Topochemically controlled solid-state methyl rearrangement in thiocyanurates
Greenberg, Mark; Shteiman, Vitaly; Kaftory, Menahem; Acta Crystallographica Section B 57 (2001) 428–434; doi:10.1107/S0108768101005171

data_2103638
_publ_section_title
;
 Topochemically controlled solid-state methyl rearrangement in
 thiocyanurates
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              428
_journal_page_last               434
_journal_paper_doi               10.1107/S0108768101005171
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C6 H9 N3 O2 S1'
_chemical_formula_sum            'C6 H9 N3 O2 S'
_chemical_formula_weight         187.22
_chemical_name_common            9a
_chemical_name_systematic
;
 4,6-Dimethoxy-3-methyl-1,3,5-triazine-2(3H)-thione
;
_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'
_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                   15.231(5)
_cell_length_b                   6.778(3)
_cell_length_c                   8.626(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.5
_cell_measurement_theta_min      7.2
_cell_volume                     890.5(6)
_computing_cell_refinement       'Philips PW 1100/20 (Philips, 1973)'
_computing_data_collection       'Philips PW 1100/20 (Philips, 1973)'
_computing_data_reduction        'Philips PW 1100/20 (Philips, 1973)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Philips PW 1100 diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71070
_diffrn_reflns_av_R_equivalents  .0546
_diffrn_reflns_av_sigmaI/netI    .0603
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            981
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.67
_diffrn_standards_decay_%        4.2
_diffrn_standards_interval_time  '120 min.'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .328
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Light yellow'
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             392
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .27
_exptl_crystal_size_min          .19
_refine_diff_density_max         .203
_refine_diff_density_min         -.362
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         857
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          .1025
_refine_ls_R_factor_gt           .0609
_refine_ls_shift/su_max          .000
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.2249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1540
_reflns_number_gt                560
_reflns_number_total             857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            av0037.cif
_cod_data_source_block           9a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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_database_code               2103638
_cod_database_fobs_code          2103638