Refinement of a twinned structure with <i>SHELXL</i>93: <i>meso</i>-2,2'-[1,6-bis(methylamino)-3,4-dithia-1,6-hexanediyl]diphenol
Bolte, Michael; Acta Crystallographica Section C 50 (1994) 1368–1370; doi:10.1107/S0108270193014507

data_2009917
_publ_section_title
;
 Refinement of a twinned structure with <i>SHELXL</i>93:
 <i>meso</i>-2,2'-[1,6-bis(methylamino)-3,4-dithia-1,6-hexanediyl]diphenol
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1368
_journal_page_last               1370
_journal_paper_doi               10.1107/S0108270193014507
_journal_volume                  50
_journal_year                    1994
_chemical_formula_sum            'C18 H24 N2 O2 S2'
_chemical_formula_weight         364.51
_chemical_name_systematic
;
 meso-2,2'-[1,6-Bis(methylamino)-3,4-dithia-1,6-hexanediyl]diphenol
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 92.36(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.618(3)
_cell_length_b                   7.4360(10)
_cell_length_c                   19.242(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      46.60
_cell_measurement_theta_min      25.30
_cell_volume                     946.1(6)
_computing_cell_refinement       'SDP (Enraf-Nonius, 1985)'
_computing_data_collection       'SDP (Enraf-Nonius, 1985)'
_computing_data_reduction        'SDP (Enraf-Nonius, 1985)'
_computing_molecular_graphics    'SHELXTL XP (Sheldrick, 1991)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4 4-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'highly oriented graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0125
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            2026
_diffrn_reflns_theta_max         55.08
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        1.70
_diffrn_standards_interval_time  92
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.648
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   N/A
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.405
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.133
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2002
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      2.301
_refine_ls_restrained_S_obs      1.110
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_obs          0.0777
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w=1/[\s^2^(Fo^2^) + (0.1310P)^2^ + 1.4059P]
where P = (Fo^2^ + 2Fc^2^)/3
;
_refine_ls_wR_factor_all         0.4129
_refine_ls_wR_factor_obs         0.2039
_reflns_number_observed          1930
_reflns_number_total             2026
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1127.cif
_cod_data_source_block           ab11h5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2009917