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_7243580
_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, H0.25 O0.13, C7 H5 N O3 S'
_chemical_formula_sum            'C31 H37.25 N O7.12 S2'
_chemical_formula_weight         601.99
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2021-03-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-14 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.404(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.321(6)
_cell_length_b                   6.4135(15)
_cell_length_c                   22.097(5)
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    298(1)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.62
_cell_volume                     3062.8(12)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (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 0.994
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            16159
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.745
_diffrn_reflns_theta_min         1.611
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             1277
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 1729 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         8823
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1119
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.729
_reflns_Friedel_fraction_full    0.929
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                5560
_reflns_number_total             8823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00830g6.cif
_cod_data_source_block           mo_210305a_0m
_cod_depositor_comments
'Adding full bibliography for 7243578--7243582.cif.'
_cod_database_code               7243580
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.843
_olex2_refinement_description
;
1. Restrained distances
 H8A-O8
 0.85 with sigma of 0.001
 H8A_$1-H8A
 1.35 with sigma of 0.02
2. Others
 Fixed Sof: O8(0.125) H8A(0.25)
 Fixed Uiso: H2A(0.061) H2B(0.061) H3A(0.072) H3B(0.072) H5(0.063) H7A(0.069)
 H7B(0.069) H8(0.056) H9(0.047) H10(0.043) H11A(0.051) H11B(0.051) H12A(0.049)
 H12B(0.049) H14(0.043) H15A(0.058) H15B(0.058) H16A(0.06) H16B(0.06)
 H18A(0.051) H18B(0.051) H19A(0.059) H19B(0.059) H21A(0.101) H21B(0.101)
 H21C(0.101) H22A(0.081) H22B(0.081) H22C(0.081) H24A(0.135) H24B(0.135)
 H24C(0.135) H8A(0.246) H28(0.077) H29(0.107) H30(0.11) H31(0.101) H1(0.071)
 Fixed X: H2A(0.1025) H2B(0.0646) H3A(0.0184) H3B(0.0072) H5(0.1499)
 H7A(0.234399) H7B(0.217) H8(0.3098) H9(0.2478) H10(0.2017) H11A(0.1392)
 H11B(0.1645) H12A(0.2359) H12B(0.2147) H14(0.3106) H15A(0.3941) H15B(0.365901)
 H16A(0.407) H16B(0.434999) H18A(0.3791) H18B(0.320601) H19A(0.443999)
 H19B(0.3944) H21A(0.107301) H21B(0.151601) H21C(0.0831) H22A(0.2658)
 H22B(0.312301) H22C(0.2418) H24A(0.4359) H24B(0.3749) H24C(0.4188) O8(0.5)
 H8A(0.470099) H28(0.006499) H29(0.0825) H30(0.183201) H31(0.2134) H1(0.0757)
 Fixed Y: H2A(0.627101) H2B(0.8254) H3A(0.8378) H3B(0.615901) H5(0.638101)
 H7A(0.847) H7B(1.061701) H8(0.9712) H9(1.120701) H10(0.7187) H11A(0.8563)
 H11B(1.0814) H12A(0.75) H12B(0.9472) H14(0.7862) H15A(0.946199) H15B(1.1715)
 H16A(1.189) H16B(0.9636) H18A(0.6569) H18B(0.6568) H19A(0.7433) H19B(0.6195)
 H21A(1.177) H21B(1.2076) H21C(1.1347) H22A(1.286399) H22B(1.3198) H22C(1.2857)
 H24A(0.425) H24B(0.311601) H24C(0.4087) H8A(0.8343) H28(-0.364699) H29(-
 0.5647) H30(-0.458899) H31(-0.151899) H1(0.306399)
 Fixed Z: H2A(0.116) H2B(0.075) H3A(0.143101) H3B(0.1084) H5(0.311101)
 H7A(0.351301) H7B(0.311601) H8(0.3265) H9(0.2173) H10(0.163401) H11A(0.051101)
 H11B(0.0787) H12A(0.073) H12B(0.023701) H14(0.200399) H15A(0.289499)
 H15B(0.2644) H16A(0.195901) H16B(0.220901) H18A(0.166301) H18B(0.0884)
 H19A(0.128901) H19B(0.060901) H21A(0.120501) H21B(0.202399) H21C(0.171801)
 H22A(0.0684) H22B(0.1497) H22C(0.121001) H24A(0.4032) H24B(0.3866)
 H24C(0.461801) O8(0) H8A(0.0009) H28(0.3701) H29(0.4642) H30(0.5235)
 H31(0.496699) H1(0.3121)
;
_olex2_submission_special_instructions 'No special instructions were received'