Chemical and Structural Diversity of Hybrid Layered Double Perovskite Halides.
Mao, Lingling; Teicher, Samuel M. L.; Stoumpos, Constantinos C.; Kennard, Rhys M.; DeCrescent, Ryan A.; Wu, Guang; Schuller, Jon A.; Chabinyc, Michael L.; Cheetham, Anthony K.; Seshadri, Ram; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b09945

data_4129204
_publ_section_title
;
 Chemical and Structural Diversity of Hybrid Layered Double Perovskite
 Halides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b09945
_journal_year                    2019
_chemical_formula_moiety         '0.5(Ag2 Bi2 Br14 Cs2), C6 H20 N2'
_chemical_formula_sum            'C6 H20 Ag Bi Br7 Cs N2'
_chemical_formula_weight         1129.37
_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     direct
_audit_creation_date             2019-03-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.503(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.053(4)
_cell_length_b                   7.997(3)
_cell_length_c                   18.536(8)
_cell_measurement_reflns_used    1238
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.09
_cell_measurement_theta_min      2.59
_cell_volume                     1165.4(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.900
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.1371
_diffrn_reflns_Laue_measured_fraction_full 0.924
_diffrn_reflns_Laue_measured_fraction_max 0.900
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4810
_diffrn_reflns_point_group_measured_fraction_full 0.924
_diffrn_reflns_point_group_measured_fraction_max 0.900
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.678
_diffrn_reflns_theta_min         1.125
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    21.907
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.218
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_refine_diff_density_max         5.786
_refine_diff_density_min         -4.368
_refine_diff_density_rms         0.517
_refine_ls_extinction_coef       0.00051(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         2138
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.2065
_refine_ls_R_factor_gt           0.1304
_refine_ls_shift/su_max          0.297
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+373.8861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2742
_refine_ls_wR_factor_ref         0.3171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1272
_reflns_number_total             2138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09945_si_004.cif
_cod_data_source_block           p21m
_cod_original_cell_volume        1165.5(9)
_cod_database_code               4129204
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. 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
2. Restrained distances
 N2-C4 = C4-C5
 1.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 N1-C1
 1.5 with sigma of 0.02
 C2-C3
 1.5 with sigma of 0.02
 C1-C2
 1.5 with sigma of 0.02
 N1-C1 = C1-C2
 1.5 with sigma of 0.02
 C1-C2 = C2-C3
 1.5 with sigma of 0.02
 N2-C5
 2.719 with sigma of 0.04
 N1-C2
 2.719 with sigma of 0.04
 C1-C3
 2.719 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N2) = Uiso(C4) = Uiso(C5)
Uiso(N2) = Uiso(C4) = Uiso(C5) = Uiso(C6)
Uiso(C1) = Uiso(C3)
Uiso(N1) = Uiso(C1) = Uiso(C3)
Uiso(N1) = Uiso(C1) = Uiso(C2) = Uiso(C3)
4. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5) H5A(0.5) H5B(0.5) H4A(0.5) H4B(0.5)
 H6A(0.5) H6B(0.5) H6C(0.5) H1A(0.5) H1B(0.5) H1C(0.5) H1D(0.5) H1E(0.5)
 H3A(0.5) H3B(0.5) H3C(0.5) H2D(0.5) H2E(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C4(H4A,H4B), C1(H1D,H1E), C2(H2D,H2E)
5.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C6(H6A,H6B,H6C), N1(H1A,H1B,H1C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              254
_shelx_hkl_checksum              3724
_olex2_submission_special_instructions 'No special instructions were received'