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#$Date: 2016-09-10 01:19:59 +0200 (Sat 10 de Sep de 2016) $
#$Revision: 186362 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/57/7225713.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_7225713
loop_
_publ_author_name
'Wojciechowska, Martyna'
'Szklarz, Przemysław'
'Białońska, Agata'
'Baran, Jan'
'Janicki, Rafał'
'Medycki, Wojciech'
'Durlak, Piotr'
'Piecha-Bisiorek, Anna'
'Jakubas, Ryszard'
_publ_section_title
;
 Enormous lattice distortion through an isomorphous phase transition in an
 organic--inorganic hybrid based on haloantimonate(iii)
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              6184
_journal_paper_doi               10.1039/C6CE01008C
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C8 H20 N, Br4 Sb'
_chemical_formula_sum            'C8 H20 Br4 N Sb'
_chemical_formula_weight         571.64
_chemical_name_systematic
;
Bis(diisobutylammonium) octabromodiantimonate(III)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2016-04-20 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.32(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.046(2)
_cell_length_b                   18.186(3)
_cell_length_c                   14.839(3)
_cell_measurement_reflns_used    11923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.8817
_cell_measurement_theta_min      2.9750
_cell_volume                     1621.7(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3359
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.779
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.779
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21768
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.779
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         36.972
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.530
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.077
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28c (release 15-05-2013 CrysAlis171 .NET)
(compiled May 15 2013,09:16:53)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.359
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         6414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0325
_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)+(0.0387P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4633
_reflns_number_total             6414
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6ce01008c3.cif
_cod_data_source_block           SbBrDIBA100K
_cod_depositor_comments
'Adding full bibliography for 7225712--7225715.cif.'
_cod_database_code               7225713
_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.
;
_shelx_estimated_absorpt_t_min   0.069
_shelx_estimated_absorpt_t_max   0.231
_shelxl_version_number           2014-3
_solvent_exptl_crystal_recrystallization_method water
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Sb Sb 0.48461(3) 0.59610(2) 0.11203(2) 0.01299(5) Uani 1 1 d . .
Br1 Br 0.08094(5) 0.55957(2) 0.10983(2) 0.01968(7) Uani 1 1 d . .
Br2 Br 0.58887(5) 0.43330(2) 0.10982(2) 0.01498(7) Uani 1 1 d . .
Br3 Br 0.38888(6) 0.73622(2) 0.11832(2) 0.02096(7) Uani 1 1 d . .
Br4 Br 0.56745(5) 0.59120(2) 0.28344(2) 0.01981(7) Uani 1 1 d . .
N N 0.1273(4) 0.37722(13) 0.20212(18) 0.0162(5) Uani 1 1 d . .
H1 H 0.0015 0.4047 0.1906 0.019 Uiso 1 1 calc R U
H2 H 0.2127 0.3853 0.1563 0.019 Uiso 1 1 calc R U
C1 C 0.0632(5) 0.29781(16) 0.2013(2) 0.0179(6) Uani 1 1 d . .
H1A H -0.0584 0.2907 0.2401 0.021 Uiso 1 1 calc R U
H1B H 0.1923 0.2682 0.2272 0.021 Uiso 1 1 calc R U
C2 C -0.0131(5) 0.27075(16) 0.1057(2) 0.0173(6) Uani 1 1 d . .
H2A H -0.1283 0.3055 0.0772 0.021 Uiso 1 1 calc R U
C3 C 0.1773(6) 0.26822(19) 0.0474(2) 0.0265(7) Uani 1 1 d . .
H3A H 0.2483 0.3167 0.0474 0.040 Uiso 1 1 calc R U
H3B H 0.1200 0.2548 -0.0147 0.040 Uiso 1 1 calc R U
H3C H 0.2866 0.2316 0.0719 0.040 Uiso 1 1 calc R U
C4 C -0.1207(6) 0.19519(18) 0.1127(3) 0.0266(7) Uani 1 1 d . .
H4A H -0.1773 0.1779 0.0520 0.040 Uiso 1 1 calc R U
H4B H -0.2440 0.1989 0.1502 0.040 Uiso 1 1 calc R U
H4C H -0.0098 0.1603 0.1405 0.040 Uiso 1 1 calc R U
C5 C 0.2529(5) 0.40357(16) 0.2897(2) 0.0177(6) Uani 1 1 d . .
