Layered Halide Double Perovskites: Dimensional Reduction of Cs<sub>2</sub>AgBiBr<sub>6</sub>.
Connor, Bridget A.; Leppert, Linn; Smith, Matthew D.; Neaton, Jeffrey B.; Karunadasa, Hemamala I.; Journal of the American Chemical Society 140 (2018) 5235–5240; doi:10.1021/jacs.8b01543

data_4132094
_publ_section_title
;
 Layered Halide Double Perovskites: Dimensional Reduction of
 Cs<sub>2</sub>AgBiBr<sub>6</sub>.
;
_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 Br8, 4(C4 H12 N)'
_chemical_formula_sum            'C16 H48 Ag Bi Br8 N4'
_chemical_formula_weight         1252.71
_chemical_name_systematic
'tetra(butylammonium) octabromoargentobismuthate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.081(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.0451(15)
_cell_length_b                   8.1328(4)
_cell_length_c                   8.4296(4)
_cell_measurement_reflns_used    6118
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      38.33
_cell_measurement_theta_min      3.37
_cell_volume                     1854.11(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      298.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'PHOTON 100 Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w 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     0.9919
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7934
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        36.523
_diffrn_reflns_theta_max         38.315
_diffrn_reflns_theta_min         2.102
_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    7.126
_exptl_absorpt_correction_T_max  0.4401
_exptl_absorpt_correction_T_min  0.2902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0891 before and 0.0463 after correction. 
The Ratio of minimum to maximum transmission is 0.6594. 
The \l/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    2.244
_exptl_crystal_description       plate
_exptl_crystal_F_000             1164
_exptl_crystal_recrystallization_method
;
Crystallized by slow cooling an HBr solution containing 
a 1:1:10 ratio of BiBr3, AgBr, and butylamine.
;
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2020
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0366
_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/[\s^2^(Fo^2^)+(0.0407P)^2^+4.4244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1799
_reflns_number_total             2020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01543_si_003.cif
_cod_data_source_block           monoc_merge_a
_cod_database_code               4132094
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.330
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8259(18) 0.1741(18)
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
 N1-C1
 1.48 with sigma of 0.02
 C1-C2
 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
 C1-C3
 2.515 with sigma of 0.02
 C2-C4
 2.515 with sigma of 0.02
 N2-C5
 1.48 with sigma of 0.02
 C5-C6
 1.54 with sigma of 0.02
 C6-C7
 1.54 with sigma of 0.02
 C7-C8
 1.54 with sigma of 0.02
 N2-C6
 2.515 with sigma of 0.02
 C5-C7
 2.515 with sigma of 0.02
 C6-C8
 2.515 with sigma of 0.02
 N1-C2
 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
 N2, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C1, C2, 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
N1 \\sim C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Others
 Fixed Sof: N2(0.5) H2A(0.5) H2B(0.5) H2C(0.5) C5(0.5) H5A(0.5) H5B(0.5)
 C3(0.5) H3A(0.5) H3B(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(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) C2(0.5) H2D(0.5) H2E(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C1(H1D,H1E), C2(H2D,H2E)
7.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C8(H8A,H8B,H8C), N1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              95088
_shelx_hkl_checksum              70191
_olex2_submission_special_instructions 'No special instructions were received'