Definitive Structural Characterization of the Conventional Low-Temperature Host Structure in Urea Inclusion Compounds
Yeo, L.; Harris, K. D. M.; Acta Crystallographica Section B 53 (1997) 822–830; doi:10.1107/S0108768197005417

data_2101918
_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_paper_doi               10.1107/S0108768197005417
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C1 H4 N2 O1 , 0.09C12 H24 Br2'
_chemical_formula_sum            'C2.08 H6.16 Br0.18 N2 O'
_chemical_formula_weight         84
_chemical_name_systematic
;
 1,12-dibromododecane/urea inclusion
;
_space_group_IT_number           178
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 61 2 (0 0 5)'
_symmetry_space_group_name_H-M   'P 61 2 2'
_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                   8.2201(13)
_cell_length_b                   8.2201(13)
_cell_length_c                   11.0342(12)
_cell_measurement_reflns_used
' 3714 (post-refined using complete data set).'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.64
_cell_measurement_theta_min      2.5
_cell_volume                     645.69(16)
_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  0.0840
_diffrn_reflns_av_sigmaI/netI    0.0324
_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       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3714
_diffrn_reflns_theta_max         25.32
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    1.09
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_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         -0.200
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   4.(10)
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.220
_refine_ls_goodness_of_fit_obs   1.219
_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         395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_restrained_S_obs      1.219
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_obs          0.1099
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+1.0780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3018
_refine_ls_wR_factor_obs         0.2987
_reflns_number_observed          387
_reflns_number_total             395
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ha0155.cif
_cod_data_source_block           DB12rt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+1.0780P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+1.0780P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        645.7(2)
_cod_original_sg_symbol_H-M      'P 61 22'
_cod_original_formula_sum        'C2.08 H6.16 Br0.18 N2 O1'
_cod_database_code               2101918