Crystal structure of bis(2-(2′-hydroxy-5′-methoxyphenyl)-1H-benzimidazole)boron – tetrahydrofuran (1/1), C36H37N4O6B
Yin, Guo-jie; Zhang, Bin; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 615–617; doi:10.1515/ncrs-2016-0377

data_8106620
_publ_section_title
;
 Crystal structure of
 bis(2-(2&#x2032;-hydroxy-5&#x2032;-methoxyphenyl)-1H-benzimidazole)boron
 -- tetrahydrofuran (1/1), C36H37N4O6B
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              615
_journal_page_last               617
_journal_paper_doi               10.1515/ncrs-2016-0377
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C28 H21 B N4 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C36 H37 B N4 O6'
_chemical_formula_weight         632.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 103.301(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3404(4)
_cell_length_b                   19.8285(10)
_cell_length_c                   17.8985(9)
_cell_measurement_reflns_used    1906
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.3127
_cell_measurement_theta_min      2.9360
_cell_volume                     3226.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -18.00   20.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000   30.0000 38

  2 omega  -15.00   25.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.2104  -99.0000 -150.0000 40

  3 omega   35.00   61.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9448  178.0000 -180.0000 26

  4 omega  -29.00   93.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9448    0.0000   90.0000 122
;
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0144087000
_diffrn_orient_matrix_UB_12      -0.0319366000
_diffrn_orient_matrix_UB_13      0.0145509000
_diffrn_orient_matrix_UB_21      -0.0640016000
_diffrn_orient_matrix_UB_22      0.0132599000
_diffrn_orient_matrix_UB_23      0.0096402000
_diffrn_orient_matrix_UB_31      -0.0422958000
_diffrn_orient_matrix_UB_32      -0.0091576000
_diffrn_orient_matrix_UB_33      -0.0368110000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6642
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         2.941
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92373
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3295
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+1.2396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1712
_refine_ls_wR_factor_ref         0.2086
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1919
_reflns_number_total             3295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2016-0377_suppl.cif
_cod_data_source_block           zbb1
_cod_database_code               8106620
_chemical_oxdiff_formula         'C16 H15 O2 N2 B1 Li1'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.982
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C26A, C26, C23, C23A, C22A, C22, C20A, C20, O21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C22A)=
 Sof(H22C)=Sof(H22D)=Sof(C20A)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(1)
 Fixed Sof: H3(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C26A(H26C,
 H26D), C23A(H23C,H23D), C22A(H22C,H22D), C20A(H20C,H20D)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), C9(H9), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18)
4.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'