#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_contact_author ; Dr. Charles G. Riordan Department of Chemistry and Biochemistry University of Delaware, Newark, DE 19716 USA ; _publ_contact_author_phone '+302 831 1073' _publ_contact_author_fax '+302 831 6335' _publ_contact_author_email riordan@udel.edu _publ_requested_journal 'J. Chem. Soc. Dalton' # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, characterization and reactivity of copper(I) imidazole complexes based on a cavitand ligand design ; loop_ _publ_author_name _publ_author_address 'Voo, J.K.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 U. S. A. ; 'Lam, K.C.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 U. S. A. ; 'Rheingold, A.L.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 U. S. A. ; 'Riordan, Charles G.' ; University of Delaware Department of Chemistry and Biochemistry Newark, DE 19716 U. S. A. ; # 3. Results data_cgr73 _database_code_CSD 163539 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H37 B Cl Cu F4 N6 S3' _chemical_formula_weight 733.61 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' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' _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 8.4150(2) _cell_length_b 12.8962(2) _cell_length_c 15.3722(2) _cell_angle_alpha 90.4394(6) _cell_angle_beta 99.6345(5) _cell_angle_gamma 93.8131(4) _cell_volume 1640.75(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Plate _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7555 _exptl_absorpt_correction_T_max 0.9075 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9720 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5705 _reflns_number_gt 5404 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5705 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 1.793 _refine_ls_restrained_S_all 1.793 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 Cu1 Cu 0.91008(5) 0.17156(3) 0.22322(3) 0.0281(2) Uani 1 1 d . . . S1 S 0.68949(11) -0.07246(7) 0.12322(6) 0.0301(3) Uani 1 1 d . . . S2 S 0.66457(11) 0.39928(7) 0.15669(6) 0.0277(3) Uani 1 1 d . . . S3 S 0.99435(10) 0.15281(7) 0.46711(6) 0.0272(3) Uani 1 1 d . . . N1 N 0.9490(4) -0.1511(2) 0.2275(2) 0.0352(7) Uani 1 1 d . . . N2 N 0.9559(4) 0.0213(2) 0.23237(19) 0.0268(6) Uani 1 1 d . . . N3 N 0.6683(3) 0.3076(2) -0.00410(19) 0.0247(6) Uani 1 1 d . . . N4 N 0.8087(3) 0.2263(2) 0.10704(19) 0.0245(6) Uani 1 1 d . . . N5 N 1.0954(4) 0.3562(2) 0.4465(2) 0.0319(7) Uani 1 1 d . . . N6 N 1.0108(3) 0.2717(2) 0.3190(2) 0.0283(7) Uani 1 1 d . . . C1 C 0.5599(4) 0.0464(2) 0.2441(2) 0.0203(6) Uani 1 1 d . . . C2 C 0.5078(4) 0.1385(3) 0.2016(2) 0.0206(7) Uani 1 1 d . . . C3 C 0.5393(4) 0.2338(2) 0.2472(2) 0.0208(6) Uani 1 1 d . . . C4 C 0.6238(4) 0.2392(2) 0.3351(2) 0.0201(6) Uani 1 1 d . . . C5 C 