data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H22 B20' _chemical_formula_weight 286.42 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' _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 7.0165(12) _cell_length_b 9.8852(16) _cell_length_c 12.375(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.440(3) _cell_angle_gamma 90.00 _cell_volume 858.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 952 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 27.60 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 292 _exptl_absorpt_coefficient_mu 0.045 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.689716 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 SMART CCD DIFFRACTOMETER' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5667 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 28.02 _reflns_number_total 2055 _reflns_number_gt 1445 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'BRUKER SMART CCD DIFFRACTOMETER' _computing_cell_refinement 'BRUKER SMART CCD DIFFRACTOMETER' _computing_data_reduction 'BRUKER SMART CCD DIFFRACTOMETER' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SIEMENS SHELXTL' _computing_publication_material 'SIEMENS 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^)+(0.1080P)^2^+0.3603P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2055 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.2311 _refine_ls_wR_factor_gt 0.2103 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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 C1 C 0.0052(3) 0.44136(18) 0.04026(14) 0.0327(4) Uani 1 1 d . . . C2 C -0.1555(3) 0.4412(2) 0.14126(17) 0.0466(6) Uani 1 1 d . . . H2 H -0.2671 0.5189 0.1480 0.056 Uiso 1 1 calc R . . B3 B -0.1704(3) 0.3185(2) 0.03928(19) 0.0411(5) Uani 1 1 d . . . H3 H -0.2879 0.3136 -0.0200 0.049 Uiso 1 1 calc R . . B4 B 0.0685(3) 0.2799(2) 0.00339(19) 0.0416(6) Uani 1 1 d . . . H4 H 0.1053 0.2497 -0.0794 0.050 Uiso 1 1 calc R . . B5 B 0.2241(3) 0.3820(2) 0.08328(19) 0.0415(5) Uani 1 1 d . . . H5 H 0.3617 0.4179 0.0525 0.050 Uiso 1 1 calc R . . B6 B 0.0784(3) 0.4781(2) 0.16677(16) 0.0378(5) Uani 1 1 d . . . H6 H 0.1228 0.5807 0.1904 0.045 Uiso 1 1 calc R . . B7 B -0.2012(4) 0.2748(3) 0.1771(2) 0.0486(6) Uani 1 1 d . . . H7 H -0.3398 0.2404 0.2076 0.058 Uiso 1 1 calc R . . B8 B -0.0587(4) 0.1715(3) 0.0924(2) 0.0503(6) Uani 1 1 d . . . H8 H -0.1037 0.0692 0.0683 0.060 Uiso 1 1 calc R . . B9 B 0.1841(4) 0.2116(3) 0.1185(2) 0.0503(6) Uani 1 1 d . . . H9 H 0.2969 0.1350 