#------------------------------------------------------------------------------
#$Date: 2019-11-25 08:11:49 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240463 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/98/4129810.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_4129810
loop_
_publ_author_name
'Guo, Yunlong'
'Shoyama, Kazutaka'
'Sato, Wataru'
'Matsuo, Yutaka'
'Inoue, Kento'
'Harano, Koji'
'Liu, Chao'
'Tanaka, Hideyuki'
'Nakamura, Eiichi'
_publ_section_title
;
 Chemical Pathways Connecting Lead(II) Iodide and Perovskite via Polymeric
 Plumbate(II) Fiber.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15907
_journal_page_last               15914
_journal_paper_doi               10.1021/jacs.5b10599
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C2 H6 I2 O Pb S'
_chemical_formula_sum            'C2 H6 I2 O Pb S'
_chemical_formula_weight         539.12
_chemical_name_common            INT-2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7962(11)
_cell_length_b                   4.5112(3)
_cell_length_c                   11.1382(6)
_cell_measurement_reflns_used    905
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      68.195
_cell_measurement_theta_min      7.957
_cell_volume                     894.20(9)
_computing_cell_refinement       'Rapid Auto (Rigaku)'
_computing_data_collection       'Rapid Auto (Rigaku)'
_computing_data_reduction        'Rapid Auto (Rigaku)'
_computing_molecular_graphics    Mercury
_computing_publication_material  Mercury
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Rigaku Rapid II'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5527
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.195
_diffrn_reflns_theta_min         7.957
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    92.444
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.3599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical Absorption Correction March 2001 T Higashi'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    4.005
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         3.446
_refine_diff_density_min         -3.499
_refine_diff_density_rms         0.598
_refine_ls_extinction_coef       0.00011(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0758
_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)+(0.0001P)²+124.0021P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                814
_reflns_number_total             905
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b10599_si_003.cif
_cod_data_source_block           Pb2I4DMSO2
_cod_database_code               4129810
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.012
_shelx_estimated_absorpt_t_max   0.458
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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 0.45896(8) 0.7500 0.68363(13) 0.0298(6) Uani 1 2 d S T P . .
I1 I 0.60815(13) 0.7500 0.50865(19) 0.0302(7) Uani 1 2 d S T P A .
I2 I 0.53401(12) 0.2500 0.8409(2) 0.0304(7) Uani 1 2 d S T P A .
S1 S 0.3283(5) 0.2500 0.8098(8) 0.032(2) Uani 1 2 d S T P . .
O1 O 0.3423(19) 0.597(8) 0.791(3) 0.041(9) Uani 0.5 1 d . . P A 1
C1 C 0.312(3) 0.2500 0.970(3) 0.045(11) Uani 1 2 d S T P A .
H1 H 0.3022 0.4529 0.9974 0.068 Uiso 0.5 1 calc R U P . .
H1A H 0.2687 0.1245 0.9888 0.068 Uiso 0.5 1 calc R U P . .
H1B H 0.3567 0.1726 1.0114 0.068 Uiso 0.5 1 calc R U P . .
C2 C 0.234(2) 0.2500 0.753(4) 0.058(13) Uani 1 2 d S T P A .
H2 H 0.2133 0.4516 0.7566 0.087 Uiso 0.5 1 calc R U P . .
H2A H 0.2336 0.1804 0.6698 0.087 Uiso 0.5 1 calc R U P . .
H2B H 0.2026 0.1180 0.8023 0.087 Uiso 0.5 1 calc R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'
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 32.2(16) . 8_575
O1 Pb1 I2 83.5(8) . .
O1 Pb1 I2 106.5(8) 8_575 .
O1 Pb1 I2 106.5(8) . 1_565
O1 Pb1 I2 83.5(8) 8_575 1_565
I2 Pb1 I2 91.35(7) . 1_565
O1 Pb1 I1 162.8(8) . .
O1 Pb1 I1 162.8(8) 8_575 .
I2 Pb1 I1 89.28(6) . .
I2 Pb1 I1 89.28(6) 1_565 .
O1 Pb1 I1 79.8(8) . 5_666
O1 Pb1 I1 101.5(9) 8_575 5_666
I2 Pb1 I1 91.42(4) . 5_666
I2 Pb1 I1 173.39(7) 1_565 5_666
I1 Pb1 I1 84.75(6) . 5_666
O1 Pb1 I1 101.5(8) . 5_676
O1 Pb1 I1 79.8(8) 8_575 5_676
I2 Pb1 I1 173.39(7) . 5_676
I2 Pb1 I1 91.42(4) 1_565 5_676
I1 Pb1 I1 84.75(6) . 5_676
I1 Pb1 I1 85.22(6) 5_666 5_676
Pb1 I1 Pb1 95.25(6) . 5_666
Pb1 I1 Pb1 95.25(6) . 5_676
Pb1 I1 Pb1 85.22(6) 5_666 5_676
Pb1 I2 Pb1 91.35(7) . 1_545
O1 S1 O1 157(3) 8_565 .
O1 S1 C2 95.8(14) 8_565 .
O1 S1 C2 95.8(14) . .
O1 S1 C1 98.7(14) 8_565 .
O1 S1 C1 98.7(14) . .
C2 S1 C1 101(2) . .
O1 O1 S1 168.3(13) 8_575 .
O1 O1 Pb1 73.9(8) 8_575 .
S1 O1 Pb1 117.6(18) . .
S1 C1 H1 109.5 . .
S1 C1 H1A 109.5 . .
H1 C1 H1A 109.5 . .
S1 C1 H1B 109.5 . .
H1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
S1 C2 H2 109.5 . .
S1 C2 H2A 109.5 . .
H2 C2 H2A 109.5 . .
S1 C2 H2B 109.5 . .
H2 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.50(3) .
Pb1 O1 2.50(3) 8_575
Pb1 I2 3.1531(18) .
Pb1 I2 3.1531(18) 1_565
Pb1 I1 3.294(3) .
Pb1 I1 3.3317(19) 5_666
Pb1 I1 3.3317(19) 5_676
I1 Pb1 3.3317(19) 5_666
I1 Pb1 3.3317(19) 5_676
I2 Pb1 3.1531(18) 1_545
S1 O1 1.60(3) 8_565
S1 O1 1.60(3) .
S1 C2 1.80(4) .
S1 C1 1.81(4) .
O1 O1 1.38(7) 8_575
C1 H1 0.9800 .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C2 H2 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 S1 O1 O1 179.99(15) 8_565 8_575
C2 S1 O1 O1 60(7) . 8_575
C1 S1 O1 O1 -42(7) . 8_575
O1 S1 O1 Pb1 -10(9) 8_565 .
C2 S1 O1 Pb1 -130(2) . .
C1 S1 O1 Pb1 128(2) . .
