6,6'-Dimethyl-2,2'-[1,3-diazinane-1,3-diylbis(methylene)]diphenol
Rivera, Augusto; González, Derly Marcela; Ríos-Motta, Jaime; Fejfarová, Karla; Dušek, Michal; Acta Crystallographica Section E 68 (2012) o698–o699; doi:10.1107/S1600536812005284

data_2233949
_publ_section_title
;
 6,6'-Dimethyl-2,2'-[1,3-diazinane-1,3-diylbis(methylene)]diphenol
;
_journal_coeditor_code           NK2137
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o698
_journal_page_last               o699
_journal_paper_doi               10.1107/S1600536812005284
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C20 H26 N2 O2'
_chemical_formula_moiety         'C20 H26 N2 O2'
_chemical_formula_sum            'C20 H26 N2 O2'
_chemical_formula_weight         326.4
_chemical_name_systematic
;
6,6'-Dimethyl-2,2'-[1,3-diazinane-1,3-diylbis(methylene)]diphenol
;
_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'
_cell_angle_alpha                90
_cell_angle_beta                 107.936(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.2788(5)
_cell_length_b                   9.72150(10)
_cell_length_c                   12.4508(2)
_cell_measurement_reflns_used    10886
_cell_measurement_temperature    120
_cell_measurement_theta_max      67.03
_cell_measurement_theta_min      2.97
_cell_volume                     3602.00(10)
_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 0.99
_diffrn_measured_fraction_theta_max 0.99
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20724
_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        67.14
_diffrn_reflns_theta_max         67.14
_diffrn_reflns_theta_min         2.97
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.2035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.14
_refine_ls_extinction_coef       9E2(3)
_refine_ls_extinction_method
'B--C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_ref   1.61
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    98
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.0025
_refine_ls_shift/su_mean         0.0004
_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          0.0951
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                2750
_reflns_number_total             3210
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            nk2137.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2233949
_cod_database_fobs_code          2233949