#------------------------------------------------------------------------------ #$Date: 2016-03-25 22:13:40 +0000 (Fri, 25 Mar 2016) $ #$Revision: 180066 $ #$URL: svn://www.crystallography.net/cod/cif/7/05/12/7051261.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_7051261 loop_ _publ_author_name 'Gerald Lesley, M. J.' 'Norman, Nicholas C.' 'Guy Orpen, A.' 'Starbuck, Jonathan' _publ_section_title ; Synthetic routes to cyclic and unsymmetric diborane(4) compounds ; _journal_issue 3 _journal_name_full 'New Journal of Chemistry' _journal_page_first 115 _journal_paper_doi 10.1039/a909645k _journal_volume 24 _journal_year 2000 _chemical_formula_sum 'C5 H8 B N O' _chemical_formula_weight 108.93 _chemical_name_systematic ; ? ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.96(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 11.931(7) _cell_length_b 11.105(11) _cell_length_c 8.929(5) _cell_measurement_temperature 173(2) _cell_volume 1182.9(15) _computing_cell_refinement 'SMART (Siemens, 1995b)' _computing_data_collection 'SMART (Siemens, 1995b)' _computing_data_reduction 'SMART (Siemens, 1995b)' _computing_molecular_graphics 'SHELXTL (Siemens, 1995a)' _computing_publication_material 'SHELXTL (Siemens, 1995a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 2799 _diffrn_reflns_theta_full 23.99 _diffrn_reflns_theta_max 23.99 _diffrn_reflns_theta_min 2.51 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_T_max 0.989572 _exptl_absorpt_correction_T_min 0.674175 _exptl_absorpt_correction_type 'SADABS (Sheldrick, 1997)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 464 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.206 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.042 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 75 _refine_ls_number_reflns 930 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0402 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.1063 _reflns_number_gt 652 _reflns_number_total 930 _reflns_threshold_expression >2sigma(I) _cod_data_source_file a909645k.txt _cod_data_source_block 6 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1182.8(15) _cod_original_sg_symbol_H-M C2/c _cod_database_code 7051261 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' 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 0.03304(19) 0.94904(17) 0.1876(2) 0.0426(6) Uani 1 1 d . . . H1 H 0.0553 1.0231 0.1438 0.051 Uiso 1 1 calc R . . C2 C 0.06686(17) 0.84117(17) 0.1261(2) 0.0375(5) Uani 1 1 d . . . H2 H 0.1129 0.8416 0.0402 0.045 Uiso 1 1 calc R . . C3 C 0.03475(16) 0.73255(16) 0.1875(2) 0.0298(5) Uani 1 1 d . . . C4 C 0.21298(17) 0.44007(19) 0.0327(2) 0.0418(6) Uani 1 1 d . . . H4A H 0.1997 0.3810 -0.0472 0.063 Uiso 1 1 calc R . . H4B H 0.2879 0.4277 0.0767 0.063 Uiso 1 1 calc R . . H4C H 0.2078 0.5216 -0.0089 0.063 Uiso 1 1 calc R . . C5 C 0.13381(17) 0.30669(18) 0.2178(3) 0.0417(6) Uani 1 1 d . . . H5A H 0.2116 0.2880 0.2461 0.062 Uiso 1 1 calc R . . H5B H 0.1058 0.2461 0.1466 0.062 Uiso 1 1 calc R . . H5C H 0.0874 0.3061 0.3073 0.062 Uiso 1 1 calc R . . B1 B 0.05464(18) 0.5154(2) 0.1895(3) 0.0298(6) Uani 1 1 d . . . N1 N 0.12880(13) 0.42509(14) 0.14842(17) 0.0316(4) Uani 1 1 d . . . O1 O 0.07586(11) 0.62895(11) 0.12498(14) 0.0348(4) 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 0.0565(15) 0.0271(12) 0.0438(14) 0.0029(10) -0.0099(10) -0.0052(10) C2 0.0448(13) 0.0352(13) 0.0326(12) 0.0030(10) -0.0008(9) -0.0078(10) C3 0.0325(11) 0.0258(11) 0.0310(12) -0.0023(9) -0.0036(8) 0.0011(8) C4 0.0371(12) 0.0505(14) 0.0383(12) -0.0041(11) 0.0088(9) 0.0053(10) C5 0.0392(13) 0.0350(13) 0.0508(15) -0.0003(11) 0.0017(10) 0.0061(9) B1 0.0320(13) 0.0287(13) 0.0286(13) -0.0013(10) -0.0044(9) -0.0037(10) N1 0.0301(9) 0.0307(10) 0.0342(10) -0.0019(8) 0.0035(7) 0.0006(7) O1 0.0392(8) 0.0315(9) 0.0339(8) -0.0003(6) 0.0091(6) -0.0016(6) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 C1 C2 119.84(12) 2 . ? C1 C2 C3 120.9(2) . . ? O1 C3 C2 117.80(17) . . ? O1 C3 C3 122.96(10) . 2 ? C2 C3 C3 119.21(12) . 2 ? N1 B1 O1 114.68(18) . . ? N1 B1 B1 131.52(13) . 2 ? O1 B1 B1 113.73(11) . 2 ? B1 N1 C5 124.17(17) . . ? B1 N1 C4 123.49(17) . . ? C5 N1 C4 112.32(16) . . ? C3 O1 B1 121.00(16) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C1 1.376(4) 2 ? C1 C2 1.381(3) . ? C2 C3 1.382(3) . ? C3 O1 1.373(2) . ? C3 C3 1.401(4) 2 ? C4 N1 1.463(3) . ? C5 N1 1.454(3) . ? B1 N1 1.391(3) . ? B1 O1 1.411(3) . ? B1 B1 1.707(4) 2 ?