0.1109 0.060 Uiso 1 1 calc R . . B10 B 0.1914(4) 0.3392(3) 0.2210(2) 0.0498(6) Uani 1 1 d . . . H10 H 0.3087 0.3468 0.2802 0.060 Uiso 1 1 calc R . . B11 B -0.0465(4) 0.3775(3) 0.25695(19) 0.0489(6) Uani 1 1 d . . . H11 H -0.0844 0.4102 0.3390 0.059 Uiso 1 1 calc R . . B12 B 0.0178(4) 0.2090(3) 0.2265(2) 0.0521(7) Uani 1 1 d . . . H12 H 0.0227 0.1305 0.2895 0.062 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 C1 0.0312(9) 0.0368(9) 0.0302(9) -0.0025(7) 0.0012(7) 0.0026(7) C2 0.0459(12) 0.0540(13) 0.0399(11) -0.0015(9) 0.0047(9) 0.0018(9) B3 0.0386(12) 0.0423(12) 0.0425(12) -0.0014(9) -0.0017(9) -0.0054(9) B4 0.0466(13) 0.0366(11) 0.0418(12) -0.0041(9) 0.0037(10) 0.0059(9) B5 0.0329(11) 0.0479(13) 0.0435(12) 0.0046(10) -0.0017(9) 0.0056(9) B6 0.0375(11) 0.0466(12) 0.0292(10) -0.0001(8) -0.0020(8) 0.0009(9) B7 0.0450(13) 0.0531(14) 0.0477(14) 0.0086(11) 0.0068(10) -0.0042(11) B8 0.0565(16) 0.0396(13) 0.0547(15) 0.0010(10) 0.0033(12) -0.0022(10) B9 0.0482(14) 0.0457(13) 0.0570(15) 0.0099(11) 0.0025(11) 0.0103(10) B10 0.0458(13) 0.0600(15) 0.0435(13) 0.0093(11) -0.0084(10) 0.0031(11) B11 0.0525(14) 0.0587(15) 0.0356(12) 0.0037(10) 0.0040(10) 0.0005(11) B12 0.0549(15) 0.0511(14) 0.0502(14) 0.0124(11) 0.0008(12) 0.0038(11) _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 C1 C1 1.530(3) 3_565 ? C1 B6 1.684(3) . ? C1 C2 1.690(3) . ? C1 B4 1.719(3) . ? C1 B5 1.725(3) . ? C1 B3 1.730(3) . ? C2 B6 1.708(3) . ? C2 B7 1.734(3) . ? C2 B11 1.736(3) . ? C2 B3 1.753(3) . ? B3 B7 1.774(3) . ? B3 B8 1.775(3) . ? B3 B4 1.779(3) . ? B4 B9 1.768(3) . ? B4 B5 1.781(3) . ? B4 B8 1.781(4) . ? B5 B6 1.741(3) . ? B5 B9 1.762(3) . ? B5 B10 1.772(3) . ? B6 B10 1.719(3) . ? B6 B11 1.737(3) . ? B7 B12 1.773(4) . ? B7 B8 1.777(4) . ? B7 B11 1.780(4) . ? B8 B9 1.776(4) . ? B8 B12 1.779(4) . ? B9 B12 1.781(4) . ? B9 B10 1.789(4) . ? B10 B11 1.772(4) . ? B10 B12 1.774(4) . ? B11 B12 1.768(4) . ? 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 C1 B6 117.05(19) 3_565 . ? C1 C1 C2 116.99(18) 3_565 . ? B6 C1 C2 60.85(12) . . ? C1 C1 B4 122.79(18) 3_565 . ? B6 C1 B4 111.67(15) . . ? C2 C1 B4 111.77(15) . . ? C1 C1 B5 119.77(19) 3_565 . ? B6 C1 B5 61.43(12) . . ? C2 C1 B5 111.66(15) . . ? B4 C1 B5 62.26(13) . . ? C1 C1 B3 119.83(19) 3_565 . ? B6 C1 B3 111.72(15) . . ? C2 C1 B3 61.67(12) . . ? B4 C1 B3 62.08(13) . . ? B5 C1 B3 113.30(15) . . ? C1 C2 B6 59.40(12) . . ? C1 C2 B7 108.39(16) . . ? B6 C2 B7 109.50(17) . . ? C1 C2 B11 108.53(16) . . ? B6 C2 B11 60.55(13) . . ? B7 C2 B11 