Crystal structures of (5<i>RS</i>)-(<i>Z</i>)-4-[5-(furan-2-yl)-3-phenyl-4,5-dihydro-1<i>H</i>-pyrazol-1-yl]-4-oxobut-2-enoic acid and (5<i>RS</i>)-(<i>Z</i>)-4-[5-(furan-2-yl)-3-(thiophen-2-yl)-4,5-dihydro-1<i>H</i>-pyrazol-1-yl]-4-oxobut-2-enoic acid
Borisova, Kseniya K.; Toze, Flavien A. A.; Yagafarov, Nniyaz Z.; Zubkov, Fedor I.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Khrustalev, Victor N.; Acta Crystallographica Section E 72 (2016) 1557–1561; doi:10.1107/S2056989016013992

data_2241878
_publ_section_title
;
 Crystal structures of
 (5<i>RS</i>)-(<i>Z</i>)-4-[5-(furan-2-yl)-3-phenyl-4,5-dihydro-1<i>H</i>-pyrazol-1-yl]-4-oxobut-2-enoic
 acid and
 (5<i>RS</i>)-(<i>Z</i>)-4-[5-(furan-2-yl)-3-(thiophen-2-yl)-4,5-dihydro-1<i>H</i>-pyrazol-1-yl]-4-oxobut-2-enoic
 acid
;
_journal_coeditor_code           XU5892
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1557
_journal_page_last               1561
_journal_paper_doi               10.1107/S2056989016013992
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C15 H12 N2 O4 S'
_chemical_formula_moiety         'C15 H12 N2 O4 S'
_chemical_formula_sum            'C15 H12 N2 O4 S'
_chemical_formula_weight         316.33
_chemical_name_systematic
'(5<i>RS</i>)-(<i>Z</i>)-4-[5-(Furan-2-yl)-3-(thiophen-2-yl)-4,5-dihydro-1<i>H</i>-pyrazol-1-yl]-4-oxobut-2-enoic acid'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 98.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6702(19)
_cell_length_b                   13.150(3)
_cell_length_c                   11.240(2)
_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.0
_cell_measurement_theta_min      3.6
_cell_volume                     1414.4(5)
_computing_cell_refinement
;
<i>i</i>MOSFLM (Battye <i>et al.</i>, 2011)
;
_computing_data_collection
;
<i>Automar</i> (MarXperts, 2015)
;
_computing_data_reduction
;
<i>i</i>MOSFLM (Battye <i>et al.</i>, 2011)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'MAR CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96990
_diffrn_reflns_av_R_equivalents  0.0870
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17279
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.485
_diffrn_reflns_theta_min         3.549
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SCALA; Evans, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.523
_refine_ls_extinction_coef       0.029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         2961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+1.1417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1140
_refine_ls_wR_factor_ref         0.1185
_reflns_number_gt                2685
_reflns_number_total             2961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            xu5892sup1.cif
_cod_data_source_block           II
_cod_database_code               2241878
_cod_database_fobs_code          2241878
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.886
_shelx_hkl_checksum              88482
_shelx_res_checksum              60748
_shelxl_version_number           2014/6