#------------------------------------------------------------------------------
#$Date: 2019-10-29 23:39:34 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220466 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/30/4003047.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_4003047
loop_
_publ_author_name
'Dahlman, Clayton J.'
'DeCrescent, Ryan A.'
'Venkatesan, Naveen R.'
'Kennard, Rhys M.'
'Wu, Guang'
'Everest, Michael A.'
'Schuller, Jon A.'
'Chabinyc, Michael L.'
_publ_section_title
;
 Controlling Solvate Intermediate Growth for Phase-Pure Organic Lead
 Iodide Ruddlesden--Popper (C4H9NH3)2(CH3NH3)n−1PbnI3n+1 Perovskite
 Thin Films
;
_journal_issue                   15
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5832
_journal_paper_doi               10.1021/acs.chemmater.9b01952
_journal_volume                  31
_journal_year                    2019
_chemical_formula_sum            'C7 H19 I3 N2 O Pb'
_chemical_formula_weight         735.13
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                89.59(2)
_cell_angle_beta                 82.08(2)
_cell_angle_gamma                83.28(2)
_cell_formula_units_Z            2
_cell_length_a                   4.618(6)
_cell_length_b                   12.470(17)
_cell_length_c                   15.10(2)
_cell_measurement_reflns_used    1370
_cell_measurement_temperature    260(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.72
_cell_volume                     855(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      260(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.1688
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_number            3519
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.558
_diffrn_reflns_theta_min         1.362
_exptl_absorpt_coefficient_mu    15.263
_exptl_absorpt_correction_T_max  0.745376
_exptl_absorpt_correction_T_min  0.457690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.855
_exptl_crystal_description       needle
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.508
_refine_diff_density_min         -1.792
_refine_diff_density_rms         0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         3519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.1146
_refine_ls_R_factor_gt           0.0492
_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)+(0.0322P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1976
_reflns_number_total             3519
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm9b01952_si_003.cif
_cod_data_source_block           twin4
_cod_database_code               4003047
_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   0.150
_shelx_estimated_absorpt_t_max   0.516
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Pb1 Pb 0.85384(10) 0.40911(4) 0.86876(3) 0.03270(16) Uani 1 1 d . .
I1 I 0.27557(16) 0.59709(6) 0.89850(5) 0.0343(2) Uani 1 1 d . .
I3 I 0.94365(18) 0.44560(7) 0.66833(5) 0.0405(2) Uani 1 1 d . .
I2 I 0.41786(18) 0.23037(7) 0.85965(6) 0.0453(3) Uani 1 1 d . .
O005 O 0.8123(18) 0.7838(6) 0.7145(6) 0.046(2) Uani 1 1 d . .
N2 N 0.385(2) 0.6661(7) 0.6517(6) 0.047(3) Uani 1 1 d . .
H2A H 0.5195 0.7002 0.6731 0.070 Uiso 1 1 calc R U
H2B H 0.3998 0.5978 0.6698 0.070 Uiso 1 1 calc R U
H2G H 0.2059 0.6986 0.6718 0.070 Uiso 1 1 calc R U
N1 N 0.908(2) 0.8932(8) 0.8226(7) 0.044(3) Uani 1 1 d . .
C1 C 0.794(3) 0.8112(10) 0.7919(9) 0.047(4) Uani 1 1 d . .
H1 H 0.6885 0.7704 0.8340 0.056 Uiso 1 1 calc R U
C00A C 0.433(3) 0.6687(12) 0.5519(8) 0.060(4) Uani 1 1 d . .
H00A H 0.2887 0.6305 0.5282 0.072 Uiso 1 1 calc R U
H00B H 0.6275 0.6335 0.5296 0.072 Uiso 1 1 calc R U
C3 C 1.074(3) 0.9620(11) 0.7644(10) 0.071(5) Uani 1 1 d . .
H3A H 1.2723 0.9559 0.7777 0.107 Uiso 1 1 calc R U
H3B H 0.9857 1.0355 0.7732 0.107 Uiso 1 1 calc R U
H3C H 1.0743 0.9408 0.7034 0.107 Uiso 1 1 calc R U
C2 C 0.878(4) 0.9179(12) 0.9181(9) 0.102(7) Uani 1 1 d . .
