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_7242593
_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(C19 H28 N4 O6 S2), C3 H8 O, 3(H2 O)'
_chemical_formula_sum            'C41 H70 N8 O16 S4'
_chemical_formula_weight         1059.29
_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     dual
_audit_creation_date             2020-10-10
_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            4
_cell_length_a                   14.1543(3)
_cell_length_b                   16.7550(4)
_cell_length_c                   23.7148(6)
_cell_measurement_reflns_used    26307
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      33.4980
_cell_measurement_theta_min      2.0530
_cell_volume                     5624.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       CrystalClear(Rigaku,2008)
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.989
_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    3.00    --  -30.00  45.00   0.00  180
  2  \w   -120.00  30.00   1.00    3.00    --  -30.00  45.00  90.00  150
  3  \w   -120.00   0.00   1.00    3.00    --  -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      -0.0197696000
_diffrn_orient_matrix_UB_12      0.0013437000
_diffrn_orient_matrix_UB_13      -0.0274612000
_diffrn_orient_matrix_UB_21      0.0453310000
_diffrn_orient_matrix_UB_22      -0.0068451000
_diffrn_orient_matrix_UB_23      -0.0117806000
_diffrn_orient_matrix_UB_31      -0.0080888000
_diffrn_orient_matrix_UB_32      -0.0417689000
_diffrn_orient_matrix_UB_33      0.0010755000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44974
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 4481 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       0.0046(13)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         11421
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0530P)^2^+3.2485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.822
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                10647
_reflns_number_total             11421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00284h2.cif
_cod_data_source_block           r20201005a
_cod_depositor_comments
'Adding full bibliography for 7242591--7242593.cif.'
_cod_database_code               7242593
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.959
_reflns_odcompleteness_completeness 98.96
_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) groups, All O(H,H) groups
2. Restrained distances
 H16C-H16D
 1.45 with sigma of 0.01
 O16A-H16C = O16A-H16D
 0.85 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O16 \\sim O16A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(O16) \\sim Ueq, Uanis(O16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O16A)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(O16)=Sof(H16A)=Sof(H16B)=FVAR(1)
 Fixed Sof: O14(0.5) H14A(0.5) H14B(0.5) O14A(0.2) H14C(0.2) H14D(0.2)
 O14B(0.3) H14E(0.3) H14F(0.3)
5.a Riding coordinates:
 O14(H14A,H14B), O16(H16A,H16B), O16A(H16C,H16D), O14A(H14C,H14D), O14B(H14E,
 H14F)
5.b Free rotating group:
 O15(H15A,H15B)
5.c Ternary CH refined with riding coordinates:
 C3(H3A), C6(H6), C10(H10), C12(H12), C22(H22), C25(H25), C29(H29), C31(H31)
5.d Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C13(H13A,H13B), C17(H17A,H17B), C27(H27A,H27B), C32(H32A,H32B),
 C36(H36A,H36B), C40(H40A,H40B), C41(H41A,H41B)
5.e Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N5(H5), N6(H6A), N7(H7)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C)
5.g Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_res_checksum              87803
_shelx_hkl_checksum              42237
_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 1.254
_oxdiff_exptl_absorpt_empirical_full_min 0.670