#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/50/1505080.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_1505080
loop_
_publ_author_name
'Udachin, Konstantin A.'
'Ratcliffe, Christopher I.'
'Ripmeester, John A.'
_publ_section_title
;
 Structure, dynamics and ordering in structure i ether clathrate hydrates
 from single-crystal X-ray diffraction and 2H NMR spectroscopy.
;
_journal_issue                   39
_journal_name_full               'The journal of physical chemistry. B'
_journal_page_first              11366
_journal_page_last               11372
_journal_paper_doi               10.1021/jp071342v
_journal_volume                  111
_journal_year                    2007
_chemical_formula_sum            'C3 H21.33 O8.67'
_chemical_formula_weight         196.20
_chemical_name_common            'Trimethylene oxide hydrate'
_chemical_name_systematic
; 
 ? 
;
_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            6
_cell_length_a                   12.069(3)
_cell_length_b                   12.069(3)
_cell_length_c                   12.069(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1758.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0045
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18936
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9564
_exptl_absorpt_correction_T_min  0.9511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.061
_refine_diff_density_min         -0.058
_refine_diff_density_rms         0.012
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         441
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.350
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0138
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0211P)²+0.0173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0386
_reflns_number_gt                382
_reflns_number_total             441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp071342vsi20070215_051250.cif
_cod_data_source_block           ku138
_cod_original_cell_volume        1757.8(7)
_cod_original_sg_symbol_H-M      Pm-3n
_cod_database_code               1505080
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
O1A O 0.5167(3) 0.1396(2) -0.0103(4) 0.0135(12) Uani 0.04 1 d PDU A -1
C1A C 0.4562(5) 0.2165(4) -0.0796(5) 0.043(3) Uani 0.04 1 d PDU A -1
H1A1 H 0.3747 0.2106 -0.0723 0.052 Uiso 0.04 1 calc PR A -1
H1A2 H 0.4789 0.2150 -0.1584 0.052 Uiso 0.04 1 calc PR A -1
C2A C 0.5064(6) 0.3113(3) -0.0141(5) 0.0195(17) Uani 0.04 1 d PDU A -1
H2A1 H 0.5557 0.3598 -0.0583 0.023 Uiso 0.04 1 calc PR A -1
H2A2 H 0.4515 0.3554 0.0279 0.023 Uiso 0.04 1 calc PR A -1
C3A C 0.5675(6) 0.2267(4) 0.0554(5) 0.031(3) Uani 0.04 1 d PDU A -1
H3A1 H 0.6491 0.2305 0.0480 0.037 Uiso 0.04 1 calc PR A -1
H3A2 H 0.5450 0.2262 0.1343 0.037 Uiso 0.04 1 calc PR A -1
C2B C 0.5095(5) 0.1838(3) -0.0438(4) 0.0608(17) Uani 0.09 1 d PDU B -2
H2B1 H 0.5084 0.1103 -0.0075 0.073 Uiso 0.09 1 calc PR B -2
H2B2 H 0.5272 0.1770 -0.1236 0.073 Uiso 0.09 1 calc PR B -2
C1B C 0.4074(4) 0.2534(4) -0.0204(5) 0.056(2) Uani 0.09 1 d PDU B -2
H1B1 H 0.3715 0.2837 -0.0876 0.067 Uiso 0.09 1 calc PR B -2
H1B2 H 0.3527 0.2169 0.0287 0.067 Uiso 0.09 1 calc PR B -2
O1B O 0.4791(4) 0.3309(4) 0.0358(4) 0.130(3) Uani 0.09 1 d PDU B -2
C3B C 0.5795(4) 0.2689(4) 0.0164(5) 0.042(2) Uani 0.09 1 d PDU B -2
H3B1 H 0.6150 0.2406 0.0848 0.050 Uiso 0.09 1 calc PR B -2
H3B2 H 0.6339 0.3074 -0.0315 0.050 Uiso 0.09 1 calc PR B -2
O1 O 0.61826(3) 0.5000 0.19495(3) 0.03650(9) Uani 1 2 d SD . .
O2 O 0.18367(2) 0.18367(2) 0.18367(2) 0.03662(10) Uani 1 3 d S . .
O3 O 0.5000 0.0000 0.2500 0.03704(16) Uani 1 8 d S . .
H1 H 0.2203(6) 0.2203(6) 0.2203(6) 0.053(5) Uiso 0.50 3 d SP . .
H2 H 0.2172(6) 0.1296(7) 0.1620(7) 0.046(2) Uiso 0.50 1 d P . .
H3 H 0.4482(11) 0.5000 0.1853(9) 0.054(4) Uiso 0.50 2 d SP . .
H4 H 0.3651(6) 0.5533(6) 0.2291(7) 0.040(2) Uiso 0.50 1 d P . .
H5 H 0.3500(11) 0.5000 0.1402(11) 0.044(3) Uiso 0.50 2 d SP . .
H6 H 0.4473(9) 0.0000 0.2107(10) 0.050(4) Uiso 0.50 2 d SP . .
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
O1A 0.012(3) 0.0155(13) 0.014(2) 0.0037(19) 0.007(3) 0.0079(14)
C1A 0.053(5) 0.041(5) 0.037(5) 0.005(4) -0.005(4) -0.027(4)
C2A 0.026(3) 0.018(2) 0.014(4) 0.002(2) -0.002(4) -0.002(4)
C3A 0.031(4) 0.024(6) 0.038(5) 0.011(4) -0.004(4) -0.009(4)
C2B 0.048(3) 0.079(3) 0.056(3) -0.045(3) 0.004(5) -0.005(5)
C1B 0.042(2) 0.053(3) 0.074(6) -0.008(4) -0.010(3) -0.001(2)
O1B 0.102(6) 0.156(4) 0.134(6) -0.067(4) 0.014(5) 0.049(5)
C3B 0.036(2) 0.043(2) 0.046(5) -0.031(3) -0.012(3) 0.016(2)
O1 0.03723(18) 0.03620(17) 0.03606(18) 0.000 -0.00105(14) 0.000
O2 0.03662(10) 0.03662(10) 0.03662(10) 0.00093(10) 0.00093(10) 0.00093(10)
O3 0.0361(2) 0.0361(2) 0.0389(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
C1A O1A C3A 93.7(3)
O1A C1A C2A 88.9(3)
C3A C2A C1A 88.5(3)
O1A C3A C2A 88.9(3)
C3B C2B C1B 89.4(3)
O1B C1B C2B 87.7(3)
C3B O1B C1B 95.2(3)
O1B C3B C2B 87.7(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1A C1A 1.448(5)
O1A C3A 1.452(5)
C1A C2A 1.517(5)
C2A C3A 1.513(5)
C2B C3B 1.516(5)
C2B C1B 1.517(5)
C1B O1B 1.444(5)
O1B C3B 1.443(5)
