Gas Hydrate Single-Crystal Structure Analyses
Michael T. Kirchner; Roland Boese; W. Edward Billups; Lewis R. Norman; Journal of the American Chemical Society 126 (2004) 9407–9412; doi:10.1021/ja049247c

data_4112808
_publ_section_title
;
 Gas Hydrate Single-Crystal Structure Analyses
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9407
_journal_page_last               9412
_journal_paper_doi               10.1021/ja049247c
_journal_volume                  126
_journal_year                    2004
_chemical_formula_moiety         '8(C3 H8) 14.9(C H4) 136(H2 O)'
_chemical_formula_sum            'C38.9 H395.6 O136'
_chemical_formula_weight         3059.60
_chemical_name_systematic
; 
  clathrate hydrate of propane, methane and ethanole
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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            1
_cell_length_a                   17.1925(10)
_cell_length_b                   17.1925(10)
_cell_length_c                   17.1925(10)
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.886
_cell_measurement_theta_min      3.351
_cell_volume                     5081.8(5)
_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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  '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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5236
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       cylindric
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.3
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.116
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         343
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+2.2093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                308
_reflns_number_total             343
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049247csi20040211_052141.cif
_cod_data_source_block           wk8xmk21
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_database_code               4112808