#------------------------------------------------------------------------------ #$Date: 2016-03-22 11:26:18 +0200 (Tue, 22 Mar 2016) $ #$Revision: 178899 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/11/28/4112810.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_4112810 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 '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 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 0.30797(18) 0.11699(17) 0.0358(6) Uani 1 2 d S . . H1 H 0.0000 0.322(5) 0.043(5) 0.054 Uiso 0.50 2 d SP . . H2 H 0.056(4) 0.274(4) 0.146(4) 0.054 Uiso 0.50 1 d P . . H3 H 0.0000 0.367(7) 0.154(6) 0.054 Uiso 0.50 2 d SP . . O2 O 0.18388(11) 0.18388(11) 0.18388(11) 0.0359(7) Uani 1 3 d S . . H4 H 0.223(3) 0.223(3) 0.223(3) 0.054 Uiso 0.50 3 d SP . . H5 H 0.160(4) 0.126(4) 0.220(4) 0.054 Uiso 0.50 1 d P . . O3 O 0.0000 0.5000 0.2500 0.0364(10) Uani 1 8 d S . . H6 H 0.0000 0.441(5) 0.201(6) 0.055 Uiso 0.50 2 d SP . . X1 H 0.0000 0.0000 0.0000 0.050 Uiso 0.00 24 dum SPD A 1 C1 C 0.0000 0.0000 0.0521(17) 0.050 Uiso 0.08(3) 4 d SPD . 2 C2 C 0.0000 0.0335(11) 0.0400(13) 0.050 Uiso 0.059(15) 2 d SPD . 3 X2 H 0.2500 0.5000 0.0000 0.050 Uiso 0.00 8 dum SPD B 1 C3 C 0.259(2) 0.4512(11) 0.0000 0.096(12) Uani 0.42(5) 2 d SPD . 4 C4 C 0.2982(9) 0.5000 0.0000 0.23(5) Uani 0.30(10) 4 d SPD . 5 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 0.0355(11) 0.0359(12) 0.0359(11) -0.0001(9) 0.000 0.000 O2 0.0359(7) 0.0359(7) 0.0359(7) 0.0001(6) 0.0001(6) 0.0001(6) O3 0.0367(14) 0.0367(14) 0.036(2) 0.000 0.000 0.000 C3 0.07(2) 0.093(11) 0.129(13) 0.000 0.000 0.041(11) C4 0.05(3) 0.42(13) 0.21(8) 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 119(4) H1 O1 H3 111(6) H2 O1 H3 101(4) H4 O2 H5 111(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O1 H1 0.90(6) . O1 H2 0.85(5) . O1 H3 0.83(8) . O2 H4 0.81(6) . O2 H5 0.86(4) . O3 H6 0.92(6) . C1 C1 1.24(4) 25