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_4130583
_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_absolute_configuration ad
_chemical_formula_moiety         'I8 Pb3, 2(C2 H6 O S), 2(C H6 N)'
_chemical_formula_sum            'C6 H26 I8 N2 O2 Pb3 S2'
_chemical_formula_weight         1859.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2b'
_space_group_name_H-M_alt        'P b c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-17
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   4.6212(6)
_cell_length_b                   27.219(7)
_cell_length_c                   26.841(4)
_cell_measurement_reflns_used    2016
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.6200
_cell_measurement_theta_min      4.0410
_cell_volume                     3376.2(11)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -67.00   52.25   0.7500   11.5000
omega____ theta____ kappa____ phi______ frames
    -       14.4699  -19.0000  120.0000 159

  2 omega   28.00   46.75   0.7500   11.5000
omega____ theta____ kappa____ phi______ frames
    -       14.4699   19.0000  120.0000 25
;
_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      -0.0570420000
_diffrn_orient_matrix_UB_12      0.0140040000
_diffrn_orient_matrix_UB_13      -0.0199329000
_diffrn_orient_matrix_UB_21      0.0556191000
_diffrn_orient_matrix_UB_22      0.0217361000
_diffrn_orient_matrix_UB_23      0.0109217000
_diffrn_orient_matrix_UB_31      0.1318598000
_diffrn_orient_matrix_UB_32      -0.0030822000
_diffrn_orient_matrix_UB_33      -0.0133258000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10664
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.76
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    22.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71142
_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_density_diffrn    3.658
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.020
_refine_diff_density_min         -3.561
_refine_diff_density_rms         0.517
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.488(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         5166
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+128.3324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                3574
_reflns_number_total             5166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b04924_si_002.cif
_cod_data_source_block           jxj-1-150905-perovskite-dmso
_cod_original_cell_volume        3376.2(12)
_cod_database_code               4130583
_reflns_odcompleteness_completeness 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B,H1C} of C1, {H0AA,H0AB,H0AC} of N0AA
 At 1.5 times of:
  {H1AA,H1AB,H1AC} of C1AA, {H3A,H3B,H3C} of C3, {H15A,H15B,H15C} of C15,
  {H2A,H2B,H2C} of N2, {H4A,H4B,H4C} of C4, {H13A,H13B,H13C} of C13
2. Rigid bond restraints
 N0AA, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N2, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1AA)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C15) = Uanis(C3) = Uanis(C1) = Uanis(C13)
4.a Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C3(H3A,H3B,H3C), C1AA(H1AA,H1AB,
 H1AC), N0AA(H0AA,H0AB,H0AC), C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
;
_olex2_submission_special_instructions 'No special instructions were received'