#------------------------------------------------------------------------------
#$Date: 2019-11-25 13:34:58 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240985 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/05/4130585.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4130585
loop_
_publ_author_name
'Cao, Jing'
'Jing, Xiaojing'
'Yan, Juanzhu'
'Hu, Chengyi'
'Chen, Ruihao'
'Yin, Jun'
'Li, Jing'
'Zheng, Nanfeng'
_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_sum            'C4 H12 I2 O2 Pb S2'
_chemical_formula_weight         617.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6978(4)
_cell_length_b                   10.8575(4)
_cell_length_c                   8.7607(3)
_cell_measurement_reflns_used    2925
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.6980
_cell_measurement_theta_min      4.6390
_cell_volume                     1302.93(8)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Atlas
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4567
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         3.338
_exptl_absorpt_coefficient_mu    17.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18471
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.124
_refine_diff_density_min         -2.986
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         1494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0298P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1350
_reflns_number_total             1494
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b04924_si_003.cif
_cod_data_source_block           jxj-1-150822-jiaben
_cod_original_cell_volume        1302.93(7)
_cod_database_code               4130585
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pb1 Pb 0.2500 0.7500 0.22399(3) 0.00545(11) Uani 1 2 d S T P
I1 I 0.22999(3) 0.96842(3) -0.00570(4) 0.00843(12) Uani 1 1 d . . .
S1 S 0.51050(9) 0.67619(11) 0.16086(15) 0.0096(3) Uani 1 1 d . . .
O1 O 0.4305(3) 0.7721(3) 0.1843(6) 0.0169(9) Uani 1 1 d . . .
C1 C 0.4933(4) 0.5636(5) 0.3053(7) 0.0163(9) Uani 1 1 d . . .
H1A H 0.4884 0.6034 0.4028 0.025 Uiso 1 1 calc R U .
H1B H 0.5479 0.5080 0.3059 0.025 Uiso 1 1 calc R U .
H1C H 0.4345 0.5184 0.2854 0.025 Uiso 1 1 calc R U .
C2 C 0.6179(5) 0.7465(4) 0.2373(8) 0.0163(9) Uani 1 1 d . . .
H2A H 0.6433 0.8049 0.1652 0.025 Uiso 1 1 calc R U .
H2B H 0.6662 0.6843 0.2570 0.025 Uiso 1 1 calc R U .
H2C H 0.6020 0.7881 0.3308 0.025 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Pb1 O1 164.1(2) 2_565 .
O1 Pb1 I1 84.08(9) 2_565 .
O1 Pb1 I1 85.66(10) . .
O1 Pb1 I1 85.67(10) 2_565 2_565
O1 Pb1 I1 84.08(9) . 2_565
I1 Pb1 I1 99.745(15) . 2_565
O1 Pb1 I1 104.22(10) 2_565 7_656
O1 Pb1 I1 87.11(9) . 7_656
I1 Pb1 I1 85.720(9) . 7_656
I1 Pb1 I1 169.235(14) 2_565 7_656
O1 Pb1 I1 87.11(9) 2_565 8_576
O1 Pb1 I1 104.22(10) . 8_576
I1 Pb1 I1 169.235(14) . 8_576
I1 Pb1 I1 85.720(9) 2_565 8_576
I1 Pb1 I1 90.461(13) 7_656 8_576
Pb1 I1 Pb1 84.897(9) . 7_655
O1 S1 C1 106.2(3) . .
O1 S1 C2 104.4(2) . .
C1 S1 C2 97.8(3) . .
S1 O1 Pb1 131.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.509(4) 2_565
Pb1 O1 2.509(4) .
Pb1 I1 3.1222(4) .
Pb1 I1 3.1222(4) 2_565
Pb1 I1 3.3626(4) 7_656
Pb1 I1 3.3626(4) 8_576
I1 Pb1 3.3626(4) 7_655
S1 O1 1.526(4) .
S1 C1 1.775(6) .
S1 C2 1.788(6) .
