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_2019764
_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          'C15 H18 N2 O3 S, 0.105H2 O'
_chemical_formula_moiety         'C15 H18 N2 O3 S, 0.105(H2 O)'
_chemical_formula_sum            'C15 H18.21 N2 O3.105 S'
_chemical_formula_weight         308.26
_chemical_name_systematic
'Ethyl (4<i>RS</i>)-4-(4-methoxyphenyl)-6-methyl-2-sulfanylidene-1,2,3,4-tetrahydropyrimidine-5-carboxylate 0.105-hydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 102.0080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1455(6)
_cell_length_b                   7.3171(2)
_cell_length_c                   25.0493(8)
_cell_measurement_reflns_used    4024
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.306
_cell_measurement_theta_min      1.662
_cell_volume                     3253.08(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0149
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.306
_diffrn_reflns_theta_min         3.011
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             1304.4
_exptl_crystal_size_max          0.519
_exptl_crystal_size_mid          0.480
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.228
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0493P)^2^+2.7236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1014
_reflns_number_gt                3447
_reflns_number_total             4023
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3572sup1.cif
_cod_data_source_block           II
_cod_database_code               2019764
_cod_database_fobs_code          2019764
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.961
_shelx_hkl_checksum              50627
_shelx_res_checksum              15071
_shelxl_version_number           2.014