61.70(15) . . ? C1 C2 B3 60.29(12) . . ? B6 C2 B3 109.41(16) . . ? B7 C2 B3 61.16(14) . . ? B11 C2 B3 111.46(17) . . ? C1 B3 C2 58.03(12) . . ? C1 B3 B7 104.82(16) . . ? C2 B3 B7 58.90(14) . . ? C1 B3 B8 105.06(16) . . ? C2 B3 B8 106.04(17) . . ? B7 B3 B8 60.09(15) . . ? C1 B3 B4 58.66(12) . . ? C2 B3 B4 106.09(16) . . ? B7 B3 B4 108.04(17) . . ? B8 B3 B4 60.17(14) . . ? C1 B4 B9 104.99(16) . . ? C1 B4 B3 59.26(12) . . ? B9 B4 B3 107.95(17) . . ? C1 B4 B5 59.02(12) . . ? B9 B4 B5 59.56(14) . . ? B3 B4 B5 108.35(16) . . ? C1 B4 B8 105.24(16) . . ? B9 B4 B8 60.06(15) . . ? B3 B4 B8 59.81(14) . . ? B5 B4 B8 107.78(17) . . ? C1 B5 B6 58.12(11) . . ? C1 B5 B9 104.99(17) . . ? B6 B5 B9 106.23(17) . . ? C1 B5 B10 104.87(16) . . ? B6 B5 B10 58.58(14) . . ? B9 B5 B10 60.82(15) . . ? C1 B5 B4 58.72(12) . . ? B6 B5 B4 106.17(16) . . ? B9 B5 B4 59.86(14) . . ? B10 B5 B4 108.40(17) . . ? C1 B6 C2 59.75(12) . . ? C1 B6 B10 109.11(17) . . ? C2 B6 B10 109.98(18) . . ? C1 B6 B11 108.80(17) . . ? C2 B6 B11 60.53(13) . . ? B10 B6 B11 61.68(15) . . ? C1 B6 B5 60.45(12) . . ? C2 B6 B5 109.97(16) . . ? B10 B6 B5 61.61(14) . . ? B11 B6 B5 111.73(18) . . ? C2 B7 B12 105.98(18) . . ? C2 B7 B3 59.95(13) . . ? B12 B7 B3 108.01(18) . . ? C2 B7 B8 106.77(17) . . ? B12 B7 B8 60.15(16) . . ? B3 B7 B8 59.97(14) . . ? C2 B7 B11 59.20(14) . . ? B12 B7 B11 59.68(15) . . ? B3 B7 B11 108.47(17) . . ? B8 B7 B11 108.18(18) . . ? B3 B8 B9 107.74(17) . . ? B3 B8 B7 59.94(14) . . ? B9 B8 B7 107.90(19) . . ? B3 B8 B12 107.71(18) . . ? B9 B8 B12 60.12(16) . . ? B7 B8 B12 59.81(15) . . ? B3 B8 B4 60.02(13) . . ? B9 B8 B4 59.59(14) . . ? B7 B8 B4 107.80(18) . . ? B12 B8 B4 107.60(18) . . ? B5 B9 B4 60.58(13) . . ? B5 B9 B8 108.82(17) . . ? B4 B9 B8 60.34(14) . . ? B5 B9 B12 107.82(18) . . ? B4 B9 B12 108.11(17) . . ? B8 B9 B12 60.01(15) . . ? B5 B9 B10 59.86(14) . . ? B4 B9 B10 108.20(17) . . ? B8 B9 B10 107.97(19) . . ? B12 B9 B10 59.60(15) . . ? B6 B10 B11 59.65(14) . . ? B6 B10 B5 59.80(13) . . ? B11 B10 B5 108.63(17) . . ? B6 B10 B12 106.24(18) . . ? B11 B10 B12 59.80(16) . . ? B5 B10 B12 107.68(18) . . ? B6 B10 B9 106.00(17) . . ? B11 B10 B9 107.86(19) . . ? B5 B10 B9 59.32(14) . . ? B12 B10 B9 59.96(16) . . ? C2 B11 B6 58.92(13) . . ? C2 B11 B12 106.12(18) . . ? B6 B11 B12 105.76(18) . . ? C2 B11 B10 106.29(17) . . ? B6 B11 B10 58.67(14) . . ? B12 B11 B10 60.17(15) . . ? C2 B11 B7 59.09(14) . . ? B6 B11 B7 106.16(16) . . ? B12 B11 B7 59.97(15) . . ? B10 B11 B7 108.08(19) . . ? B11 B12 B7 60.36(15) . . ? B11 