0.6756(4) 0.1474(3) 0.3764(2) 0.0200(6) Uani 1 1 d . . . C6 C 0.6440(4) 0.0509(2) 0.3314(2) 0.0204(6) Uani 1 1 d . . . C7 C 0.5347(4) -0.0551(3) 0.1941(2) 0.0272(7) Uani 1 1 d . . . H7A H 0.4265 -0.0593 0.1567 0.033 Uiso 1 1 calc R . . H7B H 0.5370 -0.1126 0.2365 0.033 Uiso 1 1 calc R . . C8 C 0.8714(4) -0.0651(3) 0.1987(2) 0.0283(8) Uani 1 1 d . . . C9 C 1.0903(5) -0.1169(4) 0.2834(3) 0.0406(10) Uani 1 1 d . . . H9A H 1.1695 -0.1588 0.3138 0.049 Uiso 1 1 calc R . . C10 C 1.0928(4) -0.0113(3) 0.2859(2) 0.0320(8) Uani 1 1 d . . . H10A H 1.1755 0.0334 0.3193 0.038 Uiso 1 1 calc R . . C11 C 0.8927(7) -0.2601(3) 0.2086(4) 0.0539(13) Uani 1 1 d . . . H11A H 0.7892 -0.2638 0.1681 0.081 Uiso 1 1 calc R . . H11B H 0.8788 -0.2945 0.2637 0.081 Uiso 1 1 calc R . . H11C H 0.9725 -0.2950 0.1813 0.081 Uiso 1 1 calc R . . C12 C 0.4190(4) 0.1326(3) 0.1063(2) 0.0249(7) Uani 1 1 d . . . H12A H 0.4594 0.0755 0.0745 0.030 Uiso 1 1 calc R . . H12B H 0.4428 0.1984 0.0767 0.030 Uiso 1 1 calc R . . C13 C 0.2361(5) 0.1140(4) 0.1009(3) 0.0406(10) Uani 1 1 d . . . H13A H 0.1841 0.1104 0.0388 0.061 Uiso 1 1 calc R . . H13B H 0.1953 0.1714 0.1309 0.061 Uiso 1 1 calc R . . H13C H 0.2120 0.0485 0.1294 0.061 Uiso 1 1 calc R . . C14 C 0.4926(4) 0.3327(3) 0.2003(2) 0.0260(7) Uani 1 1 d . . . H14A H 0.4540 0.3803 0.2419 0.031 Uiso 1 1 calc R . . H14B H 0.4026 0.3160 0.1509 0.031 Uiso 1 1 calc R . . C15 C 0.7157(4) 0.3061(3) 0.0853(2) 0.0234(7) Uani 1 1 d . . . C16 C 0.7358(4) 0.2276(3) -0.0408(2) 0.0280(8) Uani 1 1 d . . . H16A H 0.7258 0.2106 -0.1018 0.034 Uiso 1 1 calc R . . C17 C 0.8199(4) 0.1774(3) 0.0276(2) 0.0288(8) Uani 1 1 d . . . H17A H 0.8779 0.1176 0.0220 0.035 Uiso 1 1 calc R . . C18 C 0.5566(5) 0.3784(3) -0.0537(2) 0.0343(8) Uani 1 1 d . . . H18A H 0.5252 0.4288 -0.0127 0.051 Uiso 1 1 calc R . . H18B H 0.4601 0.3381 -0.0839 0.051 Uiso 1 1 calc R . . H18C H 0.6105 0.4154 -0.0973 0.051 Uiso 1 1 calc R . . C19 C 0.6557(4) 0.3425(3) 0.3835(2) 0.0252(7) Uani 1 1 d . . . H19A H 0.6693 0.3981 0.3407 0.030 Uiso 1 1 calc R . . H19B H 0.7574 0.3420 0.4264 0.030 Uiso 1 1 calc R . . C20 C 0.5171(5) 0.3661(3) 0.4324(3) 0.0403(10) Uani 1 1 d . . . H20A H 0.5418 0.4335 0.4633 0.060 Uiso 1 1 calc R . . H20B H 0.5043 0.3116 0.4754 0.060 Uiso 1 1 calc R . . H20C H 0.4166 0.3681 0.3899 0.060 Uiso 1 1 calc R . . C21 C 0.7736(4) 0.1527(3) 0.4683(2) 0.0238(7) Uani 1 1 d . . . H21A H 0.7398 0.0924 0.5020 0.029 Uiso 1 1 calc R . . H21B H 0.7513 0.2167 0.4989 0.029 Uiso 1 1 calc R . . C22 C 1.0335(4) 0.2638(3) 0.4071(2) 0.0259(7) Uani 1 1 d . . . C23 C 1.1165(5) 0.4238(3) 0.3806(3) 0.0381(9) Uani 1 1 d . . . H23A H 1.1608 0.4936 0.3879 0.046 Uiso 1 1 calc R . . C24 C 1.0622(4) 0.3725(3) 0.3026(3) 0.0357(9) Uani 1 1 d . . . H24A H 1.0599 0.4014 0.2458 0.043 Uiso 1 1 calc R . . C25 C 1.1431(6) 