From 2D to 3D: a facile and effective procedure for fabrication of planar CH3NH3PbI3perovskite solar cells
Zhang, Yu; Li, Fengzhu; Jiang, Ke-Jian; Huang, Jin-Hua; Wang, Huijia; Fan, Haochen; Wang, Pengcheng; Liu, Cai-Ming; Zhang, Li-Peng; Song, YanLin; Journal of Materials Chemistry A 6 (2018) 17867–; doi:10.1039/C8TA07048B

data_7237197
_publ_section_title
;
 From 2D to 3D: a facile and effective procedure for fabrication of planar
 CH3NH3PbI3perovskite solar cells
;
_journal_issue                   37
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              17867
_journal_paper_doi               10.1039/C8TA07048B
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'I14 Pb4, 6(C3 H10 N)'
_chemical_formula_sum            'C18 H60 I14 N6 Pb4'
_chemical_formula_weight         2966.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-07-09 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.16(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7287(17)
_cell_length_b                   22.221(4)
_cell_length_c                   15.080(3)
_cell_measurement_reflns_used    9264
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.4850
_cell_measurement_theta_min      1.3506
_cell_volume                     2924.3(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13373
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.525
_diffrn_reflns_theta_min         1.351
_exptl_absorpt_coefficient_mu    18.888
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.368
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.056
_refine_diff_density_max         9.110
_refine_diff_density_min         -8.579
_refine_diff_density_rms         0.761
_refine_ls_abs_structure_details
;
 Flack x determined using 5161 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         13373
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+479.7127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                12885
_reflns_number_total             13373
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta07048b2.cif
_cod_data_source_block           mx6644d_tw
_cod_original_cell_volume        2924.5(10)
_cod_database_code               7237197
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.273
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.804(5)
 0.196(5)
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
 C10-C11
 1.54 with sigma of 0.01
 C80-C16 = C80-C21
 1.54 with sigma of 0.01
 C3-C2 = C6-C5 = C5-C4 = C2-C1 = C9-C8 = C8-C7 = C12-C11 = C14-C13 = C15-C14
 1.54 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
N6 \\sim C16 \\sim C21 \\sim C80: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq,
Uanis(C15) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C16) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C80) \\sim Ueq,
Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N5) \\sim
Ueq, Uanis(N1) \\sim Ueq, Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,
 H12B), C14(H14A,H14B), C15(H15A,H15B), C2(H2D,H2E), C3(H3D,H3E), C21(H21A,
 H21B), C80(H80A,H80B)
5.b Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N3(H3A,H3B,H3C), N4(H4D,H4E,H4F), C4(H4A,H4B,H4C), N5(H5C,
 H5D,H5E), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C1(H1A,
 H1B,H1C), N1(H1D,H1E,H1F), N6(H6C,H6D,H6E), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              75034
_shelx_hkl_checksum              83872
_olex2_submission_special_instructions 'No special instructions were received'