Identifying the Molecular Structures of Intermediates for Optimizing the Fabrication of High-Quality Perovskite Films.
Cao, Jing; Jing, Xiaojing; Yan, Juanzhu; Hu, Chengyi; Chen, Ruihao; Yin, Jun; Li, Jing; Zheng, Nanfeng; Journal of the American Chemical Society 138 (2016) 9919–9926; doi:10.1021/jacs.6b04924

data_4130582
_publ_section_title
;
 Identifying the Molecular Structures of Intermediates for Optimizing the
 Fabrication of High-Quality Perovskite Films.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9919
_journal_page_last               9926
_journal_paper_doi               10.1021/jacs.6b04924
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'I5 Pb, C2 H6 O S, 3(C H6 N)'
_chemical_formula_sum            'C5 H25 I5 N3 O Pb S'
_chemical_formula_weight         1017.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-29
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.122(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.641(2)
_cell_length_b                   12.4157(9)
_cell_length_c                   19.0841(19)
_cell_measurement_reflns_used    2303
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      65.6510
_cell_measurement_theta_min      4.6490
_cell_volume                     4497.9(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega   27.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  -45.0000  -60.0000 26

  2 omega   73.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  -45.0000  -60.0000 25

  3 omega   77.00  152.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  -15.0000 -120.0000 75

  4 omega   87.00  160.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609   61.0000  -60.0000 73

  5 omega   95.00  152.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  125.0000 -180.0000 57

  6 omega   16.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  -45.0000 -150.0000 80

  7 omega   35.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       40.7547 -125.0000    0.0000 34

  8 omega   16.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       91.1609  -45.0000  150.0000 60

  9 omega  -48.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7547   37.0000 -120.0000 79

 10 omega -115.00  -16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.7547  -57.0000   90.0000 99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0581696000
_diffrn_orient_matrix_UB_12      0.0825606000
_diffrn_orient_matrix_UB_13      -0.0082729000
_diffrn_orient_matrix_UB_21      0.0419401000
_diffrn_orient_matrix_UB_22      0.0386444000
_diffrn_orient_matrix_UB_23      0.0823437000
_diffrn_orient_matrix_UB_31      0.0380328000
_diffrn_orient_matrix_UB_32      0.0839882000
_diffrn_orient_matrix_UB_33      -0.0295917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_av_unetI/netI     0.0968
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8115
_diffrn_reflns_point_group_measured_fraction_full 0.932
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.779
_diffrn_reflns_theta_min         4.255
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    69.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.004
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         5.204
_refine_diff_density_min         -9.406
_refine_diff_density_rms         0.911
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          5.198
_refine_ls_shift/su_mean         0.233
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2000
_refine_ls_wR_factor_ref         0.2290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2720
_reflns_number_total             3798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04924_si_006.cif
_cod_data_source_block           jxj-20160429-3
_cod_database_code               4130582
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 Pb01, I06, I04, I02, I05, I03
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Pb01: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(N5) \\sim Ueq, Uanis(I02) \\sim Ueq, Uanis(I03) \\sim Ueq,
Uanis(I04) \\sim Ueq, Uanis(I05) \\sim Ueq, Uanis(I06) \\sim Ueq, Uanis(S007)
\\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(N4) \\sim Ueq, : with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(I05) \\sim Ueq, Uanis(I06) \\sim Ueq, Uanis(I02) \\sim Ueq, Uanis(I03)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), C3(H3A,H3B,H3C), N4(H4A,H4B,H4C), N5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              12764
_shelx_hkl_checksum              54942
_olex2_date_sample_data_collection 2016-04-29
_olex2_submission_special_instructions 'No special instructions were received'