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_7243578
_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           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-02 deposited with the CCDC.	2021-09-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.529(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8237(9)
_cell_length_b                   6.3425(2)
_cell_length_c                   23.2717(9)
_cell_measurement_reflns_used    10462
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      33.5900
_cell_measurement_theta_min      1.8760
_cell_volume                     2975.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -120.00  60.00   1.00    2.00    --  -30.00  45.00   0.00  180
  2  \w   -120.00  30.00   1.00    2.00    --  -30.00  45.00  90.00  150
  3  \w   -120.00   0.00   1.00    2.00    --  -30.00  45.00 180.00  120
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0270073000
_diffrn_orient_matrix_UB_12      0.0075224000
_diffrn_orient_matrix_UB_13      -0.0097156000
_diffrn_orient_matrix_UB_21      -0.0225392000
_diffrn_orient_matrix_UB_22      0.0062949000
_diffrn_orient_matrix_UB_23      -0.0314215000
_diffrn_orient_matrix_UB_31      -0.0005247000
_diffrn_orient_matrix_UB_32      0.1114722000
_diffrn_orient_matrix_UB_33      0.0024579000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0721
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            18338
_diffrn_reflns_point_group_measured_fraction_full 0.939
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.655
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2664 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       0.0043(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         9920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.686
_reflns_Friedel_fraction_full    0.866
_reflns_Friedel_fraction_max     0.738
_reflns_number_gt                8240
_reflns_number_total             9920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00830g6.cif
_cod_data_source_block           r20210130f
_cod_depositor_comments
'Adding full bibliography for 7243578--7243582.cif.'
_cod_original_formula_sum        'C31 H38 N O7.50 S2'
_cod_database_code               7243578
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C5(H5), C12(H12), C13(H13), C14(H14)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C10(H10A,H10B), C11(H11A,
 H11B), C15(H15A,H15B), C21(H21A,H21B), C22(H22A,H22B)
3.d Aromatic/amide H refined with riding coordinates:
 C17(H17), N1(H1), C28(H28), C29(H29), C30(H30), C31(H31)
3.e Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              79567
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.232
_oxdiff_exptl_absorpt_empirical_full_min 0.722