############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_global _audit_creation_method 'PLATON option' _journal_date_recd_electronic 2012-05-09 _journal_date_accepted 2012-05-21 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2012 _journal_volume 68 _journal_issue 6 _journal_page_first m842 _journal_page_last m842 _journal_paper_category QM _journal_paper_doi 10.1107/S1600536812023185 _journal_coeditor_code VM2176 _publ_contact_author_name ; Dr. Mehmet Akkurt ; _publ_contact_author_address ; Department of Physics Faculty of Sciences Erciyes University 38039 Kayseri Turkey ; _publ_contact_author_email akkurt@erciyes.edu.tr _publ_contact_author_fax '+90-352-4374933' _publ_contact_author_phone '+90-352-4374901 ext. 33106' _publ_section_title ;\ Dibromido{N'-[1-(pyridin-2-yl)ethylidene]picolinohydrazide-\ \k^2^N',O}cadmium ; loop_ _publ_author_name _publ_author_address 'Mehmet Akkurt' ; Department of Physics, Faculty of Sciences, Erciyes University, 38039 Kayseri, Turkey ; 'Ali Akbar Khandar' ; Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, 51666 Tabriz, Iran ; 'Muhammad Nawaz Tahir' ; Department of Physics, University of Sargodha, Sargodha, Pakistan ; 'Seyed Abolfazl Hosseini Yazdi' ; Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, 51666 Tabriz, Iran ; 'Farhad Akbari Afkhami' ; Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, 51666 Tabriz, Iran ; data_I _chemical_name_systematic ; Dibromido{N'-[1-(pyridin-2-yl)ethylidene]picolinohydrazide- \k^2^N',O}cadmium ; _chemical_name_common ? _chemical_formula_moiety 'C13 H12 Br2 Cd N4 O' _chemical_formula_sum 'C13 H12 Br2 Cd N4 O' _chemical_formula_structural ? _chemical_formula_iupac '[Cd Br2 (C13 H12 N4 O)]' _chemical_formula_weight 512.48 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 8.1336(3) _cell_length_b 13.6111(5) _cell_length_c 14.6102(5) _cell_angle_alpha 90 _cell_angle_beta 90.5500(10) _cell_angle_gamma 90 _cell_volume 1617.38(10) _cell_formula_units_Z 4 _cell_measurement_reflns_used 545 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 18.3 _cell_measurement_temperature 296(2) _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 6.294 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2005)' _exptl_absorpt_correction_T_min 0.267 _exptl_absorpt_correction_T_max 0.365 _exptl_special_details ; ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEXII CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15317 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 28.09 _diffrn_reflns_theta_full 28.09 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_reduction_process ; ; _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > \s(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _reflns_number_total 3874 _reflns_number_gt 2859 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.0623 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _refine_ls_number_reflns 3874 _refine_ls_number_parameters 195 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.5132P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.465 _refine_diff_density_min -0.537 _refine_ls_extinction_method 'none' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . 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' Br Br -0.2901 2.4595 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 ' 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' _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2009)' _computing_data_reduction 'SAINT (Bruker, 2009)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2009)' _computing_publication_material 'WinGX (Farrugia, 1999) and PLATON (Spek, 2009)' 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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd1 0.32238(3) 0.16938(2) 0.27655(2) 0.04290(10) Uani d . 1.000 . . Br Br1 0.04606(5) 0.15378(3) 0.35202(3) 0.06260(10) Uani d . 1.000 . . Br Br2 0.42596(5) 0.34049(2) 0.23982(3) 0.05500(10) Uani d . 1.000 . . O O1 0.2555(3) 0.10824(15) 0.12175(14) 0.0493(8) Uani d . 1.000 . . N N1 0.5195(3) 0.12698(18) 0.38976(17) 0.0438(9) Uani d . 1.000 . . N N2 0.4511(3) 0.02135(16) 0.24438(15) 0.0370(8) Uani d . 1.000 . . N N3 0.4106(3) -0.02318(18) 0.16427(17) 0.0401(8) Uani d D 1.000 . . N N4 0.3565(3) -0.11450(19) 0.01147(18) 0.0495(10) Uani d . 1.000 . . C C1 0.5632(5) 0.1867(2) 0.4579(2) 0.0555(11) Uani d . 1.000 . . C C2 0.6781(5) 0.1618(3) 0.5230(2) 0.0585(11) Uani d . 1.000 . . C C3 0.7498(4) 0.0712(3) 0.5186(2) 0.0585(14) Uani d . 1.000 . . C C4 0.7079(4) 0.0090(2) 0.4477(2) 0.0487(11) Uani d . 1.000 . . C C5 0.5925(4) 0.0390(2) 0.3832(2) 0.0385(9) Uani d . 1.000 . . C C6 0.5464(3) -0.0217(2) 0.3021(2) 0.0377(9) Uani d . 1.000 . . C C7 0.6137(5) -0.1226(2) 0.2915(2) 0.0577(11) Uani d . 1.000 . . C C8 0.3114(4) 0.0268(2) 0.1050(2) 0.0392(9) Uani d . 1.000 . . C C9 0.2810(4) -0.0274(2) 0.01743(19) 0.0381(9) Uani d . 1.000 . . C C10 0.1844(4) 0.0113(2) -0.0505(2) 0.0473(11) Uani d . 1.000 . . C C11 0.1592(4) -0.0425(2) -0.1296(2) 0.0523(11) Uani d . 1.000 . . C C12 0.2361(5) -0.1319(2) -0.1370(2) 0.0543(11) Uani d . 1.000 . . C C13 0.3333(5) -0.1652(2) -0.0658(2) 0.0569(13) Uani d . 