H2C H 0.7457 0.8728 0.9505 0.153 Uiso 1 1 calc R U
H2F H 0.8008 0.9923 0.9283 0.153 Uiso 1 1 calc R U
H2E H 1.0670 0.9049 0.9382 0.153 Uiso 1 1 calc R U
C4 C 0.403(4) 0.7880(14) 0.5216(10) 0.102(7) Uani 1 1 d . .
H4A H 0.2111 0.8215 0.5487 0.123 Uiso 1 1 calc R U
H4B H 0.5487 0.8233 0.5470 0.123 Uiso 1 1 calc R U
C5 C 0.429(5) 0.8111(15) 0.4333(13) 0.132(8) Uani 1 1 d . .
H5A H 0.2919 0.7714 0.4078 0.159 Uiso 1 1 calc R U
H5B H 0.6252 0.7804 0.4074 0.159 Uiso 1 1 calc R U
C6 C 0.389(4) 0.9172(13) 0.4018(11) 0.120(7) Uani 1 1 d . .
H6A H 0.1927 0.9492 0.4229 0.179 Uiso 1 1 calc R U
H6B H 0.4194 0.9163 0.3376 0.179 Uiso 1 1 calc R U
H6C H 0.5281 0.9586 0.4233 0.179 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'
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'
I I -0.4742 1.8119 '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'
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
I3 Pb1 I2 94.56(4) . .
I3 Pb1 I2 93.13(4) . 1_655
I2 Pb1 I2 92.33(11) . 1_655
I3 Pb1 I1 90.59(5) . 1_655
I2 Pb1 I1 174.47(3) . 1_655
I2 Pb1 I1 89.42(11) 1_655 1_655
I3 Pb1 I1 91.93(4) . .
I2 Pb1 I1 89.19(11) . .
I2 Pb1 I1 174.59(3) 1_655 .
I1 Pb1 I1 88.60(11) 1_655 .
Pb1 I1 Pb1 88.60(11) 1_455 .
Pb1 I2 Pb1 92.33(11) . 1_455
C00A N2 H2A 109.5 . .
C00A N2 H2B 109.5 . .
H2A N2 H2B 109.5 . .
C00A N2 H2G 109.5 . .
H2A N2 H2G 109.5 . .
H2B N2 H2G 109.5 . .
C1 N1 C3 122.0(11) . .
C1 N1 C2 122.0(12) . .
C3 N1 C2 116.0(12) . .
O005 C1 N1 126.4(12) . .
O005 C1 H1 116.8 . .
N1 C1 H1 116.8 . .
N2 C00A C4 108.8(11) . .
N2 C00A H00A 109.9 . .
C4 C00A H00A 109.9 . .
N2 C00A H00B 109.9 . .
C4 C00A H00B 109.9 . .
H00A C00A H00B 108.3 . .
N1 C3 H3A 109.5 . .
N1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N1 C2 H2C 109.5 . .
N1 C2 H2F 109.5 . .
H2C C2 H2F 109.5 . .
N1 C2 H2E 109.5 . .
H2C C2 H2E 109.5 . .
H2F C2 H2E 109.5 . .
C5 C4 C00A 119.8(16) . .
C5 C4 H4A 107.4 . .
C00A C4 H4A 107.4 . .
C5 C4 H4B 107.4 . .
C00A C4 H4B 107.4 . .
H4A C4 H4B 106.9 . .
C4 C5 C6 122.4(18) . .
C4 C5 H5A 106.7 . .
C6 C5 H5A 106.7 . .
C4 C5 H5B 106.7 . .
C6 C5 H5B 106.7 . .
H5A C5 H5B 106.6 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I3 3.035(4) .
Pb1 I2 3.189(3) .
Pb1 I2 3.212(3) 1_655
Pb1 I1 3.288(3) 1_655
Pb1 I1 3.324(3) .
I1 Pb1 3.288(3) 1_455
I2 Pb1 3.212(3) 1_455
O005 C1 1.209(14) .
N2 C00A 1.493(14) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2G 0.8900 .
N1 C1 1.318(14) .
N1 C3 1.433(15) .
N1 C2 1.460(16) .
C1 H1 0.9300 .
C00A C4 1.550(19) .
C00A H00A 0.9700 .
C00A H00B 0.9700 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C2 H2C 0.9600 .
C2 H2F 0.9600 .
C2 H2E 0.9600 .
C4 C5 1.35(2) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.402(19) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
