#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/25/2012570.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_2012570 loop_ _publ_author_name 'Guzei, Ilia A.' 'Roberts, John' 'Saulys, Dovas A.' _publ_section_title ; Pseudosymmetry in pyridinium tetrachloro(oxo)pyridineniobate(V) pyridine solvate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m141 _journal_page_last m143 _journal_paper_doi 10.1107/S0108270101021886 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '(C5 H6 N) [Nb Cl4 O (C5 H5 N)] , C5 H5 N' _chemical_formula_moiety 'C5 H6 N + , C5 H5 Cl4 N Nb O - , C5 H5 N' _chemical_formula_sum 'C15 H16 Cl4 N3 Nb O' _chemical_formula_weight 489.02 _chemical_name_systematic ; pyridinium tetrachloro(oxo)pyridineniobate(V) pyridine solvate ; _space_group_IT_number 30 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2 -2bc' _symmetry_space_group_name_H-M 'P n c 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.3355(3) _cell_length_b 9.4033(4) _cell_length_c 14.1728(7) _cell_measurement_reflns_used 5722 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 977.61(8) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXTL (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full .999 _diffrn_measured_fraction_theta_max .999 _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .030 _diffrn_reflns_av_sigmaI/netI .027 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 7522 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 2.60 _diffrn_standards_decay_% <1 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_T_max .721 _exptl_absorpt_correction_T_min .646 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Blessing, 1995)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 488 _exptl_crystal_size_max .41 _exptl_crystal_size_mid .32 _exptl_crystal_size_min .30 _refine_diff_density_max .57 _refine_diff_density_min -.29 _refine_ls_abs_structure_details 'Flack (1983); 952 Friedel pairs' _refine_ls_abs_structure_Flack -.03(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 2000 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all .020 _refine_ls_R_factor_gt .020 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0357P)^2^+0.0707P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .054 _refine_ls_wR_factor_ref .054 _reflns_number_gt 1975 _reflns_number_total 2000 _reflns_threshold_expression I>2\s(I) _cod_data_source_file fr1359.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 'Orthorhombic' changed to 'orthorhombic' 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: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 2012570 _cod_database_fobs_code 2012570 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -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 Nb .0000 .0000 .02797(3) .02526(9) Uani d S 1 . . Nb Cl1 .20434(7) .19501(6) .05364(3) .04146(15) Uani d . 1 . . Cl Cl2 -.25238(7) .16099(5) .04506(3) .03758(13) Uani d . 1 . . Cl O .0000 .0000 -.0924(2) .0428(7) Uani d S 1 . . O N1 .0000 .0000 .2034(3) .0251(6) Uani d S 1 . . N N2 .5000 .0000 .4232(3) .0390(9) Uani d S 1 . . N H2A .5000 .0000 .4853 .047 Uiso calc SPR .50 . . H N3 .5000 .0000 .6177(3) .0338(8) Uani d S 1 . . N H3A .5000 .0000 .5556 .041 Uiso calc SPR .50 . . H C1 -.0335(3) .1185(2) .25262(17) .0331(4) Uani d . 1 . . C H1 -.0568 .2040 .2190 .040 Uiso calc R 1 . . H C2 -.0359(3) .1224(3) .3501(2) .0445(6) Uani d . 1 . . C H2 -.0620 .2083 .3827 .053 Uiso calc R 1 . . H C3 .0000 .0000 .3984(3) .0503(12) Uani d S 1 . . C H3 .0000 .0000 .4654 .060 Uiso calc SR 1 . . H C4 .4598(3) .1197(3) .37807(18) .0403(5) Uani d . 1 . . C H4 .4325 .2036 .4127 .048 Uiso calc R 1 . . H C5 .4577(3) .1220(2) .28134(18) .0383(5) Uani d . 1 . . C H5 .4275 .2070 .2487 .046 Uiso calc R 1 . . H C6 .5000 .0000 .2317(3) .0317(9) Uani d S 1 . . C H6 .5000 .0000 .1646 .038 Uiso calc SR 1 . . H C7 .3472(4) -.0147(2) .6669(2) .0435(6) Uani d . 1 . . C H7 .2362 -.0253 .6331 .052 Uiso calc R 1 . . H C8 .3403(6) -.0155(2) .7633(3) .0626(11) Uani d . 