#------------------------------------------------------------------------------
#$Date: 2019-11-22 23:34:15 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231575 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/34/4003401.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_4003401
loop_
_publ_author_name
'Oswald, Iain W. H.'
'Koegel, Alexandra A.'
'Neilson, James R.'
_publ_section_title
;
 General Synthesis Principles for Ruddlesden--Popper Hybrid Perovskite
 Halides from a Dynamic Equilibrium
;
_journal_issue                   23
_journal_name_full               'Chemistry of Materials'
_journal_page_first              8606
_journal_paper_doi               10.1021/acs.chemmater.8b03817
_journal_volume                  30
_journal_year                    2018
_chemical_formula_sum            'C20 H1.25 I10 N6 Pb3'
_chemical_formula_weight         2216.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-06-26 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   54.188(4)
_cell_length_b                   8.9661(6)
_cell_length_c                   8.7984(6)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      3.01
_cell_volume                     4274.7(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'APEX3 (Bruker-AXS, 2015)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'VESTA (Momma and Izumi, 2017)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      302(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'HELIOS optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1446
_diffrn_reflns_av_unetI/netI     0.0937
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       68
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            31226
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.815
_diffrn_reflns_theta_min         2.302
_diffrn_source                   'I\ms microfocus tube'
_exptl_absorpt_coefficient_mu    19.028
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    3.443
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3757
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.655
_refine_diff_density_min         -2.190
_refine_diff_density_rms         0.430
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.28(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         4589
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1468
_refine_ls_R_factor_gt           0.0723
_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)+(0.1083P)²+26.8974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.2174
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2438
_reflns_number_total             4589
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b03817_si_005.cif
_cod_data_source_block           shelx
_cod_database_code               4003401
_shelx_shelxl_version_number     2017/1
_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.
;
_publcif_funding_html
;
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-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 0.500000 0.2468(2) 0.4317(5) 0.0396(5) Uani 1 2 d S T P
Pb2 Pb 0.61886(2) 0.24967(18) 0.4325(3) 0.0397(4) Uani 1 1 d . . .
I1 I 0.61420(6) 0.5415(4) 0.2270(5) 0.0604(10) Uani 1 1 d . . .
I2 I 0.500000 0.0472(5) 0.7286(8) 0.0716(15) Uani 1 2 d S T P
I3 I 0.55852(4) 0.2442(4) 0.4356(10) 0.0683(8) Uani 1 1 d . . .
I4 I 0.67564(5) 0.2942(4) 0.4131(5) 0.0636(9) Uani 1 1 d . . .
I5 I 0.500000 0.5400(6) 0.6385(8) 0.0746(17) Uani 1 2 d S T P
I6 I 0.61932(7) 0.0392(4) 0.1440(5) 0.0702(12) Uani 1 1 d . . .
C1 C 0.552(2) 0.804(14) 0.521(15) 0.23(4) Uiso 1 1 d D . .
H1A H 0.549227 0.905342 0.487274 0.339 Uiso 1 1 calc R U .
H1B H 0.563682 0.801891 0.599999 0.339 Uiso 1 1 calc R U .
H1C H 0.536162 0.766079 0.558915 0.339 Uiso 1 1 calc R U .
N1 N 0.5596(15) 0.715(11) 0.396(15) 0.23(4) Uiso 1 1 d D . .
H1D H 0.560419 0.619533 0.424521 0.339 Uiso 1 1 calc R U .
H1E H 0.574497 0.744873 0.365757 0.339 Uiso 1 1 calc R U .
H1F H 0.549020 0.723461 0.318971 0.339 Uiso 1 1 calc R U .
N2 N 0.6617(8) 0.319(5) 1.000(5) 0.081(13) Uiso 1 1 d . . .
H2A H 0.656803 0.277074 1.086438 0.122 Uiso 1 1 calc R U .
H2B H 0.648762 0.359892 0.953355 0.122 Uiso 1 1 calc R U .
H2C H 0.672781 0.389882 1.020209 0.122 Uiso 1 1 calc R U .
C2 C 0.6727(11) 0.207(7) 0.902(10) 0.10(2) Uiso 1 1 d . . .
H2D H 0.670337 0.235461 0.796765 0.125 Uiso 1 1 calc R U .
H2E H 0.664400 0.112440 0.918067 0.125 Uiso 1 1 calc R U .