B12 B10 60.03(15) . . ? B7 B12 B10 108.28(18) . . ? B11 B12 B8 108.64(17) . . ? B7 B12 B8 60.04(15) . . ? B10 B12 B8 108.53(18) . . ? B11 B12 B9 108.42(18) . . ? B7 B12 B9 107.89(18) . . ? B10 B12 B9 60.44(15) . . ? B8 B12 B9 59.87(15) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.297 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.056 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H36 B20 Cu2' _chemical_formula_weight 595.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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 7.036(3) _cell_length_b 9.412(3) _cell_length_c 11.529(4) _cell_angle_alpha 92.363(7) _cell_angle_beta 95.143(8) _cell_angle_gamma 105.407(7) _cell_volume 731.4(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 824 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.81 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 302 _exptl_absorpt_coefficient_mu 1.466 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.5917 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 4926 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3441 _reflns_number_gt 2782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0632P)^2^+0.3774P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3441 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1300 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 Cu1 Cu 0.73857(6) 0.30787(4) 0.28377(3) 0.05937(17) Uani 1 1 d . . . C2 C 0.8950(3) 0.5078(2) 0.32118(18) 0.0336(4) Uani 1 1 d . . . C1 C 1.0109(3) 0.5598(2) 0.45606(17) 0.0290(4) Uani 1 1 d . . . C11 C 0.4278(5) 0.2390(4) 0.1052(3) 0.0627(8) Uani 1 1 d . . . C12 C 0.4346(5) 0.1681(4) 0.2101(3) 0.0678(9) Uani 1 1 d . . . H12A H 0.3239 0.1562 0.2580 0.081 Uiso 1 1 calc R . . C13 C 0.5718(6) 0.0930(3) 0.2342(3) 0.0680(9) Uani 1 1 d . . . H13A H 0.5496 0.0205 0.2936 0.082 Uiso 1 1 calc R . . C14 C 0.7158(7) 0.0905(4) 0.1573(4) 0.0813(11) Uani 1 1 d . . . H14A H 0.8089 0.0305 0.1718 0.098 Uiso 1 1 calc R . . C15 C 0.7081(6) 0.1608(5) 0.0535(4) 0.0819(11) Uani 1 1 d . . . H15A H 0.8009 0.1596 0.0012 0.098 Uiso 1 1 calc R . . C16 C 0.5655(5) 0.2309(4) 0.0289(3) 0.0622(8) Uani 1 1 d . . . H16A H 0.5603 0.2750 -0.0416 0.075 Uiso 1 1 calc R . . C17 C 0.2754(8) 0.3203(7) 0.0799(4) 0.1072(16) Uani 1 1 d . . . H17A H 0.2910 0.3622 0.0056 0.161 Uiso 1 1 calc R . . H17B H 0.2914 0.3978 0.1397 0.161 Uiso 1 1 calc R . . H17C H 0.1456 0.2533 0.0779 0.161 Uiso 1 1 calc R . . B3 B 1.1508(4) 0.5460(3) 0.3431(2) 0.0336(5) Uani 1 1 d . . . H3 