# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_{[B10C2H11]C}2_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-bis(1,2-dicarba-closo-dodecaborane(11)-8-yl)ethyne ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [B10 C2 H11]2 C2 ; _chemical_formula_sum 'C6 H22 B20' _chemical_formula_weight 310.44 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 11.4869(10) _cell_length_b 11.6934(11) _cell_length_c 6.8962(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 926.30(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4038 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.11 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.113 _exptl_crystal_density_method none _exptl_crystal_F_000 316 _exptl_absorpt_coefficient_mu 0.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.99 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7733 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.14 _reflns_number_total 1114 _reflns_number_gt 996 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.1183P)^2^+0.1514P] 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 noref _refine_ls_abs_structure_details ; Compound is a weak anomalous scatterer and no conclusions about the absolute structure are justified ; _refine_ls_number_reflns 1114 _refine_ls_number_parameters 162 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.188 _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 C1 C 0.2155(3) 0.2458(3) 0.6256(6) 0.0271(8) Uani 1 1 d . . . H1 H 0.170(4) 0.251(3) 0.714(8) 0.028(11) Uiso 1 1 d . . . C2 C 0.1686(3) 0.2561(2) 0.4033(5) 0.0215(7) Uani 1 1 d . . . H2 H 0.090(3) 0.264(2) 0.389(6) 0.018(9) Uiso 1 1 d . . . B3 B 0.2411(3) 0.3709(3) 0.5015(6) 0.0270(8) Uani 1 1 d . . . H3B H 0.192(3) 0.446(3) 0.534(6) 0.036(11) Uiso 1 1 d . . . B4 B 0.3490(4) 0.3067(3) 0.6526(5) 0.0293(9) Uani 1 1 d . . . H4B H 0.368(4) 0.347(3) 0.794(6) 0.039(12) Uiso 1 1 d . . . B5 B 0.3290(3) 0.1551(3) 0.6419(6) 0.0305(9) Uani 1 1 d . . . H5B H 0.344(4) 0.106(5) 0.770(9) 0.074(17) Uiso 1 1 d . . . B6 B 0.2109(3) 0.1251(3) 0.4862(6) 0.0289(9) Uani 1 1 d . . . H6B H 0.140(3) 0.067(3) 0.512(6) 0.030(10) Uiso 1 1 d . . . B7 B 0.2646(3) 0.3254(3) 0.2585(6) 0.0203(7) Uani 1 1 d . . . H7B H 0.241(3) 0.371(3) 0.145(7) 0.027(10) Uiso 1 1 d . . . B8 B 0.3873(3) 0.3555(3) 0.4142(6) 0.0262(8) Uani 1 1 d . . . B9 B 0.4399(3) 0.2193(4) 0.5002(7) 0.0291(8) Uani 1 1 d . . . H9B H 0.538(3) 0.197(4) 0.522(7) 0.040(12) Uiso 1 1 d . . . B10 B 0.3534(3) 0.1085(3) 0.3991(7) 0.0300(8) Uani 1 1 d . . . H10B H 0.401(5) 0.030(4) 0.375(10) 0.068(15) Uiso 1 1 d . . . B11 B 0.2465(3) 0.1739(3) 0.2498(6) 0.0221(7) Uani 1 1 d . . . H11B H 0.208(3) 0.144(3) 0.140(6) 0.019(8) Uiso 1 1 d . . . B12 B 0.3881(3) 0.2323(3) 0.2586(6) 0.0258(8) Uani 1 1 d . . . H12B H 0.436(5) 0.223(4) 0.143(10) 0.066(17) Uiso 1 1 d . . . C3 C 0.4676(3) 0.4586(3) 0.3919(6) 0.0328(8) 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 C1 0.0261(16) 0.0319(18) 0.0232(17) 0.0011(13) 0.0084(15) -0.0036(12) C2 0.0149(13) 0.0232(15) 0.0264(16) 0.0014(13) 0.0025(12) -0.0008(10) B3 0.0364(19) 0.0201(18) 0.0246(18) -0.0035(15) 0.0053(17) -0.0022(14) B4 0.040(2) 0.0276(18) 0.0206(18) -0.0022(16) -0.0022(17) -0.0111(15) B5 0.034(2) 0.0309(18) 0.027(2) 0.0101(18) -0.0035(17) 0.0024(15) B6 0.038(2) 0.0164(16) 0.033(2) 0.0078(15) -0.0014(19) -0.0057(15) B7 0.0229(15) 0.0176(14) 0.0205(16) 0.0015(13) 0.0000(14) -0.0044(12) B8 0.0325(17) 0.0254(16) 0.0206(16) 0.0019(16) -0.0036(16) -0.0114(14) B9 0.0213(17) 0.039(2) 0.0270(17) 0.0019(19) -0.0070(16) -0.0029(15) B10 0.0271(17) 0.0278(18) 0.0351(19) -0.0006(19) -0.0078(17) 0.0082(14) B11 0.0211(15) 0.0180(15) 0.0272(18) -0.0041(14) -0.0048(15) 0.0014(11) B12 0.0140(14) 0.042(2) 0.0214(18) -0.0021(16) -0.0006(15) -0.0032(13) C3 0.0330(16) 0.0321(17) 0.0334(18) -0.0001(16) -0.0011(14) -0.0100(14) _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 C2 1.629(5) . y C1 B5 1.685(5) . y C1 B4 1.701(5) . y C1 B6 1.709(5) . y C1 B3 1.720(5) . y C1 H1 0.81(5) . n C2 B11 1.687(5) . y C2 B7 1.694(5) . y C2 B6 1.706(5) . y C2 B3 1.718(5) . y C2 H2 0.91(4) . n B3 B7 1.779(6) . y B3 B4 1.785(6) . y B3 B8 1.793(5) . y B3 H3B 1.07(4) . n B4 B5 1.788(5) . y B4 B8 1.795(6) . y B4 B9 1.800(6) . y B4 H4B 1.11(4) . n B5 B6 1.766(6) . y B5 B9 1.772(6) . y B5 B10 1.783(6) . y B5 H5B 1.07(6) . n B6 B10 1.754(6) . y B6 B11 1.775(6) . y B6 H6B 1.08(3) . n B7 B11 1.785(5) . y B7 B12 1.788(5) . y B7 B8 1.807(5) . y B7 H7B 0.99(4) . n B8 C3 1.527(5) . y B8 B12 1.796(6) . y B8 B9 1.804(6) . y B9 B10 1.775(6) . y B9 B12 1.776(6) . y B9 H9B 1.17(4) . n B10 B11 1.776(5) . y B10 B12 1.787(6) . y B10 H10B 1.08(5) . n B11 B12 1.765(5) . y B11 H11B 0.94(4) . n B12 H12B 0.97(6) . n C3 C3 1.220(7) 2_665 y 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 C1 B5 111.4(3) . . y C2 C1 B4 111.7(3) . . y B5 C1 B4 63.8(2) . . y C2 C1 B6 61.4(2) . . y B5 C1 B6 62.7(2) . . y B4 C1 B6 115.8(3) . . y C2 C1 B3 61.7(2) . . y B5 C1 B3 115.9(3) . . y B4 C1 B3 62.9(2) . . y B6 C1 B3 115.4(3) . . y C2 C1 H1 119(3) . . n B5 C1 H1 120(3) . . n B4 C1 H1 118(3) . . n B6 C1 H1 118(3) . . n B3 C1 H1 115(3) . . n C1 C2 B11 111.9(3) . . y C1 C2 B7 112.0(2) . . y B11 C2 B7 63.7(2) . . y C1 C2 B6 61.6(2) . . y B11 C2 B6 63.1(2) . . y B7 C2 B6 116.2(3) . . y C1 C2 B3 61.7(2) . . y B11 C2 B3 115.8(2) . . y B7 C2 B3 62.8(2) . . y B6 C2 B3 115.5(3) . . y C1 C2 H2 116(3) . . n B11 C2 H2 121(2) . . n B7 C2 H2 122(2) . . n B6 C2 H2 114(2) . . n B3 C2 H2 116(2) . . n C2 B3 C1 56.6(2) . . y C2 B3 B7 57.9(2) . . y C1 B3 B7 103.9(3) . . y C2 B3 B4 103.8(3) . . y C1 B3 B4 58.0(2) . . y B7 B3 B4 108.6(3) . . y C2 B3 B8 104.0(3) . . y C1 B3 B8 104.0(3) . . y B7 B3 B8 60.8(2) . . y B4 B3 B8 60.2(2) . . y C2 B3 H3B 118(2) . . n C1 B3 H3B 121(2) . . n B7 B3 H3B 122(2) . . n B4 B3 H3B 126(2) . . n B8 B3 H3B 130(2) . . n C1 B4 B3 59.1(2) . . y C1 B4 B5 57.7(2) . . y B3 B4 B5 107.7(3) . . y C1 B4 B8 104.7(3) . . y B3 B4 B8 60.1(2) . . y B5 B4 B8 108.0(3) . . y C1 B4 B9 102.8(2) . . y B3 B4 B9 107.5(3) . . y B5 B4 B9 59.2(2) . . y B8 B4 B9 60.2(2) . . y C1 B4 H4B 117(2) . . n B3 B4 H4B 118(2) . . n B5 B4 H4B 119(2) . . n B8 B4 H4B 129(2) . . n B9 B4 H4B 130(2) . . n C1 B5 B6 59.3(2) . . y C1 B5 B9 104.7(3) . . y B6 B5 B9 107.5(3) . . y C1 B5 B10 104.6(3) . . y B6 B5 B10 59.3(2) . . y B9 B5 B10 59.9(2) . . y C1 B5 B4 58.6(2) . . y B6 B5 B4 108.7(3) . . y B9 B5 B4 60.7(2) . . y B10 B5 B4 108.8(3) . . y C1 B5 H5B 121(3) . . n B6 B5 H5B 121(3) . . n B9 B5 H5B 125(3) . . n B10 B5 H5B 126(3) . . n B4 B5 H5B 119(3) . . y C2 B6 C1 57.0(2) . . y C2 B6 B10 104.5(3) . . y C1 B6 B10 104.8(3) . . y C2 B6 B5 104.1(3) . . y C1 B6 B5 58.0(2) . . y B10 B6 B5 60.9(2) . . y C2 B6 B11 57.9(2) . . y C1 B6 B11 104.1(2) . . y B10 B6 B11 60.4(2) . . y B5 B6 B11 108.5(3) . . y C2 B6 H6B 114.1(19) . . n C1 B6 H6B 117(2) . . n B10 B6 H6B 133.7(19) . . n B5 B6 H6B 127(2) . . n B11 B6 H6B 122(2) . . n C2 B7 B3 59.3(2) . . y C2 B7 B11 57.94(19) . . y B3 B7 B11 108.1(2) . . y C2 B7 B12 103.0(2) . . y B3 B7 B12 107.6(3) . . y B11 B7 B12 59.22(19) . . y C2 B7 B8 104.5(3) . . y B3 B7 B8 60.0(2) . . y B11 B7 B8 107.7(2) . . y B12 B7 B8 59.9(2) . . y C2 B7 H7B 123(2) . . n B3 B7 H7B 123(2) . . n B11 B7 H7B 119(2) . . n B12 B7 H7B 123(2) . . n B8 B7 H7B 126(2) . . n C3 B8 B3 121.4(3) . . y C3 B8 B4 119.5(3) . . y B3 B8 B4 59.7(2) . . y C3 B8 B12 124.8(3) . . y B3 B8 B12 106.6(2) . . y B4 B8 B12 107.1(3) . . y C3 B8 B9 121.9(3) . . y B3 B8 B9 107.0(3) . . y B4 B8 B9 60.0(2) . . y B12 B8 B9 59.1(2) . . y C3 B8 B7 124.4(3) . . y B3 B8 B7 59.2(2) . . y B4 B8 B7 106.9(3) . . y B12 B8 B7 59.5(2) . . y B9 B8 B7 106.6(2) . . y B5 B9 B10 60.4(2) . . y B5 B9 B12 108.2(2) . . y B10 B9 B12 60.4(2) . . y B5 B9 B4 60.1(2) . . y B10 B9 B4 108.6(3) . . y B12 B9 B4 107.7(3) . . y B5 B9 B8 108.3(3) . . y B10 B9 B8 109.1(3) . . y B12 B9 B8 60.2(2) . . y B4 B9 B8 59.8(2) . . y B5 B9 H9B 122(2) . . n B10 B9 H9B 115(2) . . n B12 B9 H9B 118(2) . . n B4 B9 H9B 128(2) . . n B8 B9 H9B 124(2) . . n B6 B10 B9 107.9(3) . . y B6 B10 B11 60.4(2) . . y B9 B10 B11 107.5(3) . . y B6 B10 B5 59.9(2) . . y B9 B10 B5 59.7(2) . . y B11 B10 B5 107.7(3) . . y B6 B10 B12 107.7(3) . . y B9 B10 B12 59.8(2) . . y B11 B10 B12 59.4(2) . . y B5 B10 B12 107.2(3) . . y B6 B10 H10B 128(3) . . n B9 B10 H10B 113(3) . . n B11 B10 H10B 129(3) . . n B5 B10 H10B 119(4) . . n B12 B10 H10B 119(3) . . n C2 B11 B12 104.3(2) . . y C2 B11 B6 59.0(2) . . y B12 B11 B6 107.8(3) . . y C2 B11 B10 104.4(3) . . y B12 B11 B10 60.6(2) . . y B6 B11 B10 59.2(2) . . y C2 B11 B7 58.32(18) . . y B12 B11 B7 60.48(19) . . y B6 B11 B7 108.4(2) . . y B10 B11 B7 109.1(2) . . y C2 B11 H11B 118(2) . . n B12 B11 H11B 127(2) . . n B6 B11 H11B 121(2) . . n B10 B11 H11B 129(2) . . n B7 B11 H11B 116(2) . . n B11 B12 B9 107.9(3) . . y B11 B12 B10 60.0(2) . . y B9 B12 B10 59.8(2) . . y B11 B12 B7 60.30(18) . . y B9 B12 B7 108.6(3) . . y B10 B12 B7 108.5(2) . . y B11 B12 B8 109.0(2) . . y B9 B12 B8 60.7(2) . . y B10 B12 B8 108.9(3) . . y B7 B12 B8 60.5(2) . . y B11 B12 H12B 117(3) . . n B9 B12 H12B 125(3) . . n B10 B12 H12B 119(3) . . n B7 B12 H12B 121(3) . . n B8 B12 H12B 126(3) . . n C3 C3 B8 174.2(2) 2_665 . y _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.473 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 961327' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_[B10C2H11]2C6H4_(6) _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(1,2-dicarba-closo-dodecaborane-8-yl)benzene ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [B10 C2 H11]2 (C6 H4) ; _chemical_formula_sum 'C10 H26 B20' _chemical_formula_weight 362.51 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 'P 1 21/c 1' 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 7.1373(5) _cell_length_b 11.1008(8) _cell_length_c 13.1767(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.339(1) _cell_angle_gamma 90.00 _cell_volume 1043.12(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3655 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.09 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method none _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.99 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 7616 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1844 _reflns_number_gt 1400 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0662P)^2^+0.2081P] 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 noref _refine_ls_number_reflns 1844 _refine_ls_number_parameters 188 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1257 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 0.4115(3) 0.41881(16) 0.26789(14) 0.0307(5) Uani 1 1 d . . . H1 H 0.493(3) 0.4638(18) 0.2287(15) 0.042(6) Uiso 1 1 d . . . C2 C 0.2684(3) 0.33032(17) 0.20408(14) 0.0316(5) Uani 1 1 d . . . H2 H 0.280(3) 0.3304(18) 0.1316(17) 0.047(6) Uiso 1 1 d . . . B3 B 0.4521(3) 0.26683(19) 0.27282(16) 0.0294(5) Uani 1 1 d . . . H3B H 0.568(3) 0.2329(18) 0.2319(15) 0.052(6) Uiso 1 1 d . . . B4 B 0.4772(3) 0.35968(19) 0.38194(16) 0.0291(5) Uani 1 1 d . . . H4B H 0.617(3) 0.3786(16) 0.4110(14) 0.038(5) Uiso 1 1 d . . . B5 B 0.3105(3) 0.47899(19) 0.37022(17) 0.0321(5) Uani 1 1 d . . . H5B H 0.349(3) 0.5712(18) 0.3944(14) 0.043(5) Uiso 1 1 d . . . B6 B 0.1812(3) 0.4608(2) 0.25325(17) 0.0325(5) Uani 1 1 d . . . H6B H 0.151(3) 0.5320(19) 0.2001(15) 0.045(5) Uiso 1 1 d . . . B7 B 0.2240(3) 0.2033(2) 0.27006(16) 0.0299(5) Uani 1 1 d . . . H7B H 0.204(3) 0.1203(17) 0.2274(14) 0.038(5) Uiso 1 1 d . . . B8 B 0.3535(3) 0.21968(18) 0.38782(15) 0.0235(5) Uani 1 1 d . . . B9 B 0.2654(3) 0.35236(18) 0.44732(16) 0.0290(5) Uani 1 1 d . . . H9B H 0.269(3) 0.3613(17) 0.5321(15) 0.043(6) Uiso 1 1 d . . . B10 B 0.0827(3) 0.4157(2) 0.36758(17) 0.0335(5) Uani 1 1 d . . . H10B H -0.039(3) 0.4672(18) 0.3957(15) 0.046(6) Uiso 1 1 d . . . B11 B 0.0577(3) 0.3225(2) 0.25786(18) 0.0356(6) Uani 1 1 d . . . H11B H -0.062(3) 0.3117(18) 0.2049(15) 0.047(6) Uiso 1 1 d . . . B12 B 0.1086(3) 0.25616(19) 0.37831(16) 0.0296(5) Uani 1 1 d . . . H12B H 0.004(3) 0.1980(18) 0.4168(14) 0.041(5) Uiso 1 1 d . . . C3 C 0.4310(2) 0.10482(15) 0.44730(12) 0.0221(4) Uani 1 1 d . . . C4 C 0.6091(2) 0.10231(16) 0.49542(13) 0.0259(4) Uani 1 1 d . . . H4 H 0.689(2) 0.1765(16) 0.4948(13) 0.027(5) Uiso 1 1 d . . . C5 C 0.6757(2) 0.00010(16) 0.54642(13) 0.0263(4) Uani 1 1 d . . . H5 H 0.802(3) 0.0020(16) 0.5774(13) 0.032(5) 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 C1 0.0361(10) 0.0260(11) 0.0305(11) 0.0045(8) 0.0091(8) -0.0020(8) C2 0.0448(11) 0.0306(11) 0.0197(10) 0.0020(8) 0.0047(8) 0.0015(8) B3 0.0340(11) 0.0264(11) 0.0286(12) 0.0038(9) 0.0110(9) 0.0033(9) B4 0.0331(11) 0.0235(11) 0.0307(12) 0.0031(9) 0.0009(9) -0.0024(9) B5 0.0465(13) 0.0213(11) 0.0287(12) 0.0017(9) 0.0040(10) 0.0038(10) B6 0.0386(12) 0.0274(12) 0.0316(12) 0.0038(10) 0.0043(10) 0.0081(10) B7 0.0365(12) 0.0260(12) 0.0272(11) 0.0000(9) 0.0005(9) -0.0019(9) B8 0.0262(10) 0.0225(11) 0.0220(10) -0.0005(8) 0.0046(8) -0.0007(8) B9 0.0410(12) 0.0224(11) 0.0240(12) 0.0015(9) 0.0074(9) 0.0041(9) B10 0.0350(11) 0.0333(12) 0.0329(12) 0.0067(10) 0.0102(9) 0.0102(10) B11 0.0320(12) 0.0375(13) 0.0367(13) 0.0081(10) -0.0047(10) 0.0009(10) B12 0.0259(10) 0.0309(12) 0.0326(12) 0.0064(10) 0.0066(9) 0.0008(9) C3 0.0255(9) 0.0222(9) 0.0191(9) -0.0016(7) 0.0072(7) 0.0003(7) C4 0.0270(9) 0.0218(9) 0.0293(10) -0.0003(8) 0.0051(7) -0.0037(8) C5 0.0237(9) 0.0253(10) 0.0299(10) 0.0015(8) 0.0019(7) 0.0000(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 C1 C2 1.626(3) . y C1 B4 1.689(3) . y C1 B5 1.692(3) . y C1 B6 1.712(3) . y C1 B3 1.712(3) . y C1 H1 0.93(2) . n C2 B11 1.691(3) . y C2 B7 1.694(3) . y C2 B3 1.714(3) . y C2 B6 1.714(3) . y C2 H2 0.96(2) . n B3 B4 1.772(3) . y B3 B7 1.773(3) . y B3 B8 1.776(3) . y B3 H3B 1.07(2) . n B4 B9 1.772(3) . y B4 B5 1.783(3) . y B4 B8 1.791(3) . y B4 H4B 1.073(18) . n B5 B10 1.770(3) . y B5 B9 1.772(3) . y B5 B6 1.775(3) . y B5 H5B 1.103(19) . n B6 B10 1.761(3) . y B6 B11 1.773(3) . y B6 H6B 1.07(2) . n B7 B12 1.776(3) . y B7 B11 1.781(3) . y B7 B8 1.783(3) . y B7 H7B 1.085(19) . n B8 C3 1.584(3) . y B8 B12 1.794(3) . y B8 B9 1.794(3) . y B9 B12 1.771(3) . y B9 B10 1.786(3) . y B9 H9B 1.12(2) . n B10 B11 1.781(3) . y B10 B12 1.786(3) . y B10 H10B 1.12(2) . n B11 B12 1.774(3) . y B11 H11B 1.088(19) . n B12 H12B 1.126(19) . n C3 C5 1.396(2) 3_656 y C3 C4 1.397(2) . y C4 C5 1.392(2) . y C4 H4 1.002(18) . n C5 C3 1.396(2) 3_656 y C5 H5 0.974(19) . n 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 C1 B4 111.78(15) . . y C2 C1 B5 111.79(15) . . y B4 C1 B5 63.66(12) . . y C2 C1 B6 61.74(12) . . y B4 C1 B6 115.89(15) . . y B5 C1 B6 62.86(12) . . y C2 C1 B3 61.72(12) . . y B4 C1 B3 62.80(12) . . y B5 C1 B3 115.82(14) . . y B6 C1 B3 115.64(15) . . y C2 C1 H1 115.2(12) . . n B4 C1 H1 122.9(12) . . n B5 C1 H1 121.5(12) . . n B6 C1 H1 113.9(12) . . n B3 C1 H1 116.1(12) . . n C1 C2 B11 111.40(15) . . y C1 C2 B7 111.36(15) . . y B11 C2 B7 63.50(12) . . y C1 C2 B3 61.61(12) . . y B11 C2 B3 115.57(15) . . y B7 C2 B3 62.70(12) . . y C1 C2 B6 61.59(12) . . y B11 C2 B6 62.74(13) . . y B7 C2 B6 115.55(15) . . y B3 C2 B6 115.43(15) . . y C1 C2 H2 115.9(12) . . n B11 C2 H2 121.9(12) . . n B7 C2 H2 122.4(12) . . n B3 C2 H2 115.6(12) . . n B6 C2 H2 114.9(12) . . n C1 B3 C2 56.67(11) . . y C1 B3 B4 57.94(11) . . y C2 B3 B4 103.86(14) . . y C1 B3 B7 103.75(14) . . y C2 B3 B7 58.08(12) . . y B4 B3 B7 108.09(15) . . y C1 B3 B8 104.51(14) . . y C2 B3 B8 104.54(14) . . y B4 B3 B8 60.63(11) . . y B7 B3 B8 60.31(11) . . y C1 B3 H3B 117.4(11) . . n C2 B3 H3B 117.7(11) . . n B4 B3 H3B 124.0(11) . . n B7 B3 H3B 125.0(11) . . n B8 B3 H3B 131.8(11) . . n C1 B4 B3 59.26(11) . . y C1 B4 B9 103.83(15) . . y B3 B4 B9 107.91(15) . . y C1 B4 B5 58.27(12) . . y B3 B4 B5 108.46(15) . . y B9 B4 B5 59.77(12) . . y C1 B4 B8 104.85(14) . . y B3 B4 B8 59.77(11) . . y B9 B4 B8 60.47(11) . . y B5 B4 B8 108.64(15) . . y C1 B4 H4B 117.5(10) . . n B3 B4 H4B 117.7(10) . . n B9 B4 H4B 129.3(10) . . n B5 B4 H4B 119.5(10) . . n B8 B4 H4B 127.3(10) . . n