#------------------------------------------------------------------------------
#$Date: 2019-11-25 13:33:46 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240981 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/05/4130581.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_4130581
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_moiety         '0.5(C4 H12 I4 O4 Pb2 S2)'
_chemical_formula_sum            'C2 H6 I2 O2 Pb S'
_chemical_formula_weight         555.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2c 2n'
_space_group_name_H-M_alt        'P n a m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-08-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3119 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.796(3)
_cell_length_b                   11.1352(17)
_cell_length_c                   4.5144(6)
_cell_measurement_reflns_used    722
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      26.9660
_cell_measurement_theta_min      3.6460
_cell_volume                     894.6(2)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(11)
_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 0.997
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -83.00    6.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.5867  -38.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  2 omega  -35.00   63.00   1.0000    8.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.5867   19.0000  120.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0327274000
_diffrn_orient_matrix_UB_12      0.0144616000
_diffrn_orient_matrix_UB_13      0.0818428000
_diffrn_orient_matrix_UB_21      0.0193117000
_diffrn_orient_matrix_UB_22      0.0133836000
_diffrn_orient_matrix_UB_23      -0.1337488000
_diffrn_orient_matrix_UB_31      -0.0120449000
_diffrn_orient_matrix_UB_32      0.0605654000
_diffrn_orient_matrix_UB_33      0.0099871000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.1243
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            4266
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         27.452
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    25.927
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36251
_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    4.122
_exptl_crystal_description
;
;
_exptl_crystal_F_000             952
_refine_diff_density_max         2.938
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         1155
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.994
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0238P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                765
_reflns_number_total             1155
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b04924_si_005.cif
_cod_data_source_block           jxj-1-150823-pbi2.dmso-2
_cod_database_code               4130581
_shelxl_version_number           2013-2
_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.
;
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H2C(0.5) H3A(0.5) H3B(0.5) H3C(0.5)
4.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, -y-1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.04026(6) 0.31693(9) 0.7500 0.0175(3) Uani 1 2 d S T P . .
I3 I -0.03377(10) 0.15927(14) 1.2500 0.0161(4) Uani 1 2 d S T P . .
I6 I 0.10900(11) 0.50737(14) 0.2500 0.0187(5) Uani 1 2 d S T P . .
S1 S 0.1722(4) 0.1893(6) 0.2500 0.0247(17) Uani 1 2 d S T P . .
O9 O 0.1536(19) 0.200(3) 0.605(8) 0.167(14) Uani 1 1 d . U . . .
C2 C 0.1852(17) 0.035(3) 0.2500 0.036(8) Uani 1 2 d S TU P . .
H2A H 0.1474 -0.0031 0.3778 0.054 Uiso 0.5 1 calc GR . . A -1
H2B H 0.2355 0.0157 0.3245 0.054 Uiso 0.5 1 calc GR . . A -1
H2C H 0.1799 0.0038 0.0477 0.054 Uiso 0.5 1 calc GR . . A -1
C3 C 0.2605(18) 0.239(3) 0.2500 0.034(8) Uani 1 2 d S T P . .
H3A H 0.2621 0.3201 0.3336 0.051 Uiso 0.5 1 calc GR . . B -1
H3B H 0.2796 0.2407 0.0464 0.051 Uiso 0.5 1 calc GR . . B -1
H3C H 0.2918 0.1853 0.3699 0.051 Uiso 0.5 1 calc GR . . B -1
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
I3 Pb1 I3 91.60(5) 1_554 .
I3 Pb1 I6 174.15(5) . .
I3 Pb1 I6 174.15(5) 1_554 1_556
I3 Pb1 I6 91.31(3) 1_554 .
I3 Pb1 I6 91.31(3) . 1_556
I3 Pb1 I6 89.64(5) 1_554 5_566
I3 Pb1 I6 89.64(5) . 5_566
I6 Pb1 I6 85.30(5) 5_566 1_556
I6 Pb1 I6 85.30(5) 5_566 .
I6 Pb1 I6 85.35(5) . 1_556
O9 Pb1 I3 103.5(8) . .
O9 Pb1 I3 81.8(8) . 1_554
O9 Pb1 I3 103.5(8) 6_557 1_554
O9 Pb1 I3 81.8(8) 6_557 .
O9 Pb1 I6 102.4(8) 6_557 .
O9 Pb1 I6 164.4(8) . 5_566
O9 Pb1 I6 102.4(8) . 1_556
O9 Pb1 I6 164.4(8) 6_557 5_566
O9 Pb1 I6 81.9(8) 6_557 1_556
O9 Pb1 I6 81.9(8) . .
O9 Pb1 O9 30.4(17) . 6_557
Pb1 I3 Pb1 91.60(5) . 1_556
Pb1 I6 Pb1 85.35(5) 1_554 .
Pb1 I6 Pb1 94.70(5) 5_566 1_554
Pb1 I6 Pb1 94.70(5) 5_566 .
O9 S1 O9 155(2) . 6_556
O9 S1 C2 95.5(11) 6_556 .
O9 S1 C2 95.5(11) . .
O9 S1 C3 99.7(12) 6_556 .
O9 S1 C3 99.7(12) . .
C3 S1 C2 101.8(15) . .
S1 O9 Pb1 117.2(17) . .
O9 O9 Pb1 74.8(8) 6_557 .
O9 O9 S1 167.6(12) 6_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I3 3.1484(14) 1_554
Pb1 I3 3.1484(14) .
Pb1 I6 3.3299(15) 1_556
Pb1 I6 3.3299(15) .
Pb1 I6 3.299(2) 5_566
Pb1 O9 2.49(3) .
Pb1 O9 2.49(3) 6_557
I3 Pb1 3.1484(14) 1_556
I6 Pb1 3.299(2) 5_566
I6 Pb1 3.3299(15) 1_554
S1 O9 1.64(4) .
S1 O9 1.64(4) 6_556
S1 C2 1.74(3) .
S1 C3 1.67(3) .
O9 O9 1.31(7) 6_557
