Guest size effects on a robust structure of semiclathrate hydrates and their thermophysical properties.
Muromachi, Sanehiro; Takeya, Satoshi; Physical chemistry chemical physics : PCCP 26 (2024) 3315–3321; doi:10.1039/d3cp04252a

data_7247882
_publ_section_title
;
 Guest size effects on a robust structure of semiclathrate hydrates and
 their thermophysical properties.
;
_journal_issue                   4
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              3315
_journal_page_last               3321
_journal_paper_doi               10.1039/d3cp04252a
_journal_volume                  26
_journal_year                    2024
_chemical_formula_sum            'C10 H3.5 Cl0.5 N6.5 O18'
_chemical_formula_weight         520.42
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.43538(16)
_cell_length_b                   23.43538(16)
_cell_length_c                   12.39150(13)
_cell_measurement_temperature    100(2)
_cell_volume                     6805.62(10)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            96053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.425
_diffrn_reflns_theta_min         2.666
_exptl_absorpt_coefficient_mu    1.248
_exptl_crystal_density_diffrn    1.016
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.838
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 5369 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.522(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1004
_refine_ls_number_reflns         14228
_refine_ls_number_restraints     502
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.756
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1345P)^2^+3.7897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2222
_refine_ls_wR_factor_ref         0.2305
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                12682
_reflns_number_total             14228
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04252a1.cif
_cod_data_source_block           sv16-n42_auto
_cod_depositor_comments          'Adding full bibliography for 7247882.cif.'
_cod_original_cell_volume        6805.62(11)
_cod_original_formula_sum        'C10 H3.50 Cl0.50 N6.50 O18'
_cod_database_code               7247882
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              47726