C1 B5 B10 104.40(15) . . y C1 B5 B9 103.70(14) . . y B10 B5 B9 60.55(12) . . y C1 B5 B6 59.12(12) . . y B10 B5 B6 59.57(13) . . y B9 B5 B6 107.92(16) . . y C1 B5 B4 58.07(11) . . y B10 B5 B4 108.44(15) . . y B9 B5 B4 59.81(12) . . y B6 B5 B4 108.19(15) . . y C1 B5 H5B 119.2(10) . . n B10 B5 H5B 126.2(10) . . n B9 B5 H5B 128.3(10) . . n B6 B5 H5B 118.0(10) . . n B4 B5 H5B 120.5(10) . . n C1 B6 C2 56.67(11) . . y C1 B6 B10 103.96(15) . . y C2 B6 B10 104.29(15) . . y C1 B6 B11 103.68(15) . . y C2 B6 B11 57.98(12) . . y B10 B6 B11 60.52(13) . . y C1 B6 B5 58.03(12) . . y C2 B6 B5 103.90(14) . . y B10 B6 B5 60.07(13) . . y B11 B6 B5 108.07(15) . . y C1 B6 H6B 116.2(11) . . n C2 B6 H6B 116.3(11) . . n B10 B6 H6B 133.7(11) . . n B11 B6 H6B 125.0(11) . . n B5 B6 H6B 124.6(11) . . n C2 B7 B3 59.22(12) . . y C2 B7 B12 103.87(15) . . y B3 B7 B12 107.92(15) . . y C2 B7 B11 58.17(12) . . y B3 B7 B11 108.30(15) . . y B12 B7 B11 59.83(12) . . y C2 B7 B8 105.11(15) . . y B3 B7 B8 59.91(11) . . y B12 B7 B8 60.54(12) . . y B11 B7 B8 108.82(15) . . y C2 B7 H7B 117.6(10) . . n B3 B7 H7B 116.5(10) . . n B12 B7 H7B 130.0(10) . . n B11 B7 H7B 120.9(10) . . n B8 B7 H7B 126.1(10) . . n C3 B8 B3 121.12(14) . . y C3 B8 B7 120.42(15) . . y B3 B8 B7 59.78(12) . . y C3 B8 B4 123.85(15) . . y B3 B8 B4 59.59(11) . . y B7 B8 B4 106.86(14) . . y C3 B8 B12 122.39(14) . . y B3 B8 B12 107.03(14) . . y B7 B8 B12 59.55(11) . . y B4 B8 B12 106.38(14) . . y C3 B8 B9 124.46(15) . . y B3 B8 B9 106.80(14) . . y B7 B8 B9 106.61(14) . . y B4 B8 B9 59.25(11) . . y B12 B8 B9 59.17(12) . . y B12 B9 B5 108.04(15) . . y B12 B9 B4 108.18(15) . . y B5 B9 B4 60.42(12) . . y B12 B9 B10 60.27(12) . . y B5 B9 B10 59.69(12) . . y B4 B9 B10 108.24(15) . . y B12 B9 B8 60.40(11) . . y B5 B9 B8 109.01(15) . . y B4 B9 B8 60.28(11) . . y B10 B9 B8 109.07(15) . . y B12 B9 H9B 123.6(10) . . n B5 B9 H9B 120.3(10) . . n B4 B9 H9B 119.7(10) . . n B10 B9 H9B 122.5(10) . . n B8 B9 H9B 121.0(10) . . n B6 B10 B5 60.36(12) . . y B6 B10 B11 60.06(13) . . y B5 B10 B11 107.93(15) . . y B6 B10 B9 107.93(15) . . y B5 B10 B9 59.76(12) . . y B11 B10 B9 107.18(15) . . y B6 B10 B12 107.83(15) . . y B5 B10 B12 107.46(14) . . y B11 B10 B12 59.65(12) . . y B9 B10 B12 59.47(12) . . y B6 B10 H10B 118.8(10) . . n B5 B10 H10B 121.2(10) . . n B11 B10 H10B 120.9(10) . . n B9 B10 H10B 124.5(10) . . n B12 B10 H10B 124.1(10) . . n C2 B11 B6 59.29(12) . . y C2 B11 B12 104.09(15) . . y B6 B11 B12 107.85(16) . . y C2 B11 B10 104.44(15) . . y B6 B11 B10 59.42(12) . . y B12 B11 B10 60.32(12) . . y C2 B11 B7 58.33(12) . . y B6 B11 B7 108.45(15) . . y B12 B11 B7 59.95(12) . . y B10 B11 B7 108.32(15) . . y C2 B11 H11B 115.2(10) . . n B6 B11 H11B 116.9(11) . . n B12 B11 H11B 130.9(11) . . n B10 B11 H11B 129.5(11) . . n B7 B11 H11B 118.6(11) . . n B9 B12 B11 108.11(15) . . y B9 B12 B7 107.90(15) . . y B11 B12 B7 60.22(12) . . y B9 B12 B10 60.26(12) . . y B11 B12 B10 60.03(13) . . y B7 B12 B10 108.31(14) . . y B9 B12 B8 60.43(11) . . y B11 B12 B8 108.63(14) . . y B7 B12 B8 59.91(11) . . y B10 B12 B8 109.07(14) . . y B9 B12 H12B 122.2(10) . . n B11 B12 H12B 121.7(10) . . n B7 B12 H12B 120.8(10) . . n B10 B12 H12B 122.4(10) . . n B8 B12 H12B 120.2(10) . . n C5 C3 C4 116.39(16) 3_656 . y C5 C3 B8 121.39(15) 3_656 . y C4 C3 B8 122.22(15) . . y C5 C4 C3 121.44(16) . . y C5 C4 H4 119.4(10) . . n C3 C4 H4 119.1(10) . . n C4 C5 C3 122.17(16) . 3_656 y C4 C5 H5 118.4(11) . . n C3 C5 H5 119.4(11) 3_656 . n _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.205 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.036 _database_code_depnum_ccdc_archive 'CCDC 961328' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_{[B10C2H11]C2}2C6H4_(9) _chemical_name_systematic ; 1,4-bis(1,2-dicarba-closo-dodecaborane(11)-8yl-ethynyl)benzene, chloroform solvate ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; {[B10 C2 H11] C2}2 C6 H4, C H Cl3 ; _chemical_formula_sum 'C15 H27 B20 Cl3' _chemical_formula_weight 529.92 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 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 23.4549(9) _cell_length_b 11.1387(4) _cell_length_c 23.2584(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.488(2) _cell_angle_gamma 90.00 _cell_volume 5654.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9820 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 23.70 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method none _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 0.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.95 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 51767 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0552 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.91 _reflns_number_total 15629 _reflns_number_gt 8798 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0845P)^2^+0.9854P] 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 noref _refine_ls_number_reflns 15629 _refine_ls_number_parameters 930 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1176 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1481 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.01499(12) -0.4065(2) 0.83496(15) 0.0609(8) Uani 1 1 d . . . H1C H 0.0150(13) -0.498(3) 0.8332(14) 0.095(10) Uiso 1 1 d . . . C2 C -0.03681(13) -0.3341(3) 0.77887(14) 0.0764(10) Uani 1 1 d . . . H2C H -0.0655(14) -0.385(3) 0.7470(14) 0.098(11) Uiso 1 1 d . . . B3 B 0.03757(14) -0.3345(3) 0.78165(16) 0.0629(9) Uani 1 1 d . . . H3B H 0.0493(12) -0.388(3) 0.7511(13) 0.090(9) Uiso 1 1 d . . . B4 B 0.08259(12) -0.3321(3) 0.86094(14) 0.0515(7) Uani 1 1 d . . . H4B H 0.1243(11) -0.386(2) 0.8781(11) 0.066(7) Uiso 1 1 d . . . B5 B 0.03154(12) -0.3343(3) 0.90112(14) 0.0508(7) Uani 1 1 d . . . H5B H 0.0432(11) -0.393(2) 0.9436(12) 0.076(8) Uiso 1 1 d . . . B6 B -0.04471(12) -0.3386(3) 0.84781(14) 0.0524(7) Uani 1 1 d . . . H6B H -0.0791(11) -0.398(2) 0.8510(12) 0.076(8) Uiso 1 1 d . . . B7 B -0.00767(12) -0.1995(3) 0.76434(14) 0.0623(9) Uani 1 1 d . . . H7B H -0.0245(12) -0.165(3) 0.7177(13) 0.086(9) Uiso 1 1 d . . . B8 B 0.06921(10) -0.1988(2) 0.81623(11) 0.0391(6) Uani 1 1 d . . . B9 B 0.06607(12) -0.1998(3) 0.89198(13) 0.0468(6) Uani 1 1 d . . . H9B H 0.1006(10) -0.160(2) 0.9324(11) 0.058(7) Uiso 1 1 d . . . B10 B -0.01166(12) -0.2047(3) 0.88546(14) 0.0498(7) Uani 1 1 d . . . H10B H -0.0278(12) -0.163(2) 0.9223(12) 0.080(8) Uiso 1 1 d . . . B11 B -0.05708(13) -0.2031(3) 0.80681(16) 0.0659(10) Uani 1 1 d . . . H11B H -0.0995(12) -0.167(2) 0.7934(12) 0.077(8) Uiso 1 1 d . . . B12 B 0.01185(13) -0.1177(3) 0.83375(14) 0.0509(7) Uani 1 1 d . . . H12B H 0.0125(13) -0.014(3) 0.8324(14) 0.103(10) Uiso 1 1 d . . . C3 C 0.12044(10) -0.1374(2) 0.80003(10) 0.0449(5) Uani 1 1 d . . . C4 C 0.15946(9) -0.0920(2) 0.78529(10) 0.0430(5) Uani 1 1 d . . . C5 C 0.20674(8) -0.0417(2) 0.76636(9) 0.0367(5) Uani 1 1 d . . . C6 C 0.23502(10) -0.1130(2) 0.73530(11) 0.0465(6) Uani 1 1 d . . . H6A H 0.2228 -0.1944 0.7264 0.056 Uiso 1 1 calc R . . C7 C 0.28079(9) -0.0666(2) 0.71723(10) 0.0417(5) Uani 1 1 d . . . H7A H 0.2996 -0.1163 0.6960 0.050 Uiso 1 1 calc R . . C8 C 0.29928(8) 0.05194(18) 0.73008(8) 0.0309(4) Uani 1 1 d . . . C9 C 0.27067(10) 0.1228(2) 0.76070(10) 0.0420(5) Uani 1 1 d . . . H9A H 0.2827 0.2043 0.7695 0.050 Uiso 1 1 calc R . . C10 C 0.22506(10) 0.0767(2) 0.77860(10) 0.0437(5) Uani 1 1 d . . . H10A H 0.2061 0.1267 0.7995 0.052 Uiso 1 1 calc R . . C13 C 0.38703(9) 0.14775(18) 0.69883(8) 0.0332(4) Uani 1 1 d . . . C14 C 0.34721(8) 0.10207(18) 0.71221(8) 0.0326(4) Uani 1 1 d . . . C11 C 0.49200(10) 0.4226(2) 0.66839(10) 0.0392(5) Uani 1 1 d . . . H11C H 0.4930(10) 0.505(2) 0.6728(10) 0.050(7) Uiso 1 1 d . . . C12 C 0.54411(10) 0.3439(2) 0.72035(10) 0.0406(5) Uani 1 1 d . . . H12C H 0.5741(10) 0.392(2) 0.7523(11) 0.051(7) Uiso 1 1 d . . . B13 B 0.47106(12) 0.3447(2) 0.72113(11) 0.0391(6) Uani 1 1 d . . . H13B H 0.4633(10) 0.399(2) 0.7574(11) 0.058(7) Uiso 1 1 d . . . B14 B 0.42355(11) 0.3504(2) 0.64207(11) 0.0356(5) Uani 1 1 d . . . H14B H 0.3837(10) 0.405(2) 0.6290(10) 0.048(6) Uiso 1 1 d . . . B15 B 0.47145(10) 0.3592(2) 0.59789(11) 0.0351(5) Uani 1 1 d . . . H15B H 0.4604(9) 0.423(2) 0.5577(10) 0.052(6) Uiso 1 1 d . . . B16 B 0.54905(11) 0.3586(2) 0.64915(11) 0.0351(5) Uani 1 1 d . . . H16B H 0.5839(9) 0.419(2) 0.6449(10) 0.049(6) Uiso 1 1 d . . . B17 B 0.51583(11) 0.2109(2) 0.73358(11) 0.0383(6) Uani 1 1 d . . . H17B H 0.5354(9) 0.173(2) 0.7807(10) 0.048(6) Uiso 1 1 d . . . B18 B 0.43778(10) 0.2112(2) 0.68265(10) 0.0283(5) Uani 1 1 d . . . B19 B 0.43765(10) 0.2203(2) 0.60557(10) 0.0308(5) Uani 1 1 d . . . H19B H 0.4015(8) 0.1849(17) 0.5659(9) 0.029(5) Uiso 1 1 d . . . B20 B 0.51501(10) 0.2262(2) 0.60970(10) 0.0314(5) Uani 1 1 d . . . H20B H 0.5299(9) 0.1893(19) 0.5715(10) 0.047(6) Uiso 1 1 d . . . B21 B 0.56325(11) 0.2195(2) 0.68892(12) 0.0385(6) Uani 1 1 d . . . H21B H 0.6081(9) 0.1874(19) 0.7038(9) 0.043(6) Uiso 1 1 d . . . B22 B 0.49426(10) 0.1340(2) 0.66149(11) 0.0326(5) Uani 1 1 d . . . H22B H 0.4953(10) 0.034(2) 0.6593(11) 0.058(7) Uiso 1 1 d . . . C21 C 0.23132(10) 0.2620(2) 0.57286(10) 0.0410(5) Uani 1 1 d . . . H21C H 0.2650(11) 0.284(2) 0.6116(11) 0.062(7) Uiso 1 1 d . . . C22 C 0.19886(14) 0.3705(2) 0.52668(12) 0.0551(7) Uani 1 1 d . . . H22C H 0.2130(12) 0.442(3) 0.5406(12) 0.075(9) Uiso 1 1 d . . . B23 B 0.24704(13) 0.2786(3) 0.50705(13) 0.0498(7) Uani 1 1 d . . . H23B H 0.2936(10) 0.312(2) 0.5122(10) 0.063(7) Uiso 1 1 d . . . B24 B 0.23443(10) 0.1363(2) 0.53386(11) 0.0358(5) Uani 1 1 d . . . H24B H 0.2751(10) 0.077(2) 0.5545(10) 0.061(7) Uiso 1 1 d . . . B25 B 0.18092(10) 0.1525(2) 0.57080(11) 0.0343(5) Uani 1 1 d . . . H25B H 0.1881(10) 0.105(2) 0.6125(11) 0.055(7) Uiso 1 1 d . . . B26 B 0.15918(11) 0.3062(2) 0.56716(11) 0.0407(6) Uani 1 1 d . . . H26B H 0.1577(10) 0.355(2) 0.6069(10) 0.052(6) Uiso 1 1 d . . . B27 B 0.17650(17) 0.3291(2) 0.45148(14) 0.0575(8) Uani 1 1 d . . . H27B H 0.1798(11) 0.397(2) 0.4184(12) 0.079(8) Uiso 1 1 d . . . B28 B 0.19735(10) 0.1757(2) 0.45392(10) 0.0322(5) Uani 1 1 d . . . B29 B 0.15678(10) 0.0974(2) 0.49406(10) 0.0314(5) Uani 1 1 d . . . H29B H 0.1430(10) 0.007(2) 0.4831(10) 0.054(7) Uiso 1 1 d . . . B30 B 0.11075(10) 0.2015(3) 0.51549(11) 0.0406(6) Uani 1 1 d . . . H30B H 0.0688(10) 0.176(2) 0.5195(10) 0.055(7) Uiso 1 1 d . . . B31 B 0.12284(16) 0.3445(3) 0.48884(13) 0.0587(8) Uani 1 1 d . . . H31B H 0.0939(12) 0.416(3) 0.4796(12) 0.084(9) Uiso 1 1 d . . . B32 B 0.12039(11) 0.2158(3) 0.44326(11) 0.0431(6) Uani 1 1 d . . . H32B H 0.0826(10) 0.207(2) 0.3980(11) 0.061(7) Uiso 1 1 d . . . C23 C 0.21459(9) 0.11946(18) 0.40190(9) 0.0355(5) Uani 1 1 d . . . C24 C 0.22578(9) 0.08060(18) 0.35908(9) 0.0330(4) Uani 1 1 d . . . C25 C 0.23902(8) 0.03712(16) 0.30677(8) 0.0279(4) Uani 1 1 d . . . C26 C 0.19503(9) -0.02367(19) 0.25862(9) 0.0362(5) Uani 1 1 d . . . H26A H 0.1559 -0.0386 0.2605 0.043 Uiso 1 1 calc R . . C27 C 0.20757(8) -0.06275(19) 0.20801(9) 0.0352(5) Uani 1 1 d . . . H27A H 0.1769 -0.1040 0.1754 0.042 Uiso 1 1 calc R . . C28 C 0.26487(8) -0.04199(16) 0.20445(8) 0.0274(4) Uani 1 1 d . . . C29 C 0.30880(8) 0.01940(18) 0.25231(9) 0.0330(4) Uani 1 1 d . . . H29A H 0.3479 0.0348 0.2503 0.040 Uiso 1 1 calc R . . C30 C 0.29621(8) 0.05849(18) 0.30302(9) 0.0332(4) Uani 1 1 d . . . H30A H 0.3268 0.1002 0.3355 0.040 Uiso 1 1 calc R . . C33 C 0.28995(9) -0.12803(18) 0.11038(9) 0.0336(5) Uani 1 1 d . . . C34 C 0.27850(8) -0.08733(17) 0.15249(9) 0.0320(4) Uani 1 1 d . . . C31 C 0.31717(10) -0.3760(2) -0.01095(11) 0.0426(5) Uani 1 1 d . . . H31C H 0.3068(11) -0.461(2) -0.0234(11) 0.065(7) Uiso 1 1 d . . . C32 C 0.27181(10) -0.2804(2) -0.05912(11) 0.0439(6) Uani 1 1 d . . . H32C H 0.2405(11) -0.315(2) -0.0933(11) 0.058(7) Uiso 1 1 d . . . B33 B 0.26463(12) -0.3013(2) 0.01092(13) 0.0464(7) Uani 1 1 d . . . H33B H 0.2267(11) -0.350(2) 0.0111(11) 0.064(7) Uiso 1 1 d . . . B34 B 0.34148(12) -0.3253(2) 0.06302(12) 0.0407(6) Uani 1 1 d . . . H34B H 0.3506(10) -0.390(2) 0.1018(10) 0.061(7) Uiso 1 1 d . . . B35 B 0.39007(11) -0.3235(2) 0.01944(11) 0.0358(5) Uani 1 1 d . . . H35B H 0.4276(9) -0.3841(19) 0.0293(9) 0.043(6) Uiso 1 1 d . . . B36 B 0.34394(10) -0.2994(2) -0.05935(11) 0.0365(5) Uani 1 1 d . . . H36B H 0.3467(9) -0.3464(19) -0.0996(10) 0.049(6) Uiso 1 1 d . . . B37 B 0.26086(10) -0.1568(2) -0.02230(12) 0.0411(6) Uani 1 1 d . . . H37B H 0.2174(11) -0.116(2) -0.0391(11) 0.063(7) Uiso 1 1 d . . . B38 B 0.30659(10) -0.1814(2) 0.05729(10) 0.0300(5) Uani 1 1 d . . . B39 B 0.38407(9) -0.1949(2) 0.06162(10) 0.0297(5) Uani 1 1 d . . . H39B H 0.4234(9) -0.1659(19) 0.1039(10) 0.045(6) Uiso 1 1 d . . . B40 B 0.38585(10) -0.1795(2) -0.01375(10) 0.0327(5) Uani 1 1 d . . . H40B H 0.4230(9) -0.1426(18) -0.0234(9) 0.042(6) Uiso 1 1 d . . . B41 B 0.30987(12) -0.1554(2) -0.06547(11) 0.0405(6) Uani 1 1 d . . . H41B H 0.2949(9) -0.1106(19) -0.1095(10) 0.046(6) Uiso 1 1 d . . . B42 B 0.33451(10) -0.0915(2) 0.00938(10) 0.0295(5) Uani 1 1 d . . . H42B H 0.3391(9) -0.001(2) 0.0163(9) 0.044(6) Uiso 1 1 d . . . C15 C 0.06659(10) -0.2509(2) 0.57293(11) 0.0496(6) Uani 1 1 d D A 1 H15A H 0.0329 -0.2086 0.5395 0.059 Uiso 1 1 calc R A 1 Cl1 Cl 0.06871(7) -0.2016(2) 0.64738(7) 0.0665(6) Uani 0.609(3) 1 d PD A 1 Cl2 Cl 0.13861(10) -0.2086(3) 0.57044(11) 0.0913(11) Uani 0.609(3) 1 d PD A 1 Cl3 Cl 0.05504(10) -0.40415(12) 0.56569(9) 0.0738(5) Uani 0.609(3) 1 d PD A 1 Cl1X Cl 0.0631(3) -0.1407(8) 0.6156(5) 0.077(2) Uiso 0.134(3) 1 d PD B 2 Cl2X Cl 0.1405(3) -0.2471(8) 0.5683(3) 0.0201(12) Uiso 0.134(3) 1 d PD B 2 Cl3X Cl 0.0458(3) -0.3888(6) 0.5901(4) 0.0450(16) Uiso 0.134(3) 1 d PD B 2 Cl1Y Cl 0.0598(4) -0.2492(7) 0.6460(4) 0.0431(19) Uiso 0.110(2) 1 d PD C 3 Cl2Y Cl 0.0972(4) -0.1342(7) 0.5533(4) 0.075(3) Uiso 0.110(2) 1 d PD C 3 Cl3Y Cl 0.0811(3) -0.3877(6) 0.5571(3) 0.055(2) Uiso 0.110(2) 1 d PD C 3 Cl1Z Cl 0.0569(3) -0.1034(6) 0.5860(4) 0.078(2) Uiso 0.147(3) 1 d P D 4 Cl2Z Cl 0.13688(18) -0.2897(6) 0.5612(2) 0.0353(12) Uiso 0.147(3) 1 d P D 4 Cl3Z Cl 0.0494(3) -0.3533(7) 0.6131(4) 0.0745(19) Uiso 0.147(3) 1 d P D 4 C16 C 0.43436(9) 0.25370(19) 0.92770(9) 0.0359(5) Uani 1 1 d D E 1 H16 H 0.4724 0.2173 0.9581 0.043 Uiso 1 1 calc R E 1 Cl4 Cl 0.4372(2) 0.2375(6) 0.8528(2) 0.0416(10) Uani 0.480(4) 1 d PD E 1 Cl5 Cl 0.4326(3) 0.4065(4) 0.9472(2) 0.0432(9) Uani 0.480(4) 1 d PD E 1 Cl6 Cl 0.3725(3) 0.1720(7) 0.9298(3) 0.0795(17) Uani 0.480(4) 1 d PD E 1 Cl4X Cl 0.4398(3) 0.2305(6) 0.8561(2) 0.0706(16) Uani 0.520(4) 1 d PD F 2 Cl5X Cl 0.4364(3) 0.4063(5) 0.9429(2) 0.0670(14) Uani 0.520(4) 1 d PD F 2 Cl6X Cl 0.36591(17) 0.1923(6) 0.92962(17) 0.0541(9) Uani 0.520(4) 1 d PD F 2 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 0.0591(16) 0.0433(15) 0.101(2) -0.0046(15) 0.0535(16) -0.0089(13) C2 0.0562(16) 0.119(3) 0.0617(18) -0.0298(18) 0.0309(15) -0.0523(18) B3 0.0626(18) 0.068(2) 0.080(2) -0.0318(17) 0.0522(18) -0.0335(16) B4 0.0383(13) 0.0505(17) 0.075(2) 0.0134(15) 0.0314(14) 0.0069(13) B5 0.0411(14) 0.0542(18) 0.0648(19) 0.0151(15) 0.0286(14) 0.0045(13) B6 0.0393(14) 0.0590(19) 0.0690(19) 0.0003(15) 0.0319(14) -0.0073(13) B7 0.0356(14) 0.106(3) 0.0399(16) 0.0189(17) 0.0071(12) -0.0134(16) B8 0.0336(12) 0.0461(15) 0.0414(14) 0.0057(11) 0.0182(11) -0.0039(11) B9 0.0441(14) 0.0571(18) 0.0429(15) 0.0045(13) 0.0204(12) -0.0098(13) B10 0.0524(15) 0.0494(17) 0.0620(18) 0.0068(14) 0.0380(14) 0.0025(13) B11 0.0323(13) 0.095(3) 0.072(2) 0.0318(19) 0.0218(14) 0.0123(16) B12 0.0547(16) 0.0461(17) 0.0621(18) 0.0142(14) 0.0335(14) 0.0076(13) C3 0.0407(12) 0.0534(15) 0.0435(13) 0.0032(11) 0.0186(10) -0.0086(11) C4 0.0371(11) 0.0539(15) 0.0380(12) 0.0027(10) 0.0135(9) -0.0122(10) C5 0.0305(10) 0.0484(13) 0.0302(11) 0.0043(9) 0.0100(8) -0.0094(9) C6 0.0462(12) 0.0380(13) 0.0606(15) -0.0052(11) 0.0259(11) -0.0154(10) C7 0.0407(11) 0.0414(13) 0.0497(13) -0.0062(10) 0.0244(10) -0.0086(10) C8 0.0275(9) 0.0398(12) 0.0239(9) 0.0022(8) 0.0076(8) -0.0068(8) C9 0.0460(12) 0.0393(13) 0.0473(13) -0.0082(10) 0.0250(11) -0.0144(10) C10 0.0427(12) 0.0501(14) 0.0458(13) -0.0080(11) 0.0252(10) -0.0119(10) C13 