4,4'-Dichloro-2,2'-[(3a<i>R</i>,7a<i>R</i>/3a<i>S</i>,7a<i>S</i>)-2,3,3a,4,5,6,7,7a-octahydro-1<i>H</i>-1,3-benzimidazole-1,3-diyl)bis(methylene)]diphenol
Rivera, Augusto; Quiroga, Diego; Ríos-Motta, Jaime; Dušek, Michal; Fejfarová, Karla; Acta Crystallographica Section E 66 (2010) o2643–; doi:10.1107/S160053681003792X

data_2227220
_publ_section_title
;
 4,4'-Dichloro-2,2'-[(3a<i>R</i>,7a<i>R</i>/3a<i>S</i>,7a<i>S</i>)-2,3,3a,4,5,6,7,7a-octahydro-1<i>H</i>-1,3-benzimidazole-1,3-diyl)bis(methylene)]diphenol
;
_journal_coeditor_code           BT5333
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2643
_journal_paper_doi               10.1107/S160053681003792X
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C21 H24 Cl2 N2 O2'
_chemical_formula_moiety         'C21 H24 Cl2 N2 O2'
_chemical_formula_sum            'C21 H24 Cl2 N2 O2'
_chemical_formula_weight         407.3
_chemical_name_systematic
;
4,4'-Dichloro-2,2'-[(3a<i>R</i>,7a<i>R</i>/3a<i>S</i>,7a<i>S</i>)-
2,3,3a,4,5,6,7,7a-octahydro-1<i>H</i>-1,3-benzimidazole-1,3-
diyl)bis(methylene)]diphenol
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.9529(2)
_cell_length_b                   18.3846(5)
_cell_length_c                   8.9704(3)
_cell_measurement_reflns_used    10371
_cell_measurement_temperature    120
_cell_measurement_theta_max      62.4231
_cell_measurement_theta_min      4.8077
_cell_volume                     981.74(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_refinement
'<i>JANA2006</i> (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur diffractometer with an Atlas
(Gemini ultra Cu) detector
;
_diffrn_measurement_method       'Rotation method data acquisition using \w'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.008
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12720
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2008). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        62.49
_diffrn_reflns_theta_max         62.49
_diffrn_reflns_theta_min         4.81
_exptl_absorpt_coefficient_mu    3.107
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis Pro (Oxford Diffraction, 2009), based on expressions derived
by
Clark & Reid (1995)]
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.3775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.3595
_exptl_crystal_size_mid          0.2101
_exptl_crystal_size_min          0.1145
_refine_diff_density_max         0.11
_refine_diff_density_min         -0.11
_refine_ls_abs_structure_details 'Flack (1983), 615 Friedel pairs'
_refine_ls_abs_structure_Flack   0.320(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.50
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    45
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1566
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.0098
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(I)+0.0016I^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                1517
_reflns_number_total             1566
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bt5333.cif
_cod_data_source_block           I
_cod_database_code               2227220
_cod_database_fobs_code          2227220