C3 C 0.7001(8) 0.187(5) 0.932(7) 0.062(11) Uiso 1 1 d . . .
C4 C 0.7169(9) 0.270(5) 0.845(6) 0.064(13) Uiso 1 1 d . . .
H4 H 0.711691 0.344036 0.778731 0.076 Uiso 1 1 calc R U .
C5 C 0.7312(12) 0.055(8) 1.051(8) 0.10(2) Uiso 1 1 d . . .
H5 H 0.736394 -0.022655 1.113567 0.124 Uiso 1 1 calc R U .
C6 C 0.7492(10) 0.142(8) 0.978(7) 0.094(19) Uiso 1 1 d . . .
H6 H 0.765657 0.134960 1.006049 0.113 Uiso 1 1 calc R U .
C7 C 0.7420(10) 0.236(6) 0.864(6) 0.077(16) Uiso 1 1 d . . .
H7 H 0.753717 0.277518 0.798729 0.093 Uiso 1 1 calc R U .
C8 C 0.7067(11) 0.079(7) 1.035(7) 0.096(19) Uiso 1 1 d . . .
H8 H 0.695081 0.025299 1.089900 0.115 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'
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'
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
I2 Pb1 I3 89.26(13) . .
I2 Pb1 I3 89.26(13) . 4_655
I3 Pb1 I3 178.5(3) . 4_655
I2 Pb1 I2 89.72(7) . 2_654
I3 Pb1 I2 90.01(11) . 2_654
I3 Pb1 I2 90.01(11) 4_655 2_654
I2 Pb1 I5 89.7(2) . .
I3 Pb1 I5 89.99(11) . .
I3 Pb1 I5 89.99(11) 4_655 .
I2 Pb1 I5 179.5(3) 2_654 .
I2 Pb1 I5 177.9(2) . 2_664
I3 Pb1 I5 90.74(13) . 2_664
I3 Pb1 I5 90.74(13) 4_655 2_664
I2 Pb1 I5 92.4(2) 2_654 2_664
I5 Pb1 I5 88.15(7) . 2_664
I4 Pb2 I6 91.42(11) . .
I4 Pb2 I6 97.37(10) . 3
I6 Pb2 I6 89.07(5) . 3
I4 Pb2 I1 86.68(10) . .
I6 Pb2 I1 92.03(16) . .
I6 Pb2 I1 175.78(10) 3 .
I4 Pb2 I1 92.71(10) . 3_565
I6 Pb2 I1 175.87(10) . 3_565
I6 Pb2 I1 90.18(16) 3 3_565
I1 Pb2 I1 88.44(5) . 3_565
I4 Pb2 I3 172.95(11) . .
I6 Pb2 I3 90.34(14) . .
I6 Pb2 I3 89.48(13) 3 .
I1 Pb2 I3 86.44(12) . .
I1 Pb2 I3 85.59(14) 3_565 .
Pb2 I1 Pb2 158.50(17) . 3_564
Pb1 I2 Pb1 158.6(3) . 2_655
Pb1 I3 Pb2 178.3(2) . .
Pb1 I5 Pb1 161.2(3) . 2_665
Pb2 I6 Pb2 162.32(17) . 3_554
N2 C2 C3 112(5) . .
C8 C3 C4 124(5) . .
C8 C3 C2 117(5) . .
C4 C3 C2 119(5) . .
C3 C4 C7 117(5) . .
C8 C5 C6 123(7) . .
C7 C6 C5 119(6) . .
C6 C7 C4 119(5) . .
C5 C8 C3 116(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.166(7) .
Pb1 I3 3.171(2) .
Pb1 I3 3.172(2) 4_655
Pb1 I2 3.184(6) 2_654
Pb1 I5 3.197(7) .
Pb1 I5 3.211(7) 2_664
Pb2 I4 3.107(3) .
Pb2 I6 3.162(5) .
Pb2 I6 3.190(5) 3
Pb2 I1 3.190(4) .
Pb2 I1 3.207(5) 3_565
Pb2 I3 3.270(3) .
C1 N1 1.43(6) .
N2 C2 1.45(7) .
C2 C3 1.52(7) .
C3 C8 1.37(8) .
C3 C4 1.40(7) .
C4 C7 1.40(7) .
C5 C8 1.35(7) .
C5 C6 1.40(8) .
C6 C7 1.37(7) .
