#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2221722.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_2221722 loop_ _publ_author_name 'Yang, Zhao' 'Wang, Zhi-Xiang' _publ_section_title ; Phenyl N-(4-fluorophenyl)carbamate ; _journal_coeditor_code HK2663 _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1036 _journal_volume 65 _journal_year 2009 _chemical_formula_iupac 'C13 H10 F N O2' _chemical_formula_moiety 'C13 H10 F N O2' _chemical_formula_sum 'C13 H10 F N O2' _chemical_formula_weight 231.22 _chemical_name_systematic ; Phenyl N-(4-fluorophenyl)carbamate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 96.62(3) _cell_angle_beta 92.82(3) _cell_angle_gamma 91.19(3) _cell_formula_units_Z 4 _cell_length_a 5.8860(12) _cell_length_b 7.8540(16) _cell_length_c 24.761(5) _cell_measurement_reflns_used 25 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 12 _cell_measurement_theta_min 8 _cell_volume 1135.3(4) _computing_cell_refinement 'CAD-4 Software (Enraf--Nonius, 1989)' _computing_data_collection 'CAD-4 Software (Enraf--Nonius, 1989)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Enraf--Nonius CAD-4' _diffrn_measurement_method \w/2\q _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 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 4548 _diffrn_reflns_theta_full 25.27 _diffrn_reflns_theta_max 25.27 _diffrn_reflns_theta_min 1.66 _diffrn_standards_decay_% 1 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_correction_T_min 0.9898 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.128 _refine_diff_density_min -0.129 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 4110 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.000 _refine_ls_R_factor_all 0.1788 _refine_ls_R_factor_gt 0.0726 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.052P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1214 _refine_ls_wR_factor_ref 0.1574 _reflns_number_gt 1662 _reflns_number_total 4110 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hk2663.cif _[local]_cod_data_source_block I _cod_database_code 2221722 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy N N1 0.0390(6) -0.6473(4) 0.26993(14) 0.0831(11) Uani d . 1 H H1A -0.0691 -0.7213 0.2599 0.100 Uiso calc R 1 N N2 0.6939(5) -0.2644(4) 0.22504(13) 0.0755(11) Uani d . 1 H H2C 0.6083 -0.3507 0.2300 0.091 Uiso calc R 1 F F1 -0.0366(5) -0.3165(3) 0.47653(11) 0.1065(9) Uani d . 1 F F2 1.1428(5) -0.3284(4) 0.03482(12) 0.1253(11) Uani d . 1 O O1 0.1510(5) -0.7508(4) 0.19019(13) 0.1045(12) Uani d . 1 O O2 0.3575(5) -0.5355(4) 0.23766(11) 0.0916(10) Uani d . 1 O O3 0.5300(5) -0.1536(4) 0.29759(12) 0.0938(11) Uani d . 1 O O4 0.8164(4) -0.0021(3) 0.26628(10) 0.0724(8) Uani d . 1 C C1 0.3835(12) -0.7830(7) 0.0572(2) 0.1033(18) Uani d . 1 H H1B 0.3416 -0.7637 0.0218 0.124 Uiso calc R 1 C C2 0.2332(9) -0.7392(6) 0.0984(3) 0.0934(16) Uani d . 