Experimental and computational approaches to produce and characterise isostructural solvates
Braun, Doris E.; Gelbrich, Thomas; Griesser, Ulrich J.; CrystEngComm 21 (2019) 5533–; doi:10.1039/C9CE00856J

data_7233417
_publ_section_title
;
 Experimental and computational approaches to produce and characterise
 isostructural solvates
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5533
_journal_paper_doi               10.1039/C9CE00856J
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         '2(C12 H12 N2 O2 S), C2 H3 N'
_chemical_formula_sum            'C26 H27 N5 O4 S2'
_chemical_formula_weight         537.64
_chemical_name_systematic        'Dapsone acetonitrile hemisolvate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.818(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5132(2)
_cell_length_b                   16.1830(3)
_cell_length_c                   18.9865(4)
_cell_measurement_reflns_used    11098
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.5810
_cell_measurement_theta_min      3.2610
_cell_volume                     2591.44(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.9g (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23182
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         2.740
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0480P)^2^+1.5077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4510
_reflns_number_total             5290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce00856j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7233417--7233418.cif.'
_cod_database_code               7233417
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2014/6
_shelx_res_checksum              25764