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_7246272
_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, C7 H14 N O, C12 H24 O6'
_chemical_formula_sum            'C19 H38 Cl N O11'
_chemical_formula_weight         491.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m 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            4
_cell_length_a                   15.6730(17)
_cell_length_b                   10.8757(9)
_cell_length_c                   14.2780(15)
_cell_measurement_reflns_used    2403
_cell_measurement_temperature    365.01(11)
_cell_measurement_theta_max      28.7610
_cell_measurement_theta_min      1.9380
_cell_volume                     2433.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      365.01(11)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.800
_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    -92.00  18.00   0.50    2.07    --  -11.30 -38.00  71.00  220
  2  \w     -8.00  18.00   0.50    2.07    --   10.52 -99.00  60.00   52
  3  \w     30.00  56.00   0.50    2.07    --   10.52 -99.00  60.00   52
  4  \w      0.00  12.50   0.50    2.07    --  -11.30 -99.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0365057000
_diffrn_orient_matrix_UB_12      -0.0268204000
_diffrn_orient_matrix_UB_13      0.0213556000
_diffrn_orient_matrix_UB_21      -0.0157640000
_diffrn_orient_matrix_UB_22      0.0159414000
_diffrn_orient_matrix_UB_23      0.0447697000
_diffrn_orient_matrix_UB_31      -0.0218270000
_diffrn_orient_matrix_UB_32      -0.0571209000
_diffrn_orient_matrix_UB_33      0.0023762000
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.800
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9854
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.800
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_min         1.929
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_refine_diff_density_max         1.561
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.479
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     487
_refine_ls_restrained_S_all      2.665
_refine_ls_R_factor_all          0.3081
_refine_ls_R_factor_gt           0.2497
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6230
_refine_ls_wR_factor_ref         0.6590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1253
_reflns_number_total             2842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01419j2.cif
_cod_data_source_block           wwj-210815-11-365k_auto
_cod_depositor_comments
'Adding full bibliography for 7246270--7246275.cif.'
_cod_database_code               7246272
_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. Restrained distances
 O0-O4 = O6-O7
 2.731 with sigma of 0.02
 O5-C4B = O8-C4A
 2.247 with sigma of 0.02
 C2B-O0 = C2A-O6
 2.284 with sigma of 0.02
 C4B-C2B = C4A-C2A
 1.842 with sigma of 0.02
 C2B-C3B
 2.131 with sigma of 0.02
 C5B-C0 = C5A-C1
 1.475 with sigma of 0.02
 C3A-C2A
 2.131 with sigma of 0.02
 C4B-C5B = C4A-C5A
 2.234 with sigma of 0.02
 O5-O0 = O8-O6
 2.706 with sigma of 0.02
 C5B-O4 = C5A-O7
 2.259 with sigma of 0.02
 C0-C7B = C1-C7A
 2.22 with sigma of 0.02
 C4B-C2B = C4A-C2A = C3B_$1-C3B = C3A_$1-C3A = C4B-C2B = C4A-C2A = C5A-C1 =
 C5B-C0 = C7B_$1-C7B = C7A_$1-C7A = C5B-C0 = C5A-C1
 1.5 with sigma of 0.02
 O7-C7A = O4-C7B = O7-C1 = O4-C0 = O0-C5B = O6-C5A = O0-C4B = O6-C4A = O5-C2B =
  O8-C2A = O5-C3B = O8-C3A = O5-C3B = O8-C3A = O5-C2B = O8-C2A = O0-C4B = O6-
 C4A = O0-C5B = O6-C5A = O7-C1 = O4-C0 = O7-C7A = O4-C7B
 1.4 with sigma of 0.02
 C1-C7B = C0-C7A = C5B-C4B = C4A-C5A = C2B-C3B = C2A-C3A = C3A-C2A = C3B-C2B =
 C4A-C5A = C4B-C5B = C0-C7B = C1-C7A
 2.37 with sigma of 0.02
 C7B_$1-C7B \\sim C5B-C0 \\sim C4B-C2B \\sim C3B_$1-C3B \\sim C4B-C2B \\sim
C5B-C0
 with sigma of 0.02
 O4-C7B \\sim O4-C0 \\sim O0-C5B \\sim O0-C4B \\sim O5-C2B \\sim O5-C3B \\sim
O5-C3B \\sim O5-C2B \\sim O0-C4B
 \\sim O0-C5B \\sim O4-C0 \\sim O4-C7B
 with sigma of 0.02
 Cl01-O2 \\sim Cl01-O1 \\sim Cl01-O3
 with sigma of 0.02
 Cl01-O2 \\sim Cl01-O3_$1 \\sim Cl01-O3 \\sim Cl01-O1
 with sigma of 0.02
 O3-O1 \\sim O3-O2 \\sim O3-O3_$1 \\sim O3_$1-O2 \\sim O3_$1-O1 \\sim O2-O1