0.3772(4) 0.5411(3) 0.0461(11) Uani 1 1 d . . . H25A H 1.1148 0.3157 0.5738 0.069 Uiso 1 1 calc R . . H25B H 1.0864 0.4361 0.5583 0.069 Uiso 1 1 calc R . . H25C H 1.2599 0.3941 0.5546 0.069 Uiso 1 1 calc R . . C26 C 0.7060(4) -0.0478(3) 0.3763(2) 0.0252(7) Uani 1 1 d . . . H26A H 0.7284 -0.0965 0.3305 0.030 Uiso 1 1 calc R . . H26B H 0.8093 -0.0292 0.4161 0.030 Uiso 1 1 calc R . . C27 C 0.5888(5) -0.1035(3) 0.4297(3) 0.0333(8) Uani 1 1 d . . . H27A H 0.6365 -0.1655 0.4562 0.050 Uiso 1 1 calc R . . H27B H 0.4869 -0.1239 0.3906 0.050 Uiso 1 1 calc R . . H27C H 0.5681 -0.0566 0.4764 0.050 Uiso 1 1 calc R . . B1 B 0.3542(6) -0.3615(3) 0.2909(3) 0.0318(9) Uani 1 1 d . . . F1 F 0.4826(7) -0.4140(5) 0.3222(3) 0.138(2) Uani 1 1 d . . . F2 F 0.2584(6) -0.4254(4) 0.2320(3) 0.1149(19) Uani 1 1 d . . . F3 F 0.2752(4) -0.3379(2) 0.36206(17) 0.0528(7) Uani 1 1 d . . . F4 F 0.3869(7) -0.2731(2) 0.2495(3) 0.1047(16) 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 Cu1 0.0229(3) 0.0362(3) 0.0261(3) 0.0093(2) 0.00466(19) 0.0057(2) S1 0.0346(5) 0.0362(5) 0.0202(5) -0.0027(4) 0.0041(4) 0.0079(4) S2 0.0357(5) 0.0256(4) 0.0233(5) 0.0050(3) 0.0081(4) 0.0052(4) S3 0.0201(5) 0.0332(5) 0.0269(5) 0.0098(4) -0.0014(3) 0.0043(3) N1 0.0402(19) 0.0350(17) 0.0339(17) 0.0025(13) 0.0107(14) 0.0172(14) N2 0.0264(15) 0.0350(16) 0.0210(14) 0.0086(12) 0.0072(11) 0.0085(12) N3 0.0249(15) 0.0280(14) 0.0212(14) 0.0047(11) 0.0035(11) 0.0024(12) N4 0.0244(14) 0.0259(14) 0.0245(14) 0.0057(11) 0.0075(11) 0.0032(11) N5 0.0214(15) 0.0315(16) 0.0420(18) -0.0030(13) 0.0034(13) 0.0010(12) N6 0.0213(15) 0.0302(15) 0.0331(16) 0.0100(13) 0.0035(12) 0.0003(12) C1 0.0154(15) 0.0257(16) 0.0200(15) 0.0026(12) 0.0033(12) 0.0020(12) C2 0.0129(15) 0.0336(17) 0.0159(15) 0.0050(12) 0.0045(12) 0.0007(12) C3 0.0171(15) 0.0266(16) 0.0196(15) 0.0029(13) 0.0039(12) 0.0063(12) C4 0.0178(15) 0.0223(15) 0.0218(16) 0.0000(12) 0.0064(12) 0.0054(12) C5 0.0166(15) 0.0285(16) 0.0157(15) 0.0023(12) 0.0040(12) 0.0039(12) C6 0.0167(15) 0.0260(16) 0.0198(15) 0.0048(12) 0.0059(12) 0.0026(12) C7 0.0265(18) 0.0316(17) 0.0233(17) 0.0004(14) 0.0046(14) -0.0018(14) C8 0.0323(19) 0.0304(17) 0.0267(17) 0.0012(14) 0.0152(15) 0.0106(15) C9 0.039(2) 0.053(2) 0.031(2) 0.0107(18) 0.0018(17) 0.0208(19) C10 0.0263(19) 0.042(2) 0.0290(18) 0.0070(16) 0.0054(15) 0.0089(16) C11 0.071(3) 0.031(2) 0.059(3) 0.002(2) -0.001(2) 0.025(2) C12 0.0162(16) 0.0377(18) 0.0208(16) -0.0001(14) 0.0026(12) 0.0039(13) C13 0.023(2) 0.074(3) 0.0256(19) 0.0021(19) 0.0058(15) 0.0018(19) C14 0.0269(18) 0.0321(17) 0.0206(16) 0.0084(14) 0.0035(13) 0.0151(14) C15 0.0199(16) 0.0281(16) 0.0234(16) 0.0071(13) 0.0058(13) 0.0042(13) C16 0.0296(19) 0.0266(16) 0.0280(18) -0.0007(14) 0.0088(14) -0.0056(14) C17 0.0276(18) 0.0264(17) 0.0325(19) 0.0003(14) 0.0058(15) 0.0015(14) C18 