H 1.2307 0.4611 0.3335 0.040 Uiso 1 1 calc R . . B7 B 1.0332(4) 0.6095(3) 0.2222(2) 0.0395(6) Uani 1 1 d . . . H7 H 1.0371 0.5666 0.1325 0.047 Uiso 1 1 calc R . . B11 B 0.8216(5) 0.6541(3) 0.2660(2) 0.0438(6) Uani 1 1 d . . . H11 H 0.6881 0.6406 0.2046 0.053 Uiso 1 1 calc R . . B6 B 0.8049(4) 0.6179(3) 0.4145(2) 0.0376(5) Uani 1 1 d . . . H6 H 0.6620 0.5795 0.4507 0.045 Uiso 1 1 calc R . . B4 B 1.2315(4) 0.6937(3) 0.4528(2) 0.0362(5) Uani 1 1 d . . . H4 H 1.3645 0.7051 0.5142 0.043 Uiso 1 1 calc R . . B8 B 1.2465(4) 0.7290(3) 0.3032(2) 0.0405(6) Uani 1 1 d . . . H8 H 1.3895 0.7645 0.2667 0.049 Uiso 1 1 calc R . . B12 B 1.0412(5) 0.7966(3) 0.2558(2) 0.0448(6) Uani 1 1 d . . . H12 H 1.0515 0.8768 0.1884 0.054 Uiso 1 1 calc R . . B10 B 0.8980(5) 0.8018(3) 0.3756(2) 0.0455(6) Uani 1 1 d . . . H10 H 0.8150 0.8846 0.3860 0.055 Uiso 1 1 calc R . . B5 B 1.0167(4) 0.7392(3) 0.4971(2) 0.0378(5) Uani 1 1 d . . . H5 H 1.0111 0.7804 0.5871 0.045 Uiso 1 1 calc R . . B9 B 1.1632(5) 0.8488(3) 0.3991(2) 0.0438(6) Uani 1 1 d . . . H9 H 1.2527 0.9624 0.4248 0.053 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 Cu1 0.0695(3) 0.0437(2) 0.0450(2) -0.00420(14) -0.00702(16) -0.01394(17) C2 0.0367(11) 0.0344(11) 0.0258(9) -0.0015(8) -0.0007(8) 0.0047(9) C1 0.0296(10) 0.0291(10) 0.0254(9) -0.0016(7) 0.0027(7) 0.0038(8) C11 0.0578(17) 0.0705(19) 0.0462(15) -0.0079(13) -0.0098(13) 0.0006(15) C12 0.0650(19) 0.0669(19) 0.0457(15) -0.0001(13) -0.0021(14) -0.0237(16) C13 0.083(2) 0.0408(15) 0.0600(18) 0.0027(13) -0.0052(17) -0.0151(15) C14 0.087(3) 0.0528(19) 0.091(3) -0.0160(18) -0.018(2) 0.0077(18) C15 0.075(2) 0.087(3) 0.073(2) -0.023(2) 0.0105(19) 0.007(2) C16 0.071(2) 0.071(2) 0.0361(13) -0.0024(13) 0.0056(13) 0.0056(16) C17 0.095(3) 0.156(5) 0.076(3) -0.002(3) -0.009(2) 0.052(3) B3 0.0365(12) 0.0348(12) 0.0281(11) 0.0003(9) 0.0073(9) 0.0061(10) B7 0.0487(15) 0.0399(13) 0.0276(11) 0.0024(9) 0.0044(10) 0.0081(11) B11 0.0492(16) 0.0493(15) 0.0340(13) 0.0076(11) 0.0001(11) 0.0163(13) B6 0.0379(13) 0.0420(13) 0.0343(12) 0.0042(10) 0.0033(10) 0.0134(11) B4 0.0341(12) 0.0355(12) 0.0328(12) -0.0001(9) 0.0032(9) -0.0009(10) B8 0.0460(14) 0.0368(13) 0.0362(13) 0.0048(10) 0.0109(11) 0.0041(11) B12 0.0629(18) 0.0385(13) 0.0346(13) 0.0076(10) 0.0086(12) 0.0144(13) B10 0.0625(18) 0.0427(14) 0.0387(14) 0.0063(11) 0.0119(13) 0.0244(13) B5 0.0499(15) 0.0316(12) 0.0315(12) -0.0028(9) 0.0081(10) 0.0098(11) B9 0.0600(17) 0.0284(12) 0.0391(13) 0.0015(10) 0.0100(12) 