#------------------------------------------------------------------------------
#$Date: 2023-03-26 10:09:57 +0200 (Sun 26 de Mar de 2023) $
#$Revision: 282068 $
#$URL: svn://www.crystallography.net/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_compound_source        Synthetic
_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_mineral           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)'
_database_code_amcsd             0019155
_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/[σ²(Fo²)+(0.0367P)²+0.1641P] where P=(Fo²+2Fc²)/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_
_space_group_symop_operation_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)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0019155
