#------------------------------------------------------------------------------
#$Date: 2019-11-24 17:09:04 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238738 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/79/7237907.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_7237907
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           62
_space_group_name_Hall           '-P 2bc 2a'
_space_group_name_H-M_alt        'P m n b'
_atom_sites_solution_hydrogens   geom
_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(5)
_cell_length_b                   11.0894(4)
_cell_length_c                   17.9031(7)
_cell_measurement_reflns_used    4574
_cell_measurement_temperature    269.96(16)
_cell_measurement_theta_max      22.2050
_cell_measurement_theta_min      3.2150
_cell_volume                     1695.19(13)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      269.96(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0310
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            14590
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_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  0.86914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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_size_max          0.25
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1720
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0747
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1603P)²+2.5609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2412
_refine_ls_wR_factor_ref         0.2702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1186
_reflns_number_total             1720
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9tc02849h3.cif
_cod_data_source_block           pnma
_cod_database_code               7237907
_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 0.918
_oxdiff_exptl_absorpt_empirical_full_max 1.110
_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, -y+1/2, z+1/2'
'x+1/2, -y, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x-1/2, y, z'
'x-1/2, -y-1/2, z-1/2'
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 0.250000 0.65479(9) -0.56825(5) 0.1052(6) Uani 1 2 d S T P
Cl1 Cl 0.0502(5) 0.7746(4) -0.6275(3) 0.1649(15) Uani 1 1 d . . .
Cl2 Cl 0.250000 0.5111(5) -0.6754(3) 0.165(2) Uani 1 2 d S T P
Cl3 Cl 0.250000 0.8129(10) -0.4455(5) 0.274(6) Uani 1 2 d S T P
Cl4 Cl 0.000000 0.500000 -0.500000 0.186(2) Uani 1 2 d S . P
C1 C 0.250000 0.5157(17) -0.2254(12) 0.292(9) Uani 1 2 d DS TU P
H11 H 0.158129 0.509106 -0.193741 0.351 Uiso 0.5 1 calc R U P
H12 H 0.341871 0.509107 -0.193741 0.351 Uiso 0.5 1 calc R U P
C2 C 0.250000 0.6324(19) -0.2619(10) 0.296(9) Uani 1 2 d DS TU P
H21 H 0.342128 0.677824 -0.247272 0.355 Uiso 0.5 1 calc R U P
H22 H 0.157872 0.677823 -0.247272 0.355 Uiso 0.5 1 calc R U P
C3 C 0.250000 0.6132(17) -0.3420(10) 0.297(9) Uani 1 2 d DS TU P
H31 H 0.157494 0.648070 -0.364852 0.357 Uiso 0.5 1 calc R U P
H32 H 0.342506 0.648071 -0.364852 0.357 Uiso 0.5 1 calc R U P
N4 N 0.250000 0.4830(17) -0.3491(11) 0.294(9) Uani 1 2 d DS TU P
H41 H 0.334077 0.461114 -0.375199 0.353 Uiso 0.5 1 calc R U P
H42 H 0.165923 0.461114 -0.375199 0.353 Uiso 0.5 1 calc R U P
C5 C 0.250000 0.4177(19) -0.2790(10) 0.294(9) Uani 1 2 d DS TU P
H51 H 0.342663 0.367753 -0.273916 0.352 Uiso 0.5 1 calc R U P
H52 H 0.157337 0.367753 -0.273916 0.352 Uiso 0.5 1 calc R U P
C11 C -0.250000 0.801(2) -0.3553(8) 0.222(8) Uani 1 2 d DS TU P
H111 H -0.318692 0.739230 -0.335077 0.267 Uiso 0.5 1 calc R U P
H112 H -0.169821 0.818601 -0.318501 0.267 Uiso 0.5 1 calc R U P
N21 N -0.179(3) 0.759(2) -0.4241(9) 0.221(8) Uani 0.5 1 d D U P
H211 H -0.075843 0.771877 -0.423128 0.266 Uiso 0.5 1 calc R U P
H212 H -0.195396 0.680328 -0.429955 0.266 Uiso 0.5 1 calc R U P
C31 C -0.250000 0.8260(19) -0.4848(7) 0.214(8) Uani 1 2 d DS TU P
H311 H -0.169428 0.861999 -0.515779 0.257 Uiso 0.5 1 calc R U P
H312 H -0.312166 0.772307 -0.515625 0.257 Uiso 0.5 1 calc R U P
C41 C -0.349(4) 0.919(2) -0.4532(9) 0.212(8) Uani 0.5 1 d D U P
H411 H -0.313031 0.998246 -0.469086 0.255 Uiso 0.5 1 calc R U P
H412 H -0.456221 0.908750 -0.469475 0.255 Uiso 0.5 1 calc R U P
C51 C -0.339(3) 0.909(2) -0.3726(9) 0.216(8) Uani 0.5 1 d D U P
H511 H -0.286818 0.979058 -0.351822 0.259 Uiso 0.5 1 calc R U P
H512 H -0.442771 0.903440 -0.351151 0.259 Uiso 0.5 1 calc R U 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
_geom_angle_site_symmetry_3
Cl1 Sb1 Cl1 90.2(2) . 7_655
Cl1 Sb1 Cl2 90.79(16) . .
