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_7246275
_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         'C7 H14 N O, C12 H24 O6, B F4'
_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   mixed
_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                   17.3460(16)
_cell_length_b                   15.8138(15)
_cell_length_c                   17.761(2)
_cell_measurement_reflns_used    4322
_cell_measurement_temperature    350.0
_cell_measurement_theta_max      16.556
_cell_measurement_theta_min      2.820
_cell_volume                     4872.0(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      350.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3608
_diffrn_reflns_av_unetI/netI     0.2792
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            66604
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.820
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4290
_refine_ls_number_restraints     685
_refine_ls_restrained_S_all      0.878
_refine_ls_R_factor_all          0.3809
_refine_ls_R_factor_gt           0.1034
_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^)+(0.1410P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2335
_refine_ls_wR_factor_ref         0.3176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                944
_reflns_number_total             4290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01419j2.cif
_cod_data_source_block           11
_cod_depositor_comments
'Adding full bibliography for 7246270--7246275.cif.'
_cod_database_code               7246275
_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
 F1-B1 = F2-B1 = F3-B1 = F4-B1
 1.33 with sigma of 0.01
 F4-F3 = F4A-F2A = F4A-F1A = F3A-F1A
 2.2 with sigma of 0.02
 F3A-F2A
 2.2 with sigma of 0.02
 O5-C12 = C11-C12 = O6-C11 = O6-C10 = C10-C9 = O7-C9 = O7-C8 = C7-C8 = O3-C7 =
 O3-C6 = C6-C5 = O4-C5 = O4-C4 = C3-C4 = O2-C3 = O2-C2 = C2-C1 = O5-C1
 1.48 with sigma of 0.01
 O1B-C18 \\sim O1A-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(B1) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(B2)
\\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O1B) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1, F2, F3, F4, B1, O1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1B, F4A, F1A, B2, F2A, F3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F4A)=Sof(F1A)=Sof(B2)=Sof(F2A)=Sof(F3A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(B1)=FVAR(1)
 Sof(O1B)=Sof(H1BA)=Sof(H18A)=1-FVAR(2)
 Sof(H18)=Sof(O1A)=Sof(H1AA)=FVAR(2)
6.a Riding coordinates:
 N1(H1C,H1D)
6.b Ternary CH refined with riding coordinates:
 C18(H18A), C18(H18), C16(H16), C13(H13)
6.c Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C14(H14A,H14B), C19(H19A,H19B), C17(H17A,H17B), C6(H6A,H6B),
 C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C12(H12A,H12B), C10(H10A,H10B), C5(H5A,
 H5B), C11(H11A,H11B), C4(H4A,H4B), C7(H7A,H7B), C1(H1A,H1B), C2(H2A,H2B)
6.d Idealised tetrahedral OH refined as rotating group:
 O1B(H1BA), O1A(H1AA)
;
_shelx_res_checksum              5933
_shelx_hkl_checksum              41314
_olex2_submission_special_instructions 'No special instructions were received'