#------------------------------------------------------------------------------
#$Date: 2019-11-24 17:09:04 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/79/7237909.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7237909
loop_
_publ_author_name
'Ksiądzyna, Martyna'
'Gągor, Anna'
'Piecha-Bisiorek, Anna'
'Ciżman, Agnieszka'
'Medycki, Wojciech'
'Jakubas, Ryszard'
_publ_section_title
;
 Exploring a hybrid ferroelectric with a 1-D perovskite-like structure:
 bis(pyrrolidinium) pentachloroantimonate(iii)
;
_journal_issue                   33
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10360
_journal_paper_doi               10.1039/C9TC02849H
_journal_volume                  7
_journal_year                    2019
_chemical_formula_sum            'C8 H20 Cl5 N2 Sb'
_chemical_formula_weight         443.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-27 deposited with the CCDC.	2019-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5385(6)
_cell_length_b                   11.0894(5)
_cell_length_c                   17.9031(4)
_cell_measurement_reflns_used    3401
_cell_measurement_temperature    254.99(10)
_cell_measurement_theta_max      24.8040
_cell_measurement_theta_min      3.0000
_cell_volume                     1695.19(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      254.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12609
_diffrn_reflns_point_group_measured_fraction_full 0.795
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.679
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.643
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       needle
_exptl_crystal_F_000             872
_exptl_crystal_preparation       ferroelectric
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1373P)²+1.1179P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1814
_refine_ls_wR_factor_ref         0.1974
_reflns_Friedel_coverage         0.541
_reflns_Friedel_fraction_full    0.578
_reflns_Friedel_fraction_max     0.578
_reflns_number_gt                2240
_reflns_number_total             2743
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9tc02849h3.cif
_cod_data_source_block           Pmn21-trans
_cod_database_code               7237909
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.876
_oxdiff_exptl_absorpt_empirical_full_max 1.338
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sb1 Sb 0.000000 -0.42274(14) 0.4930(9) 0.0901(5) Uani 1 2 d S T P
Sb2 Sb -0.500000 -0.11229(14) 0.3563(9) 0.0889(5) Uani 1 2 d S T P
Cl10 Cl 0.1993(8) -0.5366(6) 0.5562(10) 0.154(2) Uani 1 1 d . . .
Cl12 Cl -0.7004(7) 0.0115(6) 0.3006(9) 0.141(2) Uani 1 1 d . . .
Cl21 Cl -0.500000 -0.2464(8) 0.2462(10) 0.137(3) Uani 1 2 d S T P
Cl20 Cl 0.000000 -0.2700(9) 0.5962(10) 0.150(3) Uani 1 2 d S T P
Cl30 Cl 0.000000 -0.6030(13) 0.3851(11) 0.236(8) Uani 1 2 d S T P
Cl31 Cl 0.500000 1.0392(9) -0.5102(11) 0.190(5) Uani 1 2 d S T P
Cl40 Cl -0.2512(8) -0.2731(7) 0.4160(9) 0.155(2) Uani 1 1 d . . .
