#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/16/2011621.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2011621 loop_ _publ_author_name 'Sakamoto, Jun' 'Nakagawa, Takashi' 'Kanehisa, Nobuko' 'Kai, Yasushi' 'Katsura, Masahiro' _publ_section_title ; 1H,1'H-2,2'-Bibenzimidazole ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e596 _journal_page_last e597 _journal_paper_doi 10.1107/S0108270100014761 _journal_volume 56 _journal_year 2000 _chemical_formula_moiety 'C14 H10 N4' _chemical_formula_sum 'C14 H10 N4' _chemical_formula_weight 234.26 _space_group_IT_number 72 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-I 2 2c' _symmetry_space_group_name_H-M 'I b a m' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.331(3) _cell_length_b 10.183(2) _cell_length_c 9.962(2) _cell_measurement_reflns_used 25 _cell_measurement_temperature 296.2 _cell_measurement_theta_max 14.9 _cell_measurement_theta_min 12.4 _cell_volume 1149.5(4) _computing_cell_refinement ; MSC/AFC Diffractometer Control Software ; _computing_data_collection ; MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1990) ; _computing_data_reduction ; TEXSAN (Molecular Structure Corporation and Rigaku Corporation, 1999) ; _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku AFC-5R' _diffrn_measurement_method \w-2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .7107 _diffrn_reflns_av_R_equivalents .015 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_number 985 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.50 _diffrn_standards_decay_% .55 _diffrn_standards_interval_count 150 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu .085 _exptl_absorpt_correction_T_max .996 _exptl_absorpt_correction_T_min .937 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_size_max .30 _exptl_crystal_size_mid .10 _exptl_crystal_size_min .10 _refine_diff_density_max .48 _refine_diff_density_min -.43 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment refall _refine_ls_number_parameters 55 _refine_ls_number_reflns 703 _refine_ls_R_factor_gt .0425 _refine_ls_shift/su_max .004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.045(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1274 _reflns_number_gt 321 _reflns_number_total 703 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0384.cif _cod_data_source_block I _cod_original_cell_volume 1149.4(4) _cod_database_code 2011621 _cod_database_fobs_code 2011621 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,z -x,y,1/2-z x,-y,1/2-z -x,-y,-z x,y,-z x,-y,1/2+z -x,y,1/2+z 1/2+x,1/2+y,1/2+z 1/2-x,1/2-y,1/2+z 1/2-x,1/2+y,-z 1/2+x,1/2-y,-z 1/2-x,1/2-y,1/2-z 1/2+x,1/2+y,1/2-z 1/2+x,1/2-y,z 1/2-x,1/2+y,z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 .87990(10) .0477(2) -.1130(2) .0569(6) Uani d . 1.00 . . N C1 .9404(2) .0241(3) .0000 .0504(10) Uani d S 1.00 . . C C2 .7704(2) .0931(2) -.0694(2) .0513(6) Uani d . 1.00 . . C C3 .6723(2) .1345(3) -.1406(3) .0743(9) Uani d . 1.00 . . C C4 .5757(2) .1744(3) -.0691(3) .0669(8) Uani d . 