#------------------------------------------------------------------------------
#$Date: 2008-04-03 11:11:48 +0100 (Thu, 03 Apr 2008) $
#$Revision: 326 $
#$URL: svn://www.crystallography.net/cod/cif/2/2101917.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_2101917
loop_
_publ_author_name
'Yeo, L.'
'Harris, K. D. M.'
_publ_section_title
;
 Definitive Structural Characterization of the Conventional
 Low-Temperature Host Structure in Urea Inclusion Compounds
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              822
_journal_page_last               830
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C1 H4 N2 O1 , 0.07C10 H22 Br2'
_chemical_formula_sum            'C1.7 H5.54 Br0.14 N2 O1'
_chemical_formula_weight         88
_chemical_name_systematic
;
 1,10-dibromodecane/urea inclusion
;
_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   'P 61 22'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   8.271(3)
_cell_length_b                   8.271(3)
_cell_length_c                   11.083(3)
_cell_measurement_reflns_used
' 3351 (post-refined using complete data set).'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.21
_cell_measurement_theta_min      2.5
_cell_volume                     656.7(4)
_computing_cell_refinement       'R-Axis II software (Rigaku, 1994)'
_computing_data_collection       'R-Axis II software (Rigaku, 1994)'
_computing_data_reduction
' TeXsan (Molecular Structure Corporation,1993)'
_computing_molecular_graphics    'Biosym, InsightII'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution
' TeXsan (Molecular Structure Corporation,1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku R-Axis II area detector'
_diffrn_measurement_method       'image plate scanning'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3351
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.90
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       'Hexagonal needle'
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.159
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   8.(10)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.230
_refine_ls_goodness_of_fit_obs   1.240
_refine_ls_hydrogen_treatment
;
 hydrogen atoms were added to the urea molecules according to standard
 geometry and refined using a "riding" model.  The Uiso of each hydrogen
 was refined as 1.2 times the equivalent isotropic atomic displacement
 of the nitrogen atom to which it is attached.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_restrained_S_obs      1.240
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_obs          0.1133
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+1.4180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all         0.2915
_refine_ls_wR_factor_obs         0.2903
_reflns_number_observed          384
_reflns_number_total             393
_reflns_observed_criterion       >2sigma(I)
_[local]_cod_data_source_file    ha0155.cif
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'-x, -y, z+1/2'
'y, -x+y, z+5/6'
'x-y, x, z+1/6'
'y, x, -z+1/3'
'-x, -x+y, -z+2/3'
'x-y, -y, -z'
'-y, -x, -z+5/6'
'x, x-y, -z+1/6'
'-x+y, y, -z+1/2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
O1 0.6406(7) 0.3203(4) 0.0833 0.039(2) Uani d S 1 O
N1 0.9125(7) 0.4344(7) 0.1862(4) 0.045(2) Uani d . 1 N
H1A 0.8531(7) 0.3905(7) 0.2528(4) 0.054 Uiso calc R 1 H
H1B 1.0326(7) 0.4945(7) 0.1858(4) 0.054 Uiso calc R 1 H
C1 0.8183(11) 0.4092(6) 0.0833 0.035(2) Uani d S 1 C
C2 0.951(4) 0.0000 0.0000 0.183(10) Uiso d S 1 C
C3 1.009(6) 0.005(3) 0.0833 0.231(14) Uiso d S 1 C
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
O1 0.036(3) 0.048(3) 0.029(3) 0.018(2) 0.000 0.000(2)
N1 0.032(3) 0.062(4) 0.030(2) 0.015(3) -0.002(2) 0.003(2)
C1 0.043(4) 0.033(3) 0.032(4) 0.022(2) 0.000 -0.005(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 . 1.273(10) y
N1 C1 . 1.337(6) y
C1 N1 11 1.337(6) ?
C2 C3 . 1.03(2) ?
C2 C3 5_664 1.03(2) ?
C2 C2 6_545 1.891(6) ?
C2 C2 5_664 1.891(6) ?
C3 C2 6_545 1.03(2) ?
C3 C3 5_664 1.848(2) ?
C3 C3 6_545 1.848(2) ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 C1 N1 . 11 120.3(4) y
O1 C1 N1 . . 120.3(4) ?
N1 C1 N1 11 . 119.4(7) y
C3 C2 C3 . 5_664 127.(5) ?
C3 C2 C2 . 6_545 24.(3) ?
C3 C2 C2 5_664 6_545 145.(3) ?
C3 C2 C2 . 5_664 145.(3) ?
C3 C2 C2 5_664 5_664 24.(3) ?
C2 C2 C2 6_545 5_664 167.7(9) ?
C2 C3 C2 . 6_545 132.(5) ?
C2 C3 C3 . 5_664 27.(3) ?
C2 C3 C3 6_545 5_664 152.(4) ?
C2 C3 C3 . 6_545 152.(4) ?
C2 C3 C3 6_545 6_545 27.(3) ?
C3 C3 C3 5_664 6_545 177.9(13) ?