#------------------------------------------------------------------------------
#$Date: 2016-02-20 01:53:41 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105069.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_2105069
loop_
_publ_author_name
'Małuszyńska, Hanna'
'Czarnecki, Piotr'
'Czarnecka, Anna'
'Pajak, Zdzisław'
_publ_section_title
;
 Structures and phase transitions in a new ferroelectric -- pyridinium
 chlorochromate -- studied by X-ray diffraction, DSC and dielectric
 methods
;
_journal_coeditor_code           EB5013
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              128
_journal_page_last               136
_journal_paper_doi               10.1107/S0108768112005782
_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           166
_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                   9.021(2)
_cell_length_b                   9.021(2)
_cell_length_c                   9.369(4)
_cell_measurement_reflns_used    175
_cell_measurement_temperature    355.0(2)
_cell_measurement_theta_max      32.7751
_cell_measurement_theta_min      3.3750
_cell_volume                     660.3(3)
_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      355.0(2)
_diffrn_detector_area_resol_mean 10.3200
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 0.932
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1606
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.83
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.750
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.750
_refine_ls_R_factor_all          0.3315
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.897
_refine_ls_shift/su_mean         0.317
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1210P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1673
_refine_ls_wR_factor_ref         0.2681
_reflns_number_gt                44
_reflns_number_total             305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            eb5013.cif
_cod_data_source_block           r-3m
_cod_original_cell_volume        660.2(4)
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               2105069
_cod_database_fobs_code          2105069
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'
'-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 0.046(2) 0.247(15) Uani d SP 0.50 6
O O -0.0908(11) -0.182(2) 0.103(2) 0.291(7) Uani d SP 0.50 2
Cl Cl 0.0000 0.0000 0.157(4) 0.58(6) Uani d SP 0.50 6
C C 0.0000 0.1477(7) 0.5000 0.213(4) Uani d SP 0.83 2
N N 0.0000 0.1477(7) 0.5000 0.213(4) Uani d SP 0.17 2
H H0A 0.0000 0.2508 0.5000 0.255 Uiso d SR 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
Cr1 0.184(3) 0.184(3) 0.37(5) 0.0922(16) 0.000 0.000
O 0.334(15) 0.201(15) 0.295(19) 0.101(8) 0.011(5) 0.022(10)
Cl 0.75(8) 0.75(8) 0.25(2) 0.38(4) 0.000 0.000
C 0.259(8) 0.205(5) 0.193(6) 0.129(4) -0.002(4) -0.0012(19)
N 0.259(8) 0.205(5) 0.193(6) 0.129(4) -0.002(4) -0.0012(19)
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
Cr1 Cr1 Cl 19 . 180.0000(10)
Cr1 Cr1 O 19 2 110.5(11)
Cl Cr1 O . 2 69.5(11)
Cr1 Cr1 O 19 . 110.5(11)
Cl Cr1 O . . 69.5(11)
O Cr1 O 2 . 108.5(12)
Cr1 Cr1 O 19 3 110.5(11)
Cl Cr1 O . 3 69.5(11)
O Cr1 O 2 3 108.5(12)
O Cr1 O . 3 108.5(12)
Cr1 Cr1 Cl 19 19 0.0000(10)
Cl Cr1 Cl . 19 180.0000(10)
O Cr1 Cl 2 19 110.5(11)
O Cr1 Cl . 19 110.5(11)
O Cr1 Cl 3 19 110.5(11)
Cr1 Cr1 O 19 21 45.5(5)
Cl Cr1 O . 21 134.5(5)
O Cr1 O 2 21 84.9(10)
O Cr1 O . 21 84.9(10)
O Cr1 O 3 21 156.0(12)
Cl Cr1 O 19 21 45.5(5)
Cr1 Cr1 O 19 20 45.5(5)
Cl Cr1 O . 20 134.5(5)
O Cr1 O 2 20 156.0(12)
O Cr1 O . 20 84.9(10)
O Cr1 O 3 20 84.9(10)
Cl Cr1 O 19 20 45.5(5)
O Cr1 O 21 20 76.3(8)
Cr1 Cr1 O 19 19 45.5(5)
Cl Cr1 O . 19 134.5(5)
O Cr1 O 2 19 84.9(10)
O Cr1 O . 19 156.0(12)
O Cr1 O 3 19 84.9(10)
Cl Cr1 O 19 19 45.5(5)
O Cr1 O 21 19 76.3(8)
O Cr1 O 20 19 76.3(8)
Cl O Cr1 . . 40.2(14)
Cl O Cr1 . 19 64(2)
Cr1 O Cr1 . 19 24.0(12)
Cr1 Cl O . . 70.3(19)
Cr1 Cl O . 2 70.3(19)
O Cl O . 2 109.2(19)
Cr1 Cl O . 3 70.3(19)
O Cl O . 3 109.2(19)
O Cl O 2 3 109.2(19)
Cr1 Cl Cr1 . 19 0.0000(10)
O Cl Cr1 . 19 70.3(19)
O Cl Cr1 2 19 70.3(19)
O Cl Cr1 3 19 70.3(19)
N C C 21_556 21_556 0.0(4)
N C C 21_556 20_556 120.000(2)
C C C 21_556 20_556 120.000(2)
N C N 21_556 20_556 120.000(2)
C C N 21_556 20_556 120.000(2)
C C N 20_556 20_556 0.0(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cr1 Cr1 19 0.87(4)
Cr1 Cl . 1.04(3)
Cr1 O 2 1.52(2)
Cr1 O . 1.52(2)
Cr1 O 3 1.52(2)
Cr1 Cl 19 1.91(5)
Cr1 O 21 1.99(2)
Cr1 O 20 1.99(2)
Cr1 O 19 1.99(2)
O Cl . 1.511(18)
O Cr1 19 1.99(2)
Cl O 2 1.511(18)
Cl O 3 1.511(18)
Cl Cr1 19 1.91(5)
C N 21_556 1.332(6)
C C 21_556 1.332(6)
C C 20_556 1.332(6)
C N 20_556 1.332(6)
