Calorimetric and structural studies of tetrabutylammonium bromide ionic clathrate hydrates.
Rodionova, Tatyana V.; Komarov, Vladislav Yu; Villevald, Galina V.; Karpova, Tamara D.; Kuratieva, Natalia V.; Manakov, Andrey Yu; The journal of physical chemistry. B 117 (2013) 10677–10685; doi:10.1021/jp406082z

data_1512260
_publ_section_title
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 Calorimetric and structural studies of tetrabutylammonium bromide ionic
 clathrate hydrates.
;
_journal_issue                   36
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              10677
_journal_page_last               10685
_journal_paper_doi               10.1021/jp406082z
_journal_volume                  117
_journal_year                    2013
_chemical_formula_moiety         '(C16 H36 N 1+), (Br 1-) 24(H2 O)'
_chemical_formula_sum            'C16 H84 Br N O24'
_chemical_formula_weight         754.75
_chemical_melting_point          ?
_chemical_name_common            'h24 TBAB clathrate hydrate'
_chemical_name_systematic
; 
 tetra-n-butylammonium bromide clathrate hydrate 
;
_space_group_IT_number           81
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   23.492(3)
_cell_length_b                   23.492(3)
_cell_length_c                   38.021(8)
_cell_measurement_reflns_used    104787
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.66
_cell_volume                     20983(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1113
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            89024
_diffrn_reflns_theta_full        23.67
_diffrn_reflns_theta_max         23.67
_diffrn_reflns_theta_min         2.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.7033
_exptl_absorpt_correction_T_min  0.7033
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         8.657
_refine_diff_density_min         -2.108
_refine_diff_density_rms         0.420
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.49(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.830
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         16067
_refine_ls_number_restraints     170
_refine_ls_restrained_S_all      1.827
_refine_ls_R_factor_all          0.2679
_refine_ls_R_factor_gt           0.1987
_refine_ls_shift/su_max          0.808
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4307
_refine_ls_wR_factor_ref         0.4984
_reflns_number_gt                10024
_reflns_number_total             16067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp406082z_si_002.cif
_cod_data_source_block           cx3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
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_cod_database_code               1512260