#------------------------------------------------------------------------------
#$Date: 2017-11-07 03:04:18 +0200 (Tue, 07 Nov 2017) $
#$Revision: 202763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/76/1547661.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_1547661
loop_
_publ_author_name
'Wang, Ya'
'Shi, Chao'
'Han, Xiang-Bin'
_publ_section_title
;
 Mixed Bromine--Chlorine Induced Great Dielectric and Second-Order
 Nonlinear Optical Properties Changes in Phase Transitions Compounds
 [H2mdap][BiBr5(1-x)Cl5x] (x = 0.00--1.00)
;
_journal_issue                   41
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_page_first              23039
_journal_paper_doi               10.1021/acs.jpcc.7b05126
_journal_volume                  121
_journal_year                    2017
_chemical_formula_sum            'C4 H14 Bi Br1.4 Cl3.6 N2'
_chemical_formula_weight         538.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.693(3)
_cell_length_b                   7.6587(11)
_cell_length_c                   10.1094(19)
_cell_measurement_reflns_used    1684
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.457
_cell_measurement_theta_min      2.302
_cell_volume                     1369.9(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku, SCXmini'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9719
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         2.302
_exptl_absorpt_coefficient_mu    17.617
_exptl_absorpt_correction_T_max  0.007
_exptl_absorpt_correction_T_min  0.004
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    2.612
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             980.8
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.899
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.328
_refine_ls_extinction_coef       0.0100(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.277
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         1682
_refine_ls_number_restraints     190
_refine_ls_restrained_S_all      1.232
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0966P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2312
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1355
_reflns_number_total             1684
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp7b05126_si_002.cif
_cod_data_source_block           0.72_373K
_cod_depositor_comments
'Adding full bibliography for 1547653--1547662.cif.'
_cod_original_formula_sum        'C4 H14 Bi Br1.40 Cl3.60 N2'
_cod_database_code               1547661
_publcif_datablock.id            {5c10d2df-c4f0-4327-b32e-db75393fbe2a}
_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+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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
Bi1 Bi 0.06742(5) 0.7500 0.32858(8) 0.0574(5) Uani 1 2 d S TU P
Cl1 Cl -0.0576(3) 0.7500 0.1591(5) 0.0978(19) Uani 0.72 2 d S TU P
Br1 Br -0.0576(3) 0.7500 0.1591(5) 0.0978(19) Uani 0.28 2 d S TU P
Cl2 Cl 0.1227(3) 0.4973(5) 0.1786(3) 0.1028(14) Uani 0.72 1 d . U P
Br2 Br 0.1227(3) 0.4973(5) 0.1786(3) 0.1028(14) Uani 0.28 1 d . U P
Cl3 Cl 0.0000 0.5000 0.5000 0.152(3) Uani 0.72 2 d S U P
Br3 Br 0.0000 0.5000 0.5000 0.152(3) Uani 0.28 2 d S U P
Cl4 Cl 0.2016(3) 0.7500 0.4665(5) 0.0832(14) Uani 0.72 2 d S TU P
Br4 Br 0.2016(3) 0.7500 0.4665(5) 0.0832(14) Uani 0.28 2 d S TU P
N2 N 0.2046(19) 0.2500 0.425(3) 0.151(11) Uani 1 2 d DS TU P
H2D H 0.1814 0.3541 0.4183 0.181 Uiso 0.5 1 d R U P
H2A H 0.1676 0.2005 0.3769 0.181 Uiso 0.5 1 d R U P
N1 N 0.469(2) 0.2500 0.371(4) 0.177(15) Uani 1 2 d DS TU P
H1D H 0.4558 0.3521 0.4081 0.213 Uiso 0.5 1 d R U P
H1A H 0.4702 0.1996 0.4513 0.213 Uiso 0.5 1 d R U P
H1B H 0.5113 0.3004 0.3383 0.213 Uiso 0.5 1 d R U P
C1 C 0.396(2) 0.2500 0.298(4) 0.157(14) Uani 1 2 d DS TU P
H1E H 0.4107 0.1411 0.2579 0.189 Uiso 0.5 1 d R U P
H1C H 0.3968 0.3046 0.2121 0.189 Uiso 0.5 1 d R U P
C3 C 0.266(2) 0.317(7) 0.339(5) 0.153(14) Uani 0.5 1 d D U P
H3A H 0.2880 0.4189 0.3801 0.183 Uiso 0.5 1 d R U P
H3B H 0.2507 0.3466 0.2512 0.183 Uiso 0.5 1 d R U P
C2 C 0.325(2) 0.171(7) 0.357(6) 0.150(14) Uani 0.5 1 d D U P
H2B H 0.3309 0.1230 0.4440 0.180 Uiso 0.5 1 d R U P
H2C H 0.3084 0.0808 0.2981 0.180 Uiso 0.5 1 d R U P
C4 C 0.193(2) 0.2500 0.571(3) 0.137(14) Uani 1 2 d DS TU P
H4A H 0.1455 0.1952 0.5891 0.205 Uiso 0.5 1 d R U P
H4B H 0.2329 0.1867 0.6141 0.205 Uiso 0.5 1 d R U P
H4C H 0.1924 0.3681 0.6025 0.205 Uiso 0.5 1 d 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'
Bi Bi -4.1077 10.2566 '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'
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'
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
Cl2 Bi1 Br2 94.0 . 8_575
Cl2 Bi1 Cl2 94.0(2) . 8_575
Br2 Bi1 Cl2 0.0 8_575 8_575
Cl2 Bi1 Cl4 88.38(14) . .
