141(12) -0.0061(11) C2 0.0338(14) 0.0231(13) 0.0472(17) -0.0134(12) 0.0182(13) -0.0114(11) C3 0.0288(13) 0.0277(12) 0.0248(13) -0.0054(10) -0.0029(10) -0.0036(10) C11 0.054(2) 0.0413(17) 0.0352(16) -0.0130(13) 0.0110(14) -0.0047(15) C12 0.0346(16) 0.0246(14) 0.059(2) 0.0023(13) -0.0079(14) 0.0022(11) C13 0.0354(15) 0.0263(14) 0.0464(17) -0.0071(12) -0.0037(13) -0.0078(11) C21 0.0427(17) 0.0258(14) 0.0410(16) -0.0130(12) 0.0118(13) -0.0035(12) C22 0.0303(14) 0.0354(15) 0.0419(17) -0.0003(13) 0.0032(12) 0.0098(12) C23 0.0334(15) 0.0436(17) 0.0274(14) -0.0028(12) 0.0118(11) -0.0018(12) _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 Ta C1 2.219(3) . ? Ta C3 2.233(2) . ? Ta C2 2.240(3) . ? Ta Cl2 2.4501(7) . ? Ta Cl1 2.4588(6) . ? Ta P1 2.6711(7) . ? Ta P2 2.6758(7) . ? P1 C13 1.811(3) . ? P1 C11 1.816(3) . ? P1 C12 1.817(3) . ? P2 C23 1.812(3) . ? P2 C22 1.819(3) . ? P2 C21 1.824(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 Ta C3 98.71(11) . . ? C1 Ta C2 78.18(11) . . ? C3 Ta C2 77.81(11) . . ? C1 Ta Cl2 81.82(8) . . ? C3 Ta Cl2 156.48(8) . . ? C2 Ta Cl2 124.82(8) . . ? C1 Ta Cl1 154.34(8) . . ? C3 Ta Cl1 80.77(7) . . ? C2 Ta Cl1 126.05(8) . . ? Cl2 Ta Cl1 88.72(2) . . ? C1 Ta P1 125.41(8) . . ? C3 Ta P1 120.13(7) . . ? C2 Ta P1 74.85(7) . . ? Cl2 Ta P1 76.33(2) . . ? Cl1 Ta P1 74.47(2) . . ? C1 Ta P2 74.71(8) . . ? C3 Ta P2 75.63(7) . . ? C2 Ta P2 138.24(7) . . ? Cl2 Ta P2 81.92(2) . . ? Cl1 Ta P2 80.38(2) . . ? P1 Ta P2 146.85(2) . . ? C13 P1 C11 102.71(15) . . ? C13 P1 C12 102.76(14) . . ? C11 P1 C12 103.74(17) . . ? C13 P1 Ta 117.61(10) . . ? C11 P1 Ta 115.05(11) . . ? C12 P1 Ta 113.21(11) . . ? C23 P2 C22 102.11(14) . . ? C23 P2 C21 102.19(14) . . ? C22 P2 C21 102.21(14) . . ? C23 P2 Ta 117.62(10) . . ? C22 P2 Ta 117.03(10) . . ? C21 P2 Ta 113.44(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.972 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.113 # Attachment '- TaMe3Cl2[tame3s10].cif' data_tame3s10 _database_code_depnum_ccdc_archive 'CCDC 828373' #TrackingRef '- TaMe3Cl2[tame3s10].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C3 H9 Cl2 Ta' _chemical_formula_weight 296.95 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mmc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.431(2) _cell_length_b 7.431(2) _cell_length_c 8.058(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 385.36(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4941 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 32.17 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 268 _exptl_absorpt_coefficient_mu 14.841 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0949 _exptl_absorpt_correction_T_max 0.1553 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 5998 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0104 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 31.43 _reflns_number_total 273 _reflns_number_gt 247 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 273 _refine_ls_number_parameters 10 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0141 _refine_ls_R_factor_gt 0.0128 _refine_ls_wR_factor_ref 0.0333 _refine_ls_wR_factor_gt 0.0325 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _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 Ta Ta 0.6667 0.3333 0.2500 0.02235(9) Uani 1 12 d S . . Cl Cl 0.6667 0.3333 -0.03695(18) 0.0503(4) Uani 1 6 d S . . C C 0.8312(4) 0.1688(4) 0.2500 0.0444(11) Uani 1 4 d S . . H0A H 0.9809 0.2678 0.2500 0.067 Uiso 0.50 2 calc SPR . . H0B H 0.7944 0.0813 0.1507 0.067 Uiso 0.25 1 calc PR . . H0C H 0.7944 0.0813 0.3493 0.067 Uiso 0.25 1 calc PR . . 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 Ta 0.02099(10) 0.02099(10) 0.02507(13) 0.000 0.000 0.01050(5) Cl 0.0624(6) 0.0624(6) 0.0261(6) 0.000 0.000 0.0312(3) C 0.041(2) 0.041(2) 0.063(3) 0.000 0.000 0.030(2) _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 Ta C 2.117(5) . ? Ta C 2.117(5) 3_665 ? Ta C 2.117(5) 2_655 ? Ta Cl 2.3121(16) 16_556 ? Ta Cl 2.3121(16) . ? 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 C Ta C 120.0 . 3_665 ? C Ta C 120.0 . 2_655 ? C Ta C 120.0 3_665 2_655 ? C Ta Cl 90.0 . 16_556 ? C Ta Cl 90.0 3_665 16_556 ? C Ta Cl 90.0 2_655 16_556 ? C Ta Cl 90.0 . . ? C Ta Cl 90.0 3_665 . ? C Ta Cl 90.0 2_655 . ? Cl Ta Cl 180.0 16_556 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 31.43 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.141 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.124