#------------------------------------------------------------------------------
#$Date: 2019-11-25 08:12:03 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240464 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/98/4129811.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_4129811
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 I2 O2 Pb S2, 4(C0.50)'
_chemical_formula_sum            'C4 I2 O2 Pb S2'
_chemical_formula_weight         605.15
_chemical_name_common            INT-1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   notdet
_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            2
_cell_length_a                   11.0774(7)
_cell_length_b                   13.8442(8)
_cell_length_c                   4.5169(3)
_cell_measurement_reflns_used    398
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.153
_cell_measurement_theta_min      5.114
_cell_volume                     692.70(8)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.1488
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3710
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.153
_diffrn_reflns_theta_min         5.114
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    61.241
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Empirical Absorption Correction March 2001 T Higashi'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         2.193
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.292
_refine_ls_extinction_coef       0.0075(5)
_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   1.193
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0470
_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)+(0.0315P)²+4.0515P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                385
_reflns_number_total             398
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b10599_si_002.cif
_cod_data_source_block           PbI2DMSO2
_cod_database_code               4129811
_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   0.016
_shelx_estimated_absorpt_t_max   0.084
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'-x+1/2, y+1/2, z'
'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
Pb1 Pb 0.5000 0.5000 0.5000 0.0377(5) Uani 1 8 d S T P
I1 I 0.29031(9) 0.5000 0.0000 0.0501(6) Uani 1 4 d S T P
S1 S 0.5729(9) 0.7577(7) 0.655(2) 0.061(2) Uani 0.25 1 d . . P
O1 O 0.5000 0.6799(8) 0.5000 0.092(6) Uani 1 4 d S T P
C1 C 0.5000 0.8659(13) 0.5000 0.104(9) Uani 1 4 d S T P
C2 C 0.711(2) 0.748(3) 0.5000 0.102(12) Uani 0.5 2 d S T 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'
O O 0.0492 0.0322 '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'
C C 0.0181 0.0091 '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 180.0 9_666 .
O1 Pb1 I1 90.0 9_666 9_666
O1 Pb1 I1 90.0 . 9_666
O1 Pb1 I1 90.0 9_666 1_556
O1 Pb1 I1 90.000(1) . 1_556
I1 Pb1 I1 91.61(3) 9_666 1_556
O1 Pb1 I1 90.0 9_666 9_665
O1 Pb1 I1 90.000(1) . 9_665
I1 Pb1 I1 88.39(3) 9_666 9_665
I1 Pb1 I1 180.0 1_556 9_665
O1 Pb1 I1 90.0 9_666 .
O1 Pb1 I1 90.0 . .
I1 Pb1 I1 180.0 9_666 .
I1 Pb1 I1 88.39(3) 1_556 .
I1 Pb1 I1 91.61(3) 9_665 .
Pb1 I1 Pb1 88.39(3) . 1_554
S1 S1 O1 62.6(4) 10_556 .
S1 S1 S1 89.999(2) 10_556 11_655
O1 S1 S1 57.8(4) . 11_655
S1 S1 C2 65.5(6) 10_556 .
O1 S1 C2 103.6(11) . .
S1 S1 C2 155.0(6) 11_655 .
S1 S1 C1 67.7(4) 10_556 .
O1 S1 C1 99.7(8) . .
S1 S1 C1 63.9(4) 11_655 .
C2 S1 C1 107.8(11) . .
S1 S1 S1 49.1(5) 10_556 4_656
O1 S1 S1 45.2(5) . 4_656
S1 S1 S1 40.9(5) 11_655 4_656
C2 S1 S1 114.5(9) . 4_656
C1 S1 S1 54.5(5) . 4_656
S1 O1 S1 89.5(11) 10_556 11_655
S1 O1 S1 64.3(9) 10_556 4_656
S1 O1 S1 54.9(8) 11_655 4_656
S1 O1 S1 54.9(8) 10_556 .
S1 O1 S1 64.3(9) 11_655 .
S1 O1 S1 89.5(11) 4_656 .
S1 O1 Pb1 135.2(5) 10_556 .