0.0036(11) _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 C2 1.920(2) . ? Cu1 C13 2.078(3) . ? Cu1 C12 2.261(3) . ? Cu1 C14 2.424(4) . ? C2 C1 1.679(3) . ? C2 B7 1.720(3) . ? C2 B11 1.720(4) . ? C2 B3 1.731(3) . ? C2 B6 1.736(3) . ? C1 C1 1.533(4) 2_766 ? C1 B6 1.717(3) . ? C1 B3 1.722(3) . ? C1 B5 1.723(3) . ? C1 B4 1.724(3) . ? C11 C16 1.380(5) . ? C11 C12 1.408(5) . ? C11 C17 1.490(6) . ? C12 C13 1.356(6) . ? C13 C14 1.409(6) . ? C14 C15 1.394(6) . ? C15 C16 1.356(6) . ? B3 B7 1.763(4) . ? B3 B8 1.771(4) . ? B3 B4 1.778(4) . ? B7 B11 1.760(4) . ? B7 B12 1.773(4) . ? B7 B8 1.776(4) . ? B11 B6 1.768(4) . ? B11 B12 1.773(4) . ? B11 B10 1.776(4) . ? B6 B10 1.772(4) . ? B6 B5 1.784(4) . ? B4 B9 1.772(4) . ? B4 B8 1.776(4) . ? B4 B5 1.787(4) . ? B8 B12 1.779(4) . ? B8 B9 1.789(4) . ? B12 B9 1.778(4) . ? B12 B10 1.787(4) . ? B10 B5 1.768(4) . ? B10 B9 1.792(5) . ? B5 B9 1.774(4) . ? 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 C2 Cu1 C13 176.99(11) . . ? C2 Cu1 C12 143.41(13) . . ? C13 Cu1 C12 36.12(15) . . ? C2 Cu1 C14 142.20(14) . . ? C13 Cu1 C14 35.43(15) . . ? C12 Cu1 C14 61.55(15) . . ? C1 C2 B7 108.93(16) . . ? C1 C2 B11 108.67(17) . . ? B7 C2 B11 61.54(16) . . ? C1 C2 B3 60.61(13) . . ? B7 C2 B3 61.43(15) . . ? B11 C2 B3 111.55(18) . . ? C1 C2 B6 60.33(13) . . ? B7 C2 B6 111.85(18) . . ? B11 C2 B6 61.53(15) . . ? B3 C2 B6 111.81(17) . . ? C1 C2 Cu1 120.25(14) . . ? B7 C2 Cu1 122.20(15) . . ? B11 C2 Cu1 121.21(16) . . ? B3 C2 Cu1 119.59(15) . . ? B6 C2 Cu1 117.65(15) . . ? C1 C1 C2 116.8(2) 2_766 . ? C1 C1 B6 117.4(2) 2_766 . ? C2 C1 B6 61.46(14) . . ? C1 C1 B3 117.0(2) 2_766 . ? C2 C1 B3 61.19(13) . . ? B6 C1 B3 113.24(17) . . ? C1 C1 B5 121.8(2) 2_766 . ? C2 C1 B5 111.63(16) . . ? B6 C1 B5 62.47(15) . . ? B3 C1 B5 113.43(16) . . ? C1 C1 B4 121.4(2) 2_766 . ? C2 C1 B4 111.37(16) . . ? B6 C1 B4 113.82(18) . . ? B3 C1 B4 62.11(14) . . ? B5 C1 B4 62.45(15) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 C17 122.0(3) . . ? C12 C11 C17 119.8(4) . . ? C13 C12 C11 120.5(3) . . ? C13 C12 Cu1 64.54(17) . . ? C11 C12 Cu1 96.06(19) . . ? C12 C13 C14 120.6(3) . . ? C12 C13 Cu1 79.35(19) . . ? C14 C13 Cu1 85.8(2) . . ? C15 C14 C13 118.5(4) . . ? C15 C14 Cu1 95.3(3) . . ? C13 C14 Cu1 58.74(18) . . ? C16 C15 C14 120.1(4) . . ? C15 C16 C11 122.1(3) . . ? C1 B3 C2 58.20(13) . . ? C1 B3 B7 105.10(18) . . ? C2 B3 B7 58.97(14) . . ? C1 B3 B8 105.60(17) . . ? C2 B3 B8 106.60(18) . . ? B7 B3 B8 60.36(15) . . ? C1 B3 B4 59.02(13) . . ? C2 B3 B4 106.48(17) . . ? B7 B3 B4 108.10(19) . . ? B8 