#------------------------------------------------------------------------------ #$Date: 2016-03-22 11:26:18 +0200 (Tue, 22 Mar 2016) $ #$Revision: 178899 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/28/4112809.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4112809 loop_ _publ_author_name 'Michael T. Kirchner' 'Roland Boese' 'W. Edward Billups' 'Lewis R. Norman' _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(C H4), 46(H2 O)' _chemical_formula_sum 'C8 H124 O46' _chemical_formula_weight 957.07 _chemical_name_common 'Methane hydrate' _chemical_name_systematic ; clathrate hydrate of methane ; _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 11.877(3) _cell_length_b 11.877(3) _cell_length_c 11.877(3) _cell_measurement_temperature 123(2) _cell_volume 1675.4(7) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 123(2) _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _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 0.0743 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5581 _diffrn_reflns_theta_full 28.23 _diffrn_reflns_theta_max 28.23 _diffrn_reflns_theta_min 3.84 _exptl_absorpt_coefficient_mu 0.099 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.885 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Bruker AXS SADABS program multiscan V2.03' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 0.948 _exptl_crystal_F_000 540 _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 -0.148 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 30 _refine_ls_number_reflns 399 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0379 _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^)+(0.0367P)^2^+0.1641P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.0887 _reflns_number_gt 268 _reflns_number_total 399 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ja049247csi20040211_052221.cif _cod_data_source_block xdablt2a _cod_original_cell_volume 1675.6(8) _cod_database_code 4112809 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y-1/2, -x-1/2, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y-1/2, x-1/2, -z-1/2' 'y-1/2, -x-1/2, -z-1/2' '-x-1/2, -z-1/2, y-1/2' 'x-1/2, -z-1/2, -y-1/2' 'x-1/2, z-1/2, y-1/2' '-x-1/2, z-1/2, -y-1/2' '-z-1/2, -y-1/2, x-1/2' '-z-1/2, y-1/2, -x-1/2' 'z-1/2, -y-1/2, -x-1/2' 'z-1/2, y-1/2, x-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0000 0.30860(12) 0.11683(11) 0.0291(4) Uani 1 2 d S . . H1 H 0.0000 0.325(3) 0.051(3) 0.044 Uiso 0.50 2 d SP . . H2 H 0.051(3) 0.271(3) 0.134(3) 0.044 Uiso 0.50 1 d P . . H3 H 0.0000 0.360(4) 0.150(4) 0.044 Uiso 0.50 2 d SP . . O2 O 0.18345(7) 0.18345(7) 0.18345(7) 0.0286(4) Uani 1 3 d S . . H4 H 0.216(2) 0.216(2) 0.216(2) 0.043 Uiso 0.50 3 d SP . . H5 H 0.162(2) 0.128(2) 0.220(2) 0.043 Uiso 0.50 1 d P . . O3 O 0.0000 0.5000 0.2500 0.0292(6) Uani 1 8 d S . . H6 H 0.0000 0.447(3) 0.211(4) 0.044 Uiso 0.50 2 d SP . . C1 C 0.0000 0.0000 0.0000 0.0518(18) Uani 1 24 d S . . H7 H 0.0000 0.049(6) 0.086(5) 0.078 Uiso 0.33 2 d SP . . C2 C 0.2500 0.5000 0.0000 0.113(3) Uani 1 8 d S . . H8 H 0.2986 0.5000 0.0687 0.170 Uiso 0.50 2 d SP A 1 H9 H 0.2014 0.5000 0.0687 0.170 Uiso 0.50 2 d SP B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0304(7) 0.0287(7) 0.0281(7) -0.0004(5) 0.000 0.000 O2 0.0286(4) 0.0286(4) 0.0286(4) -0.0011(3) -0.0011(3) -0.0011(3) O3 0.0274(9) 0.0274(9) 0.0328(15) 0.000 0.000 0.000 C1 0.0518(18) 0.0518(18) 0.0518(18) 0.000 0.000 0.000 C2 0.080(5) 0.130(4) 0.130(4) 0.000 0.000 0.000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle H1 O1 H2 113(3) H1 O1 H3 109(4) H2 O1 H3 110(3) H4 O2 H5 109(2) H8 C2 H9 70.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 H1 0.81(4) O1 H2 0.78(3) O1 H3 0.73(5) O2 H4 0.67(5) O2 H5 0.82(3) O3 H6 0.78(4) C1 H7 1.18(5) C2 H8 1.0000(3) C2 H9 1.0000(3)