#------------------------------------------------------------------------------ #$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/00/74/2007438.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_2007438 loop_ _publ_author_name 'Bolte, Michael' 'Kettner, Markus' _publ_section_title ; The Twinned Crystal Structure of 3,4-Dimethylpyridine Hydrobromide at 157K ; _journal_issue 7 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 963 _journal_page_last 964 _journal_paper_doi 10.1107/S0108270198001164 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C7 H10 N 1+, Br 1-' _chemical_formula_sum 'C7 H10 Br N' _chemical_formula_weight 188.07 _chemical_name_systematic ; 3,4-Dimethylpyridinehydrobromide ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _audit_creation_method SHELXL-97 _cell_angle_alpha 69.9890(10) _cell_angle_beta 64.1520(10) _cell_angle_gamma 89.997(2) _cell_formula_units_Z 2 _cell_length_a 7.3367(7) _cell_length_b 7.7985(8) _cell_length_c 8.3960(9) _cell_measurement_reflns_used 2247 _cell_measurement_temperature 157 _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 1.00 _cell_volume 399.85(7) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 157 _diffrn_measurement_device_type 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'highly oriented graphite crystal' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3587 _diffrn_reflns_theta_max 26.02 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% 0.0 _diffrn_standards_interval_time 840 _diffrn_standards_number 76 _exptl_absorpt_coefficient_mu 5.055 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_type 'empirical \y scan (SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 188 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.415_(0.93\%A_from_Br1) _refine_diff_density_min -1.111_(0.80\%A_from_C41) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment 'H atoms: see text below' _refine_ls_matrix_type full _refine_ls_number_parameters 87 _refine_ls_number_reflns 1386 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_obs .0617 _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^)+(0.0429P)^2^+2.3936P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .1324 _refine_ls_wR_factor_obs .1274 _refine_ls_wR_factor_ref 0.1324 _reflns_number_gt 1243 _reflns_number_total 1386 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ha1209.cif _cod_data_source_block he22 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0429P)^2^+2.3936P] 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^)+(0.0429P)^2^+2.3936P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_database_code 2007438 _cod_database_fobs_code 2007438 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 Br1 .0527(2) .18021(17) 1.12747(18) .0430(3) Uani d . 1 . . Br N1 .1897(13) .3823(12) .6779(12) .037(2) Uani d . 1 . . N H1 .153(13) .305(13) .795(14) .02(2) Uiso d . 1 . . H C2 .2587(13) .5649(14) .6080(15) .035(2) Uani d . 1 . . C H2 .2660 .6205 .6901 .042 Uiso calc R 1 . . H C3 .3202(14) .6750(12) .4160(14) .032(2) Uani d . 1 . . C C31 .3942(18) .8784(15) .3438(19) .059(4) Uani d . 1 . . C H31A .3941 .9098 .4473 .089 Uiso calc R 1 . . H H31B .3028 .9472 .2990 .089 Uiso calc R 1 . . H H31C .5342 .9115 .2377 .089 Uiso calc R 1 . . H C4 .3021(14) .5852(13) .3043(13) .031(2) Uani d . 1 . . C C41 .3515(18) .6936(18) .0992(12) .059(3) Uani d . 1 . . C H41A .3998 .8245 .0648 .088 Uiso calc R 1 . . H H41B .2276 .6818 .0840 .088 Uiso calc R 1 . . H H41C .4592 .6449 .0155 .088 Uiso calc R 1 . . H C5 .2296(14) .3954(13) .3833(14) .036(2) Uani d . 1 . . C H5 .2170 .3346 .3071 .043 Uiso calc R 1 . . H C6 .1763(15) .2966(13) .5721(15) .036(2) Uani d . 1 . . C H6 .1298 .1665 .6262 .044 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 Br1 .0510(7) .0460(5) .0485(6) .0170(6) -.0314(7) -.0256(4) N1 .029(5) .043(5) .017(4) .006(4) -.005(4) .006(4) C2 .025(5) .042(6) .051(6) .018(4) -.028(5) -.021(5) C3 .028(5) .020(5) .044(6) .006(4) -.020(5) -.001(4) C31 .051(8) .032(6) .083(9) .006(5) -.037(7) -.002(6) C4 .026(5) .042(6) .021(5) .013(4) -.013(4) -.003(4) C41 .033(6) .093(9) .011(4) .010(8) .001(5) .009(5) C5 .030(6) .040(5) .042(6) .011(4) -.014(5) -.024(5) C6 .030(6) .016(4) .041(6) -.001(4) -.009(5) .005(4) 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' 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 C6 N1 C2 122.6(9) N1 C2 C3 121.1(9) C4 C3 C2 116.5(8) C4 C3 C31 124.0(10) C2 C3 C31 119.5(10) C5 C4 C3 120.3(8) C5 C4 C41 119.1(10) C3 C4 C41 120.5(10) C6 C5 C4 119.6(9) N1 C6 C5 119.9(9) 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 C6 . 1.315(13) ? N1 C2 . 1.341(13) ? C2 C3 . 1.399(13) ? C3 C4 . 1.395(14) ? C3 C31 . 1.495(14) ? C4 C5 . 1.391(13) ? C4 C41 . 1.506(12) ? C5 C6 . 1.372(13) ? 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 N1 C2 C3 0.2(13) N1 C2 C3 C4 1.1(13) N1 C2 C3 C31 179.3(9) C2 C3 C4 C5 -1.1(13) C31 C3 C4 C5 -179.3(9) C2 C3 C4 C41 176.1(8) C31 C3 C4 C41 -2.0(14) C3 C4 C5 C6 -0.1(13) C41 C4 C5 C6 -177.4(9) C2 N1 C6 C5 -1.6(14) C4 C5 C6 N1 1.5(14)