#------------------------------------------------------------------------------
#$Date: 2019-11-25 08:12:16 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/98/4129812.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_4129812
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         539.13
_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                   17.9494(9)
_cell_length_b                   4.5326(2)
_cell_length_c                   11.2165(6)
_cell_measurement_reflns_used    9143
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.226
_cell_measurement_theta_min      4.649
_cell_volume                     912.55(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.1011
_diffrn_reflns_av_unetI/netI     0.0661
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9143
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         68.226
_diffrn_reflns_theta_min         4.649
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    90.585
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3576
_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    3.924
_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         2.076
_refine_diff_density_min         -2.074
_refine_diff_density_rms         0.369
_refine_ls_extinction_coef       0.00016(4)
_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   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0646
_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)+(0.0416P)²+18.7748P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                826
_reflns_number_total             955
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja5b10599_si_004.cif
_cod_data_source_block           Pb2I4DMSO2
_cod_database_code               4129812
_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.
;
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
Pb1 Pb 0.45956(5) 0.7500 0.68341(9) 0.0444(4) Uani 1 2 d S T P
I1 I 0.60726(9) 0.7500 0.50764(14) 0.0456(5) Uani 1 2 d S T P
I2 I 0.53424(9) 0.2500 0.83884(15) 0.0481(5) Uani 1 2 d S T P
S1 S 0.3292(3) 1.2500 0.8103(6) 0.0454(16) Uani 1 2 d S T P
O1 O 0.3430(12) 0.906(5) 0.793(2) 0.054(7) Uani 0.5 1 d . . P
C1 C 0.3147(18) 1.2500 0.965(2) 0.064(9) Uani 1 2 d S T P
H1 H 0.3052 1.4478 0.9912 0.096 Uiso 0.5 1 calc R U P
H1A H 0.2727 1.1273 0.9834 0.096 Uiso 0.5 1 calc R U P
H1B H 0.3583 1.1750 1.0039 0.096 Uiso 0.5 1 calc R U P
C2 C 0.2368(15) 1.2500 0.760(2) 0.068(9) Uani 1 2 d S T P
H2 H 0.2172 1.4469 0.7631 0.102 Uiso 0.5 1 calc R U P
H2A H 0.2353 1.1802 0.6789 0.102 Uiso 0.5 1 calc R U P
H2B H 0.2073 1.1228 0.8093 0.102 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 32.5(11) 8_575 .
O1 Pb1 I2 83.2(6) 8_575 .
O1 Pb1 I2 106.5(5) . .
O1 Pb1 I2 106.5(5) 8_575 1_565
O1 Pb1 I2 83.2(6) . 1_565
I2 Pb1 I2 91.73(5) . 1_565
O1 Pb1 I1 162.6(5) 8_575 .
O1 Pb1 I1 162.6(5) . .
I2 Pb1 I1 89.36(4) . .
I2 Pb1 I1 89.36(4) 1_565 .
O1 Pb1 I1 79.9(5) 8_575 5_666
O1 Pb1 I1 101.8(6) . 5_666
I2 Pb1 I1 91.13(3) . 5_666
I2 Pb1 I1 173.26(5) 1_565 5_666
I1 Pb1 I1 84.57(4) . 5_666
O1 Pb1 I1 101.8(6) 8_575 5_676
O1 Pb1 I1 79.9(5) . 5_676
I2 Pb1 I1 173.26(5) . 5_676
I2 Pb1 I1 91.13(3) 1_565 5_676
I1 Pb1 I1 84.57(4) . 5_676
I1 Pb1 I1 85.41(4) 5_666 5_676
Pb1 I1 Pb1 95.43(4) . 5_666
Pb1 I1 Pb1 95.43(4) . 5_676
Pb1 I1 Pb1 85.41(4) 5_666 5_676
Pb1 I2 Pb1 91.73(5) . 1_545
O1 S1 O1 157.2(17) . 8_585
O1 S1 C1 98.2(9) . .
O1 S1 C1 98.2(9) 8_585 .
O1 S1 C2 96.2(9) . .
O1 S1 C2 96.2(9) 8_585 .
C1 S1 C2 100.4(14) . .
O1 O1 S1 168.6(9) 8_575 .
O1 O1 Pb1 73.7(5) 8_575 .
S1 O1 Pb1 117.6(12) . .
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 2.53(2) 8_575
Pb1 O1 2.53(2) .
Pb1 I2 3.1578(13) .
Pb1 I2 3.1578(13) 1_565
Pb1 I1 3.3038(19) .
Pb1 I1 3.3416(13) 5_666
Pb1 I1 3.3416(13) 5_676
I1 Pb1 3.3417(13) 5_666
I1 Pb1 3.3417(13) 5_676
I2 Pb1 3.1578(13) 1_545
S1 O1 1.59(2) .
S1 O1 1.59(2) 8_585
S1 C1 1.75(2) .
S1 C2 1.75(3) .
O1 O1 1.42(5) 8_575
C1 H1 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C2 H2 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
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 180.00(11) 8_585 8_575
C1 S1 O1 O1 44(5) . 8_575
C2 S1 O1 O1 -57(5) . 8_575
O1 S1 O1 Pb1 8(6) 8_585 .
C1 S1 O1 Pb1 -127.8(14) . .
C2 S1 O1 Pb1 130.7(13) . .