0.040(2) 0.0390(19) 0.0229(17) 0.0098(15) -0.0039(15) 0.0140(17) C19 0.0247(18) 0.0247(16) 0.0260(17) -0.0020(13) 0.0029(14) 0.0028(13) C20 0.047(2) 0.044(2) 0.035(2) -0.0107(17) 0.0192(18) 0.0119(19) C21 0.0230(17) 0.0328(17) 0.0164(15) 0.0035(13) 0.0052(13) 0.0022(14) C22 0.0181(17) 0.0312(17) 0.0281(17) 0.0060(14) 0.0011(13) 0.0067(13) C23 0.028(2) 0.0308(18) 0.056(3) 0.0032(17) 0.0086(18) 0.0019(16) C24 0.0232(19) 0.0349(19) 0.050(2) 0.0157(17) 0.0082(16) 0.0054(15) C25 0.042(2) 0.047(2) 0.047(3) -0.014(2) 0.008(2) -0.006(2) C26 0.0290(18) 0.0239(16) 0.0237(16) 0.0045(13) 0.0072(14) 0.0028(14) C27 0.041(2) 0.0280(17) 0.034(2) 0.0062(15) 0.0143(17) 0.0024(15) B1 0.046(3) 0.0220(18) 0.027(2) 0.0102(15) 0.0037(18) 0.0084(17) F1 0.129(4) 0.207(6) 0.095(3) 0.044(4) 0.022(3) 0.116(4) F2 0.144(4) 0.132(4) 0.067(2) -0.052(2) 0.051(2) -0.081(3) F3 0.081(2) 0.0464(14) 0.0358(13) 0.0000(11) 0.0240(13) 0.0041(13) F4 0.224(5) 0.0332(15) 0.075(2) 0.0074(14) 0.085(3) -0.010(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 Cu1 N6 1.990(3) . ? Cu1 N4 2.001(3) . ? Cu1 N2 2.003(3) . ? S1 C8 1.756(4) . ? S1 C7 1.856(4) . ? S2 C15 1.744(3) . ? S2 C14 1.857(4) . ? S3 C22 1.751(4) . ? S3 C21 1.860(3) . ? N1 C8 1.364(5) . ? N1 C9 1.390(6) . ? N1 C11 1.464(5) . ? N2 C8 1.333(5) . ? N2 C10 1.391(5) . ? N3 C15 1.366(4) . ? N3 C16 1.372(5) . ? N3 C18 1.477(4) . ? N4 C15 1.344(4) . ? N4 C17 1.389(5) . ? N5 C22 1.362(5) . ? N5 C23 1.368(5) . ? N5 C25 1.460(5) . ? N6 C22 1.342(5) . ? N6 C24 1.381(5) . ? C1 C6 1.407(4) . ? C1 C2 1.421(5) . ? C1 C7 1.497(4) . ? C2 C3 1.397(5) . ? C2 C12 1.528(4) . ? C3 C4 1.417(4) . ? C3 C14 1.512(4) . ? C4 C5 1.408(5) . ? C4 C19 1.506(4) . ? C5 C6 1.407(4) . ? C5 C21 1.511(4) . ? C6 C26 1.533(4) . ? C9 C10 1.360(6) . ? C12 C13 1.530(5) . ? C16 C17 1.359(5) . ? C19 C20 1.535(5) . ? C23 C24 1.359(6) . ? C26 C27 1.532(5) . ? B1 F1 1.336(6) . ? B1 F2 1.343(6) . ? B1 F4 1.345(5) . ? B1 F3 1.412(5) . ? 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 N6 Cu1 N4 119.06(12) . . ? N6 Cu1 N2 119.90(12) . . ? N4 Cu1 N2 119.42(12) . . ? C8 S1 C7 103.37(16) . . ? C15 S2 C14 103.08(16) . . ? C22 S3 C21 103.14(15) . . ? C8 N1 C9 107.2(3) . . ? C8 N1 C11 127.6(3) . . ? C9 N1 C11 125.2(3) . . ? C8 N2 C10 105.9(3) . . ? C8 N2 Cu1 132.2(2) . . ? C10 N2 Cu1 121.8(3) . . ? C15 N3 C16 108.0(3) . . ? C15 N3 C18 126.8(3) . . ? C16 N3 C18 125.1(3) . . ? C15 N4 C17 105.6(3) . . ? C15 N4 Cu1 132.6(2) . . ? C17 N4 Cu1 121.8(2) . . ? C22 N5 C23 107.1(3) . . ? C22 N5 C25 126.7(3) . . ? C23 N5 C25 126.0(3) . . ? C22 N6 C24 105.9(3) . . ? C22 N6 Cu1 131.3(2) . . ? C24 N6 Cu1 122.6(3) . . ? C6 C1 C2 120.3(3) . . ? C6 C1 C7 119.7(3) . . ? C2 C1 C7 119.9(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C12 120.7(3) . . ? C1 C2 C12 119.7(3) . . ? C2 C3 C4 