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#$Date: 2019-11-24 00:30:49 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235772 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349729.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_4349729
loop_
_publ_author_name
'Piecha-Bisiorek, Anna'
'Gągor, Anna'
'Jakubas, Ryszard'
'Ciżman, Agnieszka'
'Janicki, Rafał'
'Medycki, Wojciech'
_publ_section_title
;
 Ferroelectricity in bis(ethylammonium) pentachlorobismuthate(iii):
 synthesis, structure, polar and spectroscopic properties
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1281
_journal_paper_doi               10.1039/C7QI00254H
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C4 H16 Bi Cl5 N2'
_chemical_formula_weight         478.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-A 2 2ab'
_space_group_name_H-M_alt        'A e a m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-09 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.8318(2)
_cell_length_b                   21.9673(8)
_cell_length_c                   7.5656(4)
_cell_measurement_reflns_used    11166
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.5680
_cell_measurement_theta_min      3.0460
_cell_volume                     2963.57(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3456
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            32217
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         2.943
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.145
_exptl_crystal_description       prism
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2229
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0335P)²+4P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1917
_reflns_number_total             2229
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00254h2.cif
_cod_data_source_block           PhaseI
_cod_original_sg_symbol_H-M      Acam
_cod_database_code               4349729
_shelx_shelxl_version_number     2014/7
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x-1/2, -y, z+1/2'
'-x-1/2, y, 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
Bi1 Bi 0.63354(2) 0.13566(2) 0.0000 0.04449(9) Uani 1 2 d S T P
Cl1 Cl 0.53802(9) 0.12052(7) 0.25187(19) 0.0863(4) Uani 1 1 d . . .
Cl2 Cl 0.59715(14) 0.25380(9) 0.0000 0.0907(6) Uani 1 2 d S T P
Cl3 Cl 0.66899(12) 0.01674(9) 0.0000 0.1038(8) Uani 1 2 d S T P
Cl4 Cl 0.7500 0.15497(15) -0.2500 0.1364(12) Uani 1 2 d S T P
N1B N 0.3504(4) -0.0312(3) 0.5000 0.086(2) Uani 0.5 2 d DS TU P
H1 H 0.3114 -0.0233 0.4303 0.129 Uiso 0.25 1 calc R U P
H2 H 0.3344 -0.0486 0.5993 0.129 Uiso 0.25 1 calc R U P
H3 H 0.3818 -0.0562 0.4446 0.129 Uiso 0.25 1 calc R U P
N11B N 0.3504(4) -0.0312(3) 0.5000 0.086(2) Uani 0.5 2 d S T P
H4 H 0.3806 -0.0551 0.5627 0.129 Uiso 0.25 1 calc R U P
H5 H 0.3375 -0.0500 0.4004 0.129 Uiso 0.25 1 calc R U P
H6 H 0.3094 -0.0230 0.5627 0.129 Uiso 0.25 1 calc R U P
C1B C 0.3893(7) 0.0258(4) 0.543(2) 0.102(4) Uani 0.5 1 d D U P
H7 H 0.4414 0.0233 0.5060 0.122 Uiso 0.5 1 calc R U P
H8 H 0.3880 0.0329 0.6690 0.122 Uiso 0.5 1 calc R U P
C2B C 0.3515(7) 0.0771(5) 0.448(2) 0.108(5) Uani 0.5 1 d D U P
H9 H 0.3258 0.0616 0.3461 0.162 Uiso 0.5 1 calc R U P
H10 H 0.3883 0.1064 0.4119 0.162 Uiso 0.5 1 calc R U P
H11 H 0.3160 0.0962 0.5260 0.162 Uiso 0.5 1 calc R U P
N1A N 0.4097(7) 0.2567(5) 0.0000 0.146(3) Uani 0.5 2 d DS TU P
H12 H 0.4469 0.2507 -0.0766 0.219 Uiso 0.25 1 calc R U P
H13 H 0.4265 0.2783 0.0913 0.219 Uiso 0.25 1 calc R U P
H14 H 0.3727 0.2768 -0.0529 0.219 Uiso 0.25 1 calc R U P
N11A N 0.4097(7) 0.2567(5) 0.0000 0.146(3) Uani 0.5 2 d S T P
H15 H 0.4242 0.2791 -0.0919 0.219 Uiso 0.25 1 calc R U P
H16 H 0.4485 0.2507 0.0720 0.219 Uiso 0.25 1 calc R U P
H17 H 0.3734 0.2760 0.0581 0.219 Uiso 0.25 1 calc R U P
C1A C 0.3830(8) 0.2004(7) 0.060(3) 0.153(4) Uani 0.5 1 d D U P
H18 H 0.3804 0.2027 0.1880 0.183 Uiso 0.5 1 calc R U P
H19 H 0.4209 0.1703 0.0317 0.183 Uiso 0.5 1 calc R U P
C2A C 0.3128(7) 0.1769(7) 0.0000 0.159(4) Uani 0.5 2 d DS TU P
H20 H 0.2869 0.2077 -0.0662 0.238 Uiso 0.25 1 calc R U P
H21 H 0.2829 0.1652 0.0999 0.238 Uiso 0.25 1 calc R U P
H22 H 0.3214 0.1421 -0.0741 0.238 Uiso 0.25 1 calc R U P
C21A C 0.3128(7) 0.1769(7) 0.0000 0.159(4) Uani 0.5 2 d S T P
H23 H 0.2738 0.2058 -0.0252 0.238 Uiso 0.25 1 calc R U P
H24 H 0.3151 0.1699 0.1251 0.238 Uiso 0.25 1 calc R U P
H25 H 0.3022 0.1393 -0.0596 0.238 Uiso 0.25 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'
Bi Bi -4.1077 10.2566 '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 Bi1 Cl1 95.35(8) . 10
Cl1 Bi1 Cl2 87.99(5) . .
