Dimethyl 2,6-dimethyl-4-{3-[4-(methylsulfanyl)phenyl]-1<i>H</i>-pyrazol-4-yl}-1,4-dihydropyridine-3,5-dicarboxylate monohydrate
Islor, Arun M.; Vijesh, A. M.; Gerber, Thomas; Hosten, Eric; Betz, Richard; Acta Crystallographica Section E 68 (2012) o3302–o3303; doi:10.1107/S1600536812045333

data_2237007
_publ_section_title
;
 Dimethyl
 2,6-dimethyl-4-{3-[4-(methylsulfanyl)phenyl]-1<i>H</i>-pyrazol-4-yl}-1,4-dihydropyridine-3,5-dicarboxylate
 monohydrate
;
_journal_coeditor_code           RN2110
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3302
_journal_page_last               o3303
_journal_paper_doi               10.1107/S1600536812045333
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C21 H23 N3 O4 S, H2 O'
_chemical_formula_moiety         'C21 H23 N3 O4 S, H2 O'
_chemical_formula_sum            'C21 H25 N3 O5 S'
_chemical_formula_weight         431.50
_chemical_melting_point_gt       467
_chemical_melting_point_lt       469
_chemical_name_systematic
'Dimethyl 2,6-dimethyl-4-{3-[4-(methylsulfanyl)phenyl]-1<i>H</i>-pyrazol-4-yl}-1,4-dihydropyridine-3,5-dicarboxylate monohydrate'
_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                 110.1060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5542(2)
_cell_length_b                   14.7260(2)
_cell_length_c                   14.5377(2)
_cell_measurement_reflns_used    9343
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.48
_cell_volume                     2121.77(6)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20236
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.190
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.9500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+0.7436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                4311
_reflns_number_total             5267
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rn2110.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2237007
_cod_database_fobs_code          2237007