Chemical Approaches to Addressing the Instability and Toxicity of Lead-Halide Perovskite Absorbers.
Slavney, Adam H.; Smaha, Rebecca W.; Smith, Ian C.; Jaffe, Adam; Umeyama, Daiki; Karunadasa, Hemamala I.; Inorganic chemistry 56 (2017) 46–55; doi:10.1021/acs.inorgchem.6b01336

data_4345096
_publ_section_title
;
 Chemical Approaches to Addressing the Instability and Toxicity of
 Lead-Halide Perovskite Absorbers.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              46
_journal_page_last               55
_journal_paper_doi               10.1021/acs.inorgchem.6b01336
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'I10 Pb3, 2(C8 H11 F N), 2(C N H6)'
_chemical_formula_sum            'C18 H34 F2 I10 N4 Pb3'
_chemical_formula_weight         2235.13
_chemical_name_systematic
'bis(4-fluorophenethylammonium) bis(methylammonium) decaiodo triplumbate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.738(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.164(5)
_cell_length_b                   8.7654(14)
_cell_length_c                   8.8626(14)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.303
_cell_measurement_theta_min      3.057
_cell_volume                     2257.8(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_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            55950
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         27.846
_diffrn_reflns_theta_min         2.292
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.334
_exptl_absorpt_correction_T_max  0.3449
_exptl_absorpt_correction_T_min  0.2587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1518 before and 0.0594 after correction.
The Ratio of minimum to maximum transmission is 0.7501.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    3.270
_exptl_crystal_description       plate
_exptl_crystal_F_000             1904
_exptl_crystal_preparation
'Slow evaporation from acetonitrile/nitromethane'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.149
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.000144(17)
_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   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         4135
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+6.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0579
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2832
_reflns_number_total             4135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01336_si_005.cif
_cod_data_source_block           g_mon_0p83_a
_cod_database_code               4345096
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups
2. Shared sites
{C1A, N1B}
{C1B, N1A}
{C1C, N1D}
{C1D, N1C}
3. Restrained distances
 N1D-C1D
 1.45 with sigma of 0.02
 N1B-C1B
 1.45 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(N1A) = Uiso(N1B) = Uiso(C1A) = Uiso(C1B)
Uiso(N1C) = Uiso(N1D) = Uiso(C1C) = Uiso(C1D)
5. Others
 Fixed Sof: N1A(0.25) C1A(0.25) N1B(0.25) C1B(0.25) C1C(0.25) N1C(0.25)
 C1D(0.25) N1D(0.25)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2D,H2E), C3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C5(H5), C9(H9), C6(H6)
6.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_shelx_res_checksum              63512
_shelx_hkl_checksum              5379
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'Mitegen loop with a trace of mineral oil'
_olex2_submission_special_instructions 'No special instructions were received'