120.5(3) . . ? C2 C3 C14 119.6(3) . . ? C4 C3 C14 119.7(3) . . ? C5 C4 C3 119.3(3) . . ? C5 C4 C19 120.9(3) . . ? C3 C4 C19 119.8(3) . . ? C6 C5 C4 120.8(3) . . ? C6 C5 C21 119.3(3) . . ? C4 C5 C21 119.9(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C26 120.1(3) . . ? C1 C6 C26 120.4(3) . . ? C1 C7 S1 112.9(2) . . ? N2 C8 N1 110.8(3) . . ? N2 C8 S1 126.6(3) . . ? N1 C8 S1 122.5(3) . . ? C10 C9 N1 106.3(3) . . ? C9 C10 N2 109.7(4) . . ? C2 C12 C13 112.1(3) . . ? C3 C14 S2 112.0(2) . . ? N4 C15 N3 110.0(3) . . ? N4 C15 S2 127.1(3) . . ? N3 C15 S2 122.8(3) . . ? C17 C16 N3 106.3(3) . . ? C16 C17 N4 110.1(3) . . ? C4 C19 C20 111.6(3) . . ? C5 C21 S3 112.2(2) . . ? N6 C22 N5 110.4(3) . . ? N6 C22 S3 126.8(3) . . ? N5 C22 S3 122.8(3) . . ? C24 C23 N5 107.2(3) . . ? C23 C24 N6 109.3(4) . . ? C27 C26 C6 114.2(3) . . ? F1 B1 F2 106.2(5) . . ? F1 B1 F4 115.2(5) . . ? F2 B1 F4 107.7(4) . . ? F1 B1 F3 108.2(4) . . ? F2 B1 F3 110.6(4) . . ? F4 B1 F3 108.9(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.079 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.083 #===END data_cgr75 _database_code_CSD 163540 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H33 B Cu F4 N5 S2' _chemical_formula_weight 606.02 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' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.6841(2) _cell_length_b 8.2017(2) _cell_length_c 19.1047(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.8733(3) _cell_angle_gamma 90.00 _cell_volume 2875.07(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7630 _exptl_absorpt_correction_T_max 0.7966 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11762 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5495 _reflns_number_gt 4769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5495 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1843 _refine_ls_wR_factor_gt 0.1686 _refine_ls_goodness_of_fit_ref 1.458 _refine_ls_restrained_S_all 1.458 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.002 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 Cu1 Cu 0.53390(2) 0.37977(5) 0.18975(2) 0.03095(18) Uani 1 1 d . . . S1 S 0.70647(4) 0.20245(12) 0.26863(5) 0.0312(2) Uani 1 1 d . . . S2 S 0.41770(5) 0.14222(12) 0.04614(4) 0.0350(2) Uani 1 1 d . . . N1 N 0.72041(15) 0.2049(3) 0.12684(16) 0.0298(6) Uani 1 1 d . . . N2 N 0.61708(15) 0.3182(4) 0.14674(15) 0.0282(6) Uani 1 1 d . . . N3 N 0.31890(17) 0.3747(4) 0.07221(18) 0.0387(8) Uani 1 1 d . . . N4 N 0.42968(15) 0.4052(4) 0.13813(16) 0.0310(7) Uani 1 1 d . . . N5 N 0.53016(17) 0.4888(4) 0.28188(16) 0.0373(7) Uani 1 1 d . . . C1 C 0.57590(16) 0.0231(4) 0.26422(16) 0.0215(6) Uani 1 1 d . . . C2 C 0.53432(16) -0.0137(4) 0.19670(15) 0.0227(7) Uani 1 1 d . . . C3 C 0.45716(17) 0.0048(4) 0.18390(15) 0.0220(6) Uani 1 1 d . . . C4 C 