4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-[1,3-diazinane-1,3-diylbis(methylene)]diphenol 0.25-hydrate
Zhang, Manman; Li, Li; Yuan, Fugen; Qian, Hui; Acta Crystallographica Section E 68 (2012) o2123–; doi:10.1107/S1600536812026505

data_2235411
_publ_section_title
;
 4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-[1,3-diazinane-1,3-diylbis(methylene)]diphenol
 0.25-hydrate
;
_journal_coeditor_code           FJ2558
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2123
_journal_paper_doi               10.1107/S1600536812026505
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C34 H54 N2 O2, 0.25H2 O'
_chemical_formula_moiety         'C34 H54 N2 O2, 0.25(H2 O)'
_chemical_formula_sum            'C136 H218 N8 O9'
_chemical_formula_weight         527.30
_chemical_name_systematic
;
4,4',6,6'-Tetra-<i>tert</i>-butyl-2,2'-[1,3-diazinane-1,3-
diylbis(methylene)]diphenol 0.25-hydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7292(8)
_cell_length_b                   37.428(3)
_cell_length_c                   10.1806(9)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.58
_cell_volume                     3326.2(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'publCIF (Westrip, 2010) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29196
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.311
_refine_ls_extinction_coef       0.0034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.038
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+1.2767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                3411
_reflns_number_total             3908
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2558.cif
_cod_data_source_block           I
_cod_original_cell_volume        3326.1(5)
_cod_database_code               2235411
_cod_database_fobs_code          2235411