Reduced 3,4'-bipyrazoles carrying thiophene and thiazole substituents: structures of two intermediates and two products
Harish Chinthal, Chayanna; Yathirajan, Hemmige S.; Manju, Nagaraja; Kalluraya, Balakrishna; Foro, Sabine; Glidewell, Christopher; Acta Crystallographica Section E 77 (2021) 335–340; doi:10.1107/S2056989021002310

data_2243769
_publ_section_title
;
 Reduced 3,4'-bipyrazoles carrying thiophene and thiazole substituents:
 structures of two intermediates and two products
;
_journal_coeditor_code           DX2035
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              335
_journal_page_last               340
_journal_paper_doi               10.1107/S2056989021002310
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '2C24 H19 Cl2 N5 O S2, H2 O'
_chemical_formula_moiety         '2(C24 H19 Cl2 N5 O S2), H2 O'
_chemical_formula_sum            'C48 H40 Cl4 N10 O3 S4'
_chemical_formula_weight         1074.94
_chemical_name_systematic
'5'-(2,4-Dichlorophenoxy)-3'-methyl-1'-phenyl-5-(thiophen-2-yl)-3,4-dihydro-1'<i>H</i>,2<i>H</i>-3,4'-bipyrazole-2-carbothioamide hemihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 96.246(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0370(10)
_cell_length_b                   8.4266(6)
_cell_length_c                   19.4710(10)
_cell_measurement_reflns_used    5307
_cell_measurement_temperature    296(2)
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_cell_measurement_theta_min      2.629
_cell_volume                     2452.5(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2020)
;
_computing_publication_material
;
SHELXL-2014 (Sheldrick, 2015b) and PLATON (Spek, 2020)
;
_computing_structure_refinement
;
SHELXL-2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type
;
Oxford Diffraction Xcalibur
with Sapphire CCD detector
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10494
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.629
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       needle
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.296
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.978
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0411P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                3075
_reflns_number_total             5290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dx2035sup1.cif
_cod_data_source_block           Ib
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2243769
_cod_database_fobs_code          2243769
_shelx_estimated_absorpt_t_min   0.850
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              16432
_shelx_res_checksum              35418
_shelxl_version_number           2.014