#------------------------------------------------------------------------------ #$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/90/2009006.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_2009006 loop_ _publ_author_name 'Clark, Bernard A. J.' 'Evans, Matthew C.' 'Lloyd, Douglas' 'McNab, Hamish' 'Parsons, Simon' _publ_section_title ; 7-Phenyl-2,3,4,5-tetrahydro-1H-1,4-diazepin-5-one ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1725 _journal_page_last 1727 _journal_paper_doi 10.1107/S010827019900832X _journal_volume 55 _journal_year 1999 _chemical_formula_sum 'C11 H12 N2 O' _chemical_formula_weight 188.23 _chemical_name_systematic ; 7-Phenyl-1,2,3,4,-tetrahydro-1,4-diazepin-5-one ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2ya' _symmetry_space_group_name_H-M 'I 1 2/a 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 114.792(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 12.1685(19) _cell_length_b 13.724(2) _cell_length_c 13.315(3) _cell_measurement_reflns_used 54 _cell_measurement_temperature 220.0(2) _cell_measurement_theta_max 16 _cell_measurement_theta_min 15 _cell_volume 2018.7(6) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990b)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1995)' _computing_structure_refinement SHELX97 _computing_structure_solution 'SHELX97 (Sheldrick, 1997)' _diffrn_ambient_temperature 220.0(2) _diffrn_measured_fraction_theta_full 0.477 _diffrn_measured_fraction_theta_max 0.477 _diffrn_measurement_device_type ; Stoe Stadi-4 diffractometer equipped with an Oxford Cryosystems low-temperature device (Cosier & Glazer, 1986). ; _diffrn_measurement_method \w-\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 0.025 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4252 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 2.97 _diffrn_standards_decay_% 1 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type none _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 1.239 _exptl_crystal_density_method 'not measured' _exptl_crystal_description lath _exptl_crystal_F_000 800 _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _refine_diff_density_max 0.151 _refine_diff_density_min -0.165 _refine_ls_extinction_coef 0.0056(8) _refine_ls_extinction_method 'SHELX97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1789 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.047 _refine_ls_R_factor_gt 0.034 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.6438P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.089 _reflns_number_gt 1428 _reflns_number_total 1789 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cf1321.cif _cod_data_source_block me2824 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' 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 'Monoclinic' changed to 'monoclinic' 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^)+(0.0447P)^2^+0.6438P] 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^)+(0.0447P)^2^+0.6438P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 2009006 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' loop_ _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 _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol N1 .00168(12) -.04034(9) .21479(11) .0400(3) Uani d . 1 . . N H1 -.0539(15) -.0827(12) .2057(13) .048(5) Uiso d . 1 . . H C2 .00199(13) .04474(10) .27823(12) .0386(4) Uani d . 1 . . C H2A .0710 .0409 .3508 .046 Uiso calc R 1 . . H H2B -.0721 .0451 .2903 .046 Uiso calc R 1 . . H C3 .00966(12) .13904(10) .22285(12) .0346(3) Uani d . 1 . . C H3A -.0417 .1343 .1434 .041 Uiso calc R 1 . . H H3B -.0213 .1923 .2527 .041 Uiso calc R 1 . . H N4 .13228(10) .16128(9) .23937(10) .0329(3) Uani d . 1 . . N H4 .1569(14) .2243(11) .2544(12) .037(4) Uiso d . 1 . . H C5 .20066(11) .10458(10) .20638(11) .0307(3) Uani d . 1 . . C O51 .29813(8) .13925(7) .20970(9) .0406(3) Uani d . 1 . . O C6 .16464(12) .00686(10) .16476(11) .0322(3) Uani d . 1 . . C H6 .2112 -.0196 .1302 .039 Uiso calc R 1 . . H C7 .07678(11) -.05490(9) .16539(11) .0300(3) Uani d . 1 . . C C71 .05994(13) -.15101(9) .10852(11) .0318(3) Uani d . 1 . . C C72 -.05561(14) -.18775(11) .04568(12) .0389(4) Uani d . 1 . . C H72 -.1239 -.1515 .0388 .047 Uiso calc R 1 . . H C73 -.07060(17) -.27693(11) -.00661(13) .0494(4) Uani d . 1 . . C H73 -.1490 -.3005 -.0497 .059 Uiso calc R 1 . . H C74 .02877(18) -.33158(12) .00411(14) .0547(5) Uani d . 1 . . C H74 .0183 -.3921 -.0317 .066 Uiso calc R 1 . . H C75 .14337(18) -.29702(12) .06754(15) .0544(5) Uani d . 1 . . C H75 .2113 -.3347 .0762 .065 Uiso calc R 1 . . H C76 .15910(14) -.20709(11) .11850(13) .0416(4) Uani d . 1 . . C H76 .2378 -.1836 .1604 .050 Uiso calc R 1 . . H 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 .0418(7) .0339(7) .0587(8) -.0138(6) .0352(7) -.0112(6) C2 .0395(8) .0380(8) .0506(9) -.0081(6) .0310(7) -.0090(7) C3 .0265(7) .0350(8) .0480(8) -.0022(6) .0212(6) -.0070(6) N4 .0276(6) .0265(6) .0504(7) -.0051(5) .0220(5) -.0056(5) C5 .0254(7) .0294(7) .0409(8) -.0004(6) .0174(6) .0009(6) O51 .0300(5) .0293(5) .0723(7) -.0044(4) .0309(5) -.0058(5) C6 .0302(7) .0291(7) .0444(8) -.0003(6) .0226(6) -.0026(6) C7 .0273(7) .0302(7) .0341(7) -.0008(6) .0145(6) .0008(6) C71 .0377(8) .0286(7) .0334(7) -.0041(6) .0192(6) .0015(6) C72 .0418(8) .0362(8) .0381(8) -.0061(7) .0162(7) .0008(6) C73 .0638(11) .0411(9) .0382(8) -.0176(8) .0162(8) -.0048(7) C74 .0916(14) .0322(8) .0507(10) -.0103(9) .0399(10) -.0095(7) C75 .0744(12) .0372(9) .0699(12) .0052(8) .0483(10) -.0018(8) C76 .0440(9) .0344(8) .0545(9) -.0010(6) .0288(8) -.0011(7) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C7 N1 C2 124.86(12) N1 C2 C3 113.18(11) N4 C3 C2 112.16(12) C5 N4 C3 124.75(12) O51 C5 N4 118.24(12) O51 C5 C6 119.50(11) N4 C5 C6 122.23(12) C7 C6 C5 133.18(12) N1 C7 C6 127.15(12) N1 C7 C71 113.73(11) C6 C7 C71 119.10(12) C76 C71 C72 118.27(13) C76 C71 C7 120.81(13) C72 C71 C7 120.90(13) C73 C72 C71 120.63(15) C74 C73 C72 120.33(16) C75 C74 C73 119.67(15) C74 C75 C76 120.32(16) C75 C76 C71 120.76(15) 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 N1 C7 . 1.3460(17) ? N1 C2 . 1.4403(18) ? C2 C3 . 1.5116(19) ? C3 N4 . 1.4465(17) ? N4 C5 . 1.3408(17) ? C5 O51 . 1.2614(15) ? C5 C6 . 1.4471(19) ? C6 C7 . 1.3670(18) ? C7 C71 . 1.4916(18) ? C71 C76 . 1.390(2) ? C71 C72 . 1.395(2) ? C72 C73 . 1.382(2) ? C73 C74 . 1.379(3) ? C74 C75 . 1.377(3) ? C75 C76 . 1.382(2) ?