Characterization of tetra-n-butylphosphonium bromide semiclathrate hydrate by crystal structure analysis
Muromachi, Sanehiro; Takeya, Satoshi; Yamamoto, Yoshitaka; Ohmura, Ryo; CrystEngComm 16 (2014) 2056–; doi:10.1039/c3ce41942h

data_7213696
_publ_section_title
;
 Characterization of tetra-n-butylphosphonium bromide semiclathrate
 hydrate by crystal structure analysis
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              2056
_journal_paper_doi               10.1039/c3ce41942h
_journal_volume                  16
_journal_year                    2014
_chemical_formula_iupac          'C16 H36 P + , Br - , 38H2 O'
_chemical_formula_moiety         'C16 H36 P + , Br - , 38H2 O'
_chemical_formula_sum            'C16 H112 Br O38 P'
_chemical_formula_weight         1023.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           51
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2a'
_symmetry_space_group_name_H-M   'P m m a'
_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            2
_cell_length_a                   21.065(5)
_cell_length_b                   12.657(3)
_cell_length_c                   11.992(3)
_cell_measurement_temperature    100(3)
_cell_volume                     3197.3(13)
_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      100(3)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16672
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.8076
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.351
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3912
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.119
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+5.6858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1858
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                3457
_reflns_number_total             3912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41942h.txt
_cod_data_source_block           st05
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3197.3(14)
_cod_original_sg_symbol_H-M      'P m m a '
_cod_database_code               7213696