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_7246270
_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         'B F4, C7 H14 N O, C12 H24 O6'
_chemical_formula_sum            'C19 H38 B F4 N O7'
_chemical_formula_weight         479.31
_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
_audit_creation_date             2021-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   17.2870(6)
_cell_length_b                   15.6308(5)
_cell_length_c                   17.7593(6)
_cell_measurement_reflns_used    11744
_cell_measurement_temperature    300.80(10)
_cell_measurement_theta_max      31.7530
_cell_measurement_theta_min      2.0970
_cell_volume                     4798.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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_environment      air
_diffrn_ambient_temperature      300.80(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.863
_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     36.00  77.00   0.50    0.80    --    8.30  59.00 -51.00   82
  2  \w    -17.00  22.00   0.50    0.80    --   -8.54  62.00 140.00   78
  3  \w    -59.00  17.00   0.50    0.80    --    8.30 -19.00-120.00  152
  4  \w    -15.00  48.00   0.50    0.80    --    8.30  77.00-120.00  126
  5  \w    -18.00  39.00   0.50    0.80    --    8.30 -99.00 150.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0369513000
_diffrn_orient_matrix_UB_12      -0.0106343000
_diffrn_orient_matrix_UB_13      0.0146164000
_diffrn_orient_matrix_UB_21      0.0172438000
_diffrn_orient_matrix_UB_22      -0.0311718000
_diffrn_orient_matrix_UB_23      0.0236719000
_diffrn_orient_matrix_UB_31      0.0046134000
_diffrn_orient_matrix_UB_32      0.0312076000
_diffrn_orient_matrix_UB_33      0.0286548000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44029
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.874
_diffrn_reflns_theta_min         2.098
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.117
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
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    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         7114
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0985
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0711P)^2^+1.0036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4133
_reflns_number_total             7114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01419j2.cif
_cod_data_source_block           wj_b4_6_301k
_cod_depositor_comments
'Adding full bibliography for 7246270--7246275.cif.'
_cod_database_code               7246270
_shelx_shelxl_version_number     2018/3
_diffrn_oxdiff_digest_frames
;
019c58aa5e7b36b4073ceb55ab99ac5dfb00030e8d3
;
_diffrn_oxdiff_digest_hkl
;
019306dc8e2126b3fc0a79e56704b6a2ea9e67
;
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.50
_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
 F1-B1 \\sim F1A-B1 \\sim F2A-B1 \\sim F2-B1 \\sim F3A-B1 \\sim F3-B1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F1A \\sim F2A \\sim F2 \\sim F4 \\sim F3 \\sim F3A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F1A) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 F1, F2, F3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F1A, F2A, F3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1C), C4(H4), C6(H6)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              21793
_shelx_hkl_checksum              12050
_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 1.470
_oxdiff_exptl_absorpt_empirical_full_min 0.669