#------------------------------------------------------------------------------
#$Date: 2019-11-26 00:16:04 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242138 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/20/4132096.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_4132096
loop_
_publ_author_name
'Connor, Bridget A.'
'Leppert, Linn'
'Smith, Matthew D.'
'Neaton, Jeffrey B.'
'Karunadasa, Hemamala I.'
_publ_section_title
;
 Layered Halide Double Perovskites: Dimensional Reduction of
 Cs₂AgBiBr₆.
;
_journal_issue                   15
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5235
_journal_page_last               5240
_journal_paper_doi               10.1021/jacs.8b01543
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'Ag Bi Br7 Cs, 2(C4 H12 N)'
_chemical_formula_sum            'C8 H24 Ag Bi Br7 Cs N2'
_chemical_formula_weight         1157.42
_chemical_name_systematic
'bis(butylammonium) cesium heptabromoargentobismuthate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.755(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0848(3)
_cell_length_b                   7.9801(3)
_cell_length_c                   19.8422(8)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    298
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.49
_cell_volume                     1253.32(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'PHOTON 100 Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25350
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.411
_diffrn_reflns_theta_max         24.511
_diffrn_reflns_theta_min         2.474
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.750
_exptl_absorpt_correction_T_max  0.4321
_exptl_absorpt_correction_T_min  0.2138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.1498 before and 0.0658 after correction. 
The Ratio of minimum to maximum transmission is 0.4948. 
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.067
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.012
_refine_diff_density_max         0.990
_refine_diff_density_min         -2.236
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2483
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0275
_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)+(0.0269P)²+5.1021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2296
_reflns_number_total             2483
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b01543_si_005.cif
_cod_data_source_block           mono_p83
_cod_database_code               4132096
_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.
;
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.216
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6752(14)
 0.3248(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N2-C5
 1.48 with sigma of 0.02
 N1-C1
 1.48 with sigma of 0.02
 C6-C7
 1.54 with sigma of 0.02
 C2-C3
 1.54 with sigma of 0.02
 C3-C4
 1.54 with sigma of 0.02
 C4-C2
 2.515 with sigma of 0.02
 C1-C2
 1.54 with sigma of 0.02
 C1-C3
 2.515 with sigma of 0.02
 C5-C6 \\sim C6-C7 \\sim C7-C8
 with sigma of 0.02
 C1-C2 \\sim C2-C3 \\sim C3-C4
 with sigma of 0.02
4. Rigid bond restraints
 C5, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2, N1, C1, C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
N2 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C2 \\sim N1 \\sim C1 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Others
 Fixed Sof: Cs1(0.5) N2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C5(0.5) H5A(0.5)
 H5B(0.5) C2(0.5) H2D(0.5) H2E(0.5) C6(0.5) H6A(0.5) H6B(0.5) C7(0.5) H7A(0.5)
 H7B(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5) H1D(0.5) H1E(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C8(0.5) H8A(0.5) H8B(0.5)
 H8C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C2(H2D,H2E), C6(H6A,H6B), C7(H7A,H7B), C1(H1D,H1E), C3(H3A,H3B)
7.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N1(H1A,H1B,H1C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C)
;
_olex2_date_sample_data_collection 2016-06-29
_olex2_submission_original_sample_id mono_p83
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Bi1 Bi 0.32409(6) 0.7500 0.14011(2) 0.03190(10) Uani 1 2 d S T P . .
Ag1 Ag 0.83142(18) 0.2500 0.15818(6) 0.0582(3) Uani 1 2 d S T P . .
Br5 Br 0.07994(14) 0.49853(14) 0.14834(6) 0.0582(3) Uani 1 1 d . . . . .
Br4 Br 0.22012(19) 0.7500 -0.00357(6) 0.0568(4) Uani 1 2 d S T P . .
Br3 Br 0.4435(2) 0.7500 0.28711(7) 0.0751(5) Uani 1 2 d S T P . .
Cs1 Cs 0.24167(14) 0.2500 -0.00024(4) 0.05640(19) Uani 1 2 d . . . . .