0.42237(16) 0.0598(4) 0.23898(17) 0.0236(6) Uani 1 1 d . . . C5 C 0.46557(16) 0.0932(4) 0.30641(16) 0.0245(7) Uani 1 1 d . . . H5A H 0.4421 0.1275 0.3439 0.029 Uiso 1 1 calc R . . C6 C 0.54089(17) 0.0780(4) 0.32024(16) 0.0233(6) Uani 1 1 d . . . C7 C 0.65792(16) 0.0082(4) 0.27858(17) 0.0265(7) Uani 1 1 d . . . H7A H 0.6720 -0.0734 0.2455 0.032 Uiso 1 1 calc R . . H7B H 0.6743 -0.0331 0.3277 0.032 Uiso 1 1 calc R . . C8 C 0.67959(16) 0.2443(4) 0.17736(17) 0.0258(7) Uani 1 1 d . . . C9 C 0.6820(2) 0.2565(5) 0.06204(19) 0.0372(8) Uani 1 1 d . . . H9A H 0.6966 0.2462 0.0172 0.045 Uiso 1 1 calc R . . C10 C 0.6185(2) 0.3261(5) 0.0745(2) 0.0354(8) Uani 1 1 d . . . H10A H 0.5815 0.3722 0.0391 0.042 Uiso 1 1 calc R . . C11 C 0.7902(2) 0.1167(5) 0.1383(2) 0.0419(10) Uani 1 1 d . . . H11A H 0.8061 0.0944 0.1893 0.063 Uiso 1 1 calc R . . H11B H 0.8270 0.1834 0.1213 0.063 Uiso 1 1 calc R . . H11C H 0.7841 0.0135 0.1119 0.063 Uiso 1 1 calc R . . C12 C 0.57116(18) -0.0766(4) 0.13670(16) 0.0259(7) Uani 1 1 d . . . H12A H 0.6209 -0.0307 0.1428 0.031 Uiso 1 1 calc R . . H12B H 0.5434 -0.0383 0.0903 0.031 Uiso 1 1 calc R . . C13 C 0.5758(2) -0.2646(4) 0.13581(18) 0.0328(8) Uani 1 1 d . . . H13A H 0.5998 -0.2994 0.0969 0.049 Uiso 1 1 calc R . . H13B H 0.5265 -0.3106 0.1286 0.049 Uiso 1 1 calc R . . H13C H 0.6040 -0.3031 0.1813 0.049 Uiso 1 1 calc R . . C14 C 0.41200(19) -0.0258(5) 0.11025(17) 0.0317(8) Uani 1 1 d . . . H14A H 0.3604 -0.0408 0.1145 0.038 Uiso 1 1 calc R . . H14B H 0.4287 -0.1282 0.0911 0.038 Uiso 1 1 calc R . . C15 C 0.38788(18) 0.3120(4) 0.08858(18) 0.0299(7) Uani 1 1 d . . . C16 C 0.3167(2) 0.5111(5) 0.1131(2) 0.0409(9) Uani 1 1 d . . . H16A H 0.2758 0.5800 0.1131 0.049 Uiso 1 1 calc R . . C17 C 0.3847(2) 0.5291(5) 0.1539(2) 0.0390(9) Uani 1 1 d . . . H17A H 0.3989 0.6134 0.1877 0.047 Uiso 1 1 calc R . . C18 C 0.2573(2) 0.3099(7) 0.0202(3) 0.0644(14) Uani 1 1 d . . . H18A H 0.2728 0.2119 -0.0023 0.097 Uiso 1 1 calc R . . H18B H 0.2407 0.3924 -0.0164 0.097 Uiso 1 1 calc R . . H18C H 0.2172 0.2821 0.0446 0.097 Uiso 1 1 calc R . . C19 C 0.34001(19) 0.0817(5) 0.2309(2) 0.0338(8) Uani 1 1 d . . . H19A H 0.3195 0.1122 0.1810 0.041 Uiso 1 1 calc R . . H19B H 0.3300 0.1721 0.2620 0.041 Uiso 1 1 calc R . . C20 C 0.3020(2) -0.0728(6) 0.2501(3) 0.0516(11) Uani 1 1 d . . . H20A H 0.2494 -0.0529 0.2441 0.077 Uiso 1 1 calc R . . H20B H 0.3213 -0.1022 0.2998 0.077 Uiso 1 1 calc R . . H20C H 0.3108 -0.1622 0.2188 0.077 Uiso 1 1 calc R . . C21 C 0.58601(19) 0.1206(5) 0.39360(18) 0.0318(8) Uani 1 1 d . . . H21A H 0.6135 0.0222 0.4131 0.038 Uiso 1 1 calc R . . H21B H 0.6221 0.2049 0.3871 0.038 Uiso 1 1 calc R . . C22 C 0.5432(2) 0.1823(6) 0.44860(19) 0.0422(10) Uani 1 1 d . . . H22A H 0.5768 0.2055 0.4934 0.063 Uiso 1 1 calc R . . H22B H 0.5081 0.0989 0.4569 0.063 Uiso 