#------------------------------------------------------------------------------ #$Date: 2012-05-05 11:34:27 +0100 (Sat, 05 May 2012) $ #$Revision: 55416 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105071.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_2105071 loop_ _publ_author_name 'Ma\/luszy\'nska, Hanna' 'Czarnecki, Piotr' 'Czarnecka, Anna' 'Pajak, Zdzis\/law' _publ_section_title ; Structures and phase transitions in a new ferroelectric -- pyridinium chlorochromate -- studied by X-ray diffraction, DSC and dielectric methods ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 128 _journal_page_last 136 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety '[C5H5 NH]+ [Cl Cr O3]- ' _chemical_formula_sum 'C5 H6 Cl Cr N O3' _chemical_formula_weight 215.56 _chemical_name_systematic ; pyridinium chlorochromate ; _space_group_IT_number 8 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2y' _symmetry_space_group_name_H-M 'C 1 m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.250(9) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.7193(7) _cell_length_b 8.6842(7) _cell_length_c 6.3139(5) _cell_measurement_reflns_used 993 _cell_measurement_temperature 298.0(2) _cell_measurement_theta_max 29.1320 _cell_measurement_theta_min 3.2393 _cell_volume 420.74(6) _computing_cell_refinement 'CrysAlisPro, Oxford Diffraction Ltd., 2010' _computing_data_collection 'CrysAlisPro, Oxford Diffraction Ltd., 2010' _computing_data_reduction 'CrysAlisPro, Oxford Diffraction Ltd., 2010' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 298.0(2) _diffrn_detector_area_resol_mean 10.3200 _diffrn_measured_fraction_theta_full 0.949 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method 'omega scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 2023 _diffrn_reflns_theta_full 28.50 _diffrn_reflns_theta_max 28.98 _diffrn_reflns_theta_min 3.25 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.81872 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.64 (release 22-03-2010 CrysAlis171 .NET) (compiled Mar 22 2010,13:57:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.701 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 216 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.580 _refine_diff_density_min -0.232 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.819 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 884 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 0.818 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0371 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.015 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0816 _refine_ls_wR_factor_ref 0.0877 _reflns_number_gt 571 _reflns_number_total 884 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file eb5013.cif _[local]_cod_data_source_block exp_181 _[local]_cod_cif_authors_sg_H-M Cm _cod_database_code 2105071 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, 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 _atom_site_symmetry_multiplicity Cr Cr 0.67097(4) 0.0000 0.23471(4) 0.0721(3) Uani d S 1 2 Cl Cl 0.8777(4) 0.0000 0.4897(4) 0.1267(8) Uani d S 1 2 C C1 1.2529(7) 0.1547(4) 0.8200(8) 0.0819(13) Uani d . 1 1 H H1A 1.2548 0.2617 0.8216 0.098 Uiso d R 1 1 C C2 1.3249(6) 0.0769(5) 0.6695(8) 0.0845(13) Uani d . 1 1 H H2A 1.3750 0.1305 0.5641 0.101 Uiso d R 1 1 O O1 0.5586(5) 0.1521(4) 0.2549(7) 0.1198(13) Uani d . 1 1 C C3 1.1794(6) 0.0796(6) 0.9676(7) 0.0939(13) Uani d P 0.50 1 N N 1.1794(6) 0.0796(6) 0.9676(7) 0.0939(13) Uani d P 0.50 1 H H3A 1.1274 0.1331 1.0715 0.113 Uiso d R 1 1 O O2 0.7535(9) 0.0000 0.0184(8) 0.1201(17) Uani d S 1 2 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 Cr 0.0762(6) 0.0721(5) 0.0701(6) 0.000 0.0179(4) 0.000 Cl 0.1425(19) 0.1009(13) 0.1220(16) 0.000 -0.0522(14) 0.000 C1 0.081(3) 0.059(2) 0.104(4) -0.009(2) 0.000(3) -0.005(2) C2 0.082(3) 0.087(2) 0.086(3) -0.006(2) 0.018(3) 0.016(2) O1 0.109(3) 0.115(3) 0.137(3) 0.051(2) 0.018(2) 0.003(2) C3 0.078(3) 0.116(3) 0.086(3) 0.008(2) 0.001(2) -0.033(2) N 0.078(3) 0.116(3) 0.086(3) 0.008(2) 0.001(2) -0.033(2) O2 0.159(5) 0.126(4) 0.084(3) 0.000 0.050(4) 0.000 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 O2 Cr O1 . 2 110.23(19) O2 Cr O1 . . 110.23(19) O1 Cr O1 2 . 112.1(3) O2 Cr Cl . . 108.3(3) O1 Cr Cl 2 . 107.92(17) O1 Cr Cl . . 107.92(17) C3 C1 C2 . . 119.9(4) C2 C2 C1 2 . 120.4(3) C1 C3 N . 2 119.7(3) C1 C3 C3 . 2 119.7(3) N C3 C3 2 2 0.0(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cr O2 . 1.568(5) Cr O1 2 1.593(3) Cr O1 . 1.593(3) Cr Cl . 2.140(2) C1 C3 . 1.316(6) C1 C2 . 1.335(6) C2 C2 2 1.336(10) C3 N 2 1.383(11) C3 C3 2 1.383(11) 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 N H3A O1 4_556 0.93 2.29 3.155(6) 155.0 C1 H1A O2 3_556 0.93 2.41 3.250(4) 149.5 C2 H2A O1 1_655 0.93 2.54 3.400(6) 153.8