Desolvation induced crystal jumping: reversible hydration and dehydration of a spironolactone–saccharin cocrystal with water as the jumping-mate
Chen, Yifu; Jing, Bo; Chang, Zewei; Gong, Junbo; CrystEngComm 23 (2021) 6838–6842; doi:10.1039/D1CE00830G

data_7243579
_publ_section_title
;
 Desolvation induced crystal jumping: reversible hydration and dehydration
 of a spironolactone--saccharin cocrystal with water as the jumping-mate
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              6838
_journal_page_last               6842
_journal_paper_doi               10.1039/D1CE00830G
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H32 O4 S, C7 H5 N O3 S, 0.5(H2 O)'
_chemical_formula_sum            'C31 H38 N O7.5 S2'
_chemical_formula_weight         608.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-08
_audit_creation_method
; 
Olex2 1.3 
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) 
;
_audit_update_record
;
2021-03-27 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.7850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.2663(9)
_cell_length_b                   6.3994(2)
_cell_length_c                   22.1324(8)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      72.38
_cell_measurement_theta_min      6.07
_cell_volume                     3074.33(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(1)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            51668
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         72.379
_diffrn_reflns_theta_min         3.050
_diffrn_source_current           3.57
_diffrn_source_power             0.2497215
_diffrn_source_voltage           69.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5739
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
; 
 Flack x determined using 3931 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.079(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         8925
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0776P)^2^+0.2534P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     0.950
_reflns_number_gt                8837
_reflns_number_total             8925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00830g6.cif
_cod_data_source_block           210303c_0m
_cod_depositor_comments
'Adding full bibliography for 7243578--7243582.cif.'
_cod_original_formula_sum        'C31 H38 N O7.50 S2'
_cod_database_code               7243579
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.424
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups, All N(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups, All O(H,H) groups 
2. Others 
 Fixed Sof: H8A(0.5) H8B(0.5) 
3.a Riding coordinates: 
 O8(H8A,H8B) 
3.b Ternary CH refined with riding coordinates: 
 C8(H8), C9(H9), C10(H10), C14(H14) 
3.c Secondary CH2 refined with riding coordinates: 
 C2(H2A,H2B), C3(H3A,H3B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,H12B), 
 C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B) 
3.d Aromatic/amide H refined with riding coordinates: 
 C5(H5), N1(H1), C28(H28), C29(H29), C30(H30), C31(H31) 
3.e Idealised Me refined as rotating group: 
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C) 
;
_shelx_res_checksum              36448
_olex2_submission_special_instructions 'No special instructions were received'