0.0379(10) 0.0377(12) 0.0258(10) -0.0020(8) 0.0139(8) -0.0076(9) C14 0.0338(10) 0.0386(12) 0.0251(10) -0.0027(8) 0.0104(8) -0.0083(9) C11 0.0538(13) 0.0248(11) 0.0511(14) -0.0026(10) 0.0334(11) -0.0039(10) C12 0.0385(11) 0.0504(14) 0.0323(11) -0.0049(10) 0.0124(9) -0.0175(10) B13 0.0511(14) 0.0402(14) 0.0349(13) -0.0088(11) 0.0263(12) -0.0160(11) B14 0.0359(12) 0.0331(13) 0.0455(14) 0.0068(11) 0.0239(11) 0.0070(10) B15 0.0358(12) 0.0385(14) 0.0366(13) 0.0101(10) 0.0199(10) 0.0053(10) B16 0.0378(12) 0.0355(13) 0.0370(13) 0.0036(10) 0.0195(10) -0.0035(10) B17 0.0361(12) 0.0484(16) 0.0283(12) 0.0073(11) 0.0092(10) -0.0080(11) B18 0.0326(11) 0.0303(12) 0.0239(11) -0.0006(9) 0.0125(9) -0.0028(9) B19 0.0303(11) 0.0410(14) 0.0229(11) 0.0016(9) 0.0117(9) -0.0017(10) B20 0.0331(11) 0.0339(13) 0.0328(12) -0.0007(10) 0.0188(10) -0.0014(10) B21 0.0297(11) 0.0435(15) 0.0413(14) 0.0113(11) 0.0118(10) 0.0031(11) B22 0.0381(12) 0.0269(12) 0.0357(12) 0.0025(10) 0.0168(10) 0.0003(10) C21 0.0352(11) 0.0525(15) 0.0383(12) -0.0200(10) 0.0171(10) -0.0111(10) C22 0.093(2) 0.0315(13) 0.0585(16) -0.0174(12) 0.0491(15) -0.0156(14) B23 0.0564(16) 0.0544(18) 0.0539(17) -0.0252(14) 0.0382(14) -0.0249(14) B24 0.0285(11) 0.0447(15) 0.0338(12) -0.0131(11) 0.0110(10) 0.0015(10) B25 0.0347(12) 0.0417(14) 0.0278(12) -0.0052(10) 0.0130(10) -0.0012(10) B26 0.0450(13) 0.0453(15) 0.0371(14) -0.0116(11) 0.0214(11) 0.0041(12) B27 0.110(3) 0.0315(15) 0.0489(17) 0.0004(12) 0.0500(18) 0.0055(15) B28 0.0375(12) 0.0319(13) 0.0327(12) -0.0072(10) 0.0193(10) -0.0049(10) B29 0.0308(11) 0.0350(13) 0.0306(12) -0.0092(10) 0.0140(9) -0.0060(10) B30 0.0270(11) 0.0607(17) 0.0360(13) -0.0097(12) 0.0139(10) 0.0025(11) B31 0.084(2) 0.0542(19) 0.0418(16) 0.0042(13) 0.0280(16) 0.0376(17) B32 0.0409(13) 0.0562(17) 0.0286(13) -0.0043(11) 0.0085(11) 0.0166(12) C23 0.0421(11) 0.0334(11) 0.0378(11) -0.0070(9) 0.0227(9) -0.0048(9) C24 0.0375(10) 0.0316(11) 0.0348(11) -0.0018(8) 0.0192(9) -0.0011(9) C25 0.0358(10) 0.0246(10) 0.0274(10) -0.0003(8) 0.0163(8) 0.0036(8) C26 0.0319(10) 0.0435(13) 0.0396(12) -0.0104(9) 0.0206(9) -0.0050(9) C27 0.0308(10) 0.0424(12) 0.0339(11) -0.0111(9) 0.0136(8) -0.0044(9) C28 0.0333(9) 0.0235(10) 0.0291(10) -0.0009(8) 0.0157(8) 0.0040(8) C29 0.0300(9) 0.0367(12) 0.0376(11) -0.0037(9) 0.0185(9) -0.0023(9) C30 0.0338(10) 0.0349(12) 0.0317(10) -0.0058(8) 0.0130(8) -0.0038(9) C33 0.0390(10) 0.0293(11) 0.0411(12) -0.0053(9) 0.0249(9) -0.0022(9) C34 0.0354(10) 0.0298(11) 0.0366(11) -0.0019(8) 0.0200(9) 0.0002(8) C31 0.0548(13) 0.0297(12) 0.0570(14) -0.0169(10) 0.0368(12) -0.0114(10) C32 0.0324(11) 0.0556(15) 0.0441(13) -0.0272(11) 0.0144(10) -0.0073(10) B33 0.0438(14) 0.0446(15) 0.0664(18) -0.0263(13) 0.0385(14) -0.0193(12) B34 0.0613(16) 0.0289(13) 0.0442(15) 0.0013(11) 0.0339(13) 0.0032(12) B35 0.0406(12) 0.0328(13) 0.0398(13) -0.0055(10) 0.0216(11) 0.0063(11) B36 0.0351(12) 0.0432(14) 0.0370(13) -0.0124(11) 0.0200(10) -0.0022(11) B37 0.0275(11) 0.0505(17) 0.0404(14) -0.0171(12) 0.0068(10) 0.0048(11) B38 0.0338(11) 0.0274(12) 0.0357(12) -0.0097(9) 0.0210(10) -0.0041(9) B39 0.0270(10) 0.0334(13) 0.0282(11) -0.0056(9) 0.0095(9) 0.0021(9) B40 0.0328(11) 0.0386(13) 0.0330(12) -0.0080(10) 0.0194(10) -0.0042(10) B41 0.0478(14) 0.0451(16) 0.0279(12) -0.0057(11) 0.0131(11) 0.0041(12) B42 0.0358(11) 0.0266(12) 0.0283(11) -0.0030(9) 0.0143(9) -0.0008(9) C15 0.0421(12) 0.0542(16) 0.0484(14) 0.0136(12) 0.0118(11) 0.0042(11) Cl1 0.0650(8) 0.0807(14) 0.0627(10) -0.0228(10) 0.0339(7) 0.0096(9) Cl2 0.0642(11) 0.144(3) 0.0701(11) 0.0289(15) 0.0302(7) -0.0336(15) Cl3 0.0834(11) 0.0509(8) 0.0693(11) -0.0132(7) 0.0069(9) -0.0087(7) C16 0.0344(10) 0.0415(13) 0.0295(11) 0.0017(9) 0.0090(8) 0.0032(9) Cl4 0.0409(16) 0.066(2) 0.0272(14) 0.0089(14) 0.0229(12) 0.0175(15) Cl5 0.0566(18) 0.0365(17) 0.0312(13) -0.0009(10) 0.0097(13) 0.0136(13) Cl6 0.109(3) 0.069(2) 0.077(2) -0.0093(16) 0.054(2) -0.035(2) Cl4X 0.069(3) 0.088(3) 0.062(3) -0.011(2) 0.032(2) 0.019(2) Cl5X 0.0558(18) 0.053(2) 0.074(3) -0.0181(17) 0.0011(18) -0.0073(15) Cl6X 0.0428(9) 0.086(3) 0.0338(12) 0.0140(13) 0.0141(8) -0.0219(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 C2 1.633(4) . y C1 B5 1.652(4) . y C1 B4 1.692(4) . y C1 B6 1.711(3) . y C1 B3 1.716(4) . y C1 H1C 1.02(3) . n C2 B6 1.681(4) . y C2 B3 1.722(4) . y C2 B7 1.732(4) . y C2 B11 1.733(5) . y C2 H2C 0.98(3) . n B3 B8 1.745(4) . y B3 B4 1.758(5) . y B3 B7 1.799(5) . y B3 H3B 1.04(3) . n B4 B9 1.746(4) . y B4 B5 1.768(3) . y B4 B8 1.774(4) . y B4 H4B 1.09(3) . n B5 B10 1.725(4) . y B5 B9 1.753(4) . y B5 B6 1.765(4) . y B5 H5B 1.13(3) . n B6 B11 1.752(5) . y B6 B10 1.760(4) . y B6 H6B 1.06(3) . n B7 B12 1.762(5) . y B7 B8 1.764(4) . y B7 B11 1.777(4) . y B7 H7B 1.08(3) . n B8 C3 1.545(3) . y B8 B12 1.787(4) . y B8 B9 1.790(3) . y B9 B12 1.739(4) . y B9 B10 1.774(3) . y B9 H9B 1.09(2) . n B10 B11 1.748(4) . y B10 B12 1.782(4) . y B10 H10B 1.15(3) . n B11 B12 1.780(4) . y B11 H11B 1.01(3) . n B12 H12B 1.15(3) . n C3 C4 1.200(3) . y C4 C5 1.448(3) . y C5 C10 1.384(3) . y C5 C6 1.395(3) . y C6 C7 1.388(3) . y C6 H6A 0.9500 . n C7 C8 1.388(3) . y C7 H7A 0.9500 . n C8 C9 1.389(3) . y C8 C14 1.446(2) . y C9 C10 1.381(3) . y C9 H9A 0.9500 . n C10 H10A 0.9500 . n C13 C14 1.200(2) . y C13 B18 1.545(3) . y C11 C12 1.625(3) . y C11 B15 1.685(3) . y C11 B14 1.697(3) . y C11 B16 1.714(3) . y C11 B13 1.715(3) . y C11 H11C 0.93(2) . n C12 B17 1.697(3) . y C12 B21 1.702(3) . y C12 B16 1.710(3) . y C12 B13 1.720(3) . y C12 H12C 0.98(2) . n B13 B18 1.763(3) . y B13 B14 1.768(4) . y B13 B17 1.784(4) . y B13 H13B 1.11(2) . n B14 B19 1.771(3) . y B14 B15 1.781(3) . y B14 B18 1.782(3) . y B14 H14B 1.06(2) . n B15 B20 1.764(3) . y B15 B16 1.773(3) . y B15 B19 1.777(3) . y B15 H15B 1.13(2) . n B16 B20 1.766(3) . y B16 B21 1.772(3) . y B16 H16B 1.09(2) . n B17 B18 1.779(3) . y B17 B21 1.781(3) . y B17 B22 1.783(3) . y B17 H17B 1.10(2) . n B18 B22 1.792(3) . y B18 B19 1.795(3) . y B19 B22 1.764(3) . y B19 B20 1.783(3) . y B19 H19B 1.074(19) . n B20 B21 1.776(3) . y B20 B22 1.781(3) . y B20 H20B 1.14(2) . n B21 B22 1.782(3) . y B21 H21B 1.04(2) . n B22 H22B 1.11(2) . n C21 C22 1.610(4) . y C21 B24 1.684(3) . y C21 B25 1.687(3) . y C21 B23 1.711(3) . y C21 B26 1.720(3) . y C21 H21C 0.99(2) . n C22 B27 1.696(4) . y C22 B31 1.699(4) . y C22 B26 1.705(3) . y C22 B23 1.707(4) . y C22 H22C 0.88(3) . n B23 B24 1.767(4) . y B23 B28 1.773(3) . y B23 B27 1.777(5) . y B23 H23B 1.12(2) . n B24 B29 1.768(3) . y B24 B25 1.771(3) . y B24 B28 1.795(3) . y B24 H24B 1.12(2) . n B25 B30 1.764(3) . y B25 B29 1.773(3) . y B25 B26 1.779(4) . y B25 H25B 1.06(2) . n B26 B31 1.758(4) . y B26 B30 1.759(4) . y B26 H26B 1.08(2) . n B27 B28 1.772(4) . y B27 B31 1.780(4) . y B27 B32 1.782(4) . y B27 H27B 1.10(3) . n B28 C23 1.542(3) . y B28 B29 1.786(3) . y B28 B32 1.786(3) . y B29 B32 1.768(4) . y B29 B30 1.776(3) . y B29 H29B 1.06(2) . n B30 B31 1.770(4) . y B30 B32 1.782(3) . y B30 H30B 1.06(2) . n B31 B32 1.771(4) . y B31 H31B 1.02(3) . n B32 H32B 1.10(2) . n C23 C24 1.200(2) . y C24 C25 1.445(2) . y C25 C26 1.390(3) . y C25 C30 1.396(2) . y C26 C27 1.384(2) . y C26 H26A 0.9500 . n C27 C28 1.396(2) . y C27 H27A 0.9500 . n C28 C29 1.389(3) . y C28 C34 1.449(2) . y C29 C30 1.387(2) . y C29 H29A 0.9500 . n C30 H30A 0.9500 . n C33 C34 1.195(2) . y C33 B38 1.544(3) . y C31 C32 1.628(3) . y C31 B35 1.697(3) . y C31 B34 1.699(3) . y C31 B36 1.705(3) . y C31 B33 1.712(3) . y C31 H31C 1.00(3) . n C32 B41 1.689(4) . y C32 B37 1.690(3) . y C32 B36 1.707(3) . y C32 B33 1.714(3) . y C32 H32C 0.95(2) . n B33 B38 1.771(3) . y B33 B37 1.773(4) . y B33 B34 1.786(4) . y B33 H33B 1.05(2) . n B34 B39 1.770(3) . y B34 B35 1.781(3) . y B34 B38 1.783(3) . y B34 H34B 1.11(2) . n B35 B40 1.767(3) . y B35 B39 1.770(3) . y B35 B36 1.774(4) . y B35 H35B 1.07(2) . n B36 B40 1.764(3) . y B36 B41 1.774(4) . y B36 H36B 1.10(2) . n B37 B42 1.767(3) . y B37 B41 1.782(3) . y B37 B38 1.788(3) . y B37 H37B 1.05(2) . n B38 B39 1.789(3) . y B38 B42 1.791(3) . y B39 B42 1.766(3) . y B39 B40 1.777(3) . y B39 H39B 1.12(2) . n B40 B41 1.768(3) . y B40 B42 1.782(3) . y B40 H40B 1.06(2) . n B41 B42 1.770(3) . y B41 H41B 1.08(2) . n B42 H42B 1.02(2) . n C15 Cl3 1.727(3) . y C15 Cl2 1.775(3) . y C15 Cl1 1.800(3) . y C15 H15A 1.0000 . n C16 Cl6 1.728(6) . y C16 Cl5 1.766(5) . y C16 Cl4 1.776(4) . y C16 H16 1.0000 . n 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 C1 B5 110.9(2) . . y C2 C1 B4 111.6(2) . . y B5 C1 B4 63.84(17) . . y C2 C1 B6 60.29(17) . . y B5 C1 B6 63.27(16) . . y B4 C1 B6 116.1(2) . . y C2 C1 B3 61.83(18) . . y B5 C1 B3 114.6(2) . . y B4 C1 B3 62.11(17) . . y B6 C1 B3 114.1(2) . . y C2 C1 H1C 118.2(18) . . n B5 C1 H1C 121.3(17) . . n B4 C1 H1C 119.4(17) . . n B6 C1 H1C 117.4(16) . . n B3 C1 H1C 115.8(17) . . n C1 C2 B6 62.16(17) . . y C1 C2 B3 61.44(18) . . y B6 C2 B3 115.4(2) . . y C1 C2 B7 110.6(2) . . y B6 C2 B7 113.7(2) . . y B3 C2 B7 62.77(18) . . y C1 C2 B11 110.0(2) . . y B6 C2 B11 61.73(18) . . y B3 C2 B11 113.7(2) . . y B7 C2 B11 61.72(19) . . y C1 C2 H2C 115.0(19) . . n B6 C2 H2C 114.8(18) . . n B3 C2 H2C 115.6(18) . . n B7 C2 H2C 124.4(19) . . n B11 C2 H2C 124.4(18) . . n C1 B3 C2 56.74(16) . . y C1 B3 B8 105.3(2) . . y C2 B3 B8 105.6(2) . . y C1 B3 B4 58.30(17) . . y C2 B3 B4 104.49(19) . . y B8 B3 B4 60.85(16) . . y C1 B3 B7 103.88(19) . . y C2 B3 B7 58.88(18) . . y B8 B3 B7 59.71(17) . . y B4 B3 B7 107.5(2) . . y C1 B3 H3B 117.2(16) . . n C2 B3 H3B 119.7(16) . . n B8 B3 H3B 129.5(16) . . n B4 B3 H3B 121.2(16) . . n B7 B3 H3B 127.4(17) . . n C1 B4 B9 103.91(18) . . y C1 B4 B3 59.60(17) . . y B9 B4 B3 107.9(2) . . y C1 B4 B5 56.96(15) . . y B9 B4 B5 59.85(15) . . y B3 B4 B5 106.95(19) . . y C1 B4 B8 105.0(2) . . y B9 B4 B8 61.13(15) . . y B3 B4 B8 59.20(17) . . y B5 B4 B8 108.24(18) . . y C1 B4 H4B 117.1(13) . . n B9 B4 H4B 128.4(13) . . n B3 B4 H4B 119.2(13) . . n B5 B4 H4B 119.2(13) . . n B8 B4 H4B 128.2(13) . . n C1 B5 B10 106.9(2) . . y C1 B5 B9 105.34(19) . . y B10 B5 B9 61.32(16) . . y C1 B5 B6 60.02(17) . . y B10 B5 B6 60.56(17) . . y B9 B5 B6 109.4(2) . . y C1 B5 B4 59.20(16) . . y B10 B5 B4 109.62(19) . . y B9 B5 B4 59.45(15) . . y B6 B5 B4 109.7(2) . . y C1 B5 H5B 115.7(14) . . n B10 B5 H5B 127.0(13) . . n B9 B5 H5B 128.6(14) . . n B6 B5 H5B 117.2(13) . . n B4 B5 H5B 118.4(13) . . n C2 B6 C1 57.55(17) . . y C2 B6 B11 60.6(2) . . y C1 B6 B11 105.59(19) . . y C2 B6 B10 105.5(2) . . y C1 B6 B10 102.84(18) . . y B11 B6 B10 59.69(19) . . y C2 B6 B5 103.42(18) . . y C1 B6 B5 56.71(16) . . y B11 B6 B5 106.4(2) . . y B10 B6 B5 58.61(17) . . y C2 B6 H6B 115.8(14) . . n C1 B6 H6B 115.3(14) . . n B11 B6 H6B 126.4(14) . . n B10 B6 H6B 134.2(14) . . n B5 B6 H6B 124.5(14) . . n C2 B7 B12 104.9(2) . . y C2 B7 B8 104.3(2) . . y B12 B7 B8 60.91(16) . . y C2 B7 B11 59.18(18) . . y B12 B7 B11 60.40(18) . . y B8 B7 B11 109.3(2) . . y C2 B7 B3 58.35(18) . . y B12 B7 B3 107.1(2) . . y B8 B7 B3 58.62(16) . . y B11 B7 B3 107.9(2) . . y C2 B7 H7B 118.4(16) . . n B12 B7 H7B 128.1(16) . . n B8 B7 H7B 126.4(14) . . n B11 B7 H7B 119.6(14) . . n B3 B7 H7B 119.2(15) . . n C3 B8 B3 120.59(19) . . y C3 B8 B7 121.76(19) . . y B3 B8 B7 61.67(19) . . y C3 B8 B4 121.85(19) . . y B3 B8 B4 59.95(18) . . y B7 B8 B4 108.33(19) . . y C3 B8 B12 123.3(2) . . y B3 B8 B12 108.33(18) . . y B7 B8 B12 59.48(17) . . y B4 B8 B12 106.02(16) . . y C3 B8 B9 124.0(2) . . y B3 B8 B9 106.55(18) . . y B7 B8 B9 105.84(17) . . y B4 B8 B9 58.68(15) . . y B12 B8 B9 58.18(15) . . y B12 B9 B4 109.4(2) . . y B12 B9 B5 107.8(2) . . y B4 B9 B5 60.70(16) . . y B12 B9 B10 60.94(15) . . y B4 B9 B10 108.4(2) . . y B5 B9 B10 58.55(15) . . y B12 B9 B8 60.83(15) . . y B4 B9 B8 60.19(16) . . y B5 B9 B8 108.2(2) . . y B10 B9 B8 109.12(19) . . y B12 B9 H9B 124.1(13) . . n B4 B9 H9B 119.6(12) . . n B5 B9 H9B 118.3(12) . . n B10 B9 H9B 120.2(12) . . n B8 B9 H9B 124.4(12) . . n B5 B10 B11 108.4(2) . . y B5 B10 B6 60.84(17) . . y B11 B10 B6 59.93(19) . . y B5 B10 B9 60.13(15) . . y B11 B10 B9 107.60(18) . . y B6 B10 B9 108.67(19) . . y B5 B10 B12 107.14(18) . . y B11 B10 B12 60.57(17) . . y B6 B10 B12 108.3(2) . . y B9 B10 B12 58.57(15) . . y B5 B10 H10B 120.4(13) . . n B11 B10 H10B 122.3(13) . . n B6 B10 H10B 120.4(13) . . n B9 B10 H10B 122.0(13) . . n B12 B10 H10B 123.4(13) . . n C2 B11 B10 103.8(2) . . y C2 B11 B6 57.67(18) . . y B10 B11 B6 60.38(17) . . y C2 B11 B7 59.10(19) . . y B10 B11 B7 108.09(19) . . y B6 B11 B7 108.1(2) . . y C2 B11 B12 104.10(19) . . y B10 B11 B12 60.67(17) . . y B6 B11 B12 108.7(2) . . y B7 B11 B12 59.38(16) . . y C2 B11 H11B 126.4(16) . . n B10 B11 H11B 118.7(15) . . n B6 B11 H11B 117.3(15) . . n B7 B11 H11B 126.1(15) . . n B12 B11 H11B 124.1(16) . . n B9 B12 B7 108.2(2) . . y B9 B12 B11 107.7(2) . . y B7 B12 B11 60.23(18) . . y B9 B12 B10 60.49(15) . . y B7 B12 B10 107.2(2) . . y B11 B12 B10 58.76(17) . . y B9 B12 B8 60.99(15) . . y B7 B12 B8 59.61(16) . . y B11 B12 B8 108.2(2) . . y B10 B12 B8 108.89(19) . . y B9 B12 H12B 122.2(15) . . n B7 B12 H12B 119.5(15) . . n B11 B12 H12B 123.0(15) . . n B10 B12 H12B 124.9(15) . . n B8 B12 H12B 118.7(15) . . n C4 C3 B8 177.4(2) . . y C3 C4 C5 177.8(3) . . y C10 C5 C6 118.62(17) . . y C10 C5 C4 121.43(19) . . y C6 C5 C4 119.9(2) . . y C7 C6 C5 120.8(2) . . y C7 C6 H6A 119.6 . . n C5 C6 H6A 119.6 . . n C6 C7 C8 120.28(19) . . y C6 C7 H7A 119.9 . . n C8 C7 H7A 119.9 . . n C7 C8 C9 118.64(17) . . y C7 C8 C14 121.33(18) . . y C9 C8 C14 120.03(18) . . y C10 C9 C8 121.1(2) . . y C10 C9 H9A 119.4 . . n C8 C9 H9A 119.4 . . n C9 C10 C5 120.5(2) . . y C9 C10 H10A 119.7 . . n C5 C10 H10A 119.7 . . n C14 C13 B18 177.8(2) . . y C13 C14 C8 177.3(2) . . y C12 C11 B15 111.52(17) . . y C12 C11 B14 111.54(17) . . y B15 C11 B14 63.57(13) . . y C12 C11 B16 61.53(13) . . y B15 C11 B16 62.88(13) . . y B14 C11 B16 115.76(17) . . y C12 C11 B13 61.93(14) . . y B15 C11 B13 115.43(17) . . y B14 C11 B13 62.43(13) . . y B16 C11 B13 115.58(17) . . y C12 C11 H11C 118.2(15) . . n B15 C11 H11C 120.8(14) . . n B14 C11 H11C 119.6(14) . . n B16 C11 H11C 116.9(14) . . n B13 C11 H11C 115.2(14) . . n C11 C12 B17 111.62(16) . . y C11 C12 B21 111.39(17) . . y B17 C12 B21 63.20(14) . . y C11 C12 B16 61.80(13) . . y B17 C12 B16 115.40(17) . . y B21 C12 B16 62.60(14) . . y C11 C12 B13 61.60(13) . . y B17 C12 B13 62.97(14) . . y B21 C12 B13 115.42(17) . . y B16 C12 B13 115.53(17) . . y C11 C12 H12C 114.0(14) . . n B17 C12 H12C 124.2(13) . . n B21 C12 H12C 122.9(13) . . n B16 C12 H12C 113.5(13) . . n B13 C12 H12C 115.7(13) . . n C11 B13 C12 56.47(12) . . y C11 B13 B18 104.67(16) . . y C12 B13 B18 104.35(16) . . y C11 B13 B14 58.28(13) . . y C12 B13 B14 103.88(15) . . y B18 B13 B14 60.61(13) . . y C11 B13 B17 103.48(15) . . y C12 B13 B17 57.88(13) . . y B18 B13 B17 60.20(14) . . y B14 B13 B17 107.94(17) . . y C11 B13 H13B 115.9(12) . . n C12 B13 H13B 116.9(12) . . n B18 B13 H13B 133.1(12) . . n B14 B13 H13B 123.8(12) . . n B17 B13 H13B 125.8(12) . . n C11 B14 B13 59.29(13) . . y C11 B14 B19 104.04(15) . . y B13 B14 B19 108.17(17) . . y C11 B14 B15 57.90(13) . . y B13 B14 B15 108.15(16) . . y B19 B14 B15 60.04(13) . . y C11 B14 B18 104.62(17) . . y B13 B14 B18 59.56(13) . . y B19 B14 B18 60.68(12) . . y B15 B14 B18 108.56(15) . . y C11 B14 H14B 116.7(12) . . n B13 B14 H14B 118.1(12) . . n B19 B14 H14B 129.1(12) . . n B15 B14 H14B 118.6(11) . . n B18 B14 H14B 128.6(12) . . n C11 B15 B20 104.92(17) . . y C11 B15 B16 59.35(13) . . y B20 B15 B16 59.90(13) . . y C11 B15 B19 104.24(15) . . y B20 B15 B19 60.46(13) . . y B16 B15 B19 108.34(16) . . y C11 B15 B14 58.52(13) . . y B20 B15 B14 108.39(16) . . y B16 B15 B14 108.71(16) . . y B19 B15 B14 59.68(12) . . y C11 B15 H15B 116.1(11) . . n B20 B15 H15B 127.1(11) . . n B16 B15 H15B 115.4(11) . . n B19 B15 H15B 131.1(11) . . n B14 B15 H15B 120.8(11) . . n C12 B16 C11 56.67(13) . . y C12 B16 B20 104.19(16) . . y C11 B16 B20 103.62(15) . . y C12 B16 B21 58.48(14) . . y C11 B16 B21 104.05(15) . . y B20 B16 B21 60.25(14) . . y C12 B16 B15 103.57(15) . . y C11 B16 B15 57.77(13) . . y