#------------------------------------------------------------------------------ #$Date: 2011-06-21 23:57:19 +0300 (Tue, 21 Jun 2011) $ #$Revision: 21238 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7052604.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_7052604 loop_ _publ_author_name 'Li, Xian-Mei' 'Fan, Fan' 'Lu, Jing-Song' 'Xue, Sai-Feng' 'Zhang, Yun-Qian' 'Zhu, Qian-Jiang' 'Tao, Zhu' 'Lawrance, Geofferey A.' 'Wei, Gang' _publ_section_title ; Host--guest complexes of cucurbit[8]uril with some pentaerythritol derivative guests ; _journal_issue 5 _journal_name_full 'New Journal of Chemistry' _journal_page_first 1088 _journal_volume 35 _journal_year 2011 _chemical_formula_sum 'C15 H23 Br2 N2 O3.5' _chemical_formula_weight 447.17 _chemical_name_systematic ; ? ; _space_group_IT_number 60 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c 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 4 _cell_length_a 9.339(8) _cell_length_b 15.689(14) _cell_length_c 12.461(11) _cell_measurement_temperature 293(2) _cell_volume 1826(3) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker CCD Area Detector' _diffrn_measurement_method '\f and \w scan' _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 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10715 _diffrn_reflns_theta_full 25.08 _diffrn_reflns_theta_max 25.08 _diffrn_reflns_theta_min 2.54 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.456 _exptl_absorpt_correction_T_max 0.4546 _exptl_absorpt_correction_T_min 0.3791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2005)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.627 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 900 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.427 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 97 _refine_ls_number_reflns 1620 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.045 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0327 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.1568P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.0820 _reflns_number_gt 1128 _reflns_number_total 1620 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0nj00752h.txt _[local]_cod_data_source_block t _[local]_cod_chemical_formula_sum_orig 'C15 H23 Br2 N2 O3.50' _cod_database_code 7052604 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-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 C1 C 0.6769(5) 0.3407(2) 0.1333(3) 0.0629(11) Uani 1 1 d . . . H1 H 0.6497 0.3265 0.2028 0.075 Uiso 1 1 calc R . . C2 C 0.5788(5) 0.3737(3) 0.0639(4) 0.0729(11) Uani 1 1 d . . . H2 H 0.4845 0.3813 0.0858 0.087 Uiso 1 1 calc R . . C3 C 0.6186(5) 0.3953(2) -0.0371(4) 0.0717(12) Uani 1 1 d . . . H3 H 0.5521 0.4180 -0.0847 0.086 Uiso 1 1 calc R . . C4 C 0.7571(5) 0.3835(3) -0.0680(3) 0.0708(12) Uani 1 1 d . . . H4 H 0.7859 0.3989 -0.1368 0.085 Uiso 1 1 calc R . . C5 C 0.8548(4) 0.3488(2) 0.0025(3) 0.0577(10) Uani 1 1 d . . . H5 H 0.9489 0.3396 -0.0189 0.069 Uiso 1 1 calc R . . C6 C 0.9159(4) 0.28738(19) 0.1770(3) 0.0564(9) Uani 1 1 d . . . H6A H 0.9841 0.2542 0.1357 0.068 Uiso 1 1 calc R . . H6B H 0.8632 0.2481 0.2223 0.068 Uiso 1 1 calc R . . C7 C 1.0000 0.3501(2) 0.2500 0.0392(11) Uani 1 2 d S . . C8 C 0.8999(4) 0.40599(18) 0.3153(3) 0.0509(9) Uani 1 1 d . . . H8A H 0.9548 0.4392 0.3665 0.061 Uiso 1 1 calc R . . H8B H 0.8498 0.4451 0.2682 0.061 Uiso 1 1 calc R . . N6 N 0.8135(3) 0.32859(16) 0.1014(2) 0.0465(7) Uani 1 1 d . . . O1 O 0.7992(3) 0.3540(2) 0.3707(2) 0.0849(10) Uani 1 1 d . . . H1A H 0.7914 0.3707 0.4328 0.127 Uiso 1 1 calc R . . Br1 Br 0.77440(4) 0.41267(2) 0.61588(3) 0.06039(19) Uani 1 1 d . . . 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 C1 0.053(3) 0.075(3) 0.060(2) -0.0058(19) 0.002(2) -0.019(2) C2 0.045(3) 0.088(3) 0.086(3) -0.025(3) -0.011(2) -0.007(2) C3 0.070(3) 0.064(3) 0.081(3) -0.014(2) -0.030(3) -0.001(2) C4 0.095(4) 0.072(3) 0.045(2) 0.001(2) -0.012(2) -0.020(2) C5 0.059(3) 0.065(2) 0.049(2) -0.0080(17) 0.0020(19) -0.0088(18) C6 0.068(3) 0.046(2) 0.055(2) -0.0012(17) -0.0105(19) -0.0002(17) C7 0.047(3) 0.030(2) 0.040(2) 0.000 -0.004(2) 0.000 C8 0.049(2) 0.057(2) 0.0465(19) -0.0046(17) -0.0004(16) -0.0001(18) N6 0.050(2) 0.0438(16) 0.0454(16) -0.0071(12) -0.0049(14) -0.0048(13) O1 0.071(2) 0.124(3) 0.0599(18) -0.0176(16) 0.0153(15) -0.0336(18) Br1 0.0652(3) 0.0645(3) 0.0515(2) 0.00485(17) -0.00525(18) -0.00752(19) 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' N N 0.0061 0.0033 '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' Br Br -0.2901 2.4595 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 C1 C2 120.2(4) . . ? C3 C2 C1 120.0(4) . . ? C2 C3 C4 119.3(4) . . ? C3 C4 C5 120.1(4) . . ? N6 C5 C4 119.6(4) . . ? N6 C6 C7 114.8(2) . . ? C8 C7 C8 109.4(3) . 4_755 ? C8 C7 C6 111.6(2) . . ? C8 C7 C6 111.29(19) 4_755 . ? C8 C7 C6 111.29(19) . 4_755 ? C8 C7 C6 111.6(2) 4_755 4_755 ? C6 C7 C6 101.4(3) . 4_755 ? O1 C8 C7 109.6(3) . . ? C5 N6 C1 120.8(3) . . ? C5 N6 C6 120.3(3) . . ? C1 N6 C6 118.8(3) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N6 1.350(6) . ? C1 C2 1.361(5) . ? C2 C3 1.355(6) . ? C3 C4 1.363(6) . ? C4 C5 1.378(5) . ? C5 N6 1.329(4) . ? C6 N6 1.489(4) . ? C6 C7 1.553(4) . ? C7 C8 1.518(4) . ? C7 C8 1.518(4) 4_755 ? C7 C6 1.553(4) 4_755 ? C8 O1 1.423(4) . ?