1.00 . . C H1 .897(3) .008(4) -.196(4) .046(10) Uiso calc P .50 . . H H2 .674(2) .137(3) -.233(3) .102(9) Uiso calc . 1.00 . . H H3 .503(2) .205(2) -.119(2) .076(7) Uiso calc . 1.00 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 .0450(10) .082(2) .0450(10) .0090(10) -.0070(9) .0000(10) C1 .042(2) .052(2) .057(2) -.0060(10) .0000 .0000 C2 .0450(10) .0570(10) .0520(10) .0030(10) .0010(10) .0000(10) C3 .0600(10) .105(2) .058(2) .0220(10) -.0080(10) .005(2) C4 .0500(10) .077(2) .074(2) .0170(10) -.0070(10) -.0010(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .003 .002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H .000 .000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N .006 .003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 N1 C2 . 1_555 1_555 104.7(2) yes C1 N1 H1 . 1_555 1_555 123(2) no C2 N1 H1 . 1_555 1_555 127.0(10) no N1 C1 N1 . 1_555 6_555 114.3(3) yes N1 C1 C1 . 1_555 2_755 122.80(10) yes N1 C1 C1 . 6_555 2_755 122.80(10) yes N1 C2 C2 . 1_555 6_555 108.20(10) no N1 C2 C3 . 1_555 1_555 131.0(2) no C2 C2 C3 6_555 . 1_555 120.80(10) no C2 C3 C4 . 1_555 1_555 117.8(2) no C2 C3 H2 . 1_555 1_555 120.0(10) no C4 C3 H2 . 1_555 1_555 121.0(10) no C3 C4 C4 . 1_555 6_555 121.4(2) no C3 C4 H3 . 1_555 1_555 119.0(10) no C4 C4 H3 6_555 . 1_555 119.0(10) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N1 C1 . . 1.339(2) yes N1 C2 . . 1.394(3) yes N1 H1 . . .94(4) no C1 C1 . 2_755 1.436(6) yes C2 C2 . 6_555 1.382(4) yes C2 C3 . . 1.385(3) yes C3 C4 . . 1.367(4) yes C3 H2 . . .92(3) no C4 C4 . 6_555 1.377(5) yes C4 H3 . . 1.01(2) no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 N1 H3 2.88(2) 15_555 N1 N1 2.898(4) 4_554 N1 H1 3.19(3) 3_754 N1 H2 3.37(3) 4_554 C1 H1 2.70(3) 5_755 C1 H3 3.09(2) 12_555 C1 H3 3.09(2) 15_555 C1 H1 3.09(4) 4_554 C1 H1 3.09(4) 7_555 C1 C4 3.500(4) 12_555 C1 C4 3.500(4) 15_555 C1 H3 3.52(2) 11_645 C1 H3 3.52(2) 16_645 C1 H1 3.55(4) 3_754 C1 H1 3.55(4) 8_755 C1 C2 3.555(4) 5_755 C2 H1 2.93(3) 4_554 C2 H2 3.25(3) 4_554 C2 H3 3.38(2) 15_555 C2 H2 3.44(3) 13_654 C3 H2 3.04(3) 4_554 C3 H2 3.17(3) 13_654 C3 H3 3.20(2) 3_654 C3 H1 3.36(3) 4_554 C3 C3 3.501(6) 4_554 C4 H3 3.25(2) 3_654 C4 H2 3.47(3) 3_654 H1 H1 2.56(6) 3_754 H1 H2 3.02(4) 4_554 H1 H3 3.25(5) 15_555 H1 H3 3.37(5) 16_645 H2 H3 2.59(4) 3_654 H2 H2 2.81(5) 4_554 H2 H2 2.89(5) 13_654 H3 H3 2.61(4) 3_654 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1 N1 4_554 .94(4) 1.99(4) 2.897(3) 160(3) yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 N1 C2 1_555 1_555 6_555 6_555 -1.1(3) no N1 C1 C1 N1 1_555 1_555 2_755 2_755 .9(7) no N1 C1 C1 N1 1_555 1_555 2_755 5_755 180.0 no N1 C2 C2 N1 1_555 1_555 6_555 6_555 .0 no N1 C2 C2 C3 1_555 1_555 6_555 6_555 179.6(3) no N1 C2 C3 C4 1_555 1_555 1_555 1_555 -179.9(2) no C1 N1 C2 C2 1_555 1_555 1_555 6_555 -.6(2) no C1 N1 C2 C3 1_555 1_555 1_555 1_555 179.0(3) no C1 N1 C2 C2 1_555 6_555 6_555 1_555 .6(2) no C1 N1 C2 C3 1_555 6_555 6_555 6_555 -179.0(3) no C2 C2 C3 C4 1_555 6_555 6_555 6_555 .4(3) no C2 C3 C4 C4 1_555 1_555 1_555 6_555 .4(3) no C3 C2 C2 C3 1_555 1_555 6_555 6_555 .0 no C3 C4 C4 C3 1_555 1_555 6_555 6_555 .0 no