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_4112810
_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         '1.2(C2 H2), 6(C2 H2), 46(H2 O)'
_chemical_formula_sum            'C14.2 H60.2 O46'
_chemical_formula_weight         1037.02
_chemical_name_common            'Ethine hydrate'
_chemical_name_systematic
; 
 clathrate hydrate of ethine
;
_space_group_IT_number           223
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4n 2 3'
_symmetry_space_group_name_H-M   'P m -3 n'
_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                   11.895(3)
_cell_length_b                   11.895(3)
_cell_length_c                   11.895(3)
_cell_measurement_reflns_used    978
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      26.941
_cell_measurement_theta_min      3.425
_cell_volume                     1683.0(7)
_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      143(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0224
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       1
_diffrn_reflns_number            406
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_meas      0
_exptl_crystal_description       oligocrystaline
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.00
_exptl_crystal_size_min          0.00
_refine_diff_density_max         0.214
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.269
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         406
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0420P)^2^+1.0524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                248
_reflns_number_total             406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049247csi20040211_052401.cif
_cod_data_source_block           eiwxmk5m
_cod_original_cell_volume        1683.0(8)
_cod_database_code               4112810