The structure of the ionic clathrate hydrate of tetrabutylammonium valerate (C4H9)4NC4H9CO2·39.8H2O
Rodionova, Tatyana; Komarov, Vladislav; Lipkowski, Janusz; Kuratieva, Natalia; New Journal of Chemistry 34 (2010) 432–; doi:10.1039/b9nj00530g

data_7053355
_publ_section_title
;
 The structure of the ionic clathrate hydrate of tetrabutylammonium
 valerate (C4H9)4NC4H9CO2&#x00B7;39.8H2O
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              432
_journal_paper_doi               10.1039/b9nj00530g
_journal_volume                  34
_journal_year                    2010
_chemical_formula_moiety         '(C16 H36 N 1+), (C5 H9 O2 1-), 39.8(H2 O)'
_chemical_formula_sum            'C21 H124.6 N O41.8'
_chemical_formula_weight         1060.87
_chemical_melting_point          284.4
_chemical_name_common
'tetra-n-butylammonium valerate clathrate hydrate'
_chemical_name_systematic
;
tetra-n-butylammonium valerate clathrate hydrate
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n 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            4
_cell_length_a                   23.322(1)
_cell_length_b                   23.322(1)
_cell_length_c                   12.278(1)
_cell_measurement_reflns_used    8825
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.47
_cell_volume                     6678.2(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0085
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22268
_diffrn_reflns_theta_full        19.98
_diffrn_reflns_theta_max         19.98
_diffrn_reflns_theta_min         2.76
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.9052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'tetragonal prism'
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.7
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1723
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0672
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1369P)^2^+7.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2074
_reflns_number_gt                1575
_reflns_number_total             1723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b9nj00530g.txt
_cod_data_source_block           compound1
_cod_database_code               7053355