Diethyl 4,4'-dihydroxy-3,3'-{[(3a<i>RS</i>,7a<i>RS</i>)-2,3,3a,4,5,6,7,7a-octahydro-1<i>H</i>-1,3-benzimidazole-1,3-diyl]bis(methylene)}dibenzoate
Rivera, Augusto; Quiroga, Diego; Ríos-Motta, Jaime; Fejfarová, Karla; Dušek, Michal; Acta Crystallographica Section E 67 (2011) o2817–o2818; doi:10.1107/S1600536811039559

data_2232169
_publ_section_title
;
 Diethyl
 4,4'-dihydroxy-3,3'-{[(3a<i>RS</i>,7a<i>RS</i>)-2,3,3a,4,5,6,7,7a-octahydro-1<i>H</i>-1,3-benzimidazole-1,3-diyl]bis(methylene)}dibenzoate
;
_journal_coeditor_code           BT5654
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2817
_journal_page_last               o2818
_journal_paper_doi               10.1107/S1600536811039559
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C27 H34 N2 O6'
_chemical_formula_moiety         'C27 H34 N2 O6'
_chemical_formula_sum            'C27 H34 N2 O6'
_chemical_formula_weight         482.6
_chemical_name_systematic
;
Diethyl 4,4'-dihydroxy-3,3'-{[(3a<i>RS</i>,7a<i>RS</i>)-2,3,3a,4,5,6,7,7a-
octahydro-1<i>H</i>-1,3-benzimidazole-1,3-diyl]bis(methylene)}dibenzoate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                89.580(5)
_cell_angle_beta                 81.028(4)
_cell_angle_gamma                70.028(5)
_cell_formula_units_Z            2
_cell_length_a                   8.1132(4)
_cell_length_b                   10.9796(7)
_cell_length_c                   15.2450(8)
_cell_measurement_reflns_used    4486
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.05
_cell_measurement_theta_min      2.94
_cell_volume                     1259.19(13)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2010)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2010)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2010)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'JANA2006 (Pet\<r\'i\<cek <i>et al.</i>, 2006)'
_computing_structure_refinement  'JANA2006 (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 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Agilent 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         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11294
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program CrysAlisPro
(Agilent Technologies, 2010). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        67.21
_diffrn_reflns_theta_max         67.21
_diffrn_reflns_theta_min         2.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.456
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.24
_refine_ls_extinction_coef       9E2(2)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   1.64
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    130
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.0046
_refine_ls_shift/su_mean         0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/[\s^2^(I)+0.0009I^2^]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                3313
_reflns_number_total             4430
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            bt5654.cif
_cod_data_source_block           I
_cod_database_code               2232169
_cod_database_fobs_code          2232169