1 1 calc R . . H22C H 0.5170 0.2821 0.4310 0.063 Uiso 1 1 calc R . . C23 C 0.51311(19) 0.5612(5) 0.32708(19) 0.0328(8) Uani 1 1 d . . . C24 C 0.4897(2) 0.6562(6) 0.3837(2) 0.0471(10) Uani 1 1 d . . . H24A H 0.4762 0.7665 0.3663 0.071 Uiso 1 1 calc R . . H24B H 0.5297 0.6624 0.4250 0.071 Uiso 1 1 calc R . . H24C H 0.4475 0.6033 0.3977 0.071 Uiso 1 1 calc R . . F1 F 0.3585(2) 0.3480(7) 0.3859(2) 0.128(2) Uani 1 1 d . . . F2 F 0.37481(19) 0.4609(5) 0.4910(2) 0.0989(12) Uani 1 1 d . . . F3 F 0.3431(2) 0.2030(5) 0.4850(3) 0.1210(17) Uani 1 1 d . . . F4 F 0.26180(14) 0.3912(4) 0.43791(16) 0.0617(8) Uani 1 1 d . . . B1 B 0.3346(2) 0.3486(6) 0.4481(3) 0.0422(11) 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 Cu1 0.0243(3) 0.0265(3) 0.0436(3) 0.00077(17) 0.01050(19) 0.00237(16) S1 0.0223(4) 0.0344(5) 0.0366(5) -0.0031(4) 0.0047(3) -0.0074(3) S2 0.0469(6) 0.0336(5) 0.0235(4) 0.0004(3) 0.0044(4) 0.0030(4) N1 0.0278(14) 0.0202(15) 0.0442(16) -0.0004(12) 0.0138(12) 0.0009(12) N2 0.0247(14) 0.0229(15) 0.0385(15) -0.0034(12) 0.0095(12) -0.0039(12) N3 0.0294(16) 0.040(2) 0.0433(17) 0.0107(14) -0.0025(13) 0.0005(13) N4 0.0272(15) 0.0261(16) 0.0396(16) -0.0001(12) 0.0062(12) 0.0043(12) N5 0.0370(17) 0.0347(18) 0.0396(16) -0.0010(14) 0.0062(13) -0.0006(14) C1 0.0221(15) 0.0162(16) 0.0269(14) -0.0001(12) 0.0066(12) 0.0008(12) C2 0.0266(16) 0.0162(16) 0.0264(15) 0.0002(12) 0.0078(12) -0.0025(12) C3 0.0245(15) 0.0163(15) 0.0245(14) 0.0005(12) 0.0027(12) -0.0028(12) C4 0.0215(15) 0.0186(16) 0.0317(16) 0.0025(13) 0.0080(12) 0.0012(12) C5 0.0234(16) 0.0252(18) 0.0262(15) 0.0002(12) 0.0080(13) 0.0008(12) C6 0.0227(15) 0.0221(17) 0.0246(15) 0.0022(12) 0.0028(12) -0.0003(13) C7 0.0228(16) 0.0218(17) 0.0353(17) -0.0007(13) 0.0066(13) 0.0054(13) C8 0.0210(15) 0.0204(17) 0.0381(17) -0.0037(13) 0.0111(13) -0.0014(12) C9 0.045(2) 0.034(2) 0.0362(18) -0.0009(16) 0.0171(16) -0.0015(17) C10 0.039(2) 0.029(2) 0.0388(19) 0.0018(15) 0.0084(16) 0.0018(16) C11 0.036(2) 0.037(2) 0.058(2) 0.0025(18) 0.0231(18) 0.0112(17) C12 0.0315(17) 0.0217(17) 0.0265(15) -0.0033(13) 0.0105(13) -0.0018(13) C13 0.044(2) 0.0221(18) 0.0351(17) -0.0007(14) 0.0157(15) 0.0039(15) C14 0.0343(18) 0.0288(19) 0.0317(17) -0.0008(14) 0.0051(14) -0.0030(15) C15 0.0307(18) 0.0285(19) 0.0297(16) 0.0058(14) 0.0036(13) 0.0002(14) C16 0.0329(19) 0.033(2) 0.056(2) 0.0076(18) 0.0085(17) 0.0103(16) C17 0.0356(19) 0.032(2) 0.050(2) -0.0002(17) 0.0088(16) 0.0071(17) C18 0.038(2) 0.063(3) 0.078(3) -0.002(3) -0.023(2) 0.005(2) C19 0.0237(17) 0.039(2) 0.0384(18) -0.0043(16) 0.0042(14) 0.0007(15) C20 0.030(2) 0.059(3) 0.071(3) 0.004(2) 0.0207(19) -0.0089(19) C21 0.0293(17) 0.039(2) 0.0265(17) -0.0022(14) 0.0028(13) -0.0013(15) C22 0.044(2) 0.054(3) 0.0284(18) -0.0050(17) 0.0067(16) -0.0024(19) C23 0.0324(18) 0.030(2) 