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_1512261
_publ_section_title
;
 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-) 26.4(H2 O)'
_chemical_formula_sum            'C16 H88.8 Br N O26.4'
_chemical_formula_weight         797.97
_chemical_melting_point          ?
_chemical_name_common            'h26 TBAB clathrate hydrate'
_chemical_name_systematic
; 
 tetra-n-butylammonium bromide clathrate hydrate 
;
_space_group_IT_number           66
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_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            64
_cell_length_a                   33.115(4)
_cell_length_b                   33.158(4)
_cell_length_c                   50.499(7)
_cell_measurement_reflns_used    153577
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.70
_cell_volume                     55449(12)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1043
_diffrn_reflns_av_sigmaI/netI    0.0717
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            138647
_diffrn_reflns_theta_full        24.11
_diffrn_reflns_theta_max         24.11
_diffrn_reflns_theta_min         2.20
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.390
_exptl_absorpt_correction_T_max  0.7685
_exptl_absorpt_correction_T_min  0.5433
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             55936
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         8.720
_refine_diff_density_min         -3.502
_refine_diff_density_rms         0.681
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   6.396
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         22258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      6.396
_refine_ls_R_factor_all          0.4876
_refine_ls_R_factor_gt           0.4569
_refine_ls_shift/su_max          0.274
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.7917
_refine_ls_wR_factor_ref         0.8051
_reflns_number_gt                16168
_reflns_number_total             22258
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp406082z_si_003.cif
_cod_data_source_block           cx4
_cod_depositor_comments
;
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_original_cell_volume        55450(13)
_cod_database_code               1512261