#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060254.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4060254 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C17 H32 B10 N P' _chemical_formula_weight 389.51 _symmetry_cell_setting monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2153(11) _cell_length_b 19.240(2) _cell_length_c 11.8583(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.978(2) _cell_angle_gamma 90.00 _cell_volume 2302.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.53 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.124 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12303 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4039 _reflns_number_gt 2557 _reflns_threshold_expression >2sigma(I) _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^)+(0.1069P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4039 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1570 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 P1 P 0.86123(7) 0.07896(4) 0.33042(6) 0.0385(3) Uani 1 1 d . . . N1 N 0.7036(2) 0.08241(12) 0.3527(2) 0.0434(6) Uani 1 1 d . . . C1 C 0.9229(3) 0.17170(14) 0.3233(2) 0.0359(7) Uani 1 1 d . . . C3 C 0.8492(3) 0.05045(15) 0.1822(2) 0.0409(7) Uani 1 1 d . . . C4 C 0.8870(3) -0.02110(15) 0.1593(2) 0.0395(7) Uani 1 1 d . . . C5 C 0.9484(3) -0.07257(17) 0.2326(3) 0.0486(8) Uani 1 1 d . . . H5A H 0.968(3) -0.0557(16) 0.308(3) 0.055(9) Uiso 1 1 d . . . C6 C 0.9726(4) -0.13637(19) 0.1876(3) 0.0607(10) Uani 1 1 d . . . H6A H 1.021(3) -0.1728(18) 0.240(3) 0.062(10) Uiso 1 1 d . . . C7 C 0.9347(4) -0.14993(19) 0.0719(3) 0.0607(10) Uani 1 1 d . . . H7A H 0.952(3) -0.1966(17) 0.044(2) 0.049(9) Uiso 1 1 d . . . C8 C 0.8754(4) -0.09950(18) 0.0001(3) 0.0523(9) Uani 1 1 d . . . H8A H 0.855(3) -0.1021(19) -0.079(3) 0.074(11) Uiso 1 1 d . . . C9 C 0.8515(3) -0.03504(16) 0.0426(2) 0.0429(7) Uani 1 1 d . . . C10 C 0.7923(3) 0.02868(15) -0.0138(2) 0.0433(7) Uani 1 1 d . . . H10A H 0.8437 0.0452 -0.0706 0.052 Uiso 1 1 calc R . . H10B H 0.7019 0.0204 -0.0503 0.052 Uiso 1 1 calc R . . C11 C 0.7964(3) 0.07879(17) 0.0806(2) 0.0434(7) Uani 1 1 d . . . H11A H 0.768(3) 0.1276(16) 0.066(2) 0.047(8) Uiso 1 1 d . . . C30 C 0.6723(3) 0.04568(19) 0.4554(3) 0.0594(9) Uani 1 1 d . . . H30A H 0.5756 0.0464 0.4498 0.071 Uiso 1 1 calc R . . C31 C 0.7127(5) -0.0300(2) 0.4598(4) 0.0945(15) Uani 1 1 d . . . H31A H 0.6744 -0.0525 0.3902 0.142 Uiso 1 1 calc R . . H31B H 0.6817 -0.0521 0.5232 0.142 Uiso 1 1 calc R . . H31C H 0.8075 -0.0333 0.4687 0.142 Uiso 1 1 calc R . . C32 C 0.7264(5) 0.0841(3) 0.5640(3) 0.0938(15) Uani 1 1 d . . . H32A H 0.6977 0.1316 0.5578 0.141 Uiso 1 1 calc R . . H32B H 0.8215 0.0824 0.5758 0.141 Uiso 1 1 calc R . . H32C H 0.6943 0.0626 0.6275 0.141 Uiso 1 1 calc R . . C40 C 0.5901(3) 0.10602(17) 0.2679(3) 0.0511(8) Uani 1 1 d . . . H40A H 0.6274 0.1294 0.2068 0.061 Uiso 1 1 calc R . . C41 C 0.5074(4) 0.0459(2) 0.2133(4) 0.0820(13) Uani 1 1 d . . . H41A H 0.5634 0.0138 0.1812 0.123 Uiso 1 1 calc R . . H41B H 0.4406 0.0632 0.1540 0.123 Uiso 1 1 calc R . . H41C H 0.4659 0.0227 0.2700 0.123 Uiso 1 1 calc R . . C42 C 0.5063(3) 0.1596(2) 0.3184(3) 0.0703(11) Uani 1 1 d . . . H42A H 0.5618 0.1971 0.3508 0.106 Uiso 1 1 calc R . . H42B H 0.4647 0.1383 0.3769 0.106 Uiso 1 1 calc R . . H42C H 0.4395 0.1773 0.2595 0.106 Uiso 1 1 calc