 with sigma of 0.02
 O3-O2 \\sim O3-O3_$1 \\sim O3-O1 \\sim O3_$1-O1 \\sim O3_$1-O2 \\sim O2-O1
 with sigma of 0.02
 Cl01-O3_$1 \\sim Cl01-O1 \\sim Cl01-O3 \\sim Cl01-O2
 with sigma of 0.02
 Cl01-O2 \\sim Cl01-O2A \\sim Cl01-O3 \\sim Cl01-O3A \\sim Cl01-O1 \\sim
Cl01-O1A
 with sigma of 0.02
 O2-O3 \\sim O2-O1 \\sim O2A-O3A \\sim O2A-O1A \\sim O3-O1 \\sim O3A-O1A
 with sigma of 0.04
 O2A-O1A \\sim O3A-O1A \\sim O3A-O2A \\sim O3-O1 \\sim O2-O1
 with sigma of 0.02
 C4B-C5B \\sim C4A-C5A
 with sigma of 0.02
 O5-C3B \\sim O8-C3A \\sim O8-C2A \\sim O5-C2B \\sim O0-C4B \\sim O6-C4A \\sim
O0-C5B \\sim O6-C5A \\sim O7-C1
 \\sim O7-C7A \\sim O4-C7B \\sim O4-C0
 with sigma of 0.02
 C3A-C2A \\sim C2B-C3B
 with sigma of 0.02
 C0-C7B \\sim C1-C7A
 with sigma of 0.02
 C4B-C2B \\sim C4A-C2A \\sim C5B-C0 \\sim C5A-C1
 with sigma of 0.02
 C5B-C0 \\sim C5A-C1 \\sim C4A-C2A \\sim C4B-C2B \\sim C3B_$1-C3B \\sim
C3A_$1-C3A \\sim C4A-C2A \\sim C5A-
 C1 \\sim C5B-C0 \\sim C7B_$1-C7B \\sim C7A_$1-C7A
 with sigma of 0.02
 O6-C4A \\sim O0-C4B \\sim O6-C5A \\sim O0-C5B \\sim O7-C1 \\sim O4-C0 \\sim
O4-C7B \\sim O7-C7A \\sim O4-C7B
 \\sim O7-C7A \\sim O4-C0 \\sim O7-C1 \\sim O0-C5B \\sim O6-C5A \\sim O6-C4A
\\sim O0-C4B \\sim O8-C2A \\sim O5-C2B
 \\sim O5-C3B \\sim O8-C3A \\sim O5-C3B \\sim O8-C3A \\sim O8-C2A \\sim O5-C2B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(O0) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C4A) \\sim Ueq,
Uanis(C4B) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(O0)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq,
Uanis(O5) \\sim Ueq, Uanis(C0) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C4B)
\\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C5B) \\sim Ueq,
Uanis(C7B) \\sim Ueq, Uanis(C7B) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(C1) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C3A)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C7A) \\sim Ueq,
Uanis(C7A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O2A, O1A, O3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, O2, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0, C4B, C5B, C2B, C0, O5, O4, C3B, C7B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C4A, C5A, C2A, C1, O8, O7, C3A, C7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C3A, C2A, O3, C7A, O2, C4A, O6, C5A, O6, C2A, O7, C4A, O7, C3A, O8, C5A,
 O8, C7A, C1, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0, C7B, C3B, O0, O2A, O4, C5B, O4, O1A, O5, C4B, O5, C3B, C0, C5B, C0, C7B,
 C2B, O3A, C2B, C4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H7Aa, C3A, H2Ab, O1, H5Aa, O3, H4Aa, O2, H3Ab, O6, C7A, O7, C4A, O8, H4Ab, C1,
  H3Aa, H1a, C5A, H1b, H5Ab, C2A, H2Aa, H7Ab
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0, H5Ba, C3B, O4, H7Bb, O5, H3Bb, C0, C7B, O2A, O3A, H0b, H3Ba, C2B, C5B,
 H2Ba, H5Bb, H2Bb, H7Ba, C4B, O1A, H4Ba, H4Bb, H0a
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3A)=1-FVAR(1)
 Sof(O1A)=Sof(O2A)=0.5*(1-FVAR(2))
 Sof(O1)=Sof(O2)=0.5*FVAR(2)
 Sof(O3)=FVAR(1)
 Sof(O0)=Sof(O4)=Sof(O5)=Sof(C0)=Sof(H0a)=Sof(H0b)=Sof(C2B)=Sof(H2Ba)=
 Sof(H2Bb)=Sof(C4B)=Sof(H4Ba)=Sof(H4Bb)=Sof(C3B)=Sof(H3Ba)=Sof(H3Bb)=Sof(C5B)=
 Sof(H5Ba)=Sof(H5Bb)=Sof(C7B)=Sof(H7Ba)=Sof(H7Bb)=1-FVAR(2)
 Sof(O6)=Sof(O7)=Sof(O8)=Sof(C1)=Sof(H1a)=Sof(H1b)=Sof(C2A)=Sof(H2Aa)=
 Sof(H2Ab)=Sof(C4A)=Sof(H4Aa)=Sof(H4Ab)=Sof(C3A)=Sof(H3Aa)=Sof(H3Ab)=Sof(C5A)=
 Sof(H5Aa)=Sof(H5Ab)=Sof(C7A)=Sof(H7Aa)=Sof(H7Ab)=FVAR(2)
 Fixed Sof: H003(0.5)
6.a Ternary CH refined with riding coordinates:
 C004(H004), C005(H005)
6.b Secondary CH2 refined with riding coordinates:
 N002(H00a,H00b), C008(H00c,H00d), C00A(H00e,H00f), C0(H0a,H0b), C2B(H2Ba,
 H2Bb), C4B(H4Ba,H4Bb), C3B(H3Ba,H3Bb), C5B(H5Ba,H5Bb), C7B(H7Ba,H7Bb), C1(H1a,
 H1b), C2A(H2Aa,H2Ab), C4A(H4Aa,H4Ab), C3A(H3Aa,H3Ab), C5A(H5Aa,H5Ab), C7A(H7Aa,
 H7Ab)
6.c Idealised tetrahedral OH refined as rotating group:
 O003(H003)
;
_shelx_res_checksum              88124
_shelx_hkl_checksum              37969
_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 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.783