Br2 Br 0.56562(14) 0.50043(14) 0.12842(6) 0.0561(3) Uani 1 1 d . . . . .
Br1 Br 0.8485(2) 0.2500 0.29304(10) 0.0971(7) Uani 1 2 d S T P . .
N2 N 0.428(2) 0.214(4) 0.2531(8) 0.075(11) Uani 0.5 1 d D U . A -1
H2A H 0.4031 0.2783 0.2158 0.090 Uiso 0.5 1 calc GR . . A -1
H2B H 0.3912 0.1102 0.2427 0.090 Uiso 0.5 1 calc GR . . A -1
H2C H 0.5398 0.2121 0.2682 0.090 Uiso 0.5 1 calc GR . . A -1
C5 C 0.347(3) 0.282(5) 0.3073(11) 0.102(11) Uani 0.5 1 d D U . A -1
H5A H 0.2271 0.2574 0.2955 0.122 Uiso 0.5 1 calc R . . A -1
H5B H 0.3598 0.4029 0.3084 0.122 Uiso 0.5 1 calc R . . A -1
C2 C 0.951(4) 0.782(6) 0.3786(9) 0.143(12) Uani 0.5 1 d D U . B -1
H2D H 0.8400 0.7356 0.3793 0.172 Uiso 0.5 1 calc R . . B -1
H2E H 0.9564 0.8929 0.3985 0.172 Uiso 0.5 1 calc R . . B -1
C6 C 0.418(4) 0.213(4) 0.3781(11) 0.113(10) Uani 0.5 1 d D U . A -1
H6A H 0.5404 0.2212 0.3880 0.135 Uiso 0.5 1 calc R . . A -1
H6B H 0.3875 0.0959 0.3804 0.135 Uiso 0.5 1 calc R . . A -1
C7 C 0.346(4) 0.314(5) 0.4304(14) 0.154(13) Uani 0.5 1 d D U . A -1
H7A H 0.3431 0.4301 0.4154 0.185 Uiso 0.5 1 calc R . . A -1
H7B H 0.2297 0.2791 0.4261 0.185 Uiso 0.5 1 calc R . . A -1
N1 N 0.847(2) 0.704(2) 0.2540(8) 0.071(6) Uani 0.5 1 d D U . B -1
H1A H 0.8895 0.6829 0.2169 0.085 Uiso 0.5 1 calc GR . . B -1
H1B H 0.7544 0.7665 0.2422 0.085 Uiso 0.5 1 calc GR . . B -1
H1C H 0.8206 0.6078 0.2720 0.085 Uiso 0.5 1 calc GR . . B -1
C1 C 0.972(3) 0.794(3) 0.3051(8) 0.095(10) Uani 0.5 1 d D U . B -1
H1D H 0.9694 0.9113 0.2922 0.114 Uiso 0.5 1 calc R . . B -1
H1E H 1.0837 0.7515 0.3028 0.114 Uiso 0.5 1 calc R . . B -1
C3 C 1.086(5) 0.671(4) 0.4223(11) 0.178(15) Uani 0.5 1 d D U . B -1
H3A H 1.0668 0.5554 0.4079 0.213 Uiso 0.5 1 calc R . . B -1
H3B H 1.1961 0.7041 0.4148 0.213 Uiso 0.5 1 calc R . . B -1
C4 C 1.084(6) 0.685(6) 0.4983(10) 0.19(2) Uani 0.5 1 d D U . B -1
H4A H 0.9890 0.7515 0.5043 0.283 Uiso 0.5 1 calc GR . . B -1
H4B H 1.1864 0.7366 0.5219 0.283 Uiso 0.5 1 calc GR . . B -1
H4C H 1.0745 0.5749 0.5169 0.283 Uiso 0.5 1 calc GR . . B -1
C8 C 0.423(6) 0.314(5) 0.5058(15) 0.18(2) Uani 0.5 1 d D U . A -1
H8A H 0.5357 0.2699 0.5128 0.267 Uiso 0.5 1 calc GR . . A -1
H8B H 0.3561 0.2460 0.5298 0.267 Uiso 0.5 1 calc GR . . A -1
H8C H 0.4269 0.4268 0.5231 0.267 Uiso 0.5 1 calc GR . . A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)'
H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Ag Ag -0.9440 1.0460 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Bi Bi -3.3340 10.1060 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Br Br -0.1850 2.3450 'Calculated using XDISP in WinGX (Farrugia, 1999)'
Cs Cs -0.3730 2.0170 'Calculated using XDISP in WinGX (Farrugia, 1999)'
N N 0.0060 0.0030 'Calculated using XDISP in WinGX (Farrugia, 1999)'
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
Br5 Bi1 Br5 89.81(5) . 4_575
Br5 Bi1 Br3 92.02(3) . .