Br2 Bi1 Cl4 88.38(14) 8_575 .
Cl2 Bi1 Cl4 88.38(14) 8_575 .
Cl2 Bi1 Cl1 86.62(14) . .
Br2 Bi1 Cl1 86.62(14) 8_575 .
Cl2 Bi1 Cl1 86.62(14) 8_575 .
Cl4 Bi1 Cl1 172.66(17) . .
Cl2 Bi1 Br3 175.13(11) . 4_556
Br2 Bi1 Br3 90.67(10) 8_575 4_556
Cl2 Bi1 Br3 90.67(10) 8_575 4_556
Cl4 Bi1 Br3 93.04(9) . 4_556
Cl1 Bi1 Br3 92.38(9) . 4_556
Cl2 Bi1 Cl3 175.13(11) . 4_556
Br2 Bi1 Cl3 90.67(10) 8_575 4_556
Cl2 Bi1 Cl3 90.67(10) 8_575 4_556
Cl4 Bi1 Cl3 93.04(9) . 4_556
Cl1 Bi1 Cl3 92.38(9) . 4_556
Br3 Bi1 Cl3 0.0 4_556 4_556
Cl2 Bi1 Cl3 90.67(10) . .
Br2 Bi1 Cl3 175.13(11) 8_575 .
Cl2 Bi1 Cl3 175.13(11) 8_575 .
Cl4 Bi1 Cl3 93.04(9) . .
Cl1 Bi1 Cl3 92.38(10) . .
Br3 Bi1 Cl3 84.6 4_556 .
Cl3 Bi1 Cl3 84.61(2) 4_556 .
Bi1 Cl3 Bi1 180.0 5_566 .
C4 N2 C3 133(4) . .
C4 N2 C3 133(3) . 8_565
C3 N2 C3 40(4) . 8_565
C4 N2 H2D 90.7 . .
C3 N2 H2D 89.2 . .
C3 N2 H2D 126.8 8_565 .
C4 N2 H2A 115.8 . .
C3 N2 H2A 111.5 . .
C3 N2 H2A 94.3 8_565 .
H2D N2 H2A 90.0 . .
C1 N1 H1D 88.7 . .
C1 N1 H1A 117.8 . .
H1D N1 H1A 90.0 . .
C1 N1 H1B 122.2 . .
H1D N1 H1B 90.0 . .
H1A N1 H1B 120.0 . .
N1 C1 C2 122(4) . .
N1 C1 C2 122(4) . 8_565
C2 C1 C2 46(5) . 8_565
N1 C1 H1E 88.7 . .
C2 C1 H1E 92.5 . .
C2 C1 H1E 136.7 8_565 .
N1 C1 H1C 116.2 . .
C2 C1 H1C 122.2 . .
C2 C1 H1C 101.0 8_565 .
H1E C1 H1C 90.0 . .
C3 C3 C2 95(5) 8_565 8_565
C3 C3 N2 70(2) 8_565 .
C2 C3 N2 131(7) 8_565 .
C3 C3 C2 43(3) 8_565 .
C2 C3 C2 52(6) 8_565 .
N2 C3 C2 100(3) . .
C3 C3 H3A 144.2 8_565 .
C2 C3 H3A 57.9 8_565 .
N2 C3 H3A 108.8 . .
C2 C3 H3A 105.9 . .
C3 C3 H3B 103.5 8_565 .
C2 C3 H3B 115.3 8_565 .
N2 C3 H3B 114.0 . .
C2 C3 H3B 118.5 . .
H3A C3 H3B 108.9 . .
C3 C2 C2 85(5) 8_565 8_565
C3 C2 C1 136(7) 8_565 .
C2 C2 C1 67(2) 8_565 .
C3 C2 C3 42(6) 8_565 .
C2 C2 C3 43(3) 8_565 .
C1 C2 C3 103(3) . .
C3 C2 H2B 107.6 8_565 .
C2 C2 H2B 112.7 8_565 .
C1 C2 H2B 114.7 . .
C3 C2 H2B 117.9 . .
C3 C2 H2C 70.0 8_565 .
C2 C2 H2C 136.3 8_565 .
C1 C2 H2C 106.8 . .
C3 C2 H2C 104.6 . .
H2B C2 H2C 108.9 . .
N2 C4 H4A 108.2 . .
N2 C4 H4B 110.7 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Cl2 2.645(4) .
Bi1 Br2 2.645(4) 8_575
Bi1 Cl2 2.645(4) 8_575
Bi1 Cl4 2.754(5) .
Bi1 Cl1 2.797(5) .
Bi1 Br3 2.8447(6) 4_556
Bi1 Cl3 2.8447(6) 4_556
Bi1 Cl3 2.8447(7) .
Cl3 Bi1 2.8447(7) 5_566
N2 C4 1.487(10) .
N2 C3 1.488(10) .
N2 C3 1.488(10) 8_565
N2 H2D 0.9000 .
N2 H2A 0.9000 .
N1 C1 1.489(10) .
N1 H1D 0.9000 .
N1 H1A 0.9000 .
N1 H1B 0.8999 .
C1 C2 1.527(10) .
C1 C2 1.527(10) 8_565
C1 H1E 0.9600 .
C1 H1C 0.9600 .
C3 C3 1.03(11) 8_565
C3 C2 1.05(6) 8_565
C3 C2 1.529(10) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C2 C3 1.05(6) 8_565
C2 C2 1.20(11) 8_565
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C4 H4A 0.9601 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
