#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/19/2101917.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # 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 O' _chemical_formula_weight 88 _chemical_name_systematic ; 1,10-dibromodecane/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 8.271(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 656.6(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 _[local]_cod_data_source_block DB10rt _[local]_cod_cif_authors_sg_H-M 'P 61 22' _[local]_cod_chemical_formula_sum_orig 'C1.7 H5.54 Br0.14 N2 O1' _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 ; _cod_original_cell_volume 656.7(4) _cod_database_code 2101917 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_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_ _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_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_ _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) ? 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) ? _journal_paper_doi 10.1107/S0108768197005417