1 . . C H8 .2279 -.0264 .7958 .075 Uiso calc R 1 . . H C9 .5000 .0000 .8110(5) .071(2) Uani d S 1 . . C H9 .5000 .0000 .8781 .085 Uiso calc SR 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 Nb .02706(12) .03326(13) .01544(14) .00004(7) .000 .000 Cl1 .0431(3) .0417(2) .0396(3) -.0145(2) -.0024(3) .0132(3) Cl2 .0373(2) .0443(3) .0312(3) .01137(19) .0023(3) .0090(2) O .0417(15) .073(2) .0140(15) .0058(10) .000 .000 N1 .0274(13) .0304(13) .0175(16) -.0006(8) .000 .000 N2 .040(2) .058(2) .0188(18) -.0063(10) .000 .000 N3 .045(2) .0347(17) .0218(19) .0009(8) .000 .000 C1 .0357(10) .0354(11) .0283(12) .0014(8) -.0013(8) -.0075(9) C2 .0434(11) .0594(15) .0308(13) -.0019(11) .0009(10) -.0185(11) C3 .039(2) .091(4) .021(2) -.0095(14) .000 .000 C4 .0432(11) .0402(13) .0374(13) .0017(10) .0055(10) -.0107(10) C5 .0435(10) .0331(11) .0381(13) .0000(9) -.0046(10) .0043(9) C6 .040(2) .042(2) .0132(19) -.0105(10) .000 .000 C7 .0414(15) .0376(12) .0516(18) -.0010(8) .0030(13) -.0017(9) C8 .091(3) .0374(13) .059(2) -.0003(12) .043(2) -.0009(11) C9 .154(8) .032(3) .027(3) .0013(19) .000 .000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -2.0727 .6215 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O Nb Cl1 . . 98.733(18) ? O Nb Cl1 . 2 98.733(18) yes Cl1 Nb Cl1 . 2 162.53(4) yes O Nb Cl2 . . 95.782(17) ? Cl1 Nb Cl2 . . 89.113(18) ? Cl1 Nb Cl2 2 . 89.134(17) ? O Nb Cl2 . 2 95.782(17) yes Cl1 Nb Cl2 . 2 89.134(17) ? Cl1 Nb Cl2 2 2 89.113(18) yes Cl2 Nb Cl2 . 2 168.44(3) yes O Nb N1 . . 180.0 ? Cl1 Nb N1 . . 81.267(18) ? Cl1 Nb N1 2 . 81.267(18) yes Cl2 Nb N1 . . 84.218(17) ? Cl2 Nb N1 2 . 84.218(17) yes C1 N1 C1 . 2 117.1(3) ? C1 N1 Nb . . 121.45(17) ? C1 N1 Nb 2 . 121.45(17) ? C4 N2 C4 2_655 . 122.4(4) ? C4 N2 H2A 2_655 . 118.8 ? C4 N2 H2A . . 118.8 ? C7 N3 C7 . 2_655 116.7(4) ? C7 N3 H3A . . 121.7 ? C7 N3 H3A 2_655 . 121.7 ? N1 C1 C2 . . 123.1(3) ? N1 C1 H1 . . 118.5 ? C2 C1 H1 . . 118.5 ? C3 C2 C1 . . 118.4(3) ? C3 C2 H2 . . 120.8 ? C1 C2 H2 . . 120.8 ? C2 C3 C2 2 . 119.8(4) ? C2 C3 H3 2 . 120.1 ? C2 C3 H3 . . 120.1 ? N2 C4 C5 . . 119.8(3) ? N2 C4 H4 . . 120.1 ? C5 C4 H4 . . 120.1 ? C4 C5 C6 . . 119.6(3) ? C4 C5 H5 . . 120.2 ? C6 C5 H5 . . 120.2 ? C5 C6 C5 . 2_655 118.7(4) ? C5 C6 H6 . . 120.6 ? C5 C6 H6 2_655 . 120.6 ? N3 C7 C8 . . 123.8(4) ? N3 C7 H7 . . 118.1 ? C8 C7 H7 . . 118.1 ? C9 C8 C7 . . 117.7(4) ? C9 C8 H8 . . 121.2 ? C7 C8 H8 . . 121.2 ? C8 C9 C8 . 2_655 120.4(6) ? C8 C9 H9 . . 119.8 ? C8 C9 H9 2_655 . 119.8 ? 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 Nb O . 1.706(3) yes Nb Cl1 . 2.3962(5) ? Nb Cl1 2 2.3962(5) yes Nb Cl2 . 2.4037(5) ? Nb Cl2 2 2.4037(5) yes Nb N1 . 2.486(4) yes N1 C1 . 1.338(3) ? N1 C1 2 1.338(3) ? N2 C4 2_655 1.328(3) ? N2 C4 . 1.328(3) ? N2 H2A . .8800 ? N3 C7 . 1.327(4) ? N3 C7 2_655 1.327(4) ? N3 H3A . .8800 ? C1 C2 . 1.382(4) ? C1 H1 . .9500 ? C2 C3 . 1.365(4) ? C2 H2 . .9500 ? C3 C2 2 1.365(4) ? C3 H3 . .9500 ? C4 C5 . 1.371(4) ? C4 H4 . .9500 ? C5 C6 . 1.381(3) ? C5 H5 . .9500 ? C6 C5 2_655 1.381(3) ? C6 H6 . .9500 ? C7 C8 . 1.368(5) ? C7 H7 . .9500 ? C8 C9 . 1.361(6) ? C8 H8 . .9500 ? C9 C8 2_655 1.361(6) ? C9 H9 . .9500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H2A N3 .88 1.88 2.756(5) 180 N3 H3A N2 .88 1.88 2.756(5) 180 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_4 _geom_torsion _geom_torsion_publ_flag Cl1 Nb N1 C1 . . 51.70(10) ? Cl1 Nb N1 C1 2 . -128.30(10) ? Cl2 Nb N1 C1 . . -38.29(10) ? Cl2 Nb N1 C1 2 . 141.71(10) ? Cl1 Nb N1 C1 . 2 -128.30(10) ? Cl1 Nb N1 C1 2 2 51.70(10) yes Cl2 Nb N1 C1 . 2 141.71(10) ? Cl2 Nb N1 C1 2 2 -38.29(10) yes C1 N1 C1 C2 2 . -.46(16) ? Nb N1 C1 C2 . . 179.54(16) ? N1 C1 C2 C3 . . .9(3) ? C1 C2 C3 C2 . 2 -.43(15) ? C4 N2 C4 C5 2_655 . .43(16) ? N2 C4 C5 C6 . . -.9(3) ? C4 C5 C6 C5 . 2_655 .42(16) ? C7 N3 C7 C8 2_655 . -.06(16) ? N3 C7 C8 C9 . . .1(3) ? C7 C8 C9 C8 . 2_655 -.05(14) ? Cl1 Nb N1 C1 . . 51.70(10) ? Cl1 Nb N1 C6 . . -50.738(14) ? loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139058497