R . . C2 C 0.9780(3) 0.20438(16) 0.2107(2) 0.0403(7) Uani 1 1 d . . . B3 B 1.0918(3) 0.1719(2) 0.3194(3) 0.0464(9) Uani 1 1 d . . . B4 B 1.0286(4) 0.1965(2) 0.4437(3) 0.0484(9) Uani 1 1 d . . . H4 H 1.040(3) 0.1575(16) 0.511(3) 0.061(9) Uiso 1 1 d . . . B5 B 0.8738(4) 0.23812(19) 0.4019(3) 0.0459(9) Uani 1 1 d . . . H5 H 0.798(3) 0.2264(17) 0.450(3) 0.064(10) Uiso 1 1 d . . . B6 B 0.8422(4) 0.24135(18) 0.2514(3) 0.0423(8) Uani 1 1 d . . . H6 H 0.743(3) 0.2346(16) 0.199(2) 0.054(9) Uiso 1 1 d . . . B7 B 1.1218(4) 0.2492(2) 0.2450(3) 0.0512(10) Uani 1 1 d . . . H7 H 1.188(3) 0.2468(15) 0.187(2) 0.047(8) Uiso 1 1 d . . . B8 B 1.1540(4) 0.2468(2) 0.3959(3) 0.0562(11) Uani 1 1 d . . . H8 H 1.257(3) 0.2463(16) 0.441(3) 0.069(10) Uiso 1 1 d . . . B9 B 1.0194(4) 0.2873(2) 0.4467(3) 0.0565(11) Uani 1 1 d . . . H9 H 1.032(4) 0.315(2) 0.523(3) 0.097(13) Uiso 1 1 d . . . B10 B 0.9038(4) 0.3153(2) 0.3285(3) 0.0525(10) Uani 1 1 d . . . H10 H 0.835(3) 0.3602(18) 0.327(3) 0.068(10) Uiso 1 1 d . . . B11 B 0.9669(4) 0.29174(19) 0.2036(3) 0.0488(9) Uani 1 1 d . . . H11 H 0.942(3) 0.3159(15) 0.122(2) 0.051(8) Uiso 1 1 d . . . B12 B 1.0773(4) 0.3204(2) 0.3247(3) 0.0548(10) Uani 1 1 d . . . H12 H 1.122(3) 0.3688(16) 0.318(2) 0.050(8) Uiso 1 1 d . . . H3 H 1.136(3) 0.1180(14) 0.311(2) 0.037(7) Uiso 1 1 d . . . H2A H 0.966(3) 0.1705(15) 0.146(2) 0.049(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0392(5) 0.0387(5) 0.0359(4) -0.0001(4) 0.0005(3) 0.0011(3) N1 0.0384(14) 0.0463(15) 0.0443(14) 0.0057(12) 0.0023(11) -0.0032(11) C1 0.0332(15) 0.0411(16) 0.0319(14) -0.0054(12) 0.0007(12) -0.0002(12) C3 0.0387(16) 0.0393(16) 0.0433(17) -0.0019(14) 0.0019(13) -0.0007(13) C4 0.0355(15) 0.0395(17) 0.0450(17) -0.0043(14) 0.0110(13) -0.0047(13) C5 0.057(2) 0.0421(19) 0.0459(19) 0.0017(16) 0.0043(15) 0.0038(16) C6 0.071(2) 0.045(2) 0.070(2) 0.0112(19) 0.021(2) 0.0118(18) C7 0.078(3) 0.042(2) 0.068(2) -0.0093(19) 0.031(2) 0.0012(18) C8 0.066(2) 0.0431(19) 0.051(2) -0.0092(17) 0.0184(18) -0.0047(16) C9 0.0410(17) 0.0454(19) 0.0432(17) -0.0070(14) 0.0096(13) -0.0078(14) C10 0.0417(17) 0.0451(18) 0.0403(16) -0.0028(14) -0.0023(13) -0.0035(14) C11 0.0410(17) 0.0423(18) 0.0446(17) 0.0020(15) -0.0009(13) 0.0013(14) C30 0.057(2) 0.067(2) 0.057(2) 0.0100(18) 0.0160(17) -0.0013(18) C31 0.117(4) 0.071(3) 0.106(3) 0.041(3) 0.049(3) 0.006(3) C32 0.098(3) 0.135(4) 0.051(2) 0.010(3) 0.022(2) -0.014(3) C40 0.0363(17) 0.053(2) 0.060(2) 0.0013(17) -0.0036(15) -0.0041(15) C41 0.061(2) 0.078(3) 0.099(3) -0.008(2) -0.013(2) -0.022(2) C42 0.041(2) 0.073(3) 0.096(3) 0.002(2) 0.0080(19) 0.0076(18) C2 0.0423(17) 0.0436(18) 0.0345(15) -0.0015(14) 0.0040(13) -0.0040(14) B3 0.0341(19) 0.058(2) 0.046(2) 0.0014(18) 0.0021(16) 0.0034(17) B4 0.046(2) 0.062(3) 0.0345(19) -0.0055(18) -0.0012(16) -0.0058(18) B5 0.046(2) 0.046(2) 0.048(2) -0.0144(17) 0.0130(17) -0.0049(16) B6 0.038(2) 0.040(2) 0.048(2) -0.0042(16) 0.0026(16) 0.0001(15) B7 0.040(2) 0.063(3) 0.052(2) -0.0040(19) 0.0103(18) -0.0044(18) B8 0.041(2) 0.068(3) 0.056(2) -0.007(2) -0.0027(19) -0.0095(19) B9 0.058(2) 0.065(3) 0.046(2) -0.022(2) 0.0048(19) -0.018(2) B10 0.050(2) 0.039(2) 0.069(3) -0.0081(19) 0.009(2) -0.0039(17) B11 0.053(2) 0.042(2) 0.049(2) 0.0032(18) 0.0034(18) -0.0065(17) B12 0.050(2) 0.053(2) 0.059(2) -0.009(2) 0.0028(19) -0.0168(19) _cod_database_code 4060254