#------------------------------------------------------------------------------
#$Date: 2017-11-07 03:04:18 +0200 (Tue, 07 Nov 2017) $
#$Revision: 202763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/76/1547658.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_1547658
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 Br5 N2'
_chemical_formula_weight         698.65
_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   mixed
_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                   17.899(14)
_cell_length_b                   7.930(6)
_cell_length_c                   10.381(8)
_cell_measurement_reflns_used    1814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.500
_cell_measurement_theta_min      3.005
_cell_volume                     1473(2)
_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 0.996
_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  0.1022
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.005
_exptl_absorpt_coefficient_mu    25.480
_exptl_absorpt_correction_T_max  0.0001
_exptl_absorpt_correction_T_min  0
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    3.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240.0
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.0069(4)
_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   1.176
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         1807
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0461P)²+3.9348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1563
_reflns_number_total             1814
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jp7b05126_si_002.cif
_cod_data_source_block           0.00_343K
_cod_depositor_comments
'Adding full bibliography for 1547653--1547662.cif.'
_cod_original_formula_sum        'C4 H14 Bi Br5 N2 '
_cod_database_code               1547658
_publcif_datablock.id            {042bf452-453d-4cba-9d65-ffaeac4625cf}
_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 0.56923(3) 0.7500 0.32275(4) 0.0437(2) Uani 1 2 d S TU P
Br1 Br 0.43995(11) 0.7500 0.16086(18) 0.0825(6) Uani 1 2 d S TU P
Br2 Br 0.62402(9) 1.00544(16) 0.17056(12) 0.0774(4) Uani 1 1 d . U .
Br3 Br 0.70408(10) 0.7500 0.46311(19) 0.0772(6) Uani 1 2 d S TU P
Br4 Br 0.5000 1.0000 0.5000 0.1217(10) Uani 1 2 d S U P
C4 C 0.8093(13) 0.7500 1.060(2) 0.117(8) Uani 1 2 d DS TU P
H4A H 0.8582 0.7953 1.0764 0.175 Uiso 0.5 1 calc R U P
H4B H 0.7725 0.8181 1.1028 0.175 Uiso 0.5 1 calc R U P
H4C H 0.8067 0.6366 1.0922 0.175 Uiso 0.5 1 calc R U P
N2 N 0.7948(12) 0.7500 0.920(2) 0.155(9) Uani 1 2 d DS TU P
H2A H 0.8004 0.6434 0.8920 0.185 Uiso 0.5 1 d R U P
H2B H 0.8316 0.8115 0.8840 0.185 Uiso 0.5 1 d R U P
N1 N 0.5390(12) 0.7500 0.880(3) 0.184(12) Uani 1 2 d DS TU P
H1A H 0.4978 0.7043 0.8475 0.276 Uiso 0.5 1 calc R U P
H1B H 0.5538 0.6902 0.9484 0.276 Uiso 0.5 1 calc R U P
H1C H 0.5295 0.8555 0.9047 0.276 Uiso 0.5 1 calc R U P
C1 C 0.5986(12) 0.7500 0.782(2) 0.136(9) Uani 1 2 d DS TU P
H1D H 0.6082 0.8637 0.7551 0.163 Uiso 0.5 1 d R U P
H1E H 0.5826 0.6871 0.7081 0.163 Uiso 0.5 1 d R U P
C2 C 0.6703(15) 0.672(4) 0.835(4) 0.134(10) Uani 0.5 1 d D U P
H2C H 0.6926 0.6004 0.7714 0.160 Uiso 0.5 1 d R U P
H2D H 0.6595 0.6057 0.9099 0.160 Uiso 0.5 1 d R U P
C3 C 0.7219(14) 0.816(4) 0.875(4) 0.144(11) Uani 0.5 1 d D U P
H3A H 0.7312 0.8832 0.7997 0.173 Uiso 0.5 1 d R U P
H3B H 0.6991 0.8863 0.9386 0.173 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'
Br Br -0.2901 2.4595 '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'
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
Br2 Bi1 Br2 94.90(8) 8_575 .
Br2 Bi1 Br3 89.52(6) 8_575 .
Br2 Bi1 Br3 89.52(6) . .
Br2 Bi1 Br1 87.19(6) 8_575 .
Br2 Bi1 Br1 87.19(6) . .
Br3 Bi1 Br1 175.13(6) . .
Br2 Bi1 Br4 174.14(3) 8_575 .
Br2 Bi1 Br4 90.74(6) . .
Br3 Bi1 Br4 92.12(5) . .
Br1 Bi1 Br4 91.51(6) . .
Br2 Bi1 Br4 90.75(6) 8_575 4_646
Br2 Bi1 Br4 174.14(3) . 4_646
Br3 Bi1 Br4 92.12(5) . 4_646
Br1 Bi1 Br4 91.51(6) . 4_646
Br4 Bi1 Br4 83.57(6) . 4_646
Bi1 Br4 Bi1 180.0 5_676 .
C4 N2 C3 118(2) . 8_575
C4 N2 C3 118(2) . .
C3 N2 C3 41(3) 8_575 .
N1 C1 C2 111(2) . 8_575
N1 C1 C2 111(2) . .
C2 C1 C2 48(3) 8_575 .
C3 C2 C2 85(3) 8_575 8_575
C3 C2 C3 43(4) 8_575 .
C2 C2 C3 41.7(11) 8_575 .
C3 C2 C1 151(5) 8_575 .
C2 C2 C1 66.2(13) 8_575 .
C3 C2 C1 107.9(19) . .
C2 C3 C3 95(3) 8_575 8_575
C2 C3 N2 164(5) 8_575 .
C3 C3 N2 69.5(13) 8_575 .
C2 C3 C2 54(4) 8_575 .
C3 C3 C2 41.7(11) 8_575 .
N2 C3 C2 111(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Br2 2.7497(18) 8_575
Bi1 Br2 2.7497(18) .
Bi1 Br3 2.819(3) .
Bi1 Br1 2.860(2) .
Bi1 Br4 2.9752(14) .
Bi1 Br4 2.9752(14) 4_646
Br4 Bi1 2.9751(14) 5_676
C4 N2 1.477(10) .
N2 C3 1.482(10) 8_575
N2 C3 1.482(10) .
N1 C1 1.477(10) .
C1 C2 1.526(10) 8_575
C1 C2 1.526(10) .
C2 C3 1.02(2) 8_575
C2 C2 1.23(6) 8_575
C2 C3 1.520(10) .
C3 C2 1.02(2) 8_575
C3 C3 1.04(7) 8_575