1.000 . . H H1 0.51340 0.24800 0.46140 0.0660 Uiso c R 1.000 . . H H2 0.70680 0.20560 0.56930 0.0700 Uiso c R 1.000 . . H H3 0.82590 0.05170 0.56290 0.0700 Uiso c R 1.000 . . H H3N 0.434(4) -0.0819(15) 0.150(2) 0.056(10) Uiso d D 1.000 . . H H4 0.75670 -0.05260 0.44310 0.0580 Uiso c R 1.000 . . H H7A 0.54530 -0.15920 0.24990 0.0860 Uiso c R 1.000 . . H H7B 0.61610 -0.15480 0.34990 0.0860 Uiso c R 1.000 . . H H7C 0.72320 -0.11890 0.26780 0.0860 Uiso c R 1.000 . . H H10 0.13630 0.07280 -0.04360 0.0570 Uiso c R 1.000 . . H H11 0.09200 -0.01880 -0.17650 0.0630 Uiso c R 1.000 . . H H12 0.22280 -0.16960 -0.18970 0.0650 Uiso c R 1.000 . . H H13 0.38510 -0.22580 -0.07180 0.0680 Uiso c R 1.000 . . 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 Cd1 0.04740(10) 0.03830(10) 0.04280(10) 0.00450(10) -0.00510(10) -0.00160(10) Br1 0.0532(2) 0.0726(3) 0.0622(2) -0.0011(2) 0.0063(2) 0.0021(2) Br2 0.0638(2) 0.0413(2) 0.0598(2) -0.0049(2) -0.0091(2) 0.0024(2) O1 0.0616(15) 0.0432(13) 0.0429(12) 0.0105(11) -0.0085(11) -0.0083(10) N1 0.0503(16) 0.0397(14) 0.0412(15) -0.0023(12) -0.0086(12) 0.0021(11) N2 0.0393(14) 0.0367(13) 0.0350(14) -0.0022(11) -0.0031(11) -0.0016(10) N3 0.0476(15) 0.0354(14) 0.0373(14) -0.0005(12) -0.0045(11) -0.0063(11) N4 0.0654(19) 0.0394(15) 0.0436(16) 0.0006(13) -0.0089(13) -0.0043(12) C1 0.075(2) 0.0403(18) 0.051(2) -0.0047(17) -0.0117(18) -0.0030(15) C2 0.071(2) 0.061(2) 0.0433(19) -0.0144(19) -0.0141(17) -0.0057(16) C3 0.056(2) 0.073(3) 0.046(2) -0.0134(18) -0.0175(17) 0.0083(17) C4 0.0471(19) 0.0505(19) 0.0483(19) -0.0019(15) -0.0065(15) 0.0107(15) C5 0.0371(16) 0.0401(16) 0.0381(16) -0.0056(13) -0.0025(13) 0.0074(13) C6 0.0359(16) 0.0361(16) 0.0411(17) -0.0045(13) 0.0005(13) 0.0033(13) C7 0.065(2) 0.0458(19) 0.062(2) 0.0137(17) -0.0072(18) -0.0003(17) C8 0.0396(16) 0.0418(17) 0.0362(16) -0.0092(14) -0.0016(13) 0.0004(13) C9 0.0384(16) 0.0383(16) 0.0376(16) -0.0058(13) 0.0000(13) -0.0005(12) C10 0.0495(19) 0.0458(18) 0.0464(19) 0.0008(15) -0.0065(15) -0.0043(15) C11 0.056(2) 0.057(2) 0.0437(19) -0.0102(17) -0.0101(16) 0.0044(15) C12 0.069(2) 0.053(2) 0.0408(19) -0.0194(18) -0.0046(17) -0.0082(15) C13 0.075(3) 0.0397(18) 0.056(2) -0.0021(17) -0.0054(19) -0.0107(16) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 Br1 . . 2.5218(5) no Cd1 Br2 . . 2.5359(4) no Cd1 O1 . . 2.466(2) no Cd1 N1 . . 2.364(2) no Cd1 N2 . . 2.321(2) no O1 C8 . . 1.224(4) no N1 C1 . . 1.331(4) no N1 C5 . . 1.341(4) no N2 N3 . . 1.356(3) no N2 C6 . . 1.282(4) no N3 C8 . . 1.360(4) no N4 C9 . . 1.338(4) no N4 C13 . . 1.335(4) no N3 H3N . . 0.85(2) no C1 C2 . . 1.370(5) no C2 C3 . . 1.366(6) no C3 C4 . . 1.378(4) no C4 C5 . . 1.385(4) no C5 C6 . . 1.490(4) no C6 C7 . . 1.487(4) no C8 C9 . . 1.495(4) no C9 C10 . . 1.366(4) no C10 C11 . . 1.382(4) no C11 C12 . . 1.373(4) no C12 C13 . . 1.377(5) no C1 H1 . . 