B20 B16 B15 59.78(14) . . y B21 B16 B15 107.75(17) . . y C12 B16 H16B 117.7(11) . . n C11 B16 H16B 116.7(11) . . n B20 B16 H16B 132.9(11) . . n B21 B16 H16B 125.7(11) . . n B15 B16 H16B 123.7(11) . . n C12 B17 B18 104.64(17) . . y C12 B17 B21 58.54(13) . . y B18 B17 B21 108.76(16) . . y C12 B17 B22 104.11(15) . . y B18 B17 B22 60.43(13) . . y B21 B17 B22 60.00(13) . . y C12 B17 B13 59.16(14) . . y B18 B17 B13 59.31(13) . . y B21 B17 B13 108.45(16) . . y B22 B17 B13 107.51(17) . . y C12 B17 H17B 117.6(12) . . n B18 B17 H17B 127.8(11) . . n B21 B17 H17B 118.6(11) . . n B22 B17 H17B 128.6(12) . . n B13 B17 H17B 118.9(12) . . n C13 B18 B13 119.96(16) . . y C13 B18 B17 122.26(16) . . y B13 B18 B17 60.49(14) . . y C13 B18 B14 121.03(17) . . y B13 B18 B14 59.83(14) . . y B17 B18 B14 107.56(16) . . y C13 B18 B22 124.09(17) . . y B13 B18 B22 108.02(15) . . y B17 B18 B22 59.88(13) . . y B14 B18 B22 106.60(14) . . y C13 B18 B19 123.35(16) . . y B13 B18 B19 107.33(15) . . y B17 B18 B19 106.86(14) . . y B14 B18 B19 59.35(12) . . y B22 B18 B19 58.93(12) . . y B22 B19 B14 108.33(16) . . y B22 B19 B15 107.78(16) . . y B14 B19 B15 60.28(13) . . y B22 B19 B20 60.26(12) . . y B14 B19 B20 108.02(16) . . y B15 B19 B20 59.39(12) . . y B22 B19 B18 60.48(12) . . y B14 B19 B18 59.97(12) . . y B15 B19 B18 108.18(16) . . y B20 B19 B18 108.60(15) . . y B22 B19 H19B 125.3(10) . . n B14 B19 H19B 119.1(10) . . n B15 B19 H19B 118.3(10) . . n B20 B19 H19B 121.8(9) . . n B18 B19 H19B 123.4(10) . . n B15 B20 B16 60.32(14) . . y B15 B20 B21 108.03(17) . . y B16 B20 B21 60.06(14) . . y B15 B20 B22 107.66(14) . . y B16 B20 B22 108.27(16) . . y B21 B20 B22 60.13(13) . . y B15 B20 B19 60.15(13) . . y B16 B20 B19 108.43(15) . . y B21 B20 B19 107.66(14) . . y B22 B20 B19 59.36(12) . . y B15 B20 H20B 120.4(11) . . n B16 B20 H20B 119.7(11) . . n B21 B20 H20B 122.1(11) . . n B22 B20 H20B 123.7(11) . . n B19 B20 H20B 122.7(11) . . n C12 B21 B16 58.92(13) . . y C12 B21 B20 104.09(16) . . y B16 B21 B20 59.69(14) . . y C12 B21 B17 58.26(13) . . y B16 B21 B17 108.26(17) . . y B20 B21 B17 108.11(16) . . y C12 B21 B22 103.94(15) . . y B16 B21 B22 107.92(17) . . y B20 B21 B22 60.07(13) . . y B17 B21 B22 60.06(13) . . y C12 B21 H21B 121.9(12) . . n B16 B21 H21B 116.5(12) . . n B20 B21 H21B 122.8(11) . . n B17 B21 H21B 123.9(11) . . n B22 B21 H21B 127.5(12) . . n B19 B22 B20 60.38(12) . . y B19 B22 B21 108.21(16) . . y B20 B22 B21 59.80(13) . . y B19 B22 B17 108.03(16) . . y B20 B22 B17 107.80(16) . . y B21 B22 B17 59.94(13) . . y B19 B22 B18 60.60(12) . . y B20 B22 B18 108.79(16) . . y B21 B22 B18 108.13(16) . . y B17 B22 B18 59.69(13) . . y B19 B22 H22B 122.2(12) . . n B20 B22 H22B 121.9(11) . . n B21 B22 H22B 121.2(12) . . n B17 B22 H22B 121.3(12) . . n B18 B22 H22B 121.4(11) . . n C22 C21 B24 111.56(18) . . y C22 C21 B25 111.60(18) . . y B24 C21 B25 63.37(13) . . y C22 C21 B23 61.75(15) . . y B24 C21 B23 62.71(14) . . y B25 C21 B23 115.53(17) . . y C22 C21 B26 61.48(15) . . y B24 C21 B26 115.58(17) . . y B25 C21 B26 62.96(14) . . y B23 C21 B26 115.38(19) . . y C22 C21 H21C 116.4(15) . . n B24 C21 H21C 121.5(14) . . n B25 C21 H21C 121.7(14) . . n B23 C21 H21C 115.2(14) . . n B26 C21 H21C 115.7(13) . . n C21 C22 B27 112.09(18) . . y C21 C22 B31 111.59(19) . . y B27 C22 B31 63.26(18) . . y C21 C22 B26 62.43(14) . . y B27 C22 B26 115.5(2) . . y B31 C22 B26 62.17(16) . . y C21 C22 B23 62.02(15) . . y B27 C22 B23 62.98(17) . . y B31 C22 B23 115.56(19) . . y B26 C22 B23 116.42(19) . . y C21 C22 H22C 114.3(18) . . n B27 C22 H22C 124.1(18) . . n B31 C22 H22C 121.9(18) . . n B26 C22 H22C 112.7(17) . . n B23 C22 H22C 116.4(17) . . n C22 B23 C21 56.23(13) . . y C22 B23 B24 103.33(16) . . y C21 B23 B24 57.91(13) . . y C22 B23 B28 104.09(18) . . y C21 B23 B28 104.59(16) . . y B24 B23 B28 60.93(14) . . y C22 B23 B27 58.21(16) . . y C21 B23 B27 103.67(17) . . y B24 B23 B27 107.99(18) . . y B28 B23 B27 59.89(15) . . y C22 B23 H23B 119.1(12) . . n C21 B23 H23B 117.6(12) . . n B24 B23 H23B 123.1(12) . . n B28 B23 H23B 131.1(12) . . n B27 B23 H23B 125.7(12) . . n C21 B24 B23 59.38(14) . . y C21 B24 B29 104.27(15) . . y B23 B24 B29 107.98(18) . . y C21 B24 B25 58.40(12) . . y B23 B24 B25 108.67(17) . . y B29 B24 B25 60.13(12) . . y C21 B24 B28 104.75(18) . . y B23 B24 B28 59.69(14) . . y B29 B24 B28 60.15(12) . . y B25 B24 B28 108.49(16) . . y C21 B24 H24B 117.5(12) . . n B23 B24 H24B 117.2(12) . . n B29 B24 H24B 129.3(12) . . n B25 B24 H24B 119.9(11) . . n B28 B24 H24B 127.1(11) . . n C21 B25 B30 104.71(18) . . y C21 B25 B24 58.23(12) . . y B30 B25 B24 108.38(16) . . y C21 B25 B29 103.94(15) . . y B30 B25 B29 60.28(13) . . y B24 B25 B29 59.87(12) . . y C21 B25 B26 59.42(13) . . y B30 B25 B26 59.54(15) . . y B24 B25 B26 108.45(17) . . y B29 B25 B26 107.76(17) . . y C21 B25 H25B 117.4(12) . . n B30 B25 H25B 127.9(12) . . n B24 B25 H25B 119.2(12) . . n B29 B25 H25B 129.1(13) . . n B26 B25 H25B 118.1(12) . . n C22 B26 C21 56.09(15) . . y C22 B26 B31 58.75(17) . . y C21 B26 B31 103.84(17) . . y C22 B26 B30 104.33(17) . . y C21 B26 B30 103.52(16) . . y B31 B26 B30 60.42(17) . . y C22 B26 B25 103.02(16) . . y C21 B26 B25 57.62(13) . . y B31 B26 B25 107.73(17) . . y B30 B26 B25 59.78(14) . . y C22 B26 H26B 117.1(12) . . n C21 B26 H26B 114.6(12) . . n B31 B26 H26B 127.4(12) . . n B30 B26 H26B 134.4(12) . . n B25 B26 H26B 122.7(12) . . n C22 B27 B28 104.6(2) . . y C22 B27 B23 58.81(16) . . y B28 B27 B23 59.93(15) . . y C22 B27 B31 58.47(16) . . y B28 B27 B31 108.28(19) . . y B23 B27 B31 108.18(19) . . y C22 B27 B32 103.91(18) . . y B28 B27 B32 60.35(14) . . y B23 B27 B32 107.94(19) . . y B31 B27 B32 59.63(17) . . y C22 B27 H27B 117.5(14) . . n B28 B27 H27B 126.4(13) . . n B23 B27 H27B 116.1(14) . . n B31 B27 H27B 121.3(13) . . n B32 B27 H27B 130.4(14) . . n C23 B28 B27 121.01(18) . . y C23 B28 B23 121.00(16) . . y B27 B28 B23 60.18(17) . . y C23 B28 B29 123.68(17) . . y B27 B28 B29 107.11(16) . . y B23 B28 B29 106.96(15) . . y C23 B28 B32 122.32(18) . . y B27 B28 B32 60.11(16) . . y B23 B28 B32 107.95(17) . . y B29 B28 B32 59.32(13) . . y C23 B28 B24 123.13(18) . . y B27 B28 B24 106.99(17) . . y B23 B28 B24 59.37(14) . . y B29 B28 B24 59.19(12) . . y B32 B28 B24 106.64(15) . . y B32 B29 B24 108.63(18) . . y B32 B29 B25 108.20(17) . . y B24 B29 B25 60.01(12) . . y B32 B29 B30 60.39(14) . . y B24 B29 B30 107.96(16) . . y B25 B29 B30 59.60(13) . . y B32 B29 B28 60.36(13) . . y B24 B29 B28 60.66(13) . . y B25 B29 B28 108.80(16) . . y B30 B29 B28 108.83(17) . . y B32 B29 H29B 121.2(12) . . n B24 B29 H29B 121.7(12) . . n B25 B29 H29B 121.9(12) . . n B30 B29 H29B 121.6(12) . . n B28 B29 H29B 120.9(12) . . n B26 B30 B25 60.68(14) . . y B26 B30 B31 59.75(16) . . y B25 B30 B31 107.91(18) . . y B26 B30 B29 108.54(16) . . y B25 B30 B29 60.12(13) . . y B31 B30 B29 107.32(16) . . y B26 B30 B32 108.15(18) . . y B25 B30 B32 107.97(15) . . y B31 B30 B32 59.83(15) . . y B29 B30 B32 59.59(13) . . y B26 B30 H30B 120.2(12) . . n B25 B30 H30B 120.2(12) . . n B31 B30 H30B 122.8(12) . . n B29 B30 H30B 122.1(12) . . n B32 B30 H30B 123.3(12) . . n C22 B31 B26 59.07(15) . . y C22 B31 B30 104.13(19) . . y B26 B31 B30 59.83(15) . . y C22 B31 B32 104.22(18) . . y B26 B31 B32 108.7(2) . . y B30 B31 B32 60.44(16) . . y C22 B31 B27 58.27(17) . . y B26 B31 B27 108.7(2) . . y B30 B31 B27 108.46(18) . . y B32 B31 B27 60.24(15) . . y C22 B31 H31B 117.9(16) . . n B26 B31 H31B 116.2(15) . . n B30 B31 H31B 126.8(15) . . n B32 B31 H31B 129.5(15) . . n B27 B31 H31B 120.6(15) . . n B29 B32 B31 107.59(18) . . y B29 B32 B30 60.02(13) . . y B31 B32 B30 59.73(15) . . y B29 B32 B27 107.44(18) . . y B31 B32 B27 60.13(17) . . y B30 B32 B27 107.81(18) . . y B29 B32 B28 60.32(13) . . y B31 B32 B28 108.0(2) . . y B30 B32 B28 108.51(17) . . y B27 B32 B28 59.54(15) . . y B29 B32 H32B 126.2(13) . . n B31 B32 H32B 118.9(12) . . n B30 B32 H32B 123.7(12) . . n B27 B32 H32B 118.1(12) . . n B28 B32 H32B 121.8(12) . . n C24 C23 B28 176.1(2) . . y C23 C24 C25 178.4(2) . . y C26 C25 C30 118.66(16) . . y C26 C25 C24 121.12(16) . . y C30 C25 C24 120.21(17) . . y C27 C26 C25 120.82(17) . . y C27 C26 H26A 119.6 . . n C25 C26 H26A 119.6 . . n C26 C27 C28 120.51(18) . . y C26 C27 H27A 119.7 . . n C28 C27 H27A 119.7 . . n C29 C28 C27 118.80(16) . . y C29 C28 C34 120.97(16) . . y C27 C28 C34 120.20(17) . . y C30 C29 C28 120.66(16) . . y C30 C29 H29A 119.7 . . n C28 C29 H29A 119.7 . . n C29 C30 C25 120.55(18) . . y C29 C30 H30A 119.7 . . n C25 C30 H30A 119.7 . . n C34 C33 B38 178.4(2) . . y C33 C34 C28 178.1(2) . . y C32 C31 B35 111.45(17) . . y C32 C31 B34 111.82(16) . . y B35 C31 B34 63.28(14) . . y C32 C31 B36 61.56(13) . . y B35 C31 B36 62.86(14) . . y B34 C31 B36 115.71(17) . . y C32 C31 B33 61.69(15) . . y B35 C31 B33 115.69(16) . . y B34 C31 B33 63.15(15) . . y B36 C31 B33 115.57(18) . . y C32 C31 H31C 113.3(14) . . n B35 C31 H31C 123.5(14) . . n B34 C31 H31C 124.5(14) . . n B36 C31 H31C 113.3(13) . . n B33 C31 H31C 115.1(13) . . n C31 C32 B41 111.50(17) . . y C31 C32 B37 111.51(17) . . y B41 C32 B37 63.65(15) . . y C31 C32 B36 61.47(13) . . y B41 C32 B36 62.98(14) . . y B37 C32 B36 115.92(17) . . y C31 C32 B33 61.57(14) . . y B41 C32 B33 115.72(17) . . y B37 C32 B33 62.79(15) . . y B36 C32 B33 115.39(18) . . y C31 C32 H32C 115.0(15) . . n B41 C32 H32C 122.4(15) . . n B37 C32 H32C 122.9(14) . . n B36 C32 H32C 114.4(14) . . n B33 C32 H32C 115.3(14) . . n C31 B33 C32 56.74(13) . . y C31 B33 B38 104.35(16) . . y C32 B33 B38 104.50(16) . . y C31 B33 B37 103.80(16) . . y C32 B33 B37 57.95(14) . . y B38 B33 B37 60.59(14) . . y C31 B33 B34 58.07(14) . . y C32 B33 B34 103.84(15) . . y B38 B33 B34 60.15(14) . . y B37 B33 B34 107.97(17) . . y C31 B33 H33B 116.9(13) . . n C32 B33 H33B 117.0(13) . . n B38 B33 H33B 132.5(13) . . n B37 B33 H33B 124.7(13) . . n B34 B33 H33B 124.6(13) . . n C31 B34 B39 103.68(16) . . y C31 B34 B35 58.32(13) . . y B39 B34 B35 59.80(13) . . y C31 B34 B38 104.41(18) . . y B39 B34 B38 60.48(12) . . y B35 B34 B38 108.60(16) . . y C31 B34 B33 58.78(14) . . y B39 B34 B33 107.50(18) . . y B35 B34 B33 108.01(17) . . y B38 B34 B33 59.53(14) . . y C31 B34 H34B 119.8(12) . . n B39 B34 H34B 127.3(12) . . n B35 B34 H34B 119.6(11) . . n B38 B34 H34B 126.3(12) . . n B33 B34 H34B 119.6(11) . . n C31 B35 B40 104.15(17) . . y C31 B35 B39 103.73(15) . . y B40 B35 B39 60.32(13) . . y C31 B35 B36 58.80(13) . . y B40 B35 B36 59.74(14) . . y B39 B35 B36 107.92(17) . . y C31 B35 B34 58.40(13) . . y B40 B35 B34 108.30(16) . . y B39 B35 B34 59.78(12) . . y B36 B35 B34 108.31(17) . . y C31 B35 H35B 119.9(11) . . n B40 B35 H35B 125.3(11) . . n B39 B35 H35B 128.4(11) . . n B36 B35 H35B 117.4(11) . . n B34 B35 H35B 121.5(11) . . n C31 B36 C32 56.97(13) . . y C31 B36 B40 103.95(16) . . y C32 B36 B40 103.84(15) . . y C31 B36 B41 103.99(15) . . y C32 B36 B41 58.03(14) . . y B40 B36 B41 59.95(14) . . y C31 B36 B35 58.34(14) . . y C32 B36 B35 104.22(15) . . y B40 B36 B35 59.92(13) . . y B41 B36 B35 107.82(16) . . y C31 B36 H36B 118.4(11) . . n C32 B36 H36B 115.5(11) . . n B40 B36 H36B 133.0(11) . . n B41 B36 H36B 122.0(11) . . n B35 B36 H36B 127.3(11) . . n C32 B37 B42 103.87(15) . . y C32 B37 B33 59.26(14) . . y B42 B37 B33 107.86(18) . . y C32 B37 B41 58.16(13) . . y B42 B37 B41 59.84(13) . . y B33 B37 B41 108.29(17) . . y C32 B37 B38 104.77(18) . . y B42 B37 B38 60.48(12) . . y B33 B37 B38 59.65(14) . . y B41 B37 B38 108.57(16) . . y C32 B37 H37B 118.1(13) . . n B42 B37 H37B 130.0(13) . . n B33 B37 H37B 116.2(13) . . n B41 B37 H37B 121.6(13) . . n B38 B37 H37B 125.6(13) . . n C33 B38 B33 122.03(15) . . y C33 B38 B34 122.01(17) . . y B33 B38 B34 60.32(15) . . y C33 B38 B37 122.51(17) . . y B33 B38 B37 59.75(15) . . y B34 B38 B37 107.45(16) . . y C33 B38 B39 122.46(17) . . y B33 B38 B39 107.28(14) . . y B34 B38 B39 59.41(13) . . y B37 B38 B39 106.43(14) . . y C33 B38 B42 122.67(17) . . y B33 B38 B42 106.90(16) . . y B34 B38 B42 106.66(14) . . y B37 B38 B42 59.18(13) . . y B39 B38 B42 59.12(12) . . y B42 B39 B34 108.31(16) . . y B42 B39 B35 108.19(16) . . y B34 B39 B35 60.42(13) . . y B42 B39 B40 60.38(12) . . y B34 B39 B40 108.36(16) . . y B35 B39 B40 59.75(13) . . y B42 B39 B38 60.49(12) . . y B34 B39 B38 60.11(13) . . y B35 B39 B38 108.80(15) . . y B40 B39 B38 109.07(15) . . y B42 B39 H39B 122.5(11) . . n B34 B39 H39B 120.6(11) . . n B35 B39 H39B 120.8(11) . . n B40 B39 H39B 121.8(10) . . n B38 B39 H39B 121.2(10) . . n B36 B40 B35 60.34(14) . . y B36 B40 B41 60.31(14) . . y B35 B40 B41 108.44(17) . . y B36 B40 B39 108.10(16) . . y B35 B40 B39 59.93(13) . . y B41 B40 B39 107.69(15) . . y B36 B40 B42 107.97(15) . . y B35 B40 B42 107.64(14) . . y B41 B40 B42 59.84(12) . . y B39 B40 B42 59.51(12) . . y B36 B40 H40B 119.2(11) . . n B35 B40 H40B 121.7(11) . . n B41 B40 H40B 120.0(11) . . n B39 B40 H40B 124.4(11) . . n B42 B40 H40B 123.4(11) . . n C32 B41 B40 104.40(18) . . y C32 B41 B42 103.77(16) . . y B40 B41 B42 60.47(13) . . y C32 B41 B36 58.99(13) . . y B40 B41 B36 59.73(14) . . y B42 B41 B36 108.01(17) . . y C32 B41 B37 58.19(13) . . y B40 B41 B37 108.23(17) . . y B42 B41 B37 59.67(12) . . y B36 B41 B37 108.15(18) . . y C32 B41 H41B 117.9(11) . . n B40 B41 H41B 127.9(11) . . n B42 B41 H41B 128.6(12) . . n B36 B41 H41B 118.4(11) . . n B37 B41 H41B 119.2(11) . . n B39 B42 B37 108.36(17) . . y B39 B42 B41 108.06(16) . . y B37 B42 B41 60.49(13) . . y B39 B42 B40 60.12(12) . . y B37 B42 B40 108.26(16) . . y B41 B42 B40 59.69(13) . . y B39 B42 B38 60.40(12) . . y B37 B42 B38 60.34(14) . . y B41 B42 B38 108.98(16) . . y B40 B42 B38 108.80(16) . . y B39 B42 H42B 122.0(12) . . n B37 B42 H42B 120.3(12) . . n B41 B42 H42B 122.0(12) . . n B40 B42 H42B 123.1(11) . . n B38 B42 H42B 119.8(11) . . n Cl3 C15 Cl2 112.11(17) . . y Cl3 C15 Cl1 110.10(15) . . y Cl2 C15 Cl1 105.02(16) . . y Cl3 C15 H15A 109.8 . . n Cl2 C15 H15A 109.8 . . n Cl1 C15 H15A 109.8 . . n Cl6 C16 Cl5 113.6(4) . . y Cl6 C16 Cl4 107.9(3) . . y Cl5 C16 Cl4 111.3(3) . . y Cl6 C16 H16 107.9 . . n Cl5 C16 H16 107.9 . . n Cl4 C16 H16 107.9 . . n _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.530 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 961329' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_{[B10C2H11]C2}2_(14) _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,4-bis(1,2-dicarba-closo-dodecaborane(11)-8-yl)butadiyne ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [B10 C2 H11]2 C4 ; _chemical_formula_sum 'C8 H22 B20' _chemical_formula_weight 334.46 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 'P 1 21/n 1' 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 6.7200(8) _cell_length_b 12.6135(15) _cell_length_c 12.0553(14) _cell_angle_alpha 90.00 _cell_angle_beta 100.506(2) _cell_angle_gamma 90.00 _cell_volume 1004.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5150 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.09 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method none _exptl_crystal_F_000 340 _exptl_absorpt_coefficient_mu 0.