B3 B4 60.07(14) . . ? C2 B7 B11 59.25(15) . . ? C2 B7 B3 59.60(14) . . ? B11 B7 B3 108.23(18) . . ? C2 B7 B12 106.54(19) . . ? B11 B7 B12 60.25(17) . . ? B3 B7 B12 108.10(18) . . ? C2 B7 B8 106.85(17) . . ? B11 B7 B8 108.6(2) . . ? B3 B7 B8 60.04(15) . . ? B12 B7 B8 60.17(17) . . ? C2 B11 B7 59.22(15) . . ? C2 B11 B6 59.66(14) . . ? B7 B11 B6 108.46(19) . . ? C2 B11 B12 106.5(2) . . ? B7 B11 B12 60.23(17) . . ? B6 B11 B12 108.4(2) . . ? C2 B11 B10 106.73(19) . . ? B7 B11 B10 108.7(2) . . ? B6 B11 B10 60.00(16) . . ? B12 B11 B10 60.48(17) . . ? C1 B6 C2 58.21(13) . . ? C1 B6 B11 104.86(18) . . ? C2 B6 B11 58.81(15) . . ? C1 B6 B10 105.19(19) . . ? C2 B6 B10 106.24(19) . . ? B11 B6 B10 60.22(16) . . ? C1 B6 B5 58.94(14) . . ? C2 B6 B5 106.20(18) . . ? B11 B6 B5 107.57(19) . . ? B10 B6 B5 59.65(16) . . ? C1 B4 B9 105.09(19) . . ? C1 B4 B8 105.26(17) . . ? B9 B4 B8 60.54(15) . . ? C1 B4 B3 58.87(13) . . ? B9 B4 B3 108.04(18) . . ? B8 B4 B3 59.77(14) . . ? C1 B4 B5 58.74(14) . . ? B9 B4 B5 59.79(16) . . ? B8 B4 B5 108.22(19) . . ? B3 B4 B5 107.77(18) . . ? B3 B8 B4 60.15(14) . . ? B3 B8 B7 59.60(15) . . ? B4 B8 B7 107.56(18) . . ? B3 B8 B12 107.45(19) . . ? B4 B8 B12 107.42(19) . . ? B7 B8 B12 59.81(16) . . ? B3 B8 B9 107.61(18) . . ? B4 B8 B9 59.62(15) . . ? B7 B8 B9 107.5(2) . . ? B12 B8 B9 59.78(17) . . ? B7 B12 B11 59.53(17) . . ? B7 B12 B9 108.10(19) . . ? B11 B12 B9 108.04(19) . . ? B7 B12 B8 60.02(16) . . ? B11 B12 B8 107.87(19) . . ? B9 B12 B8 60.38(17) . . ? B7 B12 B10 107.68(19) . . ? B11 B12 B10 59.84(17) . . ? B9 B12 B10 60.36(17) . . ? B8 B12 B10 108.60(19) . . ? B5 B10 B6 60.51(15) . . ? B5 B10 B11 107.90(19) . . ? B6 B10 B11 59.78(16) . . ? B5 B10 B12 107.5(2) . . ? B6 B10 B12 107.64(19) . . ? B11 B10 B12 59.68(17) . . ? B5 B10 B9 59.76(16) . . ? B6 B10 B9 107.99(19) . . ? B11 B10 B9 107.3(2) . . ? B12 B10 B9 59.57(17) . . ? C1 B5 B10 105.06(18) . . ? C1 B5 B9 105.06(17) . . ? B10 B5 B9 60.78(17) . . ? C1 B5 B6 58.59(14) . . ? B10 B5 B6 59.84(16) . . ? B9 B5 B6 108.27(19) . . ? C1 B5 B4 58.81(13) . . ? B10 B5 B4 108.25(18) . . ? B9 B5 B4 59.69(16) . . ? B6 B5 B4 107.68(17) . . ? B4 B9 B5 60.52(15) . . ? B4 B9 B12 107.66(18) . . ? B5 B9 B12 107.7(2) . . ? B4 B9 B8 59.84(15) . . ? B5 B9 B8 108.24(18) . . ? B12 B9 B8 59.84(16) . . ? B4 B9 B10 107.86(18) . . ? B5 B9 B10 59.46(16) . . ? B12 B9 B10 60.08(17) . . ? B8 B9 B10 108.0(2) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.622 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.084 #===END