0.0358(18) 0.0039(16) 0.0068(15) -0.0017(15) C24 0.058(3) 0.045(2) 0.041(2) -0.0050(18) 0.0147(19) 0.002(2) F1 0.096(3) 0.223(6) 0.069(2) -0.023(3) 0.028(2) 0.055(3) F2 0.080(2) 0.101(3) 0.102(3) -0.011(2) -0.0168(19) -0.042(2) F3 0.073(2) 0.057(2) 0.220(5) 0.050(3) -0.007(3) 0.0024(18) F4 0.0336(13) 0.073(2) 0.0790(19) 0.0206(15) 0.0122(12) 0.0099(12) B1 0.029(2) 0.049(3) 0.049(3) -0.004(2) 0.0074(19) -0.005(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 Cu1 N2 1.956(3) . ? Cu1 N5 1.987(3) . ? Cu1 N4 2.021(3) . ? S1 C8 1.755(3) . ? S1 C7 1.861(3) . ? S2 C15 1.754(4) . ? S2 C14 1.860(4) . ? N1 C9 1.375(5) . ? N1 C8 1.377(4) . ? N1 C11 1.472(4) . ? N2 C8 1.348(4) . ? N2 C10 1.388(5) . ? N3 C15 1.368(5) . ? N3 C16 1.370(5) . ? N3 C18 1.471(5) . ? N4 C15 1.346(5) . ? N4 C17 1.388(5) . ? N5 C23 1.141(5) . ? C1 C2 1.407(4) . ? C1 C6 1.428(4) . ? C1 C7 1.510(4) . ? C2 C3 1.424(4) . ? C2 C12 1.534(4) . ? C3 C4 1.411(4) . ? C3 C14 1.519(4) . ? C4 C5 1.412(4) . ? C4 C19 1.528(4) . ? C5 C6 1.388(4) . ? C6 C21 1.533(4) . ? C9 C10 1.377(5) . ? C12 C13 1.544(5) . ? C16 C17 1.367(5) . ? C19 C20 1.531(6) . ? C21 C22 1.522(5) . ? C23 C24 1.466(5) . ? F1 B1 1.346(6) . ? F2 B1 1.361(6) . ? F3 B1 1.381(6) . ? F4 B1 1.382(5) . ? 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 N2 Cu1 N5 130.66(12) . . ? N2 Cu1 N4 126.19(12) . . ? N5 Cu1 N4 101.19(12) . . ? C8 S1 C7 102.44(15) . . ? C15 S2 C14 102.78(16) . . ? C9 N1 C8 107.2(3) . . ? C9 N1 C11 125.6(3) . . ? C8 N1 C11 127.2(3) . . ? C8 N2 C10 106.0(3) . . ? C8 N2 Cu1 128.8(2) . . ? C10 N2 Cu1 124.9(2) . . ? C15 N3 C16 107.8(3) . . ? C15 N3 C18 127.0(4) . . ? C16 N3 C18 125.2(4) . . ? C15 N4 C17 105.9(3) . . ? C15 N4 Cu1 131.5(2) . . ? C17 N4 Cu1 122.5(3) . . ? C23 N5 Cu1 164.9(3) . . ? C2 C1 C6 120.2(3) . . ? C2 C1 C7 121.0(3) . . ? C6 C1 C7 118.8(3) . . ? C1 C2 C3 120.0(3) . . ? C1 C2 C12 120.6(3) . . ? C3 C2 C12 119.3(3) . . ? C4 C3 C2 120.0(3) . . ? C4 C3 C14 119.3(3) . . ? C2 C3 C14 120.6(3) . . ? C3 C4 C5 118.5(3) . . ? C3 C4 C19 124.0(3) . . ? C5 C4 C19 117.5(3) . . ? C6 C5 C4 122.7(3) . . ? C5 C6 C1 118.5(3) . . ? C5 C6 C21 121.1(3) . . ? C1 C6 C21 120.4(3) . . ? C1 C7 S1 114.2(2) . . ? N2 C8 N1 110.5(3) . . ? N2 C8 S1 125.5(2) . . ? N1 C8 S1 123.9(3) . . ? N1 C9 C10 107.0(3) . . ? C9 C10 N2 109.4(3) . . ? C2 C12 C13 112.2(3) . . ? C3 C14 S2 113.4(2) . . ? N4 C15 N3 110.1(3) . . ? N4 C15 S2 125.7(3) . . ? N3 C15 S2 124.1(3) . . ? C17 C16 N3 106.8(3) . . ? C16 C17 N4 109.5(4) . . ? C4 C19 C20 112.5(3) . . ? C22 C21 C6 115.9(3) . . ? N5 C23 C24 178.4(4) . . ? F1 B1 F2 107.2(4) . . ? F1 B1 F3 115.0(5) . . ? F2 B1 F3 106.3(4) . . ? F1 B1 F4 111.1(4) . . ? F2 B1 F4 109.3(4) . . ? F3 B1 F4 107.8(4) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.067 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.072