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.71 _exptl_absorpt_correction_T_max 0.99 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 8555 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.13 _reflns_number_total 2214 _reflns_number_gt 1753 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0905P)^2^+0.0703P] 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 noref _refine_ls_number_reflns 2214 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 -0.0603(2) 0.83180(10) 0.14284(12) 0.0379(4) Uani 1 1 d . . . H1 H -0.137(3) 0.8324(14) 0.0726(18) 0.065(6) Uiso 1 1 d . . . C2 C -0.1575(2) 0.90113(10) 0.23364(11) 0.0362(3) Uani 1 1 d . . . H2 H -0.283(3) 0.9382(15) 0.2018(17) 0.070(6) Uiso 1 1 d . . . B3 B -0.1770(2) 0.76576(12) 0.23697(13) 0.0340(3) Uani 1 1 d . . . H3B H -0.333(3) 0.7305(13) 0.2041(15) 0.056(5) Uiso 1 1 d . . . B4 B 0.0548(3) 0.72095(11) 0.20188(13) 0.0352(4) Uani 1 1 d . . . H4B H 0.046(3) 0.6494(13) 0.1483(15) 0.059(5) Uiso 1 1 d . . . B5 B 0.1959(3) 0.83330(13) 0.17312(17) 0.0467(5) Uani 1 1 d . . . H5B H 0.274(4) 0.8308(16) 0.100(2) 0.092(7) Uiso 1 1 d . . . B6 B 0.0544(3) 0.94861(12) 0.19013(15) 0.0429(4) Uani 1 1 d . . . H6B H 0.028(3) 1.0134(14) 0.1314(15) 0.062(5) Uiso 1 1 d . . . B7 B -0.1185(3) 0.84352(12) 0.36231(13) 0.0359(4) Uani 1 1 d . . . H7B H -0.236(3) 0.8533(14) 0.4122(16) 0.062(5) Uiso 1 1 d . . . B8 B 0.0240(2) 0.72715(10) 0.34514(11) 0.0268(3) Uani 1 1 d . . . B9 B 0.2557(2) 0.76925(11) 0.30610(15) 0.0386(4) Uani 1 1 d . . . H9B H 0.402(3) 0.7212(15) 0.3326(17) 0.068(5) Uiso 1 1 d . . . B10 B 0.2555(3) 0.90995(12) 0.29695(18) 0.0480(5) Uani 1 1 d . . . H10B H 0.399(3) 0.9578(16) 0.3131(18) 0.082(6) Uiso 1 1 d . . . B11 B 0.0249(3) 0.95579(12) 0.33270(14) 0.0421(4) Uani 1 1 d . . . H11B H -0.009(3) 1.0355(15) 0.3677(15) 0.065(5) Uiso 1 1 d . . . B12 B 0.1484(3) 0.84521(11) 0.40466(14) 0.0385(4) Uani 1 1 d . . . H12B H 0.217(3) 0.8515(12) 0.4971(16) 0.059(5) Uiso 1 1 d . . . C3 C 0.01099(19) 0.62481(9) 0.41387(10) 0.0290(3) Uani 1 1 d . . . C4 C 0.00459(19) 0.54529(9) 0.46853(9) 0.0273(3) 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 C1 0.0558(9) 0.0294(7) 0.0283(7) 0.0051(5) 0.0074(6) 0.0028(6) C2 0.0417(8) 0.0310(6) 0.0356(7) 0.0069(5) 0.0065(6) 0.0094(5) B3 0.0361(8) 0.0309(7) 0.0346(7) 0.0043(6) 0.0054(6) -0.0015(6) B4 0.0513(9) 0.0252(7) 0.0330(7) 0.0044(5) 0.0177(7) 0.0041(6) B5 0.0552(11) 0.0346(8) 0.0587(11) 0.0167(7) 0.0329(9) 0.0040(7) B6 0.0568(10) 0.0230(7) 0.0510(10) 0.0103(6) 0.0156(8) -0.0006(6) B7 0.0470(9) 0.0318(7) 0.0315(8) 0.0027(6) 0.0139(7) 0.0090(6) B8 0.0333(7) 0.0212(6) 0.0273(6) 0.0022(5) 0.0092(5) -0.0003(5) B9 0.0325(8) 0.0270(7) 0.0583(10) 0.0122(6) 0.0137(7) 0.0012(6) B10 0.0439(9) 0.0272(8) 0.0711(12) 0.0131(7) 0.0060(8) -0.0074(7) B11 0.0588(11) 0.0222(7) 0.0425(9) 0.0009(6) 0.0016(8) 0.0047(7) B12 0.0485(9) 0.0231(7) 0.0396(8) 0.0017(6) -0.0032(7) -0.0002(6) C3 0.0360(7) 0.0257(6) 0.0269(6) 0.0007(5) 0.0101(5) -0.0015(5) C4 0.0367(7) 0.0239(6) 0.0226(6) -0.0020(4) 0.0087(5) -0.0025(5) _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 C2 1.628(2) . y C1 B4 1.691(2) . y C1 B5 1.693(3) . y C1 B3 1.709(2) . y C1 B6 1.712(2) . y C1 H1 0.91(2) . n C2 B7 1.6895(19) . y C2 B11 1.694(2) . y C2 B6 1.713(2) . y C2 B3 1.713(2) . y C2 H2 0.98(2) . n B3 B8 1.766(2) . y B3 B4 1.779(2) . y B3 B7 1.784(2) . y B3 H3B 1.141(17) . n B4 B5 1.774(2) . y B4 B9 1.776(2) . y B4 B8 1.778(2) . y B4 H4B 1.105(17) . n B5 B10 1.762(3) . y B5 B6 1.770(2) . y B5 B9 1.775(2) . y B5 H5B 1.11(2) . n B6 B10 1.757(3) . y B6 B11 1.768(3) . y B6 H6B 1.075(18) . n B7 B12 1.773(3) . y B7 B8 1.785(2) . y B7 B11 1.785(2) . y B7 H7B 1.086(19) . n B8 C3 1.5450(16) . y B8 B9 1.787(2) . y B8 B12 1.792(2) . y B9 B10 1.778(2) . y B9 B12 1.778(2) . y B9 H9B 1.147(19) . n B10 B11 1.779(3) . y B10 B12 1.792(3) . y B10 H10B 1.12(2) . n B11 B12 1.768(2) . y B11 H11B 1.130(18) . n B12 H12B 1.128(19) . n C3 C4 1.2051(16) . y C4 C4 1.379(2) 3_566 y 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 C1 B4 111.71(10) . . y C2 C1 B5 111.45(12) . . y B4 C1 B5 63.23(9) . . y C2 C1 B3 61.73(9) . . y B4 C1 B3 63.10(8) . . y B5 C1 B3 115.71(11) . . y C2 C1 B6 61.65(9) . . y B4 C1 B6 115.33(12) . . y B5 C1 B6 62.62(10) . . y B3 C1 B6 115.57(11) . . y C2 C1 H1 113.1(12) . . n B4 C1 H1 122.6(11) . . n B5 C1 H1 125.9(13) . . n B3 C1 H1 111.7(12) . . n B6 C1 H1 116.7(11) . . n C1 C2 B7 111.86(10) . . y C1 C2 B11 111.42(12) . . y B7 C2 B11 63.69(10) . . y C1 C2 B6 61.58(9) . . y B7 C2 B6 115.67(12) . . y B11 C2 B6 62.51(10) . . y C1 C2 B3 61.46(8) . . y B7 C2 B3 63.23(8) . . y B11 C2 B3 115.96(10) . . y B6 C2 B3 115.28(11) . . y C1 C2 H2 114.6(12) . . n B7 C2 H2 122.8(12) . . n B11 C2 H2 122.8(11) . . n B6 C2 H2 114.7(12) . . n B3 C2 H2 114.9(11) . . n C1 B3 C2 56.80(8) . . y C1 B3 B8 104.05(11) . . y C2 B3 B8 103.92(10) . . y C1 B3 B4 57.95(8) . . y C2 B3 B4 103.70(10) . . y B8 B3 B4 60.20(8) . . y C1 B3 B7 103.74(10) . . y C2 B3 B7 57.73(8) . . y B8 B3 B7 60.37(8) . . y B4 B3 B7 107.99(11) . . y C1 B3 H3B 117.6(9) . . n C2 B3 H3B 116.7(8) . . n B8 B3 H3B 132.8(9) . . n B4 B3 H3B 125.6(9) . . n B7 B3 H3B 123.7(9) . . n C1 B4 B5 58.45(9) . . y C1 B4 B9 104.15(11) . . y B5 B4 B9 59.99(10) . . y C1 B4 B8 104.31(10) . . y B5 B4 B8 108.40(11) . . y B9 B4 B8 60.38(9) . . y C1 B4 B3 58.95(8) . . y B5 B4 B3 108.35(10) . . y B9 B4 B3 107.96(10) . . y B8 B4 B3 59.54(8) . . y C1 B4 H4B 117.2(9) . . n B5 B4 H4B 120.7(9) . . n B9 B4 H4B 130.3(10) . . n B8 B4 H4B 126.9(9) . . n B3 B4 H4B 116.3(10) . . n C1 B5 B10 104.73(12) . . y C1 B5 B6 59.20(10) . . y B10 B5 B6 59.67(10) . . y C1 B5 B4 58.32(9) . . y B10 B5 B4 108.66(12) . . y B6 B5 B4 108.45(12) . . y C1 B5 B9 104.10(11) . . y B10 B5 B9 60.36(10) . . y B6 B5 B9 107.91(12) . . y B4 B5 B9 60.05(9) . . y C1 B5 H5B 116.2(13) . . n B10 B5 H5B 128.5(12) . . n B6 B5 H5B 117.4(11) . . n B4 B5 H5B 118.8(11) . . n B9 B5 H5B 130.0(12) . . n C1 B6 C2 56.77(9) . . y C1 B6 B10 104.17(11) . . y C2 B6 B10 104.47(11) . . y C1 B6 B11 104.15(11) . . y C2 B6 B11 58.22(9) . . y B10 B6 B11 60.62(11) . . y C1 B6 B5 58.18(10) . . y C2 B6 B5 104.01(10) . . y B10 B6 B5 59.96(11) . . y B11 B6 B5 108.22(12) . . y C1 B6 H6B 115.2(10) . . n C2 B6 H6B 114.9(10) . . n B10 B6 H6B 134.9(10) . . n B11 B6 H6B 124.6(9) . . n B5 B6 H6B 125.2(9) . . n C2 B7 B12 103.79(11) . . y C2 B7 B3 59.04(8) . . y B12 B7 B3 107.79(11) . . y C2 B7 B8 104.11(10) . . y B12 B7 B8 60.48(8) . . y B3 B7 B8 59.32(8) . . y C2 B7 B11 58.28(9) . . y B12 B7 B11 59.56(9) . . y B3 B7 B11 108.08(10) . . y B8 B7 B11 107.95(11) . . y C2 B7 H7B 117.0(10) . . n B12 B7 H7B 129.9(10) . . n B3 B7 H7B 117.5(10) . . n B8 B7 H7B 128.2(9) . . n B11 B7 H7B 119.7(9) . . n C3 B8 B3 121.05(11) . . y C3 B8 B4 120.80(10) . . y B3 B8 B4 60.25(9) . . y C3 B8 B7 122.74(10) . . y B3 B8 B7 60.31(8) . . y B4 B8 B7 107.98(10) . . y C3 B8 B9 121.78(11) . . y B3 B8 B9 108.01(10) . . y B4 B8 B9 59.74(9) . . y B7 B8 B9 107.32(10) . . y C3 B8 B12 123.19(11) . . y B3 B8 B12 107.73(10) . . y B4 B8 B12 107.28(10) . . y B7 B8 B12 59.43(9) . . y B9 B8 B12 59.57(9) . . y B5 B9 B4 59.96(10) . . y B5 B9 B10 59.48(10) . . y B4 B9 B10 107.87(11) . . y B5 B9 B12 107.80(11) . . y B4 B9 B12 108.01(11) . . y B10 B9 B12 60.53(10) . . y B5 B9 B8 107.97(11) . . y B4 B9 B8 59.88(8) . . y B10 B9 B8 108.80(11) . . y B12 B9 B8 60.36(9) . . y B5 B9 H9B 122.2(10) . . n B4 B9 H9B 121.1(10) . . n B10 B9 H9B 122.3(9) . . n B12 B9 H9B 121.9(10) . . n B8 B9 H9B 120.7(9) . . n B6 B10 B5 60.37(11) . . y B6 B10 B9 108.30(12) . . y B5 B10 B9 60.16(9) . . y B6 B10 B11 59.99(10) . . y B5 B10 B11 108.04(13) . . y B9 B10 B11 107.45(11) . . y B6 B10 B12 107.48(12) . . y B5 B10 B12 107.72(11) . . y B9 B10 B12 59.74(9) . . y B11 B10 B12 59.32(10) . . y B6 B10 H10B 119.9(11) . . n B5 B10 H10B 119.8(11) . . n B9 B10 H10B 122.3(11) . . n B11 B10 H10B 122.7(11) . . n B12 B10 H10B 124.3(11) . . n C2 B11 B12 103.85(10) . . y C2 B11 B6 59.26(9) . . y B12 B11 B6 108.11(12) . . y C2 B11 B10 104.31(12) . . y B12 B11 B10 60.71(10) . . y B6 B11 B10 59.39(11) . . y C2 B11 B7 58.03(9) . . y B12 B11 B7 59.88(9) . . y B6 B11 B7 108.30(11) . . y B10 B11 B7 108.46(10) . . y C2 B11 H11B 117.1(9) . . n B12 B11 H11B 128.9(9) . . n B6 B11 H11B 118.3(9) . . n B10 B11 H11B 128.6(9) . . n B7 B11 H11B 118.5(9) . . n B11 B12 B7 60.56(9) . . y B11 B12 B9 107.96(12) . . y B7 B12 B9 108.25(11) . . y B11 B12 B8 108.44(11) . . y B7 B12 B8 60.09(8) . . y B9 B12 B8 60.07(8) . . y B11 B12 B10 59.97(10) . . y B7 B12 B10 108.41(11) . . y B9 B12 B10 59.73(10) . . y B8 B12 B10 107.95(11) . . y B11 B12 H12B 120.0(8) . . n B7 B12 H12B 119.7(9) . . n B9 B12 H12B 123.7(9) . . n B8 B12 H12B 122.1(8) . . n B10 B12 H12B 122.5(9) . . n C4 C3 B8 178.74(14) . . y C3 C4 C4 179.38(17) . 3_566 y _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.13 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.283 _refine_diff_density_min -0.107 _refine_diff_density_rms 0.047 _database_code_depnum_ccdc_archive 'CCDC 961330' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(NBu4)2{[B9C2H11]C}2_(15) _chemical_name_systematic ; tetrabutylammonium bis(undecahydro-7,8-dicarba -nido-decaborate(1-)-1-yl)ethyne ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; {[B9 C2 H11] C}2 {N ((C H2)3 C H3)4}2 ; _chemical_formula_sum 'C38 H94 B18 N2' _chemical_formula_weight 773.73 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc ' _symmetry_int_tables_number 14 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 14.8236(17) _cell_length_b 18.229(2) _cell_length_c 19.262(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.120(2) _cell_angle_gamma 90.00 _cell_volume 5124.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4520 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 21.94 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.003 _exptl_crystal_density_method none _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.75 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49669 _diffrn_reflns_av_R_equivalents 0.1560 _diffrn_reflns_av_sigmaI/netI 0.1276 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9021 _reflns_number_gt 3826 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'Apex II' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0643P)^2^+2.5354P] 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 noref _refine_ls_number_reflns 9021 _refine_ls_number_parameters 682 _refine_ls_number_restraints 1103 _refine_ls_R_factor_all 0.1974 _refine_ls_R_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.2024 _refine_ls_wR_factor_gt 0.1491 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 2.306 _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 B1 B 0.5674(6) 0.6862(5) 0.1043(5) 0.034(2) Uani 1 1 d U . . B2 B 0.5499(7) 0.6254(6) 0.1722(5) 0.044(2) Uani 1 1 d U . . H2 H 0.6052 0.6162 0.2190 0.053 Uiso 1 1 calc R . . B3 B 0.5603(7) 0.5902(6) 0.0894(6) 0.054(3) Uani 1 1 d U . . H3 H 0.6205 0.5564 0.0809 0.065 Uiso 1 1 calc R . . B4 B 0.5046(7) 0.6499(6) 0.0249(5) 0.053(3) Uani 1 1 d U . . H4 H 0.5290 0.6572 -0.0265 0.064 Uiso 1 1 calc R . . B5 B 0.4556(6) 0.7215(6) 0.0660(5) 0.043(2) Uani 1 1 d U . . H5 H 0.4474 0.7773 0.0414 0.052 Uiso 1 1 calc R . . B6 B 0.4842(6) 0.7058(6) 0.1603(5) 0.040(2) Uani 1 1 d U . . H6 H 0.4956 0.7510 0.2002 0.048 Uiso 1 1 calc R . . C7 C 0.4732(6) 0.5629(6) 0.1319(6) 0.056(3) Uani 1 1 d U . . H7 H 0.482(7) 0.512(6) 0.148(5) 0.10(4) Uiso 1 1 d . . . C8 C 0.4494(7) 0.5761(6) 0.0519(5) 0.058(3) Uani 1 1 d U . . H8 H 0.437(5) 0.536(5) 0.022(4) 0.06(3) Uiso 1 1 d . . . B9 B 0.3864(7) 0.6467(7) 0.0318(6) 0.051(3) Uani 1 1 d U . . H9 H 0.334(5) 0.651(4) -0.015(4) 0.05(2) Uiso 1 1 d . . . B10 B 0.3712(7) 0.6893(6) 0.1140(5) 0.041(2) Uani 1 1 d U . . H10 H 0.314(5) 0.729(4) 0.124(3) 0.04(2) Uiso 1 1 d . . . B11 B 0.4311(7) 0.6235(6) 0.1780(6) 0.049(3) Uani 1 1 d U . . H11 H 0.413(5) 0.610(4) 0.228(4) 0.05(2) Uiso 1 1 d . . . H1 H 0.352(6) 0.625(5) 0.106(5) 0.09(3) Uiso 1 1 d . . . C1 C 0.6577(6) 0.7299(4) 0.1064(4) 0.035(2) Uani 1 1 d U A . C2 C 0.7300(6) 0.7619(4) 0.1082(4) 0.035(2) Uani 1 1 d U . . B21 B 0.8234(6) 0.8012(5) 0.1105(5) 0.038(2) Uani 1 1 d DU A 1 B22 B 0.8486(6) 0.8599(5) 0.0425(5) 0.045(2) Uani 1 1 d DU A 1 H22 H 0.7954 0.8727 -0.0048 0.054 Uiso 1 1 calc R A 1 B23 B 0.8408(7) 0.8966(6) 0.1250(6) 0.060(3) Uani 1 1 d DU A 1 H23 H 0.7836 0.9337 0.1336 0.072 Uiso 1 1 calc R A 1 B24 B 0.8907(7) 0.8345(7) 0.1893(5) 0.070(3) Uani 1 1 d DU A 1 H24 H 0.8668 0.8299 0.2411 0.084 Uiso 1 1 calc R A 1 B25 B 0.9300(7) 0.7584(6) 0.1471(5) 0.063(3) Uani 1 1 d DU A 1 H25 H 0.9319 0.7023 0.1709 0.076 Uiso 1 1 calc R A 1 B26 B 0.9035(6) 0.7740(5) 0.0552(5) 0.047(2) Uani 1 1 d DU A 1 H26 H 0.8871 0.7281 0.0164 0.056 Uiso 1 1 calc R A 1 C27 C 0.9301(7) 0.9209(6) 0.0810(6) 0.057(3) Uani 0.50 1 d PDU A 1 C28 C 0.9543(6) 0.9064(6) 0.1645(5) 0.075(3) Uani 0.50 1 d PDU A 1 B29 B 1.0058(7) 0.8273(7) 0.1788(6) 0.080(3) Uani 0.50 1 d PDU A 1 B30 B 1.0154(7) 0.7893(7) 0.1008(6) 0.058(3) Uani 1 1 d DU A 1 H30 H 1.064(6) 0.756(4) 0.093(4) 0.06(3) Uiso 1 1 d . B 1 B31 B 0.9652(7) 0.8509(6) 0.0376(6) 0.047(3) Uani 1 1 d DU A 1 H31 H 0.985(5) 0.859(4) -0.013(4) 0.06(3) Uiso 1 1 d . C 1 H21 H 1.045(9) 0.861(8) 0.127(8) 0.04(3) Uiso 0.50 1 d P D 1 C27X C 0.9543(6) 0.9064(6) 0.1645(5) 0.075(3) Uani 0.50 1 d PDU A 2 C28X C 1.0058(7) 0.8273(7) 0.1788(6) 0.080(3) Uani 0.50 1 d PDU A 2 B31X B 0.9301(7) 0.9209(6) 0.0810(6) 0.057(3) Uani 0.50 1 d PDU A 2 H21X H 1.006(10) 0.878(8) 0.063(8) 0.04(3) Uiso 0.50 1 d P E 2 H27 H 0.935(6) 0.972(5) 0.068(4) 0.08(3) Uiso 1 1 d . . . H28 H 0.969(10) 0.957(8) 0.201(8) 0.20(6) Uiso 1 1 d . . . H29 H 1.059(7) 0.823(6) 0.234(6) 0.12(4) Uiso 1 1 d . . . N1 N 0.3067(4) 0.2903(3) 0.1491(3) 0.0312(15) Uani 1 1 d U . . C3 C 0.3895(5) 0.2423(4) 0.1446(4) 0.033(2) Uani 1 1 d U . . H3A H 0.4424 0.2746 0.1419 0.040 Uiso 1 1 calc R . . H3B H 0.4044 0.2136 0.1888 0.040 Uiso 1 1 calc R . . C4 C 0.3782(5) 0.1895(4) 0.0828(4) 0.037(2) Uani 1 1 d U . . H4A H 0.3313 0.1523 0.0882 0.045 Uiso 1 1 calc R . . H4B H 0.3570 0.2167 0.0384 0.045 Uiso 1 1 calc R . . C5 C 0.4683(5) 0.1518(4) 0.0792(4) 0.039(2) Uani 1 1 d U . . H5A H 0.4900 0.1258 0.1241 0.047 Uiso 1 1 calc R . . H5B H 0.5147 0.1892 0.0729 0.047 Uiso 1 1 calc R . . C6 C 0.4586(6) 0.0971(5) 0.0184(4) 0.051(2) Uani 1 1 d U . . H6A H 0.4144 0.0590 0.0253 0.076 Uiso 1 1 calc R . . H6B H 0.5182 0.0745 0.0169 0.076 Uiso 1 1 calc R . . H6C H 0.4370 0.1227 -0.0262 0.076 Uiso 1 1 calc R . . C9 C 0.2197(5) 0.2452(4) 0.1441(4) 0.038(2) Uani 1 1 d U . . H9A H 0.2046 0.2246 0.0959 0.046 Uiso 1 1 calc R . . H9B H 0.1691 0.2786 0.1506 0.046 Uiso 1 1 calc R . . C10 C 0.2228(5) 0.1824(5) 0.1967(4) 0.041(2) Uani 1 1 d U . . H10A H 0.2725 0.1480 0.1906 0.049 Uiso 1 1 calc R . . H10B H 0.2365 0.2021 0.2453 0.049 Uiso 1 1 calc R . . C11 C 0.1324(6) 0.1416(5) 0.1862(4) 0.052(2) Uani 1 1 d U . . H11A H 0.1182 0.1230 0.1373 0.063 Uiso 1 1 calc R . . H11B H 0.0830 0.1759 0.1933 0.063 Uiso 1 1 calc R . . C12 C 0.1353(7) 0.0776(5) 0.2374(5) 0.066(3) Uani 1 1 d U . . H12A H 0.1822 0.0424 0.2290 0.098 Uiso 1 1 calc R . . H12B H 0.0754 0.0533 0.2303 0.098 Uiso 1 1 calc R . . H12C H 0.1501 0.0959 0.2859 0.098 Uiso 1 1 calc R . . C13 C 0.2954(5) 0.3448(4) 0.0883(4) 0.035(2) Uani 1 1 d U . . H13A H 0.3544 0.3705 0.0894 0.043 Uiso 1 1 calc R . . H13B H 0.2824 0.3170 0.0435 0.043 Uiso 1 1 calc R . . C14 C 0.2209(6) 0.4018(5) 0.0877(4) 0.046(2) Uani 1 1 d U . . H14A H 0.2284 0.4261 0.1343 0.055 Uiso 1 1 calc R . . H14B H 0.1602 0.3776 0.0787 0.055 Uiso 1 1 calc R . . C15 C 0.2257(6) 0.4594(5) 0.0302(5) 0.055(3) Uani 1 1 d U . . H15A H 0.1875 0.5020 0.0383 0.066 Uiso 1 1 calc R . . H15B H 0.2898 0.4768 0.0346 0.066 Uiso 1 1 calc R . . C16 C 0.1941(7) 0.4316(5) -0.0440(5) 0.065(3) Uani 1 1 d U . . H16A H 0.2314 0.3893 -0.0526 0.097 Uiso 1 1 calc R . . H16B H 0.2008 0.4706 -0.0778 0.097 Uiso 1 1 calc R . . H16C H 0.1296 0.4170 -0.0498 0.097 Uiso 1 1 calc R . . C17 C 0.3237(5) 0.3286(4) 0.2207(4) 0.037(2) Uani 1 1 d U . . H17A H 0.2666 0.3540 0.2269 0.045 Uiso 1 1 calc R . . H17B H 0.3365 0.2907 0.2579 0.045 Uiso 1 1 calc R . . C18 C 0.4017(5) 0.3842(4) 0.2324(4) 0.036(2) Uani 1 1 d U . . H18A H 0.4590 0.3607 0.2241 0.043 Uiso 1 1 calc R . . H18B H 0.3874 0.4254 0.1988 0.043 Uiso 1 1 calc R . . C19 C 0.4143(6) 0.4130(5) 0.3076(4) 0.045(2) Uani 1 1 d U . . H19A H 0.3601 0.4427 0.3133 0.054 Uiso 1 1 calc R . . H19B H 0.4181 0.3710 0.3406 0.054 Uiso 1 1 calc R . . C20 C 0.4998(6) 0.4596(5) 0.3268(4) 0.059(3) Uani 1 1 d U . . H20A H 0.5536 0.4308 0.3206 0.088 Uiso 1 1 calc R . . H20B H 0.5061 0.4753 0.3761 0.088 Uiso 1 1 calc R . . H20C H 0.4949 0.5028 0.2962 0.088 Uiso 1 1 calc R . . N2 N 0.7889(5) 0.1956(5) 0.1273(4) 0.066(2) Uani 1 1 d DU F 1 C29 C 0.7213(16) 0.2468(16) 0.1537(17) 0.052(7) Uani 0.596(10) 1 d PDU F 1 H29A H 0.6710 0.2170 0.1667 0.062 Uiso 0.596(10) 1 calc PR F 1 H29B H 0.6942 0.2796 0.1146 0.062 Uiso 0.596(10) 1 calc PR F 1 C30 C 0.763(2) 0.2949(15) 0.2181(13) 0.054(7) Uani 0.596(10) 1 d PDU F 1 H30A H 0.7905 0.2633 0.2580 0.064 Uiso 