S1 O1 Pb1 135.2(5) 11_655 .
S1 O1 Pb1 135.2(5) 4_656 .
S1 O1 Pb1 135.2(5) . .
S1 C1 S1 71.0(9) . 4_656
S1 C1 S1 52.1(7) . 11_655
S1 C1 S1 44.7(7) 4_656 11_655
S1 C1 S1 44.7(7) . 10_556
S1 C1 S1 52.1(7) 4_656 10_556
S1 C1 S1 71.0(9) 11_655 10_556
C2 C2 S1 154.2(19) 13_666 .
C2 C2 S1 154.2(19) 13_666 10_556
S1 C2 S1 49.0(11) . 10_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.491(12) 9_666
Pb1 O1 2.491(12) .
Pb1 I1 3.2397(8) 9_666
Pb1 I1 3.2397(8) 1_556
Pb1 I1 3.2397(8) 9_665
Pb1 I1 3.2398(8) .
I1 Pb1 3.2398(8) 1_554
S1 S1 1.40(2) 10_556
S1 O1 1.518(13) .
S1 S1 1.62(2) 11_655
S1 C2 1.69(3) .
S1 C1 1.839(18) .
S1 S1 2.14(2) 4_656
O1 S1 1.517(13) 10_556
O1 S1 1.517(13) 11_655
O1 S1 1.517(13) 4_656
C1 S1 1.839(18) 4_656
C1 S1 1.839(18) 11_655
C1 S1 1.839(18) 10_556
C2 C2 0.87(5) 13_666
C2 S1 1.69(3) 10_556
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
S1 S1 O1 S1 109.1(5) 11_655 10_556
C2 S1 O1 S1 -52.7(10) . 10_556
C1 S1 O1 S1 58.4(5) . 10_556
S1 S1 O1 S1 58.4(5) 4_656 10_556
S1 S1 O1 S1 -109.1(5) 10_556 11_655
C2 S1 O1 S1 -161.7(9) . 11_655
C1 S1 O1 S1 -50.6(6) . 11_655
S1 S1 O1 S1 -50.6(6) 4_656 11_655
S1 S1 O1 S1 -58.4(5) 10_556 4_656
S1 S1 O1 S1 50.6(6) 11_655 4_656
C2 S1 O1 S1 -111.1(11) . 4_656
C1 S1 O1 S1 0.001(2) . 4_656
S1 S1 O1 Pb1 121.6(5) 10_556 .
S1 S1 O1 Pb1 -129.4(6) 11_655 .
C2 S1 O1 Pb1 68.9(11) . .
C1 S1 O1 Pb1 180.000(3) . .
S1 S1 O1 Pb1 179.999(3) 4_656 .
S1 S1 C1 S1 54.8(5) 10_556 4_656
O1 S1 C1 S1 -0.001(2) . 4_656
S1 S1 C1 S1 -46.7(6) 11_655 4_656
C2 S1 C1 S1 107.8(12) . 4_656
S1 S1 C1 S1 101.6(3) 10_556 11_655
O1 S1 C1 S1 46.7(6) . 11_655
C2 S1 C1 S1 154.6(9) . 11_655
S1 S1 C1 S1 46.7(5) 4_656 11_655
O1 S1 C1 S1 -54.8(5) . 10_556
S1 S1 C1 S1 -101.6(3) 11_655 10_556
C2 S1 C1 S1 53.0(11) . 10_556
S1 S1 C1 S1 -54.8(5) 4_656 10_556
S1 S1 C2 C2 160(13) 10_556 13_666
O1 S1 C2 C2 -149(12) . 13_666
S1 S1 C2 C2 172(10) 11_655 13_666
C1 S1 C2 C2 106(12) . 13_666
S1 S1 C2 C2 165(12) 4_656 13_666
O1 S1 C2 S1 50.8(10) . 10_556
S1 S1 C2 S1 12(3) 11_655 10_556
C1 S1 C2 S1 -54.2(10) . 10_556
S1 S1 C2 S1 4.1(11) 4_656 10_556
