Ethyl (4-benzyloxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate and a redetermination of ethyl (4<i>RS</i>)-4-(4-methoxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate, as its 0.105-hydrate, both at 200K: subtly different hydrogen-bonded ribbons
Sarojini, Balladka K.; Yathirajan, Hemmige S.; Hosten, Eric C.; Betz, Richard; Glidewell, Christopher; Acta Crystallographica Section C 71 (2015) –; doi:10.1107/S2053229614026758

data_2019763
_publ_section_title
;
 Ethyl
 (4-benzyloxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate
 and a redetermination of ethyl
 (4<i>RS</i>)-4-(4-methoxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate,
 as its 0.105-hydrate, both at 200K: subtly different hydrogen-bonded
 ribbons
;
_journal_coeditor_code           SK3572
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614026758
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C21 H22 N2 O3 S'
_chemical_formula_moiety         'C21 H22 N2 O3 S'
_chemical_formula_sum            'C21 H22 N2 O3 S'
_chemical_formula_weight         382.47
_chemical_name_systematic
'Ethyl (4<i>RS</i>)-4-(4-benzyloxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                85.567(2)
_cell_angle_beta                 83.815(2)
_cell_angle_gamma                69.150(2)
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_cell_length_a                   11.0094(4)
_cell_length_b                   12.7915(5)
_cell_length_c                   14.5418(5)
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_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.381
_cell_measurement_theta_min      1.410
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_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009) and SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
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_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33717
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         2.116
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.935
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.451
_exptl_crystal_size_min          0.346
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^+0.7328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                7596
_reflns_number_total             9456
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3572sup1.cif
_cod_data_source_block           I
_cod_database_code               2019763
_cod_database_fobs_code          2019763
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.936
_shelx_hkl_checksum              64924
_shelx_res_checksum              97737
_shelxl_version_number           2.014