Br5 Bi1 Br3 92.02(3) 4_575 .
Br4 Bi1 Br5 89.46(3) . 4_575
Br4 Bi1 Br5 89.46(3) . .
Br4 Bi1 Br3 177.91(5) . .
Br4 Bi1 Br2 89.18(4) . 4_575
Br4 Bi1 Br2 89.18(4) . .
Br2 Bi1 Br5 90.38(3) 4_575 4_575
Br2 Bi1 Br5 178.62(4) . 4_575
Br2 Bi1 Br5 178.62(4) 4_575 .
Br2 Bi1 Br5 90.38(3) . .
Br2 Bi1 Br3 89.34(4) 4_575 .
Br2 Bi1 Br3 89.34(4) . .
Br2 Bi1 Br2 89.39(5) . 4_575
Br5 Ag1 Br5 87.88(7) 1_655 4_665
Br5 Ag1 Br4 83.32(4) 1_655 3_665
Br5 Ag1 Br4 83.32(4) 4_665 3_665
Br5 Ag1 Br2 164.68(5) 4_665 .
Br5 Ag1 Br2 164.68(5) 1_655 4_565
Br5 Ag1 Br2 90.57(3) 4_665 4_565
Br5 Ag1 Br2 90.57(3) 1_655 .
Br2 Ag1 Br4 81.36(4) 4_565 3_665
Br2 Ag1 Br4 81.36(4) . 3_665
Br2 Ag1 Br2 86.91(6) 4_565 .
Br1 Ag1 Br5 100.15(5) . 4_665
Br1 Ag1 Br5 100.15(5) . 1_655
Br1 Ag1 Br4 175.13(7) . 3_665
Br1 Ag1 Br2 95.12(5) . .
Br1 Ag1 Br2 95.12(5) . 4_565
Bi1 Br5 Ag1 178.89(6) . 1_455
Bi1 Br4 Ag1 170.71(7) . 3_665
Bi1 Br2 Ag1 163.92(5) . .
N2 C5 C6 114(2) . .
C1 C2 C3 112.1(17) . .
C5 C6 C7 108(3) . .
C8 C7 C6 123(3) . .
N1 C1 C2 116(2) . .
C4 C3 C2 111.8(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Bi1 Br5 2.8428(11) .
Bi1 Br5 2.8428(11) 4_575
Bi1 Br4 2.8031(14) .
Bi1 Br3 2.8796(15) .
Bi1 Br2 2.8316(11) 4_575
Bi1 Br2 2.8316(11) .
Ag1 Br5 2.8581(15) 4_665
Ag1 Br5 2.8581(15) 1_655
Ag1 Br4 3.0107(16) 3_665
Ag1 Br2 2.9057(15) 4_565
Ag1 Br2 2.9057(15) .
Ag1 Br1 2.651(2) .
Br5 Ag1 2.8581(15) 1_455
Br4 Ag1 3.0107(16) 3_665
N2 C5 1.473(18) .
C5 C6 1.51(2) .
C2 C1 1.509(14) .
C2 C3 1.528(14) .
C6 C7 1.520(16) .
C7 C8 1.50(2) .
N1 C1 1.467(16) .
C3 C4 1.515(14) .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.6752(14)
2 0.3248(14)
