Phase Behavior and Structural Characterization of Ionic Clathrate Hydrate Formed with Tetra-n-butylphosphonium Hydroxide: Discovery of Primitive Crystal Structure
Kobori, Takayuki; Muromachi, Sanehiro; Yamasaki, Tatsuro; Takeya, Satoshi; Yamamoto, Yoshitaka; Alavi, Saman; Ohmura, Ryo; Crystal Growth & Design 15 (2015) 3862–; doi:10.1021/acs.cgd.5b00484

data_4513371
_publ_section_title
;
 Phase Behavior and Structural Characterization of Ionic Clathrate Hydrate
 Formed with Tetra-n-butylphosphonium Hydroxide: Discovery of Primitive
 Crystal Structure
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3862
_journal_paper_doi               10.1021/acs.cgd.5b00484
_journal_volume                  15
_journal_year                    2015
_chemical_formula_iupac          'C16 H36 P + , OH - ,29.6H2 O'
_chemical_formula_moiety         'C16 H36 P + , OH - ,29.6H2 O'
_chemical_formula_sum            'C16 H96.2 O30.6 P'
_chemical_formula_weight         809.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           220
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I -4bd 2c 3'
_symmetry_space_group_name_H-M   'I -4 3 d'
_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            12
_cell_length_a                   24.5191(13)
_cell_length_b                   24.5191(13)
_cell_length_c                   24.5191(13)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.35
_cell_volume                     14740.5(14)
_computing_cell_refinement       'Bruker SAINT ver. 7.68A(Bruker AXS Inc.)'
_computing_data_collection       'Bruker APEX2 ver. 2009.9(Bruker AXS Inc.)'
_computing_data_reduction        'Bruker SAINT ver. 7.68A(Bruker AXS Inc.)'
_computing_publication_material  'Bruker SHEXLTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating unit'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33207
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.9614
_exptl_absorpt_correction_T_min  0.9614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4994
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0662
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1684P)^2^+1.5173P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                1918
_reflns_number_total             2175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00484_si_001.cif
_cod_data_source_block           sr01
_cod_depositor_comments          'Adding full bibliography for 4513371.cif.'
_cod_original_sg_symbol_H-M      I-43d
_cod_original_formula_sum        'C16 H96.2 O30.6 P1'
_cod_database_code               4513371