0.596(10) 1 calc PR F 1 H30B H 0.8112 0.3271 0.2056 0.064 Uiso 0.596(10) 1 calc PR F 1 C31 C 0.686(4) 0.341(2) 0.239(2) 0.061(11) Uani 0.596(10) 1 d PDU F 1 H31A H 0.6309 0.3097 0.2381 0.073 Uiso 0.596(10) 1 calc PR F 1 H31B H 0.7050 0.3588 0.2880 0.073 Uiso 0.596(10) 1 calc PR F 1 C32 C 0.659(3) 0.407(2) 0.191(3) 0.067(11) Uani 0.596(10) 1 d PDU F 1 H32A H 0.7135 0.4362 0.1883 0.101 Uiso 0.596(10) 1 calc PR F 1 H32B H 0.6146 0.4373 0.2108 0.101 Uiso 0.596(10) 1 calc PR F 1 H32C H 0.6311 0.3900 0.1441 0.101 Uiso 0.596(10) 1 calc PR F 1 C33 C 0.8712(13) 0.2463(16) 0.1070(15) 0.070(6) Uani 0.596(10) 1 d PDU F 1 H33A H 0.9048 0.2671 0.1517 0.084 Uiso 0.596(10) 1 calc PR F 1 H33B H 0.9142 0.2129 0.0888 0.084 Uiso 0.596(10) 1 calc PR F 1 C34 C 0.8517(19) 0.3092(19) 0.0551(18) 0.084(9) Uani 0.596(10) 1 d PDU F 1 H34A H 0.8048 0.3415 0.0699 0.100 Uiso 0.596(10) 1 calc PR F 1 H34B H 0.8258 0.2891 0.0081 0.100 Uiso 0.596(10) 1 calc PR F 1 C35 C 0.939(2) 0.357(2) 0.0486(19) 0.093(11) Uani 0.596(10) 1 d PDU F 1 H35A H 0.9898 0.3241 0.0416 0.112 Uiso 0.596(10) 1 calc PR F 1 H35B H 0.9247 0.3890 0.0066 0.112 Uiso 0.596(10) 1 calc PR F 1 C36 C 0.9694(13) 0.4034(12) 0.1121(11) 0.105(8) Uani 0.596(10) 1 d PDU F 1 H36A H 0.9169 0.4304 0.1236 0.157 Uiso 0.596(10) 1 calc PR F 1 H36B H 1.0161 0.4382 0.1025 0.157 Uiso 0.596(10) 1 calc PR F 1 H36C H 0.9954 0.3720 0.1520 0.157 Uiso 0.596(10) 1 calc PR F 1 C37 C 0.8383(11) 0.1446(12) 0.1790(10) 0.066(5) Uani 0.596(10) 1 d PDU F 1 H37A H 0.8752 0.1716 0.2187 0.079 Uiso 0.596(10) 1 calc PR F 1 H37B H 0.8797 0.1130 0.1569 0.079 Uiso 0.596(10) 1 calc PR F 1 C38 C 0.7651(11) 0.0985(9) 0.2048(10) 0.056(5) Uani 0.596(10) 1 d PDU F 1 H38A H 0.7210 0.1309 0.2231 0.068 Uiso 0.596(10) 1 calc PR F 1 H38B H 0.7310 0.0695 0.1653 0.068 Uiso 0.596(10) 1 calc PR F 1 C39 C 0.8106(16) 0.0473(11) 0.2630(10) 0.072(6) Uani 0.596(10) 1 d PDU F 1 H39A H 0.7633 0.0147 0.2768 0.086 Uiso 0.596(10) 1 calc PR F 1 H39B H 0.8553 0.0161 0.2442 0.086 Uiso 0.596(10) 1 calc PR F 1 C40 C 0.8598(17) 0.0870(12) 0.3283(10) 0.071(7) Uani 0.596(10) 1 d PDU F 1 H40A H 0.9141 0.1119 0.3173 0.106 Uiso 0.596(10) 1 calc PR F 1 H40B H 0.8785 0.0514 0.3662 0.106 Uiso 0.596(10) 1 calc PR F 1 H40C H 0.8184 0.1232 0.3435 0.106 Uiso 0.596(10) 1 calc PR F 1 C29X C 0.719(3) 0.245(3) 0.155(2) 0.081(13) Uani 0.404(10) 1 d PDU F 2 H29C H 0.6600 0.2184 0.1489 0.097 Uiso 0.404(10) 1 calc PR F 2 H29D H 0.7087 0.2889 0.1235 0.097 Uiso 0.404(10) 1 calc PR F 2 C30X C 0.742(3) 0.273(2) 0.231(2) 0.053(10) Uani 0.404(10) 1 d PDU F 2 H30C H 0.7324 0.2327 0.2642 0.064 Uiso 0.404(10) 1 calc PR F 2 H30D H 0.8067 0.2883 0.2426 0.064 Uiso 0.404(10) 1 calc PR F 2 C31X C 0.678(5) 0.338(3) 0.240(4) 0.063(13) Uani 0.404(10) 1 d PDU F 2 H31C H 0.6141 0.3208 0.2294 0.076 Uiso 0.404(10) 1 calc PR F 2 H31D H 0.6910 0.3541 0.2898 0.076 Uiso 0.404(10) 1 calc PR F 2 C32X C 0.690(5) 0.403(3) 0.193(4) 0.077(17) Uani 0.404(10) 1 d PDU F 2 H32D H 0.7526 0.4219 0.2046 0.116 Uiso 0.404(10) 1 calc PR F 2 H32E H 0.6464 0.4415 0.1993 0.116 Uiso 0.404(10) 1 calc PR F 2 H32F H 0.6783 0.3870 0.1431 0.116 Uiso 0.404(10) 1 calc PR F 2 C33X C 0.881(2) 0.221(3) 0.129(3) 0.070(6) Uani 0.404(10) 1 d PDU F 2 H33C H 0.9194 0.1836 0.1116 0.084 Uiso 0.404(10) 1 calc PR F 2 H33D H 0.9101 0.2356 0.1777 0.084 Uiso 0.404(10) 1 calc PR F 2 C34X C 0.866(2) 0.288(2) 0.080(2) 0.065(11) Uani 0.404(10) 1 d PDU F 2 H34C H 0.8277 0.3249 0.0984 0.079 Uiso 0.404(10) 1 calc PR F 2 H34D H 0.8359 0.2729 0.0323 0.079 Uiso 0.404(10) 1 calc PR F 2 C35X C 0.9622(16) 0.3187(15) 0.0784(15) 0.057(8) Uani 0.404(10) 1 d PDU F 2 H35C H 0.9921 0.3329 0.1265 0.068 Uiso 0.404(10) 1 calc PR F 2 H35D H 1.0005 0.2808 0.0609 0.068 Uiso 0.404(10) 1 calc PR F 2 C36X C 0.954(3) 0.385(3) 0.030(3) 0.078(12) Uani 0.404(10) 1 d PDU F 2 H36D H 0.9283 0.3700 -0.0181 0.118 Uiso 0.404(10) 1 calc PR F 2 H36E H 1.0146 0.4068 0.0313 0.118 Uiso 0.404(10) 1 calc PR F 2 H36F H 0.9133 0.4213 0.0463 0.118 Uiso 0.404(10) 1 calc PR F 2 C37X C 0.792(2) 0.1234(19) 0.1821(16) 0.066(5) Uani 0.404(10) 1 d PDU F 2 H37C H 0.7320 0.1217 0.1980 0.079 Uiso 0.404(10) 1 calc PR F 2 H37D H 0.7959 0.0788 0.1536 0.079 Uiso 0.404(10) 1 calc PR F 2 C38X C 0.8655(16) 0.1170(13) 0.2475(11) 0.063(7) Uani 0.404(10) 1 d PDU F 2 H38C H 0.9258 0.1140 0.2322 0.076 Uiso 0.404(10) 1 calc PR F 2 H38D H 0.8651 0.1628 0.2752 0.076 Uiso 0.404(10) 1 calc PR F 2 C39X C 0.858(2) 0.0531(17) 0.2958(16) 0.056(9) Uani 0.404(10) 1 d PDU F 2 H39C H 0.8021 0.0593 0.3170 0.068 Uiso 0.404(10) 1 calc PR F 2 H39D H 0.8507 0.0074 0.2677 0.068 Uiso 0.404(10) 1 calc PR F 2 C40X C 0.9395(18) 0.0459(17) 0.3536(12) 0.082(9) Uani 0.404(10) 1 d PDU F 2 H40D H 0.9937 0.0336 0.3332 0.123 Uiso 0.404(10) 1 calc PR F 2 H40E H 0.9284 0.0069 0.3861 0.123 Uiso 0.404(10) 1 calc PR F 2 H40F H 0.9499 0.0924 0.3793 0.123 Uiso 0.404(10) 1 calc PR F 2 C21 C 0.7366(6) 0.1637(5) 0.0583(4) 0.056(3) Uani 1 1 d U . . H21A H 0.6842 0.1349 0.0691 0.068 Uiso 1 1 calc R F 1 H21B H 0.7113 0.2048 0.0273 0.068 Uiso 1 1 calc R F 1 C22 C 0.7918(6) 0.1150(5) 0.0176(4) 0.055(3) Uani 1 1 d U F . H22A H 0.8198 0.0744 0.0482 0.066 Uiso 1 1 calc R . . H22B H 0.8417 0.1437 0.0026 0.066 Uiso 1 1 calc R . . C23 C 0.7292(7) 0.0842(5) -0.0465(5) 0.062(3) Uani 1 1 d U . . H23A H 0.6992 0.1253 -0.0752 0.075 Uiso 1 1 calc R F . H23B H 0.6806 0.0546 -0.0307 0.075 Uiso 1 1 calc R . . C24 C 0.7800(7) 0.0364(6) -0.0923(5) 0.071(3) Uani 1 1 d U F . H24A H 0.8235 0.0667 -0.1125 0.107 Uiso 1 1 calc R . . H24B H 0.7357 0.0145 -0.1305 0.107 Uiso 1 1 calc R . . H24C H 0.8132 -0.0026 -0.0634 0.107 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 B1 0.032(5) 0.038(5) 0.033(5) -0.005(4) 0.010(4) -0.004(4) B2 0.035(5) 0.048(6) 0.050(6) 0.012(5) 0.006(5) -0.005(4) B3 0.041(6) 0.043(6) 0.083(7) -0.016(5) 0.023(5) -0.009(5) B4 0.045(6) 0.079(8) 0.039(5) -0.015(5) 0.017(5) -0.021(5) B5 0.038(5) 0.051(6) 0.039(5) 0.009(5) 0.004(4) -0.003(5) B6 0.034(5) 0.050(6) 0.036(5) -0.005(5) 0.008(4) 0.001(5) C7 0.049(6) 0.041(6) 0.082(7) 0.009(5) 0.017(5) -0.010(5) C8 0.053(6) 0.058(6) 0.067(6) -0.032(5) 0.024(5) -0.023(5) B9 0.041(6) 0.074(8) 0.037(6) -0.002(5) 0.005(5) -0.016(5) B10 0.035(5) 0.041(7) 0.047(6) -0.001(5) 0.013(4) 0.000(5) B11 0.039(6) 0.068(7) 0.040(6) 0.012(5) 0.011(5) -0.006(5) C1 0.037(5) 0.037(5) 0.032(5) -0.002(4) 0.008(4) 0.001(4) C2 0.038(5) 0.040(5) 0.030(5) -0.004(4) 0.012(4) 0.000(4) B21 0.033(5) 0.047(6) 0.035(5) -0.004(4) 0.011(4) -0.003(4) B22 0.036(5) 0.050(6) 0.050(5) 0.008(5) 0.008(5) -0.008(5) B23 0.035(6) 0.057(6) 0.094(8) -0.031(6) 0.026(5) -0.013(5) B24 0.039(6) 0.129(10) 0.044(6) -0.018(6) 0.016(5) -0.032(6) B25 0.036(6) 0.084(7) 0.071(7) 0.035(6) 0.013(5) 0.005(5) B26 0.042(6) 0.050(6) 0.054(6) -0.002(5) 0.021(5) 0.001(5) C27 0.039(6) 0.052(6) 0.081(7) 0.008(5) 0.014(5) -0.007(5) C28 0.049(6) 0.101(7) 0.077(6) -0.037(6) 0.020(5) -0.029(5) B29 0.038(6) 0.136(9) 0.064(7) 0.029(7) 0.005(5) -0.008(6) B30 0.034(6) 0.072(9) 0.073(8) 0.013(6) 0.023(5) 0.008(6) B31 0.034(6) 0.063(8) 0.046(6) -0.002(5) 0.010(5) -0.011(5) C27X 0.049(6) 0.101(7) 0.077(6) -0.037(6) 0.020(5) -0.029(5) C28X 0.038(6) 0.136(9) 0.064(7) 0.029(7) 0.005(5) -0.008(6) B31X 0.039(6) 0.052(6) 0.081(7) 0.008(5) 0.014(5) -0.007(5) N1 0.028(4) 0.041(4) 0.026(3) -0.001(3) 0.006(3) -0.001(3) C3 0.028(4) 0.045(5) 0.028(4) -0.002(4) 0.005(4) 0.004(4) C4 0.037(5) 0.046(5) 0.029(4) -0.002(4) 0.002(4) 0.004(4) C5 0.042(5) 0.037(5) 0.040(5) 0.000(4) 0.007(4) 0.002(4) C6 0.064(6) 0.041(6) 0.051(6) -0.006(4) 0.018(5) 0.003(5) C9 0.029(5) 0.051(6) 0.035(5) -0.005(4) 0.006(4) -0.002(4) C10 0.039(5) 0.050(6) 0.035(5) -0.001(4) 0.009(4) -0.004(4) C11 0.053(6) 0.060(6) 0.045(5) -0.006(5) 0.011(5) -0.019(5) C12 0.076(7) 0.057(7) 0.069(7) -0.002(5) 0.029(6) -0.021(6) C13 0.038(5) 0.039(5) 0.031(4) 0.001(4) 0.010(4) 0.003(4) C14 0.051(6) 0.052(6) 0.037(5) -0.002(4) 0.011(4) 0.011(5) C15 0.053(6) 0.048(6) 0.065(6) 0.009(5) 0.012(5) 0.016(5) C16 0.075(7) 0.071(7) 0.051(6) 0.018(5) 0.018(5) 0.019(6) C17 0.039(5) 0.045(5) 0.029(4) -0.004(4) 0.009(4) 0.003(4) C18 0.043(5) 0.037(5) 0.029(4) 0.000(4) 0.008(4) -0.001(4) C19 0.055(6) 0.047(6) 0.034(5) -0.008(4) 0.011(4) -0.005(5) C20 0.080(7) 0.054(6) 0.039(5) -0.010(5) 0.003(5) -0.017(6) N2 0.052(5) 0.089(6) 0.051(5) -0.029(4) -0.008(4) 0.032(5) C29 0.035(11) 0.063(14) 0.052(17) -0.025(12) -0.009(11) 0.006(11) C30 0.054(17) 0.070(17) 0.039(13) -0.009(10) 0.014(9) 0.006(11) C31 0.08(2) 0.07(2) 0.043(17) 0.000(13) 0.027(18) 0.018(18) C32 0.07(3) 0.071(17) 0.070(17) 0.009(14) 0.040(16) 0.018(15) C33 0.027(8) 0.12(2) 0.06(2) -0.027(11) -0.015(10) 0.034(12) C34 0.051(15) 0.12(2) 0.08(2) -0.014(13) 0.005(14) 0.005(14) C35 0.025(13) 0.15(4) 0.11(3) -0.05(2) 0.023(17) 0.004(19) C36 0.077(15) 0.104(18) 0.14(2) -0.014(14) 0.024(14) -0.002(12) C37 0.031(12) 0.105(13) 0.058(8) -0.010(8) -0.004(9) 0.031(10) C38 0.053(12) 0.041(10) 0.064(12) -0.004(8) -0.018(9) -0.006(8) C39 0.085(18) 0.064(13) 0.062(14) -0.003(10) 0.001(11) 0.001(12) C40 0.079(15) 0.078(18) 0.051(13) 0.010(11) 0.002(12) 0.003(13) C29X 0.08(2) 0.12(3) 0.05(2) 0.006(19) 0.03(2) 0.07(2) C30X 0.030(18) 0.07(2) 0.057(19) -0.014(17) 0.014(14) 0.005(17) C31X 0.05(3) 0.06(3) 0.07(3) -0.028(19) 0.00(2) 0.00(2) C32X 0.08(4) 0.06(2) 0.11(3) -0.03(2) 0.05(3) 0.01(2) C33X 0.027(8) 0.12(2) 0.06(2) -0.027(11) -0.015(10) 0.034(12) C34X 0.028(15) 0.10(3) 0.06(3) -0.035(18) -0.016(17) 0.027(19) C35X 0.028(13) 0.083(19) 0.050(17) -0.023(12) -0.017(11) 0.034(12) C36X 0.06(3) 0.09(3) 0.08(2) -0.015(17) -0.01(2) 0.03(2) C37X 0.031(12) 0.105(13) 0.058(8) -0.010(8) -0.004(9) 0.031(10) C38X 0.077(17) 0.066(16) 0.045(13) 0.011(11) 0.008(11) -0.017(14) C39X 0.06(2) 0.05(2) 0.06(2) 0.012(16) 0.011(16) -0.018(18) C40X 0.08(2) 0.11(2) 0.057(16) 0.033(15) 0.005(13) -0.009(18) C21 0.049(6) 0.072(7) 0.043(5) -0.018(5) -0.003(4) 0.015(5) C22 0.053(6) 0.066(7) 0.045(5) -0.010(5) 0.006(5) 0.015(5) C23 0.064(7) 0.071(7) 0.051(6) -0.017(5) 0.008(5) -0.003(6) C24 0.095(8) 0.067(7) 0.053(6) -0.012(5) 0.016(6) 0.013(6) _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 B1 C1 1.552(12) . y B1 B2 1.768(13) . y B1 B4 1.774(13) . y B1 B3 1.774(14) . y B1 B5 1.810(13) . y B1 B6 1.810(13) . y B2 C7 1.699(14) . y B2 B3 1.749(15) . y B2 B6 1.752(14) . y B2 B11 1.784(14) . y B2 H2 1.1200 . n B3 C8 1.696(14) . y B3 C7 1.720(14) . y B3 B4 1.747(16) . y B3 H3 1.1200 . n B4 C8 1.703(14) . y B4 B5 1.751(15) . y B4 B9 1.782(14) . y B4 H4 1.1200 . n B5 B9 1.764(15) . y B5 B10 1.782(13) . y B5 B6 1.813(13) . y B5 H5 1.1200 . n B6 B11 1.755(15) . y B6 B10 1.780(14) . y B6 H6 1.1200 . n C7 C8 1.539(13) . y C7 B11 1.610(15) . y C7 H7 0.98(10) . n C8 B9 1.597(15) . y C8 H8 0.94(8) . n B9 B10 1.813(15) . y B9 H9 1.08(7) . n B10 B11 1.833(15) . y B10 H10 1.15(7) . n B10 H1 1.21(10) . n B11 H11 1.07(7) . n C1 C2 1.215(10) . y C2 B21 1.553(12) . y B21 B24 1.770(13) . y B21 B23 1.773(14) . y B21 B22 1.782(12) . y B21 B25 1.793(13) . y B21 B26 1.798(12) . y B22 C27 1.712(13) . y B22 B23 1.747(13) . y B22 B31 1.754(13) . y B22 B26 1.761(13) . y B22 H22 1.1200 . n B23 C28 1.729(13) . y B23 B24 1.743(15) . y B23 C27 1.751(13) . y B23 H23 1.1200 . n B24 C28 1.730(14) . y B24 B25 1.757(15) . y B24 B29 1.758(14) . y B24 H24 1.1200 . n B25 B29 1.723(15) . y B25 B30 1.764(14) . y B25 B26 1.768(13) . y B25 H25 1.1200 . n B26 B31 1.740(14) . y B26 B30 1.757(14) . y B26 H26 1.1200 . n C27 C28 1.607(13) . y C27 B31 1.657(14) . y C27 H21X 1.45(15) . n C27 H27 0.98(9) . n C28 B29 1.631(14) . y C28 H28 1.15(15) . n B29 B30 1.683(15) . y B29 H21 1.37(14) . n B29 H29 1.20(10) . n B30 B31 1.726(14) . y B30 H30 0.97(8) . n B30 H21 1.44(14) . n B31 H31 1.08(8) . n B31 H21X 0.86(15) . n N1 C9 1.518(9) . y N1 C3 1.521(9) . y N1 C13 1.522(9) . y N1 C17 1.527(9) . y C3 C4 1.517(10) . y C3 H3A 0.9900 . n C3 H3B 0.9900 . n C4 C5 1.515(10) . n C4 H4A 0.9900 . n C4 H4B 0.9900 . n C5 C6 1.526(10) . n C5 H5A 0.9900 . n C5 H5B 0.9900 . n C6 H6A 0.9800 . n C6 H6B 0.9800 . n C6 H6C 0.9800 . n C9 C10 1.524(10) . n C9 H9A 0.9900 . n C9 H9B 0.9900 . n C10 C11 1.515(10) . n C10 H10A 0.9900 . n C10 H10B 0.9900 . n C11 C12 1.523(12) . n C11 H11A 0.9900 . n C11 H11B 0.9900 . n C12 H12A 0.9800 . n C12 H12B 0.9800 . n C12 H12C 0.9800 . n C13 C14 1.515(10) . n C13 H13A 0.9900 . n C13 H13B 0.9900 . n C14 C15 1.537(11) . n C14 H14A 0.9900 . n C14 H14B 0.9900 . n C15 C16 1.511(12) . n C15 H15A 0.9900 . n C15 H15B 0.9900 . n C16 H16A 0.9800 . n C16 H16B 0.9800 . n C16 H16C 0.9800 . n C17 C18 1.524(10) . n C17 H17A 0.9900 . n C17 H17B 0.9900 . n C18 C19 1.521(10) . n C18 H18A 0.9900 . n C18 H18B 0.9900 . n C19 C20 1.516(11) . n C19 H19A 0.9900 . n C19 H19B 0.9900 . n C20 H20A 0.9800 . n C20 H20B 0.9800 . n C20 H20C 0.9800 . n N2 C37 1.462(17) . y N2 C29 1.521(19) . y N2 C21 1.532(10) . y N2 C33 1.63(2) . y C29 C30 1.55(2) . n C29 H29A 0.9900 . n C29 H29B 0.9900 . n C30 C31 1.53(2) . n C30 H30A 0.9900 . n C30 H30B 0.9900 . n C31 C32 1.52(2) . n C31 H31A 0.9900 . n C31 H31B 0.9900 . n C32 H32A 0.9800 . n C32 H32B 0.9800 . n C32 H32C 0.9800 . n C33 C34 1.52(2) . n C33 H33A 0.9900 . n C33 H33B 0.9900 . n C34 C35 1.58(3) . n C34 H34A 0.9900 . n C34 H34B 0.9900 . n C35 C36 1.49(4) . n C35 H35A 0.9900 . n C35 H35B 0.9900 . n C36 H36A 0.9800 . n C36 H36B 0.9800 . n C36 H36C 0.9800 . n C37 C38 1.52(2) . n C37 H37A 0.9900 . n C37 H37B 0.9900 . n C38 C39 1.52(2) . n C38 H38A 0.9900 . n C38 H38B 0.9900 . n C39 C40 1.52(3) . n C39 H39A 0.9900 . n C39 H39B 0.9900 . n C40 H40A 0.9800 . n C40 H40B 0.9800 . n C40 H40C 0.9800 . n C29X C30X 1.54(3) . n C29X H29C 0.9900 . n C29X H29D 0.9900 . n C30X C31X 1.54(3) . n C30X H30C 0.9900 . n C30X H30D 0.9900 . n C31X C32X 1.53(4) . n C31X H31C 0.9900 . n C31X H31D 0.9900 . n C32X H32D 0.9800 . n C32X H32E 0.9800 . n C32X H32F 0.9800 . n C33X C34X 1.53(3) . n C33X H33C 0.9900 . n C33X H33D 0.9900 . n C34X C35X 1.54(3) . n C34X H34C 0.9900 . n C34X H34D 0.9900 . n C35X C36X 1.52(4) . n C35X H35C 0.9900 . n C35X H35D 0.9900 . n C36X H36D 0.9800 . n C36X H36E 0.9800 . n C36X H36F 0.9800 . n C37X C38X 1.52(3) . n C37X H37C 0.9900 . n C37X H37D 0.9900 . n C38X C39X 1.51(3) . n C38X H38C 0.9900 . n C38X H38D 0.9900 . n C39X C40X 1.50(3) . n C39X H39C 0.9900 . n C39X H39D 0.9900 . n C40X H40D 0.9800 . n C40X H40E 0.9800 . n C40X H40F 0.9800 . n C21 C22 1.515(11) . n C21 H21A 0.9900 . n C21 H21B 0.9900 . n C22 C23 1.516(11) . n C22 H22A 0.9900 . n C22 H22B 0.9900 . n C23 C24 1.529(12) . n C23 H23A 0.9900 . n C23 H23B 0.9900 . n C24 H24A 0.9800 . n C24 H24B 0.9800 . n C24 H24C 0.9800 . n 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 B1 B2 122.7(7) . . y C1 B1 B4 122.2(7) . . y B2 B1 B4 106.3(7) . . y C1 B1 B3 122.4(7) . . y B2 B1 B3 59.2(6) . . y B4 B1 B3 59.0(6) . . y C1 B1 B5 123.5(7) . . y B2 B1 B5 106.4(6) . . y B4 B1 B5 58.5(6) . . y B3 B1 B5 105.2(7) . . y C1 B1 B6 123.9(7) . . y B2 B1 B6 58.6(5) . . y B4 B1 B6 106.2(6) . . y B3 B1 B6 105.3(7) . . y B5 B1 B6 60.1(5) . . y C7 B2 B3 59.8(6) . . y C7 B2 B6 100.9(7) . . y B3 B2 B6 108.9(7) . . y C7 B2 B1 104.9(7) . . y B3 B2 B1 60.6(6) . . y B6 B2 B1 61.9(5) . . y C7 B2 B11 55.0(6) . . y B3 B2 B11 107.2(7) . . y B6 B2 B11 59.5(6) . . y B1 B2 B11 109.5(7) . . y C7 B2 H2 127.1 . . n B3 B2 H2 120.6 . . n B6 B2 H2 122.8 . . n B1 B2 H2 120.5 . . n B11 B2 H2 122.5 . . n C8 B3 C7 53.5(5) . . y C8 B3 B4 59.3(6) . . y C7 B3 B4 102.6(7) . . y C8 B3 B2 102.1(7) . . y C7 B3 B2 58.6(6) . . y B4 B3 B2 108.3(7) . . y C8 B3 B1 104.1(8) . . y C7 B3 B1 103.7(7) . . y B4 B3 B1 60.5(6) . . y B2 B3 B1 60.2(5) . . y C8 B3 H3 126.3 . . n C7 B3 H3 126.5 . . n B4 B3 H3 121.8 . . n B2 B3 H3 122.4 . . n B1 B3 H3 122.7 . . n C8 B4 B3 58.9(6) . . y C8 B4 B5 101.0(7) . . y B3 B4 B5 108.9(7) . . y C8 B4 B1 103.8(7) . . y B3 B4 B1 60.5(6) . . y B5 B4 B1 61.8(6) . . y C8 B4 B9 54.5(6) . . y B3 B4 B9 105.9(7) . . y B5 B4 B9 59.9(6) . . y B1 B4 B9 108.7(7) . . y C8 B4 H4 127.7 . . n B3 B4 H4 121.2 . . n B5 B4 H4 122.4 . . n B1 B4 H4 121.0 . . n B9 B4 H4 123.1 . . n B4 B5 B9 60.9(6) . . y B4 B5 B10 112.0(8) . . y B9 B5 B10 