N10 N 0.047(2) -0.246(2) 0.2781(16) 0.082(6) Uiso 0.5 1 d D . P
C20 C -0.034(8) -0.178(5) 0.220(3) 0.19(3) Uiso 0.5 1 d D . P
C30 C 0.00(3) -0.244(4) 0.153(3) 0.173(16) Uiso 1 2 d D . P
C40 C -0.03(2) -0.360(8) 0.186(6) 0.33(6) Uiso 0.5 1 d D . P
C50 C -0.051(10) -0.351(6) 0.266(5) 0.26(4) Uiso 0.5 1 d D . P
C21 C 0.542(4) 0.6946(19) -0.4022(12) 0.150(7) Uiso 0.5 1 d D . P
C31 C 0.573(4) 0.699(2) -0.3226(11) 0.150(7) Uiso 0.5 1 d D . P
C41 C 0.500000 0.813(2) -0.3050(11) 0.150(7) Uiso 1 2 d DS . P
C51 C 0.636(2) 0.854(3) -0.3459(12) 0.150(7) Uiso 0.5 1 d D . P
N11 N 0.591(3) 0.816(2) -0.4203(10) 0.150(7) Uiso 0.5 1 d D . P
N13 N 0.432(5) 0.479(3) 0.3685(14) 0.200(11) Uiso 0.5 1 d D . P
C23 C 0.500000 0.441(3) 0.2980(18) 0.200(11) Uiso 1 2 d DS . P
C33 C 0.597(6) 0.334(3) 0.2934(15) 0.200(11) Uiso 0.5 1 d D . P
C43 C 0.596(6) 0.311(4) 0.3731(14) 0.200(11) Uiso 0.5 1 d D . P
C53 C 0.500000 0.390(3) 0.4184(18) 0.200(11) Uiso 1 2 d DS . P
N12 N 0.096(2) 0.027(3) 0.5055(10) 0.161(8) Uani 0.5 1 d D U P
C22 C 0.000000 0.085(3) 0.4490(8) 0.154(8) Uani 1 2 d DS TU P
C32 C -0.1328(18) 0.125(3) 0.4927(11) 0.153(8) Uani 0.5 1 d D U P
C42 C -0.053(3) 0.164(2) 0.5600(12) 0.156(8) Uani 0.5 1 d D U P
C52 C 0.000000 0.042(2) 0.5717(10) 0.158(8) Uani 1 2 d DS TU P
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
_geom_angle_site_symmetry_1
Cl10 Sb1 Cl10 90.2(4) 4
Cl10 Sb1 Cl20 90.5(3) 4
Cl10 Sb1 Cl20 90.5(3) .
Cl10 Sb1 Cl30 87.1(3) 4
Cl10 Sb1 Cl30 87.1(3) .
Cl20 Sb1 Cl30 176.5(4) .
Cl10 Sb1 Cl40 90.0(2) 4
Cl10 Sb1 Cl40 178.5(2) .
Cl20 Sb1 Cl40 88.0(2) .
Cl30 Sb1 Cl40 94.4(3) .
Cl12 Sb2 Cl12 90.5(3) 4_455
Cl12 Sb2 Cl21 90.7(2) 4_455
Cl12 Sb2 Cl21 90.7(2) .
Cl12 Sb2 Cl40 89.0(2) 4_455
Cl12 Sb2 Cl40 176.4(2) .
Cl21 Sb2 Cl40 85.7(2) .
Cl12 Sb2 Cl31 25.19(17) 4_455
Cl12 Sb2 Cl31 69.55(16) .
Cl21 Sb2 Cl31 77.58(19) .
Cl40 Sb2 Cl31 109.08(16) .
Sb2 Cl40 Sb1 173.7(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Cl10 2.402(6) 4
Sb1 Cl10 2.402(6) .
Sb1 Cl20 2.506(9) .
Sb1 Cl30 2.780(11) .
Sb1 Cl40 3.043(6) .
Sb2 Cl12 2.409(5) 4_455
Sb2 Cl12 2.409(5) .
Sb2 Cl21 2.469(7) .
Sb2 Cl40 2.972(6) .
N10 C50 1.450(13) .
N10 C20 1.460(13) .
C20 C30 1.449(13) .
C20 C30 1.44(11) 4
C30 C40 1.451(13) .
C30 C40 1.44(11) 4
C40 C50 1.453(13) .
C21 N11 1.4500(13) .
C21 C31 1.4501(13) .
C31 C41 1.4500(13) .
C41 C51 1.4500(13) .
C41 C51 1.4500(13) 4_655
C51 N11 1.4501(13) .
N13 C53 1.4500(13) .
N13 C23 1.4501(13) .
C23 C33 1.4499(13) 4_655
C23 C33 1.4500(13) .
C33 C43 1.4500(13) .
C43 C53 1.4500(13) .
N12 C22 1.4495(13) .
N12 C52 1.4496(13) .
C22 C32 1.4494(13) 4
C22 C32 1.4494(13) .
C32 C42 1.4497(13) .
C42 C52 1.4498(13) .