0.9300 no C2 H2 . . 0.9300 no C3 H3 . . 0.9300 no C4 H4 . . 0.9300 no C7 H7A . . 0.9600 no C7 H7B . . 0.9600 no C7 H7C . . 0.9600 no C10 H10 . . 0.9300 no C11 H11 . . 0.9300 no C12 H12 . . 0.9300 no C13 H13 . . 0.9300 no 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Br1 Cd1 Br2 . . . 117.98(2) no Br1 Cd1 O1 . . . 100.54(6) no Br1 Cd1 N1 . . . 105.95(6) no Br1 Cd1 N2 . . . 114.91(6) no Br2 Cd1 O1 . . . 100.76(5) no Br2 Cd1 N1 . . . 98.50(6) no Br2 Cd1 N2 . . . 127.09(6) no O1 Cd1 N1 . . . 134.55(8) no O1 Cd1 N2 . . . 67.49(8) no N1 Cd1 N2 . . . 68.01(8) no Cd1 O1 C8 . . . 114.21(19) no Cd1 N1 C1 . . . 123.3(2) no Cd1 N1 C5 . . . 117.77(19) no C1 N1 C5 . . . 118.9(3) no Cd1 N2 N3 . . . 117.17(17) no Cd1 N2 C6 . . . 122.33(18) no N3 N2 C6 . . . 120.3(2) no N2 N3 C8 . . . 117.6(2) no C9 N4 C13 . . . 116.9(3) no C8 N3 H3N . . . 117(2) no N2 N3 H3N . . . 126(2) no N1 C1 C2 . . . 123.0(3) no C1 C2 C3 . . . 118.7(3) no C2 C3 C4 . . . 119.2(3) no C3 C4 C5 . . . 119.4(3) no N1 C5 C4 . . . 120.8(3) no C4 C5 C6 . . . 122.8(3) no N1 C5 C6 . . . 116.4(3) no N2 C6 C7 . . . 125.1(3) no C5 C6 C7 . . . 120.3(2) no N2 C6 C5 . . . 114.6(2) no N3 C8 C9 . . . 113.0(2) no O1 C8 N3 . . . 123.0(3) no O1 C8 C9 . . . 124.0(3) no C8 C9 C10 . . . 121.4(3) no N4 C9 C8 . . . 114.9(3) no N4 C9 C10 . . . 123.8(3) no C9 C10 C11 . . . 118.9(3) no C10 C11 C12 . . . 118.1(3) no C11 C12 C13 . . . 119.4(3) no N4 C13 C12 . . . 123.0(3) no N1 C1 H1 . . . 118.00 no C2 C1 H1 . . . 119.00 no C1 C2 H2 . . . 121.00 no C3 C2 H2 . . . 121.00 no C2 C3 H3 . . . 120.00 no C4 C3 H3 . . . 120.00 no C3 C4 H4 . . . 120.00 no C5 C4 H4 . . . 120.00 no C6 C7 H7A . . . 109.00 no C6 C7 H7B . . . 109.00 no C6 C7 H7C . . . 109.00 no H7A C7 H7B . . . 109.00 no H7A C7 H7C . . . 109.00 no H7B C7 H7C . . . 109.00 no C9 C10 H10 . . . 121.00 no C11 C10 H10 . . . 121.00 no C10 C11 H11 . . . 121.00 no C12 C11 H11 . . . 121.00 no C11 C12 H12 . . . 120.00 no C13 C12 H12 . . . 120.00 no N4 C13 H13 . . . 119.00 no C12 C13 H13 . . . 119.00 no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Br1 Cd1 O1 C8 . . . . -107.6(2) no Br2 Cd1 O1 C8 . . . . 131.0(2) no N1 Cd1 O1 C8 . . . . 17.6(3) no N2 Cd1 O1 C8 . . . . 5.2(2) no Br1 Cd1 N1 C1 . . . . -76.1(3) no Br2 Cd1 N1 C1 . . . . 46.4(3) no O1 Cd1 N1 C1 . . . . 160.7(2) no N2 Cd1 N1 C1 . . . . 173.0(3) no Br1 Cd1 N1 C5 . . . . 105.4(2) no Br2 Cd1 N1 C5 . . . . -132.2(2) no O1 Cd1 N1 C5 . . . . -17.9(3) no N2 Cd1 N1 C5 . . . . -5.6(2) no Br1 Cd1 N2 N3 . . . . 85.55(18) no Br2 Cd1 N2 N3 . . . . -92.50(19) no O1 Cd1 N2 N3 . . . . -5.94(17) no N1 Cd1 N2 N3 . . . . -176.5(2) no Br1 Cd1 N2 C6 . . . . -88.8(2) no Br2 Cd1 N2 C6 . . . . 