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_4129207
_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
'Cl3 In0.5, Ag0.5 Cl4 In0.5, Ag0.5 Cl, 4(C3 H10 N)'
_chemical_formula_sum            'C12 H40 Ag Cl8 In N4'
_chemical_formula_weight         746.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.141(10)
_cell_angle_beta                 89.992(10)
_cell_angle_gamma                90.049(11)
_cell_formula_units_Z            2
_cell_length_a                   7.454(3)
_cell_length_b                   7.866(3)
_cell_length_c                   24.629(8)
_cell_measurement_reflns_used    1214
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.48
_cell_measurement_theta_min      2.72
_cell_volume                     1444.1(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.41
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.835
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.1251
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.835
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            9706
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.763
_diffrn_reflns_theta_min         0.827
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.224
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       plate
_exptl_crystal_F_000             744
_refine_diff_density_max         1.599
_refine_diff_density_min         -1.967
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         5690
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.1962
_refine_ls_R_factor_gt           0.0771
_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^)+(0.1291P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1999
_refine_ls_wR_factor_ref         0.2696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2206
_reflns_number_total             5690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b09945_si_001.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        1444.0(8)
_cod_database_code               4129207
_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
 C10-C11
 1.5 with sigma of 0.02
 C4-C5
 1.5 with sigma of 0.02
 C8-C9
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uiso(N1) = Uiso(C1) = Uiso(C2) = Uiso(C3)
Uiso(N2) = Uiso(C4) = Uiso(C5) = Uiso(C6)
Uiso(N3) = Uiso(C7) = Uiso(C8) = Uiso(C9)
Uiso(N4) = Uiso(C10) = Uiso(C11) = Uiso(C12)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C3(H3A,H3B,H3C), N2(H2C,H2D,H2E), C6(H6A,H6B,H6C), N3(H3D,
 H3E,H3F), C9(H9A,H9B,H9C), N4(H4C,H4D,H4E), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              33523
_shelx_hkl_checksum              4810
_olex2_submission_special_instructions 'No special instructions were received'