#------------------------------------------------------------------------------
#$Date: 2019-11-25 13:34:41 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240984 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/05/4130584.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_4130584
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            'C3 H7 I2 N O Pb'
_chemical_formula_weight         534.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 92.661(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.53212(12)
_cell_length_b                   18.2385(5)
_cell_length_c                   11.5566(4)
_cell_measurement_reflns_used    2081
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9660
_cell_measurement_theta_min      3.6460
_cell_volume                     954.23(5)
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4577
_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         27.480
_diffrn_reflns_theta_min         3.530
_exptl_absorpt_coefficient_mu    24.083
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.718
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_refine_diff_density_max         2.775
_refine_diff_density_min         -2.915
_refine_diff_density_rms         0.446
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         2181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0843
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1972
_reflns_number_total             2181
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b04924_si_004.cif
_cod_data_source_block           jxj-1-150829-bingtontg
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130584
_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+1/2'
'-x, -y, -z'
'x-1/2, -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
Pb1 Pb 0.23920(6) 0.52859(2) 0.32878(3) 0.01210(12) Uani 1 1 d . .
I1 I -0.24599(10) 0.61002(3) 0.48545(5) 0.01362(15) Uani 1 1 d . .
I2 I 0.71840(11) 0.46463(3) 0.16754(5) 0.01823(16) Uani 1 1 d . .
O0AA O 0.1937(12) 0.6421(3) 0.2194(6) 0.0220(14) Uani 1 1 d . .
N2 N -0.1238(14) 0.7015(3) 0.0946(6) 0.0137(14) Uani 1 1 d . .
C4 C 0.0601(18) 0.6485(5) 0.1224(9) 0.021(2) Uani 1 1 d . .
H4 H 0.0942 0.6132 0.0666 0.025 Uiso 1 1 calc R U
C5 C -0.2592(18) 0.7069(5) -0.0225(9) 0.024(2) Uani 1 1 d . .
H5A H -0.2067 0.7530 -0.0562 0.036 Uiso 1 1 calc R U
H5B H -0.4701 0.7039 -0.0190 0.036 Uiso 1 1 calc R U
H5C H -0.1896 0.6675 -0.0691 0.036 Uiso 1 1 calc R U
C6 C -0.2075(18) 0.7557(5) 0.1798(9) 0.021(2) Uani 1 1 d . .
H6A H -0.0744 0.7529 0.2467 0.031 Uiso 1 1 calc R U
H6B H -0.4053 0.7462 0.2021 0.031 Uiso 1 1 calc R U
H6C H -0.1981 0.8039 0.1466 0.031 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'
N N 0.0061 0.0033 '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'
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
O0AA Pb1 I2 92.97(15) . .
O0AA Pb1 I2 87.97(14) . 1_455
I2 Pb1 I2 91.783(17) . 1_455
O0AA Pb1 I1 86.67(15) . 1_655
I2 Pb1 I1 90.110(15) . 1_655
I2 Pb1 I1 174.402(17) 1_455 1_655
O0AA Pb1 I1 81.84(15) . .
I2 Pb1 I1 174.618(17) . .
I2 Pb1 I1 89.489(15) 1_455 .
I1 Pb1 I1 88.152(15) 1_655 .
O0AA Pb1 I1 169.94(16) . 3_566
I2 Pb1 I1 96.588(16) . 3_566
I2 Pb1 I1 94.850(16) 1_455 3_566
I1 Pb1 I1 90.165(14) 1_655 3_566
I1 Pb1 I1 88.513(14) . 3_566
Pb1 I1 Pb1 88.152(15) 1_455 .
Pb1 I1 Pb1 89.836(14) 1_455 3_566
Pb1 I1 Pb1 91.488(14) . 3_566
Pb1 I2 Pb1 91.782(17) . 1_655
C4 O0AA Pb1 124.8(5) . .
C4 N2 C6 121.2(8) . .
C4 N2 C5 120.9(8) . .
C6 N2 C5 117.8(7) . .
O0AA C4 N2 124.4(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O0AA 2.429(6) .
Pb1 I2 3.1504(6) .
Pb1 I2 3.1615(6) 1_455
Pb1 I1 3.2459(6) 1_655
Pb1 I1 3.2694(6) .
Pb1 I1 3.3159(6) 3_566
I1 Pb1 3.2459(6) 1_455
I1 Pb1 3.3158(6) 3_566
I2 Pb1 3.1615(6) 1_655
O0AA C4 1.254(11) .
N2 C4 1.306(11) .
N2 C6 1.459(11) .
N2 C5 1.463(11) .
