Revealing the order–disorder type phase transition mechanism in two new supramolecular clathrates
Wei, Wen-Juan; Gao, Hong-Qiang; Fang, Ming; Tang, Yun-Zhi; Wei, Yen; CrystEngComm 25 (2023) 1333–1338; doi:10.1039/D2CE01419J

data_7246273
_publ_section_title
;
 Revealing the order--disorder type phase transition mechanism in two new
 supramolecular clathrates
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1333
_journal_page_last               1338
_journal_paper_doi               10.1039/D2CE01419J
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'Cl O4, C12 H24 O6, C7 H14 N O'
_chemical_formula_sum            'C19 H38 Cl N O11'
_chemical_formula_weight         491.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-28 deposited with the CCDC.	2023-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.3155(8)
_cell_length_b                   15.6324(9)
_cell_length_c                   17.8689(9)
_cell_measurement_reflns_used    5169
_cell_measurement_temperature    300.00(10)
_cell_measurement_theta_max      26.7530
_cell_measurement_theta_min      3.9120
_cell_volume                     4836.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2137
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.855
_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    -32.00  30.00   1.00    9.28    --  -10.68 -19.00  60.00   62
  2  \w    -51.00  28.00   1.00    9.28    --   11.22 -38.00   0.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0255379000
_diffrn_orient_matrix_UB_12      0.0188146000
_diffrn_orient_matrix_UB_13      -0.0262661000
_diffrn_orient_matrix_UB_21      -0.0145585000
_diffrn_orient_matrix_UB_22      0.0411066000
_diffrn_orient_matrix_UB_23      0.0092837000
_diffrn_orient_matrix_UB_31      0.0285069000
_diffrn_orient_matrix_UB_32      0.0040755000
_diffrn_orient_matrix_UB_33      0.0282766000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.855
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17811
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.855
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.619
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0822P)^2^+1.9680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1490
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3731
_reflns_number_total             5827
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01419j2.cif
_cod_data_source_block           210815-11_auto
_cod_depositor_comments
'Adding full bibliography for 7246270--7246275.cif.'
_cod_database_code               7246273
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C00B(H00z), C00H(H2), C00I(H3)
2.b Secondary CH2 refined with riding coordinates:
 N009(H00y,H), C00C(H00,Ha), C00D(H1,Hb), C00E(H00a,H00b), C00F(H00c,H00d),
 C00G(H00e,H00f), C00J(H00g,H00h), C00K(H00i,H00j), C00L(H00k,H00l), C00M(H4,
 Hc), C00N(H00m,H00n), C00O(H00o,H00p), C00P(H5,Hd), C00Q(H00q,H00r), C00R(H00s,
 H00t), C00S(H00u,H00v), C00T(H00w,H00x)
2.c Idealised tetrahedral OH refined as rotating group:
 O008(H008)
;
_shelx_res_checksum              24097
_shelx_hkl_checksum              52254
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.818