Methyl 2-[(3,5-di-<i>tert</i>-butyl-4-hydroxybenzyl)sulfanyl]pyridine-3-carboxylate <i>n</i>-hexane hemisolvate
Ariffin, Azhar; Nordin, Nordiana; Yehye, Wagee A.; Ng, Seik Weng; Acta Crystallographica Section E 68 (2012) o1605–; doi:10.1107/S1600536812018739

data_2234922
_publ_section_title
;
 Methyl
 2-[(3,5-di-<i>tert</i>-butyl-4-hydroxybenzyl)sulfanyl]pyridine-3-carboxylate
 <i>n</i>-hexane hemisolvate
;
_journal_coeditor_code           BT5894
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1605
_journal_paper_doi               10.1107/S1600536812018739
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C22 H29 N O3 S, 0.5C6 H14'
_chemical_formula_moiety         'C22 H29 N O3 S, 0.5(C6 H14)'
_chemical_formula_sum            'C25 H36 N O3 S'
_chemical_formula_weight         430.61
_chemical_name_systematic
;
Methyl
2-[(3,5-di-<i>tert</i>-butyl-4-hydroxybenzyl)sulfanyl]pyridine-3-carboxylate
<i>n</i>-hexane hemisolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.796(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.0665(5)
_cell_length_b                   9.4818(3)
_cell_length_c                   34.6700(13)
_cell_measurement_reflns_used    9294
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5017
_cell_measurement_theta_min      2.3453
_cell_volume                     4952.4(3)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4041
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Agilent SuperNova Dual diffractometer with an Atlas detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  Mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            34553
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.35
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  0.9550
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         11426
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+3.1619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                8907
_reflns_number_total             11425
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5894.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2234922
_cod_database_fobs_code          2234922