1 H H2A 0.0941 -0.6896 0.0917 0.112 Uiso calc R 1 C C3 0.3045(9) -0.7740(6) 0.1487(2) 0.0763(14) Uani d . 1 C C4 0.5077(11) -0.8420(6) 0.1599(2) 0.0894(16) Uani d . 1 H H4A 0.5516 -0.8605 0.1953 0.107 Uiso calc R 1 C C5 0.6465(9) -0.8828(6) 0.1186(3) 0.1024(18) Uani d . 1 H H5A 0.7849 -0.9327 0.1259 0.123 Uiso calc R 1 C C6 0.5889(11) -0.8528(7) 0.0673(3) 0.108(2) Uani d . 1 H H6A 0.6871 -0.8792 0.0394 0.130 Uiso calc R 1 C C7 0.1980(8) -0.6340(6) 0.23447(19) 0.0860(15) Uani d . 1 C C8 0.0241(7) -0.5556(5) 0.32213(17) 0.0698(12) Uani d . 1 C C9 -0.1636(7) -0.5849(5) 0.35086(18) 0.0740(12) Uani d . 1 H H9A -0.2782 -0.6603 0.3349 0.089 Uiso calc R 1 C C10 -0.1859(8) -0.5051(6) 0.4028(2) 0.0861(14) Uani d . 1 H H10A -0.3134 -0.5253 0.4221 0.103 Uiso calc R 1 C C11 -0.0157(8) -0.3963(5) 0.42483(19) 0.0776(13) Uani d . 1 C C12 0.1691(8) -0.3626(5) 0.39833(18) 0.0772(13) Uani d . 1 H H12A 0.2818 -0.2868 0.4150 0.093 Uiso calc R 1 C C13 0.1923(7) -0.4407(5) 0.34595(18) 0.0784(13) Uani d . 1 H H13A 0.3192 -0.4165 0.3269 0.094 Uiso calc R 1 C C14 0.4753(10) 0.1478(6) 0.4438(2) 0.0860(15) Uani d . 1 H H14A 0.4594 0.2114 0.4774 0.103 Uiso calc R 1 C C15 0.6668(9) 0.0580(6) 0.4346(2) 0.0882(15) Uani d . 1 H H15A 0.7815 0.0618 0.4620 0.106 Uiso calc R 1 C C16 0.6942(7) -0.0391(5) 0.3851(2) 0.0744(13) Uani d . 1 H H16A 0.8265 -0.0994 0.3790 0.089 Uiso calc R 1 C C17 0.5254(8) -0.0445(5) 0.34616(18) 0.0647(11) Uani d . 1 C C18 0.3329(8) 0.0490(6) 0.35436(18) 0.0775(13) Uani d . 1 H H18A 0.2203 0.0478 0.3266 0.093 Uiso calc R 1 C C19 0.3070(9) 0.1455(6) 0.4044(2) 0.0829(14) Uani d . 1 H H19A 0.1761 0.2075 0.4107 0.099 Uiso calc R 1 C C20 0.6969(7) -0.1294(6) 0.26345(17) 0.0763(13) Uani d . 1 C C21 0.8171(7) -0.2801(5) 0.17706(16) 0.0588(10) Uani d . 1 C C22 1.0269(7) -0.2011(5) 0.17460(18) 0.0738(12) Uani d . 1 H H22A 1.0954 -0.1378 0.2054 0.089 Uiso calc R 1 C C23 1.1343(7) -0.2167(5) 0.12616(19) 0.0798(13) Uani d . 1 H H23A 1.2738 -0.1612 0.1237 0.096 Uiso calc R 1 C C24 1.0365(9) -0.3124(6) 0.08250(19) 0.0840(14) Uani d . 1 C C25 0.8320(8) -0.3995(5) 0.08437(18) 0.0813(13) Uani d . 1 H H25A 0.7693 -0.4681 0.0540 0.098 Uiso calc R 1 C C26 0.7227(7) -0.3818(5) 0.13273(17) 0.0717(12) Uani d . 1 H H26A 0.5845 -0.4393 0.1352 0.086 Uiso calc R 1 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 N1 0.078(3) 0.080(3) 0.086(3) -0.031(2) 0.023(2) -0.013(2) N2 0.082(3) 0.062(2) 0.080(3) -0.038(2) 0.023(2) -0.0024(19) F1 0.120(2) 0.102(2) 0.094(2) -0.0065(17) 0.0279(17) -0.0139(16) F2 0.140(3) 0.121(2) 0.112(2) -0.0283(19) 0.061(2) -0.0174(18) O1 0.105(3) 0.109(3) 0.091(2) -0.056(2) 0.030(2) -0.027(2) O2 0.094(2) 0.085(2) 0.091(2) -0.0490(18) 0.0269(18) -0.0119(17) O3 0.099(2) 0.086(2) 0.089(2) -0.0449(18) 0.0397(19) -0.0265(18) O4 0.0745(19) 0.0645(18) 0.0752(19) -0.0264(15) 