61.5(6) . . y B4 B5 B1 59.7(5) . . y B9 B5 B1 107.9(8) . . y B10 B5 B1 110.4(7) . . y B4 B5 B6 107.0(7) . . y B9 B5 B6 105.7(7) . . y B10 B5 B6 59.4(5) . . y B1 B5 B6 60.0(5) . . y B4 B5 H5 120.6 . . n B9 B5 H5 122.2 . . n B10 B5 H5 119.1 . . n B1 B5 H5 121.2 . . n B6 B5 H5 123.8 . . n B2 B6 B11 61.2(6) . . y B2 B6 B10 112.1(7) . . y B11 B6 B10 62.5(6) . . y B2 B6 B1 59.5(5) . . y B11 B6 B1 108.8(7) . . y B10 B6 B1 110.4(7) . . y B2 B6 B5 106.9(7) . . y B11 B6 B5 107.2(7) . . y B10 B6 B5 59.4(5) . . y B1 B6 B5 59.9(5) . . y B2 B6 H6 120.9 . . n B11 B6 H6 120.9 . . n B10 B6 H6 118.9 . . n B1 B6 H6 121.2 . . n B5 B6 H6 123.5 . . n C8 C7 B11 113.7(8) . . y C8 C7 B2 111.7(7) . . y B11 C7 B2 65.2(6) . . y C8 C7 B3 62.5(6) . . y B11 C7 B3 117.3(8) . . y B2 C7 B3 61.6(6) . . y C8 C7 H7 117(6) . . n B11 C7 H7 122(6) . . n B2 C7 H7 117(6) . . n B3 C7 H7 111(6) . . n C7 C8 B9 112.9(8) . . y C7 C8 B3 64.0(6) . . y B9 C8 B3 117.6(8) . . y C7 C8 B4 113.1(8) . . y B9 C8 B4 65.3(7) . . y B3 C8 B4 61.8(6) . . y C7 C8 H8 119(5) . . n B9 C8 H8 117(5) . . n B3 C8 H8 117(5) . . n B4 C8 H8 119(5) . . n C8 B9 B5 104.9(8) . . y C8 B9 B4 60.2(6) . . y B5 B9 B4 59.2(6) . . y C8 B9 B10 107.0(8) . . y B5 B9 B10 59.7(6) . . y B4 B9 B10 109.1(7) . . y C8 B9 H9 125(4) . . n B5 B9 H9 122(4) . . n B4 B9 H9 120(4) . . n B10 B9 H9 121(4) . . n B6 B10 B5 61.2(5) . . y B6 B10 B9 105.0(7) . . y B5 B10 B9 58.8(6) . . y B6 B10 B11 58.1(6) . . y B5 B10 B11 105.2(7) . . y B9 B10 B11 100.7(8) . . y B6 B10 H10 118(4) . . n B5 B10 H10 119(3) . . n B9 B10 H10 128(3) . . n B11 B10 H10 126(3) . . n B6 B10 H1 114(4) . . n B5 B10 H1 115(4) . . n B9 B10 H1 62(4) . . n B11 B10 H1 62(4) . . n H10 B10 H1 118(6) . . n C7 B11 B6 104.5(7) . . y C7 B11 B2 59.8(6) . . y B6 B11 B2 59.3(6) . . y C7 B11 B10 105.5(8) . . y B6 B11 B10 59.4(6) . . y B2 B11 B10 108.2(7) . . y C7 B11 H11 122(4) . . n B6 B11 H11 124(4) . . n B2 B11 H11 118(4) . . n B10 B11 H11 125(4) . . n C2 C1 B1 177.9(8) . . y C1 C2 B21 178.8(8) . . y C2 B21 B24 123.3(7) . . y C2 B21 B23 124.2(7) . . y B24 B21 B23 58.9(6) . . y C2 B21 B22 123.9(7) . . y B24 B21 B22 105.3(7) . . y B23 B21 B22 58.9(5) . . y C2 B21 B25 122.1(7) . . y B24 B21 B25 59.1(6) . . y B23 B21 B25 105.7(7) . . y B22 B21 B25 105.4(6) . . y C2 B21 B26 122.3(7) . . y B24 B21 B26 105.7(7) . . y B23 B21 B26 105.7(7) . . y B22 B21 B26 58.9(5) . . y B25 B21 B26 59.0(5) . . y C27 B22 B23 60.8(5) . . y C27 B22 B31 57.1(6) . . y B23 B22 B31 107.9(7) . . y C27 B22 B26 104.1(7) . . y B23 B22 B26 108.4(7) . . y B31 B22 B26 59.3(5) . . y C27 B22 B21 107.2(7) . . y B23 B22 B21 60.3(5) . . y B31 B22 B21 108.6(7) . . y B26 B22 B21 61.0(5) . . y C27 B22 H22 124.1 . . n B23 B22 H22 120.8 . . n B31 B22 H22 122.4 . . n B26 B22 H22 122.7 . . n B21 B22 H22 120.9 . . n C28 B23 B24 59.8(6) . . y C28 B23 B22 103.0(6) . . y B24 B23 B22 108.1(7) . . y C28 B23 C27 55.0(5) . . y B24 B23 C27 104.3(7) . . y B22 B23 C27 58.6(5) . . y C28 B23 B21 106.0(7) . . y B24 B23 B21 60.5(5) . . y B22 B23 B21 60.8(5) . . y C27 B23 B21 105.9(7) . . y C28 B23 H23 125.2 . . n B24 B23 H23 121.7 . . n B22 B23 H23 122.6 . . n C27 B23 H23 125.1 . . n B21 B23 H23 121.5 . . n C28 B24 B23 59.7(6) . . y C28 B24 B25 103.3(7) . . y B23 B24 B25 108.6(7) . . y C28 B24 B29 55.8(6) . . y B23 B24 B29 105.4(7) . . y B25 B24 B29 58.7(6) . . y C28 B24 B21 106.0(7) . . y B23 B24 B21 60.6(5) . . y B25 B24 B21 61.1(5) . . y B29 B24 B21 106.8(7) . . y C28 B24 H24 125.1 . . n B23 B24 H24 121.3 . . n B25 B24 H24 122.4 . . n B29 B24 H24 124.3 . . n B21 B24 H24 121.3 . . n B29 B25 B24 60.7(6) . . y B29 B25 B30 57.7(6) . . y B24 B25 B30 108.0(8) . . y B29 B25 B26 104.7(7) . . y B24 B25 B26 107.6(7) . . y B30 B25 B26 59.7(6) . . y B29 B25 B21 107.3(8) . . y B24 B25 B21 59.8(5) . . y B30 B25 B21 108.9(7) . . y B26 B25 B21 60.6(5) . . y B29 B25 H25 123.6 . . n B24 B25 H25 121.3 . . n B30 B25 H25 122.0 . . n B26 B25 H25 122.8 . . n B21 B25 H25 121.1 . . n B31 B26 B30 59.1(6) . . y B31 B26 B22 60.1(5) . . y B30 B26 B22 107.5(7) . . y B31 B26 B25 107.0(7) . . y B30 B26 B25 60.1(5) . . y B22 B26 B25 107.4(7) . . y B31 B26 B21 108.5(7) . . y B30 B26 B21 109.0(7) . . y B22 B26 B21 60.1(5) . . y B25 B26 B21 60.4(5) . . y B31 B26 H26 122.1 . . n B30 B26 H26 121.8 . . n B22 B26 H26 122.0 . . n B25 B26 H26 122.2 . . n B21 B26 H26 120.9 . . n C28 C27 B31 110.1(8) . . y C28 C27 B22 110.0(7) . . y B31 C27 B22 62.7(6) . . y C28 C27 B23 61.8(6) . . y B31 C27 B23 112.3(7) . . y B22 C27 B23 60.6(5) . . y C28 C27 H21X 96(6) . . n B31 C27 H21X 31(6) . . n B22 C27 H21X 94(6) . . n B23 C27 H21X 131(6) . . n C28 C27 H27 113(5) . . n B31 C27 H27 125(5) . . n B22 C27 H27 126(5) . . n B23 C27 H27 117(5) . . n H21X C27 H27 111(8) . . n C27 C28 B29 109.3(8) . . y C27 C28 B23 63.2(6) . . y B29 C28 B23 111.9(7) . . y C27 C28 B24 111.4(7) . . y B29 C28 B24 63.0(6) . . y B23 C28 B24 60.5(6) . . y C27 C28 H28 117(7) . . n B29 C28 H28 125(7) . . n B23 C28 H28 114(7) . . n B24 C28 H28 119(7) . . n C28 B29 B30 108.9(8) . . y C28 B29 B25 109.1(7) . . y B30 B29 B25 62.4(6) . . y C28 B29 B24 61.3(6) . . y B30 B29 B24 111.7(7) . . y B25 B29 B24 60.6(6) . . y C28 B29 H21 74(6) . . n B30 B29 H21 55(6) . . n B25 B29 H21 114(6) . . n B24 B29 H21 126(6) . . n C28 B29 H29 115(5) . . n B30 B29 H29 128(5) . . n B25 B29 H29 123(5) . . n B24 B29 H29 114(5) . . n H21 B29 H29 112(8) . . n B29 B30 B31 105.5(8) . . y B29 B30 B26 106.9(7) . . y B31 B30 B26 59.9(6) . . y B29 B30 B25 59.9(6) . . y B31 B30 B25 107.8(7) . . y B26 B30 B25 60.3(5) . . y B29 B30 H30 125(5) . . n B31 B30 H30 123(5) . . n B26 B30 H30 119(5) . . n B25 B30 H30 119(5) . . n B29 B30 H21 51(6) . . n B31 B30 H21 74(6) . . n B26 B30 H21 121(5) . . n B25 B30 H21 108(6) . . n H30 B30 H21 116(7) . . n C27 B31 B30 106.3(8) . . y C27 B31 B26 107.4(7) . . y B30 B31 B26 60.9(6) . . y C27 B31 B22 60.2(6) . . y B30 B31 B22 109.3(7) . . y B26 B31 B22 60.5(5) . . y C27 B31 H31 121(4) . . n B30 B31 H31 125(4) . . n B26 B31 H31 121(4) . . n B22 B31 H31 118(4) . . n C27 B31 H21X 61(10) . . n B30 B31 H21X 79(10) . . n B26 B31 H21X 134(10) . . n B22 B31 H21X 120(10) . . n H31 B31 H21X 100(10) . . n C9 N1 C3 111.7(6) . . n C9 N1 C13 109.1(6) . . n C3 N1 C13 108.2(5) . . n C9 N1 C17 107.9(5) . . n C3 N1 C17 107.9(5) . . n C13 N1 C17 112.0(6) . . n C4 C3 N1 115.5(6) . . n C4 C3 H3A 108.4 . . n N1 C3 H3A 108.4 . . n C4 C3 H3B 108.4 . . n N1 C3 H3B 108.4 . . n H3A C3 H3B 107.5 . . n C5 C4 C3 110.4(6) . . n C5 C4 H4A 109.6 . . n C3 C4 H4A 109.6 . . n C5 C4 H4B 109.6 . . n C3 C4 H4B 109.6 . . n H4A C4 H4B 108.1 . . n C4 C5 C6 111.6(7) . . n C4 C5 H5A 109.3 . . n C6 C5 H5A 109.3 . . n C4 C5 H5B 109.3 . . n C6 C5 H5B 109.3 . . n H5A C5 H5B 108.0 . . n C5 C6 H6A 109.5 . . n C5 C6 H6B 109.5 . . n H6A C6 H6B 109.5 . . n C5 C6 H6C 109.5 . . n H6A C6 H6C 109.5 . . n H6B C6 H6C 109.5 . . n N1 C9 C10 116.0(6) . . n N1 C9 H9A 108.3 . . n C10 C9 H9A 108.3 . . n N1 C9 H9B 108.3 . . n C10 C9 H9B 108.3 . . n H9A C9 H9B 107.4 . . n C11 C10 C9 110.9(7) . . n C11 C10 H10A 109.5 . . n C9 C10 H10A 109.5 . . n C11 C10 H10B 109.5 . . n C9 C10 H10B 109.5 . . n H10A C10 H10B 108.0 . . n C10 C11 C12 111.5(7) . . n C10 C11 H11A 109.3 . . n C12 C11 H11A 109.3 . . n C10 C11 H11B 109.3 . . n C12 C11 H11B 109.3 . . n H11A C11 H11B 108.0 . . n C11 C12 H12A 109.5 . . n C11 C12 H12B 109.5 . . n H12A C12 H12B 109.5 . . n C11 C12 H12C 109.5 . . n H12A C12 H12C 109.5 . . n H12B C12 H12C 109.5 . . n C14 C13 N1 115.8(6) . . n C14 C13 H13A 108.3 . . n N1 C13 H13A 108.3 . . n C14 C13 H13B 108.3 . . n N1 C13 H13B 108.3 . . n H13A C13 H13B 107.4 . . n C13 C14 C15 110.4(7) . . n C13 C14 H14A 109.6 . . n C15 C14 H14A 109.6 . . n C13 C14 H14B 109.6 . . n C15 C14 H14B 109.6 . . n H14A C14 H14B 108.1 . . n C16 C15 C14 114.0(8) . . n C16 C15 H15A 108.8 . . n C14 C15 H15A 108.8 . . n C16 C15 H15B 108.8 . . n C14 C15 H15B 108.8 . . n H15A C15 H15B 107.7 . . n C15 C16 H16A 109.5 . . n C15 C16 H16B 109.5 . . n H16A C16 H16B 109.5 . . n C15 C16 H16C 109.5 . . n H16A C16 H16C 109.5 . . n H16B C16 H16C 109.5 . . n C18 C17 N1 116.0(6) . . y C18 C17 H17A 108.3 . . n N1 C17 H17A 108.3 . . n C18 C17 H17B 108.3 . . n N1 C17 H17B 108.3 . . n H17A C17 H17B 107.4 . . n C19 C18 C17 109.5(6) . . n C19 C18 H18A 109.8 . . n C17 C18 H18A 109.8 . . n C19 C18 H18B 109.8 . . n C17 C18 H18B 109.8 . . n H18A C18 H18B 108.2 . . n C20 C19 C18 112.5(7) . . n C20 C19 H19A 109.1 . . n C18 C19 H19A 109.1 . . n C20 C19 H19B 109.1 . . n C18 C19 H19B 109.1 . . n H19A C19 H19B 107.8 . . n C19 C20 H20A 109.5 . . n C19 C20 H20B 109.5 . . n H20A C20 H20B 109.5 . . n C19 C20 H20C 109.5 . . n H20A C20 H20C 109.5 . . n H20B C20 H20C 109.5 . . n C37 N2 C29 116.3(16) . . n C37 N2 C21 117.7(11) . . n C29 N2 C21 105.1(11) . . n C37 N2 C33 102.6(11) . . n C29 N2 C33 107.3(16) . . n C21 N2 C33 107.1(12) . . n N2 C29 C30 114.9(18) . . n N2 C29 H29A 108.5 . . n C30 C29 H29A 108.5 . . n N2 C29 H29B 108.5 . . n C30 C29 H29B 108.5 . . n H29A C29 H29B 107.5 . . n C31 C30 C29 108(2) . . n C31 C30 H30A 110.1 . . n C29 C30 H30A 110.1 . . n C31 C30 H30B 110.1 . . n C29 C30 H30B 110.1 . . n H30A C30 H30B 108.4 . . n C32 C31 C30 114(2) . . n C32 C31 H31A 108.8 . . n C30 C31 H31A 108.8 . . n C32 C31 H31B 108.8 . . n C30 C31 H31B 108.8 . . n H31A C31 H31B 107.7 . . n C34 C33 N2 121.5(16) . . n C34 C33 H33A 107.0 . . n N2 C33 H33A 107.0 . . n C34 C33 H33B 107.0 . . n N2 C33 H33B 107.0 . . n H33A C33 H33B 106.7 . . n C33 C34 C35 114(2) . . n C33 C34 H34A 108.8 . . n C35 C34 H34A 108.8 . . n C33 C34 H34B 108.8 . . n C35 C34 H34B 108.8 . . n H34A C34 H34B 107.7 . . n C36 C35 C34 112(3) . . n C36 C35 H35A 109.1 . . n C34 C35 H35A 109.1 . . n C36 C35 H35B 109.1 . . n C34 C35 H35B 109.1 . . n H35A C35 H35B 107.9 . . n N2 C37 C38 105.9(12) . . n N2 C37 H37A 110.6 . . n C38 C37 H37A 110.6 . . n N2 C37 H37B 110.6 . . n C38 C37 H37B 110.6 . . n H37A C37 H37B 108.7 . . n C39 C38 C37 109.2(14) . . n C39 C38 H38A 109.8 . . n C37 C38 H38A 109.8 . . n C39 C38 H38B 109.8 . . n C37 C38 H38B 109.8 . . n H38A C38 H38B 108.3 . . n C40 C39 C38 113.8(16) . . n C40 C39 H39A 108.8 . . n C38 C39 H39A 108.8 . . n C40 C39 H39B 108.8 . . n C38 C39 H39B 108.8 . . n H39A C39 H39B 107.7 . . n C30X C29X H29C 107.8 . . n C30X C29X H29D 107.8 . . n H29C C29X H29D 107.1 . . n C31X C30X C29X 108(3) . . n C31X C30X H30C 110.0 . . n C29X C30X H30C 110.0 . . n C31X C30X H30D 110.0 . . n C29X C30X H30D 110.0 . . n H30C C30X H30D 108.4 . . n C32X C31X C30X 114(4) . . n C32X C31X H31C 108.8 . . n C30X C31X H31C 108.8 . . n C32X C31X H31D 108.8 . . n C30X C31X H31D 108.8 . . n H31C C31X H31D 107.7 . . n C31X C32X H32D 109.5 . . n C31X C32X H32E 109.5 . . n H32D C32X H32E 109.5 . . n C31X C32X H32F 109.5 . . n H32D C32X H32F 109.5 . . n H32E C32X H32F 109.5 . . n C34X C33X H33C 111.4 . . n C34X C33X H33D 111.4 . . n H33C C33X H33D 109.2 . . n C33X C34X C35X 106(2) . . n C33X C34X H34C 110.6 . . n C35X C34X H34C 110.6 . . n C33X C34X H34D 110.6 . . n C35X C34X H34D 110.6 . . n H34C C34X H34D 108.7 . . n C36X C35X C34X 109(3) . . n C36X C35X H35C 109.8 . . n C34X C35X H35C 109.8 . . n C36X C35X H35D 109.8 . . n C34X C35X H35D 109.8 . . n H35C C35X H35D 108.3 . . n C35X C36X H36D 109.5 . . n C35X C36X H36E 109.5 . . n H36D C36X H36E 109.5 . . n C35X C36X H36F 109.5 . . n H36D C36X H36F 109.5 . . n H36E C36X H36F 109.5 . . n C38X C37X H37C 107.1 . . n C38X C37X H37D 107.1 . . n H37C C37X H37D 106.8 . . n C39X C38X C37X 117(2) . . n C39X C38X H38C 108.1 . . n C37X C38X H38C 108.1 . . n C39X C38X H38D 108.1 . . n C37X C38X H38D 108.1 . . n H38C C38X H38D 107.3 . . n C40X C39X C38X 113(2) . . n C40X C39X H39C 109.0 . . n C38X C39X H39C 109.0 . . n C40X C39X H39D 109.0 . . n C38X C39X H39D 109.0 . . n H39C C39X H39D 107.8 . . n C39X C40X H40D 109.5 . . n C39X C40X H40E 109.5 . . n H40D C40X H40E 109.5 . . n C39X C40X H40F 109.5 . . n H40D C40X H40F 109.5 . . n H40E C40X H40F 109.5 . . n C22 C21 N2 115.7(7) . . n C22 C21 H21A 108.3 . . n N2 C21 H21A 108.3 . . n C22 C21 H21B 108.3 . . n N2 C21 H21B 108.3 . . n H21A C21 H21B 107.4 . . n C21 C22 C23 109.2(7) . . n C21 C22 H22A 109.8 . . n C23 C22 H22A 109.8 . . n C21 C22 H22B 109.8 . . n C23 C22 H22B 109.8 . . n H22A C22 H22B 108.3 . . n C22 C23 C24 112.8(8) . . n C22 C23 H23A 109.0 . . n C24 C23 H23A 109.0 . . n C22 C23 H23B 109.0 . . n C24 C23 H23B 109.0 . . n H23A C23 H23B 107.8 . . n C23 C24 H24A 109.5 . . n C23 C24 H24B 109.5 . . n H24A C24 H24B 109.5 . . n C23 C24 H24C 109.5 . . n H24A C24 H24C 109.5 . . n H24B C24 H24C 109.5 . . n _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.216 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.041 _database_code_depnum_ccdc_archive 'CCDC 961331' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_(NBu4)2{[B9C2H11]C2}2C6H4_(17) _chemical_name_systematic ; tetrabutylammonium 1,4-bis(1-ethynyl-undecahydro- 7,8-dicarba-nido-decaborate(1-))benzene ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; {[B9 C2 H11] C2}2 C6 H4 {N ((C H2)3 C H3)4}2 ; _chemical_formula_sum 'C46 H98 B18 N2' _chemical_formula_weight 873.84 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn ' _symmetry_int_tables_number 14 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 10.9742(16) _cell_length_b 15.710(2) _cell_length_c 16.935(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.556(3) _cell_angle_gamma 90.00 _cell_volume 2919.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6221 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.87 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.994 _exptl_crystal_density_method none _exptl_crystal_F_000 956 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Bruker SADABS 2008/1 ; _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.99 _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 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25157 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.12 _reflns_number_total 6420 _reflns_number_gt 3048 _reflns_threshold_expression I>2\s(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0867P)^2^+0.9693P] 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 noref _refine_ls_number_reflns 6420 _refine_ls_number_parameters 383 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1580 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2187 _refine_ls_wR_factor_gt 0.1771 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 B1 B -0.0339(3) 0.72053(18) 0.20256(17) 0.0428(7) Uani 1 1 d . . . B2 B 0.0450(3) 0.7178(2) 0.29384(18) 0.0482(8) Uani 1 1 d . . . H2 H 0.094(2) 0.7699(17) 0.3208(15) 0.058(8) Uiso 1 1 d . . . B3 B -0.1148(3) 0.7192(2) 0.29170(19) 0.0524(9) Uani 1 1 d . . . H3 H -0.165(3) 0.7716(19) 0.3153(17) 0.071(9) Uiso 1 1 d . . . B4 B -0.1656(3) 0.6578(2) 0.21158(19) 0.0493(8) Uani 1 1 d . . . H4 H -0.248(2) 0.6753(15) 0.1873(14) 0.045(7) Uiso 1 1 d . . . B5 B -0.0385(3) 0.6146(2) 0.1643(2) 0.0503(8) Uani 1 1 d . . . H5 H -0.038(2) 0.6023(17) 0.0990(17) 0.064(8) Uiso 1 1 d . . . B6 B 0.0956(3) 0.6528(2) 0.2167(2) 0.0499(8) Uani 1 1 d . . . H6 H 0.180(2) 0.6647(15) 0.1870(14) 0.043(7) Uiso 1 1 d . . . C7 C -0.0370(3) 0.6457(2) 0.34676(19) 0.0645(9) Uani 1 1 d . . . H7 H -0.042(3) 0.657(2) 0.403(2) 0.079(10) Uiso 1 1 d . . . C8 C -0.1526(3) 0.61327(19) 0.30348(18) 0.0573(8) Uani 1 1 d . . . H8 H -0.229(3) 0.603(2) 0.3395(18) 0.081(10) Uiso 1 1 d . . . B9 B -0.1198(3) 0.5506(2) 0.2304(2) 0.0563(9) Uani 1 1 d . . . H9 H -0.180(2) 0.4999(18) 0.2144(15) 0.061(8) Uiso 1 1 d . . . B10 B 0.0464(4) 0.5466(2) 0.2274(2) 0.0605(10) Uani 1 1 d . . . H10 H 0.102(2) 0.4947(19) 0.2024(16) 0.066(8) Uiso 1 1 d . . . B11 B 0.0860(3) 0.6099(2) 0.3128(2) 0.0544(9) Uani 1 1 d . . . H11 H 0.169(3) 0.5987(17) 0.3509(16) 0.063(8) Uiso 1 1 d . . . H12 H 0.0000 0.5245 0.2759 0.162(19) Uiso 1 1 d . . . C1 C -0.0278(3) 0.79875(17) 0.14700(15) 0.0485(7) Uani 1 1 d . . . C2 C -0.0216(3) 0.85790(17) 0.10331(15) 0.0515(7) Uani 1 1 d . . . C3 C -0.0118(3) 0.92984(16) 0.05088(15) 0.0491(7) Uani 1 1 d . . . C4 C 0.1010(3) 0.96046(19) 0.02955(18) 0.0652(9) Uani 1 1 d . . . H4A H 0.1723 0.9334 0.0496 