Structural aspects of partial solid solution formation: Two crystalline modifications of chiral derivative of 1,5-dihydro-2H-pyrrol-2-one under consideration
Lodochnikova, Olga; Kosolapova, Liliya; Saifina, Alina; Gubaidullin, Aidar Timergalievich; Fayzullin, Robert R.; Ayrat, Khamatgalimov; Litvinov, Igor; Kurbangalieva, Almira; CrystEngComm  (2017) –; doi:10.1039/C7CE01717K

data_7229579
_publ_section_title
;
 Structural aspects of partial solid solution formation: Two crystalline
 modifications of chiral derivative of 1,5-dihydro-2H-pyrrol-2-one under
 consideration
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE01717K
_journal_year                    2017
_chemical_formula_moiety         'C19 H18 Cl N O2 S'
_chemical_formula_sum            'C19 H18 Cl N O2 S'
_chemical_formula_weight         359.85
_chemical_melting_point          408
_chemical_name_systematic
rac-3-chloro-5-hydroxy-1-(4-methylbenzyl)-4-[(4-methylphenyl)sulfanyl]-1,5-dihydro-2H-pyrrol-2-one
_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-2017/1
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2017-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                113.084(2)
_cell_angle_beta                 106.754(2)
_cell_angle_gamma                97.855(2)
_cell_formula_units_Z            2
_cell_length_a                   8.0999(10)
_cell_length_b                   10.9970(13)
_cell_length_c                   11.7661(14)
_cell_measurement_reflns_used    5439
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.17
_cell_measurement_theta_min      2.73
_cell_volume                     885.35(19)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_reduction        'APEX2 v2014.11-0 (Bruker AXS)'
_computing_molecular_graphics
;
WinGX (Farrugia, 2012); ORTEP-3 (Farrugia, 2012); PLATON (Spek, 2009)
;
_computing_publication_material  'enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11081
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.849
_diffrn_reflns_theta_min         2.099
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/5
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       prism
_exptl_crystal_F_000             376
_exptl_crystal_recrystallization_method
'crystallized from benzene solution at room temperature'
_exptl_crystal_size_max          0.391
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0467P)^2^+0.3176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3907
_reflns_number_total             4512
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01717k1.cif
_cod_data_source_block           ch244
_cod_database_code               7229579
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.877
_shelx_estimated_absorpt_t_max   0.928
_shelx_res_checksum              71638