Cl1 Sb1 Cl2 90.79(16) 7_655 .
Cl1 Sb1 Cl3 90.0(2) . .
Cl1 Sb1 Cl3 90.0(2) 7_655 .
Cl2 Sb1 Cl3 178.9(3) . .
Cl1 Sb1 Cl4 89.49(11) . .
Cl1 Sb1 Cl4 177.77(13) 7_655 .
Cl2 Sb1 Cl4 87.00(10) . .
Cl3 Sb1 Cl4 92.21(19) . .
Cl1 Sb1 Cl4 177.77(13) . 3_564
Cl1 Sb1 Cl4 89.49(11) 7_655 3_564
Cl2 Sb1 Cl4 87.00(10) . 3_564
Cl3 Sb1 Cl4 92.21(19) . 3_564
Cl4 Sb1 Cl4 90.75(2) . 3_564
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Cl1 2.408(3) .
Sb1 Cl1 2.408(3) 7_655
Sb1 Cl2 2.494(5) .
Sb1 Cl3 2.811(7) .
Sb1 Cl4 2.9994(6) .
Sb1 Cl4 2.9994(6) 3_564
Cl1 H511 21.84(2) 1_464
Cl4 H412 26.456(14) 1_464
Cl4 H412 26.456(15) 5_655
C1 C2 1.4499(10) .
C1 C5 1.4499(10) .
C1 H11 0.9700 .
C1 H12 0.9700 .
C2 C3 1.4500(10) .
C2 H21 0.9700 .
C2 H22 0.9700 .
C2 H21 10.35(3) 5_665
C2 H21 10.35(3) 3_465
C3 N4 1.4499(10) .
C3 H31 0.9700 .
C3 H32 0.9700 .
N4 C5 1.4499(10) .
N4 H41 0.8900 .
N4 H42 0.8900 .
C5 H51 0.9700 .
C5 H52 0.9700 .
C11 C51 1.4501(10) .
C11 N21 1.4504(10) .
C11 H111 0.9700 .
C11 H112 0.9700 .
N21 C31 1.4502(10) .
N21 H211 0.8900 .
N21 H212 0.8900 .
N21 H311 24.560(2) 1_464
C31 C41 1.4501(10) .
C31 H311 0.9700 .
C31 H312 0.9700 .
C31 H311 23.1155 1_464
C31 H311 23.1155 7_664
C41 C51 1.4501(10) .
C41 H411 0.9700 .
C41 H412 0.9700 .
C51 H511 0.9700 .
C51 H512 0.9700 .
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
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H41 Cl4 0.89 2.68 3.448(15) 145.0 3_564 yes
N4 H42 Cl4 0.89 2.68 3.448(15) 145.0 . yes
N21 H211 Cl3 0.89 2.85 3.73(3) 170.8 . yes
N21 H212 Cl4 0.89 2.89 3.525(15) 129.6 . yes
N21 H212 Cl2 0.89 2.88 3.54(3) 132.2 5_564 yes
