Calorimetric and structural studies of tetrabutylammonium chloride ionic clathrate hydrates.
Rodionova, T.; Komarov, V.; Villevald, G.; Aladko, L.; Karpova, T.; Manakov, A.; The journal of physical chemistry. B 114 (2010) 11838–11846; doi:10.1021/jp103939q

data_1502709
_publ_section_title
;
 Calorimetric and structural studies of tetrabutylammonium chloride ionic
 clathrate hydrates.
;
_journal_issue                   36
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              11838
_journal_page_last               11846
_journal_paper_doi               10.1021/jp103939q
_journal_volume                  114
_journal_year                    2010
_chemical_formula_moiety         '(C16 H36 N 1+), (Cl-),  30(H2 O)'
_chemical_formula_sum            'C16 H96 Cl N O30'
_chemical_formula_weight         818.4
_chemical_melting_point          288.3
_chemical_name_common
;
 tetrabutylammonium chloride TS I clathrate hydrate 
;
_chemical_name_systematic
; 
 tetrabutylammonium chloride clathrate hydrate  
;
_space_group_IT_number           84
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c'
_symmetry_space_group_name_H-M   'P 42/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            5
_cell_length_a                   23.5211(7)
_cell_length_b                   23.5211(7)
_cell_length_c                   12.4880(6)
_cell_measurement_reflns_used    62834
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.60
_cell_measurement_theta_min      0.87
_cell_volume                     6908.9(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo and Scalepack(Otwinowski&Minor, 1997)'
_computing_molecular_graphics    'local program'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            35128
_diffrn_reflns_theta_full        23.81
_diffrn_reflns_theta_max         23.81
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             2185
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5586
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      2.046
_refine_ls_R_factor_all          0.1602
_refine_ls_R_factor_gt           0.1392
_refine_ls_shift/su_max          0.929
_refine_ls_shift/su_mean         0.045
_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          0.4385
_refine_ls_wR_factor_ref         0.4687
_reflns_number_gt                4289
_reflns_number_total             5586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp103939q_si_001.cif
_cod_data_source_block           s3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               1502709