H5A H 0.3957 0.3766 0.2996 0.021 Uiso 1 1 calc R U
H5B H 0.2882 0.4563 0.2833 0.021 Uiso 1 1 calc R U
C6 C 0.1321(5) 0.39424(16) 0.3720(2) 0.0166(6) Uani 1 1 d . .
H6A H 0.1012 0.3407 0.3796 0.020 Uiso 1 1 calc R U
C7 C 0.2845(6) 0.42028(19) 0.4548(2) 0.0242(7) Uani 1 1 d . .
H7A H 0.4211 0.3908 0.4610 0.036 Uiso 1 1 calc R U
H7B H 0.2081 0.4146 0.5093 0.036 Uiso 1 1 calc R U
H7C H 0.3221 0.4722 0.4472 0.036 Uiso 1 1 calc R U
C8 C -0.0874(6) 0.4353(2) 0.3641(3) 0.0321(9) Uani 1 1 d . .
H8A H -0.0610 0.4875 0.3531 0.048 Uiso 1 1 calc R U
H8B H -0.1562 0.4297 0.4205 0.048 Uiso 1 1 calc R U
H8C H -0.1868 0.4151 0.3135 0.048 Uiso 1 1 calc R U
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'
Br Br -0.2901 2.4595 '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
Br1 Sb Br4 95.02(2) . .
Br1 Sb Br3 92.254(16) . .
Br4 Sb Br3 91.057(12) . .
Br1 Sb Br2 86.831(14) . .
Br4 Sb Br2 87.603(11) . .
Br3 Sb Br2 178.305(13) . .
Br1 Sb Br2 85.48(2) . 3_665
Br4 Sb Br2 168.169(11) . 3_665
Br3 Sb Br2 100.741(12) . 3_665
Br2 Sb Br2 80.616(11) . 3_665
Br1 Sb Br1 154.295(16) . 1_655
Br4 Sb Br1 85.23(2) . 1_655
Br3 Sb Br1 113.449(11) . 1_655
Br2 Sb Br1 67.482(8) . 1_655
Br2 Sb Br1 89.22(2) 3_665 1_655
C1 N C5 114.8(2) . .
C1 N H1 108.6 . .
C5 N H1 108.6 . .
C1 N H2 108.6 . .
C5 N H2 108.6 . .
H1 N H2 107.6 . .
N C1 C2 111.8(2) . .
N C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
N C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
C3 C2 C1 111.7(3) . .
C3 C2 C4 111.5(3) . .
C1 C2 C4 108.3(3) . .
C3 C2 H2A 108.4 . .
C1 C2 H2A 108.4 . .
C4 C2 H2A 108.4 . .
C2 C3 H3A 109.5 . .
C2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 N 114.9(3) . .
C6 C5 H5A 108.5 . .
N C5 H5A 108.5 . .
C6 C5 H5B 108.5 . .
N C5 H5B 108.5 . .
H5A C5 H5B 107.5 . .
C5 C6 C8 112.4(3) . .
C5 C6 C7 108.4(3) . .
C8 C6 C7 110.8(3) . .
C5 C6 H6A 108.4 . .
C8 C6 H6A 108.4 . .
C7 C6 H6A 108.4 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb Br1 2.5261(9) .
Sb Br4 2.5393(7) .
Sb Br3 2.6170(5) .
Sb Br2 3.0280(6) .
Sb Br2 3.3163(8) 3_665
Sb Br1 3.6698(12) 1_655
N C1 1.495(4) .
N C5 1.509(4) .
N H1 0.9100 .
N H2 0.9100 .
C1 C2 1.524(4) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.515(5) .
C2 C4 1.529(4) .
C2 H2A 1.0000 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.500(4) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C8 1.515(5) .
C6 C7 1.528(4) .
C6 H6A 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
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
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455
N H2 Br2 0.91 2.60 3.398(3) 146.9 .
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455
N H2 Br2 0.91 2.60 3.398(3) 146.9 .
N H1 Br2 0.91 2.70 3.540(3) 154.5 1_455
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N C1 C2 -166.7(3)
N C1 C2 C3 68.5(3)
N C1 C2 C4 -168.2(3)
C1 N C5 C6 -58.7(3)
N C5 C6 C8 -59.6(3)
N C5 C6 C7 177.6(2)
