#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105070.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_2105070 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 160 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall 'R 3 -2"' _symmetry_space_group_name_H-M 'R 3 m :H' _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 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 8.8349(12) _cell_length_b 8.8349(12) _cell_length_c 9.3960(16) _cell_measurement_reflns_used 835 _cell_measurement_temperature 320.0(2) _cell_measurement_theta_max 28.9376 _cell_measurement_theta_min 3.4270 _cell_volume 635.15(16) _computing_cell_refinement 'CrysAlis CCD (Oxford Diffraction,2009)' _computing_data_collection 'CrysAlis CCD (Oxford Diffraction,2009)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction,2009)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 320.0(2) _diffrn_detector_area_resol_mean 10.3200 _diffrn_measured_fraction_theta_full 0.952 _diffrn_measured_fraction_theta_max 0.952 _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 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 1845 _diffrn_reflns_theta_full 28.93 _diffrn_reflns_theta_max 28.93 _diffrn_reflns_theta_min 3.43 _exptl_absorpt_coefficient_mu 1.623 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.66703 _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 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 324 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.912 _refine_diff_density_min -0.245 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 22 _refine_ls_number_reflns 401 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.975 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0493 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.004 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.1148 _reflns_number_gt 194 _reflns_number_total 401 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file eb5013.cif _[local]_cod_data_source_block r3m _[local]_cod_cif_authors_sg_H-M R3m _cod_database_code 2105070 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' 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 Cr1 0.0000 0.0000 0.2007 0.1002(7) Uani d S 1 6 Cl Cl 0.0000 0.0000 -0.0245(4) 0.1506(16) Uani d S 1 6 O O1 -0.0980(4) 0.0980(4) 0.2533(6) 0.152(2) Uani d S 1 2 C C 0.0003(7) -0.1504(6) 0.6195(5) 0.1068(14) Uani d P 0.83 1 N N 0.0003(7) -0.1504(6) 0.6195(5) 0.1068(14) Uani d P 0.17 1 H H0A 0.0003 -0.2589 0.6195 0.128 Uiso d R 1 1 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 Cr1 0.0924(8) 0.0924(8) 0.1158(14) 0.0462(4) 0.000 0.000 Cl 0.176(2) 0.176(2) 0.101(2) 0.0878(12) 0.000 0.000 O1 0.162(4) 0.162(4) 0.167(6) 0.108(4) 0.0233(19) -0.0233(19) C 0.142(3) 0.098(3) 0.096(2) 0.071(2) -0.007(2) -0.008(2) N 0.142(3) 0.098(3) 0.096(2) 0.071(2) -0.007(2) -0.008(2) 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 O1 Cr1 O1 3 2 110.7(2) O1 Cr1 O1 3 . 110.7(2) O1 Cr1 O1 2 . 110.7(2) O1 Cr1 Cl 3 . 108.2(2) O1 Cr1 Cl 2 . 108.2(2) O1 Cr1 Cl . . 108.2(2) N C C 5 5 0.0000(10) N C C 5 4 120.000(3) C C C 5 4 120.000(3) N C N 5 4 120.000(3) C C N 5 4 120.000(3) C C N 4 4 0.0(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Cr1 O1 3 1.578(5) Cr1 O1 2 1.578(5) Cr1 O1 . 1.578(5) Cr1 Cl . 2.116(4) C N 5 1.334(10) C C 5 1.334(10) C C 4 1.326(11) C N 4 1.326(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 C H0A O1 9_445 0.96 2.40 3.277(5) 152.7 _cod_database_fobs_code 2105070