0.0099(15) -0.0018(14) C1 0.112(5) 0.125(5) 0.071(4) -0.036(4) -0.012(4) 0.014(3) C2 0.081(4) 0.089(4) 0.112(5) -0.014(3) -0.010(4) 0.030(3) C3 0.065(3) 0.070(3) 0.090(4) -0.027(3) 0.014(3) -0.005(3) C4 0.099(4) 0.083(4) 0.083(4) -0.035(3) -0.008(3) 0.008(3) C5 0.080(4) 0.063(3) 0.163(6) -0.007(3) -0.009(5) 0.013(4) C6 0.081(4) 0.102(5) 0.134(6) -0.029(4) 0.032(4) -0.025(4) C7 0.081(4) 0.093(4) 0.077(3) -0.033(3) 0.015(3) -0.015(3) C8 0.069(3) 0.062(3) 0.079(3) -0.017(2) 0.015(2) 0.008(2) C9 0.066(3) 0.067(3) 0.087(3) -0.016(2) 0.010(2) 0.002(2) C10 0.083(3) 0.078(3) 0.097(4) -0.013(3) 0.025(3) 0.006(3) C11 0.081(4) 0.061(3) 0.089(4) 0.005(3) 0.024(3) -0.007(3) C12 0.081(3) 0.074(3) 0.076(3) -0.015(3) 0.000(3) 0.009(3) C13 0.075(3) 0.077(3) 0.082(3) -0.030(2) 0.009(2) 0.006(3) C14 0.093(4) 0.086(4) 0.078(4) -0.010(3) 0.020(3) 0.002(3) C15 0.090(4) 0.098(4) 0.077(4) -0.012(3) 0.002(3) 0.018(3) C16 0.055(3) 0.064(3) 0.108(4) -0.001(2) 0.015(3) 0.020(3) C17 0.065(3) 0.057(3) 0.072(3) -0.014(2) 0.012(3) 0.005(2) C18 0.077(4) 0.078(3) 0.079(3) -0.020(3) -0.004(3) 0.021(3) C19 0.080(4) 0.069(3) 0.102(4) 0.013(3) 0.022(3) 0.008(3) C20 0.081(3) 0.070(3) 0.076(3) -0.028(3) 0.017(3) -0.003(3) C21 0.059(3) 0.048(2) 0.068(3) -0.007(2) 0.003(2) 0.002(2) C22 0.054(3) 0.073(3) 0.090(3) -0.018(2) 0.002(2) -0.005(2) C23 0.068(3) 0.070(3) 0.099(4) -0.010(2) 0.029(3) -0.007(3) C24 0.099(4) 0.070(3) 0.082(4) -0.006(3) 0.032(3) -0.006(3) C25 0.093(4) 0.073(3) 0.074(3) -0.006(3) 0.009(3) -0.008(2) C26 0.072(3) 0.065(3) 0.074(3) -0.018(2) 0.007(2) -0.007(2) 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' F F 0.0171 0.0103 '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 C7 N1 C8 128.3(4) C7 N1 H1A 115.8 C8 N1 H1A 115.8 C20 N2 C21 126.8(3) C20 N2 H2C 116.6 C21 N2 H2C 116.6 C7 O1 C3 120.4(3) C20 O3 C17 118.5(3) C6 C1 C2 122.3(5) C6 C1 H1B 118.9 C2 C1 H1B 118.9 C3 C2 C1 115.4(5) C3 C2 H2A 122.3 C1 C2 H2A 122.3 C4 C3 C2 123.5(5) C4 C3 O1 118.5(6) C2 C3 O1 117.8(6) C3 C4 C5 118.9(5) C3 C4 H4A 120.6 C5 C4 H4A 120.6 C6 C5 C4 121.5(6) C6 C5 H5A 119.2 C4 C5 H5A 119.2 C5 C6 C1 118.4(6) C5 C6 H6A 120.8 C1 C6 H6A 120.8 O2 C7 N1 128.5(4) O2 C7 O1 122.5(4) N1 C7 O1 109.0(4) C9 C8 C13 118.8(4) C9 C8 N1 118.1(4) C13 C8 N1 123.0(4) C8 C9 C10 121.4(4) C8 C9 H9A 119.3 C10 C9 H9A 119.3 C11 C10 C9 117.7(4) C11 C10 H10A 121.2 C9 C10 H10A 121.2 C12 C11 C10 123.0(4) C12 C11 F1 118.9(4) C10 C11 F1 118.1(4) C11 C12 C13 119.8(4) C11 C12 H12A 120.1 C13 C12 H12A 120.1 C12 C13 C8 119.2(4) C12 C13 H13A 120.4 C8 C13 H13A 120.4 C19 C14 C15 120.5(5) C19 C14 H14A 119.7 C15 C14 H14A 119.7 C14 C15 C16 121.0(5) C14 C15 H15A 119.5 C16 C15 H15A 119.5 C17 C16 C15 118.7(4) C17 C16 H16A 120.6 C15 C16 H16A 120.6 C16 C17 C18 120.9(4) C16 C17 O3 121.9(5) C18 C17 O3 117.0(4) C17 C18 C19 119.7(4) C17 C18 H18A 120.1 C19 C18 H18A 120.1 C14 C19 