0.078 Uiso 1 1 calc R . . C5 C 0.1130(3) 1.02975(19) -0.02043(18) 0.0650(9) Uani 1 1 d . . . H5A H 0.1920 1.0495 -0.0338 0.078 Uiso 1 1 calc R . . N1 N 0.0409(2) 0.26370(13) 0.15647(12) 0.0445(6) Uani 1 1 d . B . C9 C -0.0204(3) 0.18113(16) 0.17896(16) 0.0483(7) Uani 1 1 d . . . H9A H -0.0908 0.1949 0.2128 0.058 Uiso 1 1 calc R . . H9B H -0.0531 0.1545 0.1302 0.058 Uiso 1 1 calc R . . C10 C 0.0569(3) 0.11628(17) 0.22139(19) 0.0625(9) Uani 1 1 d . . . H10A H 0.1226 0.0971 0.1859 0.075 Uiso 1 1 calc R . . H10B H 0.0957 0.1434 0.2681 0.075 Uiso 1 1 calc R . . C11 C -0.0145(3) 0.04059(16) 0.24774(17) 0.0547(8) Uani 1 1 d . . . H11A H -0.0526 0.0135 0.2009 0.066 Uiso 1 1 calc R . . H11B H -0.0808 0.0601 0.2826 0.066 Uiso 1 1 calc R . . C12 C 0.0605(3) -0.02500(19) 0.2912(2) 0.0773(10) Uani 1 1 d . . . H12A H 0.1226 -0.0480 0.2559 0.116 Uiso 1 1 calc R . . H12B H 0.0074 -0.0712 0.3089 0.116 Uiso 1 1 calc R . . H12C H 0.1002 0.0015 0.3371 0.116 Uiso 1 1 calc R . . C13 C -0.0545(3) 0.32636(19) 0.12652(17) 0.0589(8) Uani 1 1 d . . . H13A H -0.1143 0.3355 0.1691 0.071 Uiso 1 1 calc R A 1 H13B H -0.0137 0.3815 0.1169 0.071 Uiso 1 1 calc R A 1 C14 C -0.1229(3) 0.3026(2) 0.05351(19) 0.0655(9) Uani 1 1 d D B 1 H14A H -0.1722 0.2506 0.0616 0.079 Uiso 1 1 calc R B 1 H14B H -0.0672 0.2934 0.0087 0.079 Uiso 1 1 calc R B 1 C15 C -0.2052(7) 0.3817(5) 0.0397(4) 0.071(2) Uani 0.652(9) 1 d PD B 1 H15A H -0.2454 0.3976 0.0897 0.085 Uiso 0.652(9) 1 calc PR B 1 H15B H -0.1547 0.4304 0.0226 0.085 Uiso 0.652(9) 1 calc PR B 1 C16 C -0.2995(6) 0.3629(5) -0.0217(4) 0.099(3) Uani 0.652(9) 1 d PD B 1 H16A H -0.2597 0.3514 -0.0722 0.148 Uiso 0.652(9) 1 calc PR B 1 H16B H -0.3540 0.4119 -0.0276 0.148 Uiso 0.652(9) 1 calc PR B 1 H16C H -0.3468 0.3129 -0.0059 0.148 Uiso 0.652(9) 1 calc PR B 1 C15X C -0.2357(11) 0.3448(8) 0.0167(8) 0.066(4) Uani 0.348(9) 1 d PD B 2 H15C H -0.2596 0.3152 -0.0327 0.079 Uiso 0.348(9) 1 calc PR B 2 H15D H -0.3048 0.3424 0.0537 0.079 Uiso 0.348(9) 1 calc PR B 2 C16X C -0.2028(9) 0.4351(6) -0.0003(6) 0.066(3) Uani 0.348(9) 1 d PD B 2 H16D H -0.1723 0.4622 0.0482 0.099 Uiso 0.348(9) 1 calc PR B 2 H16E H -0.2750 0.4656 -0.0195 0.099 Uiso 0.348(9) 1 calc PR B 2 H16F H -0.1394 0.4367 -0.0406 0.099 Uiso 0.348(9) 1 calc PR B 2 C17 C 0.1061(3) 0.30261(17) 0.22726(16) 0.0569(8) Uani 1 1 d . . . H17A H 0.1739 0.2643 0.2426 0.068 Uiso 1 1 calc R B 1 H17B H 0.1426 0.3572 0.2103 0.068 Uiso 1 1 calc R B 1 C18 C 0.0315(4) 0.3194(2) 0.29930(17) 0.0762(11) Uani 1 1 d D B 1 H18A H -0.0007 0.2643 0.3183 0.091 Uiso 1 1 calc R B 1 H18B H -0.0394 0.3547 0.2833 0.091 Uiso 1 1 calc R B 1 C19 C 0.095(2) 0.3630(10) 0.3677(8) 0.083(5) Uani 0.52(4) 1 d PD B 1 H19A H 0.1475 0.4086 0.3468 0.100 Uiso 0.52(4) 1 calc PR B 1 H19B H 0.1479 0.3211 0.3949 0.100 Uiso 0.55(5) 1 calc PR B 1 C20 C 0.008(3) 0.4020(11) 0.4286(8) 0.095(6) Uani 0.52(4) 1 d PD B 1 H20A H -0.0472 0.4423 0.4021 0.142 Uiso 0.52(4) 1 calc PR B 1 H20B H 0.0553 0.4320 0.4692 0.142 Uiso 0.52(4) 1 calc PR B 1 H20C H -0.0400 0.3567 0.4532 0.142 Uiso 0.52(4) 1 calc PR B 1 C19X C 0.127(2) 0.3555(13) 0.3578(10) 0.084(5) Uani 0.48(4) 1 d PD B 2 H19C H 0.1934 0.3134 0.3658 0.101 Uiso 0.48(4) 1 calc PR B 2 H19D H 0.1634 0.4080 0.3358 0.101 Uiso 0.48(4) 1 calc PR B 2 C20X C 0.067(3) 0.376(3) 0.4377(11) 0.107(9) Uani 0.48(4) 1 d PD B 2 H20D H -0.0066 0.4094 0.4287 0.160 Uiso 0.48(4) 1 calc PR B 2 H20E H 0.1245 0.4079 0.4709 0.160 Uiso 0.48(4) 1 calc PR B 2 H20F H 0.0460 0.3223 0.4643 0.160 Uiso 0.48(4) 1 calc PR B 2 C21 C 0.1345(2) 0.24589(17) 0.09274(15) 0.0477(7) Uani 1 1 d . . . H21A H 0.1963 0.2064 0.1149 0.057 Uiso 1 1 calc R B . H21B H 0.0928 0.2160 0.0487 0.057 Uiso 1 1 calc R . . C22 C 0.2002(3) 0.32223(19) 0.05917(16) 0.0531(7) Uani 1 1 d . B . H22A H 0.1408 0.3602 0.0324 0.064 Uiso 1 1 calc R . . H22B H 0.2396 0.3546 0.1026 0.064 Uiso 1 1 calc R . . C23 C 0.2954(3) 0.2942(2) 0.00105(17) 0.0654(9) Uani 1 1 d . . . H23A H 0.2546 0.2659 -0.0442 0.078 Uiso 1 1 calc R B . H23B H 0.3498 0.2521 0.0268 0.078 Uiso 1 1 calc R . . C24 C 0.3711(4) 0.3675(3) -0.0291(2) 0.0938(13) Uani 1 1 d . B . H24A H 0.3182 0.4084 -0.0565 0.141 Uiso 1 1 calc R . . H24B H 0.4323 0.3459 -0.0658 0.141 Uiso 1 1 calc R . . H24C H 0.4121 0.3957 0.0154 0.141 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 B1 0.062(2) 0.0333(16) 0.0336(16) 0.0045(13) -0.0008(14) -0.0030(14) B2 0.069(2) 0.0362(17) 0.0395(18) 0.0039(14) -0.0083(16) -0.0071(16) B3 0.072(2) 0.047(2) 0.0384(18) 0.0061(15) 0.0037(16) 0.0051(17) B4 0.059(2) 0.0452(19) 0.0431(18) 0.0141(15) -0.0030(16) -0.0041(16) B5 0.071(2) 0.0358(17) 0.0439(19) -0.0010(14) 0.0016(16) -0.0107(16) B6 0.059(2) 0.0345(17) 0.057(2) 0.0047(15) 0.0035(17) -0.0024(15) C7 0.084(2) 0.070(2) 0.0396(18) 0.0170(16) -0.0066(16) -0.0082(18) C8 0.063(2) 0.0554(19) 0.0538(18) 0.0182(15) 0.0004(16) -0.0081(15) B9 0.063(2) 0.0398(19) 0.066(2) 0.0105(17) -0.0033(18) -0.0120(17) B10 0.070(2) 0.0349(18) 0.077(3) 0.0074(18) 0.005(2) -0.0038(17) B11 0.060(2) 0.0407(18) 0.063(2) 0.0176(16) -0.0097(18) -0.0057(16) C1 0.0710(19) 0.0391(15) 0.0354(14) 0.0004(13) -0.0042(13) -0.0061(14) C2 0.085(2) 0.0362(15) 0.0329(14) 0.0025(12) -0.0051(14) -0.0050(15) C3 0.083(2) 0.0327(14) 0.0315(14) 0.0027(11) -0.0060(14) -0.0090(15) C4 0.081(2) 0.0517(19) 0.063(2) 0.0232(16) -0.0108(17) -0.0006(17) C5 0.076(2) 0.0551(19) 0.063(2) 0.0247(16) -0.0028(17) -0.0081(17) N1 0.0575(14) 0.0352(12) 0.0406(12) 0.0002(10) -0.0042(11) 0.0045(10) C9 0.0594(17) 0.0375(15) 0.0478(16) -0.0021(13) -0.0010(13) 0.0010(13) C10 0.073(2) 0.0374(16) 0.077(2) 0.0065(15) -0.0158(17) 0.0001(15) C11 0.077(2) 0.0382(15) 0.0491(17) -0.0064(13) 0.0038(15) 0.0045(15) C12 0.107(3) 0.0416(18) 0.083(2) 0.0074(17) -0.015(2) 0.0019(18) C13 0.070(2) 0.0505(18) 0.0569(19) 0.0112(15) 0.0109(16) 0.0179(15) C14 0.0541(18) 0.077(2) 0.065(2) 0.0235(17) -0.0031(16) 0.0050(17) C15 0.065(5) 0.089(6) 0.058(4) 0.019(4) -0.015(3) 0.015(4) C16 0.080(5) 0.151(7) 0.065(4) -0.013(4) -0.022(4) 0.032(4) C15X 0.049(7) 0.103(11) 0.044(8) 0.009(6) -0.023(6) -0.008(7) C16X 0.084(7) 0.061(7) 0.054(6) 0.014(5) -0.011(5) 0.018(5) C17 0.095(2) 0.0339(15) 0.0421(16) -0.0001(13) -0.0058(15) -0.0025(15) C18 0.136(3) 0.0519(19) 0.0412(18) -0.0031(15) 0.0134(19) -0.031(2) C19 0.185(14) 0.035(5) 0.029(5) 0.009(4) 0.020(6) 0.003(7) C20 0.167(18) 0.083(7) 0.035(5) -0.005(4) 0.028(7) -0.015(8) C19X 0.125(9) 0.085(10) 0.041(6) -0.026(6) 0.016(6) -0.035(8) C20X 0.119(15) 0.138(19) 0.063(8) -0.029(9) 0.031(8) -0.061(13) C21 0.0520(16) 0.0470(16) 0.0440(15) -0.0034(13) -0.0056(13) 0.0073(13) C22 0.0618(18) 0.0564(18) 0.0410(16) 0.0017(14) -0.0050(14) 0.0027(15) C23 0.070(2) 0.084(2) 0.0420(17) -0.0033(16) -0.0014(15) -0.0010(18) C24 0.094(3) 0.127(3) 0.061(2) -0.014(2) 0.012(2) -0.041(3) _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 B1 C1 1.550(4) . y B1 B4 1.757(5) . y B1 B3 1.759(5) . y B1 B2 1.765(4) . y B1 B5 1.787(4) . y B1 B6 1.790(5) . y B2 C7 1.706(4) . y B2 B6 1.752(5) . y B2 B3 1.754(5) . y B2 B11 1.782(5) . y B2 H2 1.08(3) . n B3 C7 1.707(5) . y B3 C8 1.727(5) . y B3 B4 1.751(5) . y B3 H3 1.07(3) . n B4 C8 1.711(4) . y B4 B5 1.753(5) . y B4 B9 1.787(5) . y B4 H4 1.02(2) . n B5 B9 1.756(5) . y B5 B10 1.769(5) . y B5 B6 1.814(5) . y B5 H5 1.12(3) . n B6 B10 1.763(5) . y B6 B11 1.766(5) . y B6 H6 1.08(2) . n C7 C8 1.545(4) . y C7 B11 1.577(5) . y C7 H7 0.98(3) . n C8 B9 1.624(5) . y C8 H8 1.06(3) . n B9 B10 1.826(5) . y B9 H9 1.07(3) . n B9 H12 1.571(4) . n B10 B11 1.805(5) . y B10 H10 1.10(3) . n B10 H12 1.031(4) . n B11 H11 1.12(3) . n C1 C2 1.190(3) . y C2 C3 1.442(4) . y C3 C5 1.375(4) 3_575 y C3 C4 1.380(4) . y C4 C5 1.386(4) . y C4 H4A 0.9500 . n C5 C3 1.375(4) 3_575 y C5 H5A 0.9500 . n N1 C9 1.512(3) . y N1 C17 1.519(3) . y N1 C13 1.521(3) . y N1 C21 1.523(3) . y C9 C10 1.504(4) . n C9 H9A 0.9900 . n C9 H9B 0.9900 . n C10 C11 1.494(4) . n C10 H10A 0.9900 . n C10 H10B 0.9900 . n C11 C12 1.506(4) . n C11 H11A 0.9900 . n C11 H11B 0.9900 . n C12 H12A 0.9800 . n C12 H12B 0.9800 . n C12 H12C 0.9800 . n C13 C14 1.488(4) . n C13 H13A 0.9900 . n C13 H13B 0.9900 . n C14 C15 1.554(7) . n C14 H14A 0.9900 . n C14 H14B 0.9900 . n C15 C16 1.490(8) . n C15 H15A 0.9900 . n C15 H15B 0.9900 . n C16 H16A 0.9800 . n C16 H16B 0.9800 . n C16 H16C 0.9800 . n C15X C16X 1.492(13) . n C15X H15C 0.9900 . n C15X H15D 0.9900 . n C16X H16D 0.9800 . n C16X H16E 0.9800 . n C16X H16F 0.9800 . n C17 C18 1.499(4) . n C17 H17A 0.9900 . n C17 H17B 0.9900 . n C18 C19 1.509(10) . n C18 H18A 0.9900 . n C18 H18B 0.9900 . n C19 C20 1.539(13) . n C19 H19A 0.9900 . n C19 H19B 0.9900 . n C20 H20A 0.9800 . n C20 H20B 0.9800 . n C20 H20C 0.9800 . n C19X C20X 1.543(14) . n C19X H19C 0.9900 . n C19X H19D 0.9900 . n C20X H20D 0.9800 . n C20X H20E 0.9800 . n C20X H20F 0.9800 . n C21 C22 1.513(4) . n C21 H21A 0.9900 . n C21 H21B 0.9900 . n C22 C23 1.508(4) . n C22 H22A 0.9900 . n C22 H22B 0.9900 . n C23 C24 1.512(5) . n C23 H23A 0.9900 . n C23 H23B 0.9900 . n C24 H24A 0.9800 . n C24 H24B 0.9800 . n C24 H24C 0.9800 . n 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 B1 B4 122.6(2) . . y C1 B1 B3 123.8(2) . . y B4 B1 B3 59.74(19) . . y C1 B1 B2 121.8(2) . . y B4 B1 B2 107.9(2) . . y B3 B1 B2 59.71(19) . . y C1 B1 B5 121.3(2) . . y B4 B1 B5 59.30(19) . . y B3 B1 B5 106.7(2) . . y B2 B1 B5 107.9(2) . . y C1 B1 B6 120.9(3) . . y B4 B1 B6 107.9(2) . . y B3 B1 B6 106.5(2) . . y B2 B1 B6 59.03(18) . . y B5 B1 B6 60.93(18) . . y C7 B2 B6 100.2(2) . . y C7 B2 B3 59.09(19) . . y B6 B2 B3 108.4(2) . . y C7 B2 B1 102.7(2) . . y B6 B2 B1 61.17(18) . . y B3 B2 B1 59.96(18) . . y C7 B2 B11 53.69(19) . . y B6 B2 B11 59.95(19) . . y B3 B2 B11 105.4(2) . . y B1 B2 B11 107.6(2) . . y C7 B2 H2 122.9(14) . . n B6 B2 H2 126.9(14) . . n B3 B2 H2 119.4(14) . . n B1 B2 H2 126.1(14) . . n B11 B2 H2 121.6(14) . . n C7 B3 C8 53.49(18) . . y C7 B3 B4 101.8(2) . . y C8 B3 B4 58.95(18) . . y C7 B3 B2 59.04(19) . . y C8 B3 B2 103.1(2) . . y B4 B3 B2 108.7(3) . . y C7 B3 B1 102.9(2) . . y C8 B3 B1 103.6(2) . . y B4 B3 B1 60.08(18) . . y B2 B3 B1 60.33(19) . . y C7 B3 H3 124.9(16) . . n C8 B3 H3 125.0(16) . . n B4 B3 H3 123.5(16) . . n B2 B3 H3 121.3(16) . . n B1 B3 H3 125.2(16) . . n C8 B4 B3 59.81(18) . . y C8 B4 B5 101.3(2) . . y B3 B4 B5 108.6(2) . . y C8 B4 B1 104.3(2) . . y B3 B4 B1 60.18(19) . . y B5 B4 B1 61.21(19) . . y C8 B4 B9 55.28(18) . . y B3 B4 B9 107.1(2) . . y B5 B4 B9 59.5(2) . . y B1 B4 B9 108.3(2) . . y C8 B4 H4 122.8(14) . . n B3 B4 H4 115.9(14) . . n B5 B4 H4 128.4(14) . . n B1 B4 H4 122.4(14) . . n B9 B4 H4 124.7(14) . . n B4 B5 B9 61.2(2) . . y B4 B5 B10 112.0(2) . . y B9 B5 B10 62.4(2) . . y B4 B5 B1 59.50(19) . . y B9 B5 B1 108.3(2) . . y B10 B5 B1 109.3(2) . . y B4 B5 B6 107.0(2) . . y B9 B5 B6 107.0(2) . . y B10 B5 B6 58.95(19) . . y B1 B5 B6 59.60(17) . . y B4 B5 H5 122.1(14) . . n B9 B5 H5 122.7(14) . . n B10 B5 H5 118.8(14) . . n B1 B5 H5 121.1(14) . . n B6 B5 H5 121.6(14) . . n B2 B6 B10 112.1(3) . . y B2 B6 B11 60.89(19) . . y B10 B6 B11 61.5(2) . . y B2 B6 B1 59.80(18) . . y B10 B6 B1 109.4(2) . . y B11 B6 B1 107.3(2) . . y B2 B6 B5 107.3(2) . . y B10 B6 B5 59.25(19) . . y B11 B6 B5 105.7(2) . . y B1 B6 B5 59.47(18) . . y B2 B6 H6 121.9(13) . . n B10 B6 H6 118.5(13) . . n B11 B6 H6 123.8(12) . . n B1 B6 H6 121.5(12) . . n B5 B6 H6 121.8(12) . . n C8 C7 B11 114.3(3) . . y C8 C7 B2 113.9(2) . . y B11 C7 B2 65.6(2) . . y C8 C7 B3 63.9(2) . . y B11 C7 B3 117.9(3) . . y B2 C7 B3 61.86(19) . . y C8 C7 H7 118.2(19) . . n B11 C7 H7 118.7(19) . . n B2 C7 H7 115.2(19) . . n B3 C7 H7 112.1(19) . . n C7 C8 B9 112.0(3) . . y C7 C8 B4 110.9(2) . . y B9 C8 B4 64.7(2) . . y C7 C8 B3 62.6(2) . . y B9 C8 B3 116.2(2) . . y B4 C8 B3 61.24(18) . . y C7 C8 H8 115.7(17) . . n B9 C8 H8 121.8(17) . . n B4 C8 H8 121.9(17) . . n B3 C8 H8 114.3(17) . . n C8 B9 B5 104.9(2) . . y C8 B9 B4 60.00(19) . . y B5 B9 B4 59.33(19) . . y C8 B9 B10 105.7(3) . . y B5 B9 B10 59.1(2) . . y B4 B9 B10 107.8(2) . . y C8 B9 H9 120.3(15) . . n B5 B9 H9 125.6(15) . . n B4 B9 H9 119.0(14) . . n B10 B9 H9 125.7(14) . . n C8 B9 H12 88.6(2) . . n B5 B9 H12 91.9(2) . . n B4 B9 H12 124.5(2) . . n B10 B9 H12 34.31(14) . . n H9 B9 H12 116.3(14) . . n B6 B10 B5 61.80(19) . . y B6 B10 B11 59.30(19) . . y B5 B10 B11 105.9(2) . . y B6 B10 B9 106.1(2) . . y B5 B10 B9 58.5(2) . . y B11 B10 B9 101.0(3) . . y B6 B10 H10 119.4(15) . . n B5 B10 H10 120.2(14) . . n B11 B10 H10 125.8(14) . . n B9 B10 H10 126.1(15) . . n B6 B10 H12 123.7(3) . . n B5 B10 H12 115.1(3) . . n B11 B10 H12 70.4(2) . . n B9 B10 H12 59.2(2) . . n H10 B10 H12 109.5(14) . . n C7 B11 B6 105.0(2) . . y C7 B11 B2 60.7(2) . . y B6 B11 B2 59.16(18) . . y C7 B11 B10 106.7(3) . . y B6 B11 B10 59.16(19) . . y B2 B11 B10 108.7(2) . . y C7 B11 H11 122.6(14) . . n B6 B11 H11 122.3(14) . . n B2 B11 H11 117.0(14) . . n B10 B11 H11 124.1(14) . . n C2 C1 B1 178.7(3) . . y C1 C2 C3 178.9(3) . . y C5 C3 C4 117.7(3) 3_575 . y C5 C3 C2 121.9(3) 3_575 . y C4 C3 C2 120.5(3) . . y C3 C4 C5 121.6(3) . . y C3 C4 H4A 119.2 . . n C5 C4 H4A 119.2 . . n C3 C5 C4 120.7(3) 3_575 . y C3 C5 H5A 119.6 3_575 . n C4 C5 H5A 119.6 . . n C9 N1 C17 110.73(19) . . n C9 N1 C13 109.4(2) . . n C17 N1 C13 108.7(2) . . n C9 N1 C21 109.0(2) . . n C17 N1 C21 108.5(2) . . n C13 N1 C21 110.46(19) . . n C10 C9 N1 116.8(2) . . n C10 C9 H9A 108.1 . . n N1 C9 H9A 108.1 . . n C10 C9 H9B 108.1 . . n N1 C9 H9B 108.1 . . n H9A C9 H9B 107.3 . . n C11 C10 C9 112.8(3) . . n C11 C10 H10A 109.0 . . n C9 C10 H10A 109.0 . . n C11 C10 H10B 109.0 . . n C9 C10 H10B 109.0 . . n H10A C10 H10B 107.8 . . n C10 C11 C12 113.9(3) . . n C10 C11 H11A 108.8 . . n C12 C11 H11A 108.8 . . n C10 C11 H11B 108.8 . . n C12 C11 H11B 108.8 . . n H11A C11 H11B 107.7 . . n C11 C12 H12A 109.5 . . n C11 C12 H12B 109.5 . . n H12A C12 H12B 109.5 . . n C11 C12 H12C 109.5 . . n H12A C12 H12C 109.5 . . n H12B C12 H12C 109.5 . . n C14 C13 N1 117.0(2) . . n C14 C13 H13A 108.0 . . n N1 C13 H13A 108.0 . . n C14 C13 H13B 108.0 . . n N1 C13 H13B 108.0 . . n H13A C13 H13B 107.3 . . n C13 C14 C15 102.2(4) . . n C13 C14 H14A 111.3 . . n C15 C14 H14A 111.3 . . n C13 C14 H14B 111.3 . . n C15 C14 H14B 111.3 . . n H14A C14 H14B 109.2 . . n C16 C15 C14 110.1(6) . . n C16 C15 H15A 109.6 . . n C14 C15 H15A 109.6 . . n C16 C15 H15B 109.6 . . n C14 C15 H15B 109.6 . . n H15A C15 H15B 108.1 . . n C16X C15X H15C 110.3 . . n C16X C15X H15D 110.3 . . n H15C C15X H15D 108.5 . . n C15X C16X H16D 109.5 . . n C15X C16X H16E 109.5 . . n H16D C16X H16E 109.5 . . n C15X C16X H16F 109.5 . . n H16D C16X H16F 109.5 . . n H16E C16X H16F 109.5 . . n C18 C17 N1 117.2(3) . . n C18 C17 H17A 108.0 . . n N1 C17 H17A 108.0 . . n C18 C17 H17B 108.0 . . n N1 C17 H17B 108.0 . . n H17A C17 H17B 107.3 . . n C17 C18 C19 117.0(10) . . n C17 C18 H18A 108.0 . . n C19 C18 H18A 108.0 . . n C17 C18 H18B 108.0 . . n C19 C18 H18B 108.0 . . n H18A C18 H18B 107.3 . . n C18 C19 C20 114.3(11) . . n C18 C19 H19A 108.7 . . n C20 C19 H19A 108.7 . . n C18 C19 H19B 108.7 . . n C20 C19 H19B 108.7 . . n H19A C19 H19B 107.6 . . n C20X C19X H19C 109.6 . . n C20X C19X H19D 109.6 . . n H19C C19X H19D 108.1 . . n C19X C20X H20D 109.5 . . n C19X C20X H20E 109.5 . . n H20D C20X H20E 109.5 . . n C19X C20X H20F 109.5 . . n H20D C20X H20F 109.5 . . n H20E C20X H20F 109.5 . . n C22 C21 N1 116.6(2) . . n C22 C21 H21A 108.1 . . n N1 C21 H21A 108.1 . . n C22 C21 H21B 108.1 . . n N1 C21 H21B 108.1 . . n H21A C21 H21B 107.3 . . n C23 C22 C21 110.5(2) . . n C23 C22 H22A 109.6 . . n C21 C22 H22A 109.6 . . n C23 C22 H22B 109.6 . . n C21 C22 H22B 109.6 . . n H22A C22 H22B 108.1 . . n C22 C23 C24 112.7(3) . . n C22 C23 H23A 109.1 . . n C24 C23 H23A 109.1 . . n C22 C23 H23B 109.1 . . n C24 C23 H23B 109.1 . . n H23A C23 H23B 107.8 . . n C23 C24 H24A 109.5 . . n C23 C24 H24B 109.5 . . n H24A C24 H24B 109.5 . . n C23 C24 H24C 109.5 . . n H24A C24 H24C 109.5 . . n H24B C24 H24C 109.5 . . n _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.444 _refine_diff_density_min -0.139 _refine_diff_density_rms 0.039 #===END _database_code_depnum_ccdc_archive 'CCDC 961332'