Influence of intermolecular interactions and crystal structure on desolvation mechanisms of solvates
Liu, Wanying; Hou, Baohong; Huang, Xin; Zong, Shuyi; Zheng, Zhixin; Li, Shuyu; Zhao, Bugui; Liu, Songqiang; Zhou, Lina; Hao, Hongxun; CrystEngComm 23 (2021) 3557–3568; doi:10.1039/D1CE00284H

data_7242592
_publ_section_title
;
 Influence of intermolecular interactions and crystal structure on
 desolvation mechanisms of solvates
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              3557
_journal_page_last               3568
_journal_paper_doi               10.1039/D1CE00284H
_journal_volume                  23
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C19 H28 N4 O6 S2, C3 H8 O'
_chemical_formula_sum            'C22 H36 N4 O7 S2'
_chemical_formula_weight         532.67
_space_group_crystal_system      tetragonal
_space_group_IT_number           78
_space_group_name_Hall           'P 4cw'
_space_group_name_H-M_alt        'P 43'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-01 deposited with the CCDC.	2021-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.556(3)
_cell_length_b                   19.556(3)
_cell_length_c                   17.153(3)
_cell_measurement_reflns_used    10443
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9304
_cell_measurement_theta_min      1.5780
_cell_volume                     6559.9(18)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.0828
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            56819
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.019
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_min         1.579
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 3015 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(5)
_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     686
_refine_ls_number_reflns         11493
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0790
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1248P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2008
_refine_ls_wR_factor_ref         0.2148
_reflns_Friedel_coverage         0.919
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                9174
_reflns_number_total             11493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00284h2.cif
_cod_data_source_block           r20191027c1_sq
_cod_depositor_comments
'Adding full bibliography for 7242591--7242593.cif.'
_cod_original_cell_volume        6560(2)
_cod_database_code               7242592
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.961
_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) groups
2. Restrained distances
 O13-C40 = O14-C43 = O15-C46
 1.4 with sigma of 0.01
 C39-C40 = C40-C41 = C42-C43 = C43-C44 = C45-C46 = C46-C47
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C46)
\\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Fixed Sof: O14(0.5) H14(0.5) C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5)
 H43(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) O15(0.5) H15(0.5) C45(0.5)
 H45A(0.5) H45B(0.5) H45C(0.5) C46(0.5) H46(0.5) C47(0.5) H47A(0.5) H47B(0.5)
 H47C(0.5)
5.a Ternary CH refined with riding coordinates:
 C2(H2A), C5(H5), C10(H10), C12(H12), C21(H21), C25(H25), C29(H29), C31(H31),
 C40(H40), C43(H43), C46(H46)
5.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C17(H17A,H17B), C27(H27A,H27B), C32(H32A,H32B),
 C36(H36A,H36B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5A), N6(H6), N7(H7)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,
 H47B,H47C)
5.e Idealised tetrahedral OH refined as rotating group:
 O13(H13), O14(H14), O15(H15)
;
_shelx_res_checksum              91597
_shelx_hkl_checksum              96808
_shelx_fab_checksum              25937
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'