93.1(2) no O1 Cd1 N2 C6 . . . . 179.7(2) no N1 Cd1 N2 C6 . . . . 9.2(2) no Cd1 O1 C8 C9 . . . . 177.1(2) no Cd1 O1 C8 N3 . . . . -4.0(4) no Cd1 N1 C5 C6 . . . . 2.6(3) no Cd1 N1 C1 C2 . . . . -179.7(3) no C1 N1 C5 C4 . . . . 2.0(4) no C1 N1 C5 C6 . . . . -176.1(3) no C5 N1 C1 C2 . . . . -1.1(5) no Cd1 N1 C5 C4 . . . . -179.3(2) no C6 N2 N3 C8 . . . . -178.9(3) no Cd1 N2 C6 C7 . . . . 170.9(2) no Cd1 N2 N3 C8 . . . . 6.6(3) no Cd1 N2 C6 C5 . . . . -11.0(3) no N3 N2 C6 C7 . . . . -3.4(4) no N3 N2 C6 C5 . . . . 174.8(2) no N2 N3 C8 O1 . . . . -1.5(4) no N2 N3 C8 C9 . . . . 177.5(2) no C9 N4 C13 C12 . . . . -0.5(5) no C13 N4 C9 C8 . . . . -179.7(3) no C13 N4 C9 C10 . . . . -0.4(5) no N1 C1 C2 C3 . . . . -0.8(6) no C1 C2 C3 C4 . . . . 1.8(5) no C2 C3 C4 C5 . . . . -0.9(5) no C3 C4 C5 N1 . . . . -1.0(5) no C3 C4 C5 C6 . . . . 177.0(3) no N1 C5 C6 N2 . . . . 5.2(4) no C4 C5 C6 C7 . . . . 5.3(4) no C4 C5 C6 N2 . . . . -172.9(3) no N1 C5 C6 C7 . . . . -176.6(3) no O1 C8 C9 N4 . . . . 178.4(3) no N3 C8 C9 C10 . . . . -179.9(3) no O1 C8 C9 C10 . . . . -1.0(5) no N3 C8 C9 N4 . . . . -0.6(4) no N4 C9 C10 C11 . . . . 1.4(5) no C8 C9 C10 C11 . . . . -179.3(3) no C9 C10 C11 C12 . . . . -1.5(5) no C10 C11 C12 C13 . . . . 0.7(5) no C11 C12 C13 N4 . . . . 0.3(6) no 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 _geom_hbond_publ_flag C7 H7C Br2 2_645 0.96 2.91 3.810(4) 157 yes _iucr_refine_instructions_details ; TITL 237-A in P2(1)/n CELL 0.71073 8.1336 13.6111 14.6102 90.000 90.550 90.000 ZERR 4.00 0.0003 0.0005 0.0005 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR CD UNIT 52 48 16 4 8 4 MERG 2 DFIX 0.860 0.020 N3 H3N FMAP 2 PLAN 12 ACTA BOND $H CONF LIST 4 L.S. 33 TEMP 23.00 WGHT 0.024500 0.513200 FVAR 0.09193 C1 1 0.563154 0.186657 0.457866 11.00000 0.07493 0.04027 = 0.05056 -0.00301 -0.01168 -0.00472 AFIX 43 H1 2 0.513404 0.248039 0.461442 11.00000 -1.20000 AFIX 0 C2 1 0.678144 0.161752 0.523018 11.00000 0.07080 0.06090 = 0.04334 -0.00572 -0.01412 -0.01438 AFIX 43 H2 2 0.706796 0.205648 0.569270 11.00000 -1.20000 AFIX 0 C3 1 0.749769 0.071162 0.518614 11.00000 0.05580 0.07253 = 0.04584 0.00834 -0.01749 -0.01342 AFIX 43 H3 2 0.825860 0.051667 0.562926 11.00000 -1.20000 AFIX 0 C4 1 0.707884 0.008957 0.447662 11.00000 0.04715 0.05051 = 0.04833 0.01066 -0.00647 -0.00193 AFIX 43 H4 2 0.756677 -0.052619 0.443103 11.00000 -1.20000 AFIX 0 C5 1 0.592465 0.039040 0.383250 11.00000 0.03705 0.04008 = 0.03811 0.00743 -0.00253 -0.00561 C6 1 0.546376 -0.021688 0.302078 11.00000 0.03594 0.03607 = 0.04113 0.00333 0.00051 -0.00451 C7 1 0.613703 -0.122560 0.291487 11.00000 0.06470 0.04578 = 0.06177 -0.00027 -0.00724 