Characterization of a New Solvatomorph of Drospirenone by Thermogravimetry–Mass Spectrometry Combined with Other Solid-State Analysis Methods
Yuan, Penghui; Yang, Dezhi; Wang, Ruonan; Gong, Ningbo; Zhang, Li; Lu, Yang; Du, Guanhua; ACS Omega  (2020) –; doi:10.1021/acsomega.0c03531

data_4518088
_publ_section_title
;
 Characterization of a New Solvatomorph of Drospirenone by
 Thermogravimetry--Mass Spectrometry Combined with Other Solid-State
 Analysis Methods
;
_journal_name_full               'ACS Omega'
_journal_paper_doi               10.1021/acsomega.0c03531
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H30 O3&#x00EF;&#x00BC;&#x008C;C2 H6 O S'
_chemical_formula_sum            'C26 H36 O4 S'
_chemical_formula_weight         444.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2019-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3541(3)
_cell_length_b                   11.5712(3)
_cell_length_c                   32.2251(4)
_cell_measurement_reflns_used    6
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.5
_cell_measurement_theta_min      26.6
_cell_volume                     2369.34(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    ORTEPII(Johnson,1976)andPLUTON(Spek,1990)
_computing_publication_material  ' SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  ' SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    ' SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'MicroMax 002+'
_diffrn_measurement_method       \f\k
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            15032
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.115
_diffrn_reflns_theta_min         4.059
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.402
_exptl_crystal_size_mid          0.352
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Flack x determined using 1358 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.003(12)
_refine_ls_extinction_coef       0.0053(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4521
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0712P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.698
_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                3823
_reflns_number_total             4521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao0c03531_si_002.cif
_cod_data_source_block           6051
_cod_database_code               4518088
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.595
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 S1A-O1D
 1.4 with sigma of 0.02
 S1A-C2D
 1.7 with sigma of 0.02
3. Others
 Sof(H2DD)=Sof(H2DE)=Sof(H2DF)=Sof(H1DD)=Sof(H1DE)=Sof(H1DF)=Sof(S1A)=1-FVAR(1)
 Sof(S1B)=Sof(H2DA)=Sof(H2DB)=Sof(H2DC)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C004(H004), C005(H005), C006(H006), C008(H008), C009(H009), C00A(H00A),
 C00G(H00G)
4.b Secondary CH2 refined with riding coordinates:
 C00D(H00B,H00C), C00I(H00H,H00I), C00K(H00J,H00K), C00M(H00L,H00M), C00N(H00N,
 H00O), C00P(H00S,H00T), C00R(H00V,H00W), C00T(H00X,H00Y)
4.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00U)
4.d Idealised Me refined as rotating group:
 C00F(H00D,H00E,H00F), C00O(H00P,H00Q,H00R), C2D(H2DA,H2DB,H2DC), C2D(H2DD,
 H2DE,H2DF), C1D(H1DA,H1DB,H1DC), C1D(H1DD,H1DE,H1DF)
;
_shelx_res_checksum              15172
_shelx_hkl_checksum              1549
_olex2_submission_special_instructions 'No special instructions were received'