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_7242591
_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
'2(C9.5 H14 N2 O3 S), 3(C H1.5 N0.5), 2(H O0.5)'
_chemical_formula_sum            'C22 H34.5 N5.5 O7 S2'
_chemical_formula_weight         552.17
_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             2019-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2020-11-30 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                   14.406(3)
_cell_length_b                   16.682(3)
_cell_length_c                   25.020(5)
_cell_measurement_reflns_used    17086
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.9064
_cell_measurement_theta_min      1.4672
_cell_volume                     6013(2)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      133.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            57965
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.574
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.223
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Flack x determined using 4138 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_coef       0.0032(5)
_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   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         10601
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0766P)^2^+2.2587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                10140
_reflns_number_total             10601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00284h2.cif
_cod_data_source_block           shelxl_sq
_cod_depositor_comments
'Adding full bibliography for 7242591--7242593.cif.'
_cod_original_formula_sum        'C22 H34.50 N5.50 O7 S2'
_cod_database_code               7242591
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.957
_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. Restrained distances
 C26-N5 = C28-N7 = C7-N2 = C9-N3
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N9) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N11) \\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: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Free rotating group:
 O14(H14A,H14B), O13(H13C,H13D)
4.b Ternary CH refined with riding coordinates:
 C2(H2A), C5(H5), C10(H10), C11(H11), C21(H21), C24(H24), C29(H29), C31(H31)
4.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C16(H16A,H16B), C27(H27A,H27B), C32(H32A,H32B),
 C35(H35A,H35B)
4.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5A), N6(H6), N7(H7)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C18(H18A,
 H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C)
;
_shelx_res_checksum              79240
_shelx_hkl_checksum              4126
_shelx_fab_checksum              37748
_olex2_submission_special_instructions 'No special instructions were received'