C18 119.0(5) C14 C19 H19A 120.5 C18 C19 H19A 120.5 O4 C20 N2 127.1(4) O4 C20 O3 124.4(4) N2 C20 O3 108.3(3) C26 C21 C22 120.3(4) C26 C21 N2 117.4(3) C22 C21 N2 122.3(4) C21 C22 C23 119.4(4) C21 C22 H22A 120.3 C23 C22 H22A 120.3 C24 C23 C22 119.6(4) C24 C23 H23A 120.2 C22 C23 H23A 120.2 C23 C24 F2 119.6(4) C23 C24 C25 122.3(4) F2 C24 C25 118.1(4) C24 C25 C26 118.1(4) C24 C25 H25A 121.0 C26 C25 H25A 121.0 C21 C26 C25 120.2(4) C21 C26 H26A 119.9 C25 C26 H26A 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C7 1.325(5) N1 C8 1.413(4) N1 H1A 0.8600 N2 C20 1.340(4) N2 C21 1.417(4) N2 H2C 0.8600 F1 C11 1.371(4) F2 C24 1.358(4) O1 C3 1.399(5) O1 C7 1.359(4) O2 C7 1.198(4) O3 C17 1.396(5) O3 C20 1.351(4) O4 C20 1.204(4) C1 C6 1.361(7) C1 C2 1.400(6) C1 H1B 0.9300 C2 C3 1.355(6) C2 H2A 0.9300 C3 C4 1.349(6) C4 C5 1.353(6) C4 H4A 0.9300 C5 C6 1.348(7) C5 H5A 0.9300 C6 H6A 0.9300 C8 C9 1.373(5) C8 C13 1.388(5) C9 C10 1.379(5) C9 H9A 0.9300 C10 C11 1.354(5) C10 H10A 0.9300 C11 C12 1.335(5) C12 C13 1.384(5) C12 H12A 0.9300 C13 H13A 0.9300 C14 C19 1.354(6) C14 C15 1.357(6) C14 H14A 0.9300 C15 C16 1.385(6) C15 H15A 0.9300 C16 C17 1.347(5) C16 H16A 0.9300 C17 C18 1.374(5) C18 C19 1.393(6) C18 H18A 0.9300 C19 H19A 0.9300 C21 C26 1.368(5) C21 C22 1.377(5) C22 C23 1.377(5) C22 H22A 0.9300 C23 C24 1.341(5) C23 H23A 0.9300 C24 C25 1.377(6) C25 C26 1.381(5) C25 H25A 0.9300 C26 H26A 0.9300 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N1 H1A O4 1_445 0.86 2.32 3.044(4) 142.00 N2 H2C O2 . 0.86 2.08 2.931(4) 171.00 C19 H19A Cg2 1_565 0.93 2.94 3.644(4) 133.71 C23 H23A Cg1 1_665 0.93 2.97 3.710(5) 137.68 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C6 C1 C2 C3 -1.2(7) C1 C2 C3 C4 1.7(7) C1 C2 C3 O1 -173.0(4) C7 O1 C3 C4 67.3(6) C7 O1 C3 C2 -117.7(5) C2 C3 C4 C5 -2.0(7) O1 C3 C4 C5 172.7(4) C3 C4 C5 C6 1.8(7) C4 C5 C6 C1 -1.3(8) C2 C1 C6 C5 1.1(8) C8 N1 C7 O2 -4.2(9) C8 N1 C7 O1 177.7(4) C3 O1 C7 O2 7.6(8) C3 O1 C7 N1 -174.2(4) C7 N1 C8 C9 176.8(5) C7 N1 C8 C13 -4.7(7) C13 C8 C9 C10 -1.1(7) N1 C8 C9 C10 177.5(4) C8 C9 C10 C11 -0.1(7) C9 C10 C11 C12 0.6(7) C9 C10 C11 F1 -180.0(4) C10 C11 C12 C13 0.0(8) F1 C11 C12 C13 -179.4(4) C11 C12 C13 C8 -1.1(7) C9 C8 C13 C12 1.6(7) N1 C8 C13 C12 -176.9(4) C19 C14 C15 C16 -0.6(7) C14 C15 C16 C17 -0.7(6) C15 C16 C17 C18 2.3(6) C15 C16 C17 O3 -173.0(3) C20 O3 C17 C16 -63.8(6) C20 O3 C17 C18 120.8(4) C16 C17 C18 C19 -2.6(6) O3 C17 C18 C19 172.9(4) C15 C14 C19 C18 0.3(7) C17 C18 C19 C14 1.3(6) C21 N2 C20 O4 -5.8(8) C21 N2 C20 O3 170.2(4) C17 O3 C20 O4 -15.0(7) C17 O3 C20 N2 168.9(4) C20 N2 C21 C26 -150.6(4) C20 N2 C21 C22 31.2(6) C26 C21 C22 C23 4.0(6) N2 C21 C22 C23 -177.8(4) C21 C22 C23 C24 -1.9(7) C22 C23 C24 F2 -179.7(4) C22 C23 C24 C25 -1.2(8) C23 C24 C25 C26 2.1(7) F2 C24 C25 C26 -179.4(4) C22 C21 C26 C25 -3.1(6) N2 C21 C26 C25 178.6(4) C24 C25 C26 C21 0.1(7)