Capturing the metastable state in the spontaneous and reversible single-crystal-to-single-crystal phase transition of riluzolium oxalate
Mondal, Pradip Kumar; Rao, Varun; Chopra, Deepak; CrystEngComm 20 (2018) 2079–; doi:10.1039/C8CE00283E

data_7230309
_publ_section_title
;
 Capturing the metastable state in the spontaneous and reversible
 single-crystal-to-single-crystal phase transition of riluzolium oxalate
;
_journal_issue                   15
_journal_name_full               CrystEngComm
_journal_page_first              2079
_journal_paper_doi               10.1039/C8CE00283E
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C18 H12 F6 N4 O6 S2'
_chemical_formula_weight         558.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-11-20 deposited with the CCDC.
2018-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.624(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.786(3)
_cell_length_b                   20.184(3)
_cell_length_c                   11.6566(17)
_cell_measurement_reflns_used    2858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      2.69
_cell_volume                     4329.3(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_av_unetI/netI     0.2519
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9372
_diffrn_reflns_point_group_measured_fraction_full 0.594
_diffrn_reflns_point_group_measured_fraction_max 0.580
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.571
_diffrn_reflns_theta_min         2.494
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.19(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         7045
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0140P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.159
_reflns_Friedel_fraction_full    0.187
_reflns_Friedel_fraction_max     0.159
_reflns_number_gt                3956
_reflns_number_total             7045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00283e2.cif
_cod_data_source_block           RZ-OA-100K
_cod_depositor_comments
'Adding full bibliography for 7230307--7230312.cif.'
_cod_original_cell_volume        4329.4(11)
_cod_database_code               7230309
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              82486