0.01370 AFIX 137 H7A 2 0.545267 -0.159166 0.249853 11.00000 -1.50000 H7B 2 0.616079 -0.154762 0.349944 11.00000 -1.50000 H7C 2 0.723235 -0.118883 0.267826 11.00000 -1.50000 AFIX 0 C8 1 0.311390 0.026784 0.104968 11.00000 0.03963 0.04178 = 0.03623 0.00040 -0.00159 -0.00920 C9 1 0.281047 -0.027426 0.017428 11.00000 0.03835 0.03834 = 0.03758 -0.00054 0.00001 -0.00582 C10 1 0.184364 0.011269 -0.050483 11.00000 0.04954 0.04583 = 0.04639 -0.00429 -0.00652 0.00085 AFIX 43 H10 2 0.136271 0.072780 -0.043578 11.00000 -1.20000 AFIX 0 C11 1 0.159181 -0.042461 -0.129599 11.00000 0.05569 0.05664 = 0.04373 0.00437 -0.01007 -0.01018 AFIX 43 H11 2 0.092004 -0.018754 -0.176494 11.00000 -1.20000 AFIX 0 C12 1 0.236144 -0.131876 -0.137049 11.00000 0.06913 0.05315 = 0.04079 -0.00817 -0.00462 -0.01939 AFIX 43 H12 2 0.222788 -0.169562 -0.189694 11.00000 -1.20000 AFIX 0 C13 1 0.333345 -0.165242 -0.065797 11.00000 0.07479 0.03967 = 0.05570 -0.01072 -0.00545 -0.00210 AFIX 43 H13 2 0.385120 -0.225789 -0.071800 11.00000 -1.20000 AFIX 0 N1 3 0.519519 0.126979 0.389756 11.00000 0.05032 0.03971 = 0.04117 0.00212 -0.00857 -0.00227 N2 3 0.451143 0.021355 0.244375 11.00000 0.03929 0.03674 = 0.03498 -0.00162 -0.00306 -0.00216 N3 3 0.410584 -0.023181 0.164266 11.00000 0.04763 0.03538 = 0.03727 -0.00635 -0.00449 -0.00049 N4 3 0.356487 -0.114505 0.011469 11.00000 0.06542 0.03939 = 0.04357 -0.00430 -0.00888 0.00061 O1 4 0.255470 0.108244 0.121753 11.00000 0.06158 0.04318 = 0.04295 -0.00826 -0.00852 0.01054 BR1 5 0.046064 0.153783 0.352023 11.00000 0.05323 0.07259 = 0.06222 0.00213 0.00626 -0.00113 BR2 5 0.425960 0.340495 0.239819 11.00000 0.06381 0.04132 = 0.05975 0.00238 -0.00910 -0.00491 CD1 6 0.322385 0.169376 0.276552 11.00000 0.04744 0.03828 = 0.04276 -0.00155 -0.00514 0.00453 H3N 2 0.433955 -0.081896 0.149866 11.00000 0.05628 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM 237-A in P2(1)/n REM R1 = 0.0278 for 2859 Fo > 4sig(Fo) and 0.0486 for all 3874 data REM 195 parameters refined using 1 restraints END WGHT 0.0245 0.5132 REM Highest difference peak 0.465, deepest hole -0.537, 1-sigma level 0.075 Q1 1 0.5180 0.3011 0.2148 11.00000 0.05 0.47 Q2 1 0.0823 0.1606 0.4033 11.00000 0.05 0.43 Q3 1 0.4552 0.3397 0.2871 11.00000 0.05 0.43 Q4 1 0.3008 0.1169 0.2777 11.00000 0.05 0.37 Q5 1 0.1370 0.1617 0.3775 11.00000 0.05 0.36 Q6 1 0.2158 0.1129 0.3061 11.00000 0.05 0.35 Q7 1 0.3850 0.2172 0.2542 11.00000 0.05 0.34 Q8 1 0.3051 0.2360 0.2809 11.00000 0.05 0.34 Q9 1 0.1778 0.1884 0.3188 11.00000 0.05 0.32 Q10 1 0.3862 0.0958 0.2537 11.00000 0.05 0.32 Q11 1 0.7590 0.0659 0.4573 11.00000 0.05 0.30 Q12 1 0.0527 0.0942 0.3363 11.00000 0.05 0.30 ;