Hybrid Dion-Jacobson 2D Lead Iodide Perovskites.
Mao, Lingling; Ke, Weijun; Pedesseau, Laurent; Wu, Yilei; Katan, Claudine; Even, Jacky; Wasielewski, Michael R.; Stoumpos, Constantinos C.; Kanatzidis, Mercouri G.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.8b00542

data_4127192
_publ_section_title
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 Hybrid Dion-Jacobson 2D Lead Iodide Perovskites.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.8b00542
_journal_year                    2018
_chemical_formula_moiety         'I20 Pb6, 2(C6 H16 N2), 4(C H6 N)'
_chemical_formula_sum            'C16 H56 I20 N8 Pb6'
_chemical_formula_weight         4141.82
_chemical_name_systematic
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 ?
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_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2ya'
_space_group_name_H-M_alt        'P 1 a 1'
_symmetry_space_group_name_Hall  'P -2ya'
_symmetry_space_group_name_H-M   'P 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-12-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.862
_cell_length_b                   8.862
_cell_length_c                   23.032
_cell_measurement_reflns_used    3508
_cell_measurement_temperature    250
_cell_measurement_theta_max      28.184
_cell_measurement_theta_min      3.249
_cell_volume                     1808.819
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      250
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24106
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.471
_diffrn_reflns_theta_min         0.884
_exptl_absorpt_coefficient_mu    22.467
_exptl_absorpt_correction_T_max  0.74487
_exptl_absorpt_correction_T_min  0.63071
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.802
_exptl_crystal_description       plate
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.031
_exptl_crystal_size_mid          0.029
_exptl_crystal_size_min          0.029
_refine_diff_density_max         2.014
_refine_diff_density_min         -1.382
_refine_diff_density_rms         0.364
_refine_ls_abs_structure_details
;
 Flack x determined using 2081 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.491(18)
_refine_ls_extinction_coef       0.000421(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         8035
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0655P)^2^+3.2042P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.835
_reflns_Friedel_fraction_max     0.766
_reflns_number_gt                5486
_reflns_number_total             8035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00542_si_002.cif
_cod_data_source_block           3ampPb3I10
_cod_original_cell_volume        1808.8
_cod_database_code               4127192
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-C8
 1.5 with sigma of 0.02
 C2-N3
 1.5 with sigma of 0.02
 C7-C3 = C3-C1
 1.5 with sigma of 0.02
 C3-C1 = C1-N1
 1.5 with sigma of 0.02
 C1-N1 = N1-C4
 1.5 with sigma of 0.02
 N1-C4 = C4-C6
 1.5 with sigma of 0.02
 C4-C6 = C6-C7
 1.5 with sigma of 0.02
 C6-C7 = C7-C3
 1.5 with sigma of 0.02
 C6-C5 = C5-N4
 1.5 with sigma of 0.02
 C4-C6 = C6-C5
 1.5 with sigma of 0.02
 C7-C1
 2.472 with sigma of 0.04
 C3-N1
 2.472 with sigma of 0.04
 C1-C4
 2.516 with sigma of 0.04
 N1-C6
 2.457 with sigma of 0.04
 C4-C7
 2.442 with sigma of 0.04
 C6-C3
 2.472 with sigma of 0.04
 C6-N4
 2.442 with sigma of 0.04
 C4-C5
 2.442 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N2) = Uiso(C8)
Uiso(C2) = Uiso(N3)
Uiso(N4) = Uiso(C5) = Uiso(C6) = Uiso(C4) = Uiso(N1) = Uiso(C1) = Uiso(C3) =
Uiso(C7)
4.a Ternary CH refined with riding coordinates:
 C6(H6)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C3(H3A,H3B), C4(H4D,H4E), C5(H5A,H5B), C7(H7A,H7B)
4.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3C,H3D,H3E), N4(H4A,H4B,H4C), C2(H2D,H2E,H2F), C8(H8A,
 H8B,H8C)
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_olex2_submission_special_instructions 'No special instructions were received'