Cl1 Bi1 Cl2 87.99(5) 10 .
Cl1 Bi1 Cl3 91.72(5) . .
Cl1 Bi1 Cl3 91.72(5) 10 .
Cl2 Bi1 Cl3 179.57(7) . .
Cl1 Bi1 Cl4 90.58(4) . 10
Cl1 Bi1 Cl4 174.06(4) 10 10
Cl2 Bi1 Cl4 91.86(8) . 10
Cl3 Bi1 Cl4 88.46(7) . 10
Cl1 Bi1 Cl4 174.06(4) . .
Cl1 Bi1 Cl4 90.58(4) 10 .
Cl2 Bi1 Cl4 91.86(8) . .
Cl3 Bi1 Cl4 88.46(7) . .
Cl4 Bi1 Cl4 83.487(19) 10 .
Bi1 Cl4 Bi1 162.82(13) . 7_644
C1B N1B H1 109.5 . .
C1B N1B H2 109.5 . .
H1 N1B H2 109.5 . .
C1B N1B H3 109.5 . .
H1 N1B H3 109.5 . .
H2 N1B H3 109.5 . .
N1B C1B C2B 109.0(9) . .
N1B C1B H7 109.9 . .
C2B C1B H7 109.9 . .
N1B C1B H8 109.9 . .
C2B C1B H8 109.9 . .
H7 C1B H8 108.3 . .
C1B C2B H9 109.5 . .
C1B C2B H10 109.5 . .
H9 C2B H10 109.5 . .
C1B C2B H11 109.5 . .
H9 C2B H11 109.5 . .
H10 C2B H11 109.5 . .
C1A N1A H12 109.5 . .
C1A N1A H13 109.5 . .
H12 N1A H13 109.5 . .
C1A N1A H14 109.5 . .
H12 N1A H14 109.5 . .
H13 N1A H14 109.5 . .
N1A C1A C2A 120.9(14) . .
N1A C1A H18 107.1 . .
C2A C1A H18 107.1 . .
N1A C1A H19 107.1 . .
C2A C1A H19 107.1 . .
H18 C1A H19 106.8 . .
C1A C2A H20 109.5 . .
C1A C2A H21 109.5 . .
H20 C2A H21 109.5 . .
C1A C2A H22 109.5 . .
H20 C2A H22 109.5 . .
H21 C2A H22 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Cl1 2.5774(12) .
Bi1 Cl1 2.5774(12) 10
Bi1 Cl2 2.6752(19) .
Bi1 Cl3 2.6878(19) .
Bi1 Cl4 2.8408(5) 10
Bi1 Cl4 2.8408(5) .
Cl4 Bi1 2.8408(5) 7_644
N1B C1B 1.468(8) .
N1B H1 0.8900 .
N1B H2 0.8900 .
N1B H3 0.8900 .
C1B C2B 1.494(9) .
C1B H7 0.9700 .
C1B H8 0.9700 .
C2B H9 0.9600 .
C2B H10 0.9600 .
C2B H11 0.9600 .
N1A C1A 1.401(9) .
N1A H12 0.8900 .
N1A H13 0.8900 .
N1A H14 0.8900 .
C1A C2A 1.428(9) .
C1A H18 0.9700 .
C1A H19 0.9700 .
C2A H20 0.9600 .
C2A H21 0.9600 .
C2A H22 0.9600 .
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
N1B H6 Cl3 0.89 2.55 3.250(7) 135.9 15
N1B H3 Cl1 0.89 2.48 3.367(6) 172.1 2_655
N1A H16 Cl2 0.89 2.71 3.343(12) 129.4 .
N1A H13 Cl1 0.89 2.60 3.416(8) 153.2 13_655
