#------------------------------------------------------------------------------
#$Date: 2020-12-19 05:33:33 +0200 (Sat, 19 Dec 2020) $
#$Revision: 260001 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/61/7706152.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_7706152
loop_
_publ_author_name
'Guo, Yuan-Yuan'
'Yang, Lin-Jie'
'McNulty, Jason A.'
'Slawin, Alexandra M. Z.'
'Lightfoot, Philip'
_publ_section_title
;
 Structural variations in (001)-oriented layered lead halide perovskites,
 templated by 1,2,4-triazolium.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17274
_journal_page_last               17280
_journal_paper_doi               10.1039/d0dt02936j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(I5 Pb1.50), 4(C2 H4 N3), 2(H2 O)'
_chemical_formula_sum            'C8 H20 I10 N12 O2 Pb3'
_chemical_formula_weight         2206.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-08-20 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6028(12)
_cell_length_b                   20.805(2)
_cell_length_c                   19.776(3)
_cell_measurement_reflns_used    6321
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.1
_cell_volume                     3951.0(9)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20834
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.659
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    20.593
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.799
_refine_diff_density_min         -1.554
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1847
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0159
_refine_ls_R_factor_gt           0.0151
_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)+(0.0161P)²+1.7211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0336
_refine_ls_wR_factor_ref         0.0338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1797
_reflns_number_total             1847
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt02936j3.cif
_cod_data_source_block           T4Pb3I10_2H2O_93K
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               7706152
_shelx_shelxl_version_number     2018/3
_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, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'x+1/2, -y, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.500000 0.500000 0.01300(7) Uani 1 4 d S T P . .
Pb2 Pb 0.500000 0.63382(2) 0.35456(2) 0.01416(6) Uani 1 2 d S T P . .
I1 I 0.500000 0.77822(2) 0.38651(2) 0.01496(8) Uani 1 2 d S T P . .
I2 I 0.500000 0.52624(2) 0.65713(2) 0.01671(8) Uani 1 2 d S T P . .
I3 I 0.73070(2) 0.61088(2) 0.47630(2) 0.01527(7) Uani 1 1 d . . . . .
I4 I 0.250000 0.64058(2) 0.250000 0.03375(11) Uani 1 2 d S T P . .
N1 N 0.5715(3) 0.56166(14) 0.82751(15) 0.0175(6) Uani 1 1 d . . . . .
H1 H 0.624312 0.589765 0.808591 0.021 Uiso 0.5 1 calc R U P . .
N2 N 0.500000 0.4801(2) 0.8844(3) 0.0320(12) Uani 1 2 d S T P . .
H2 H 0.500001 0.446230 0.909342 0.038 Uiso 1 2 calc R U P . .
N3 N 0.9294(3) 0.70940(14) 0.84030(16) 0.0200(7) Uani 1 1 d . . . . .
H3 H 0.876559 0.694610 0.808838 0.024 Uiso 0.5 1 calc R U P . .
N4 N 1.000000 0.7537(2) 0.9320(2) 0.0169(9) Uani 1 2 d S T P . .
H4 H 0.999998 0.773002 0.970448 0.020 Uiso 1 2 calc R U P . .
C1 C 0.6127(4) 0.51137(18) 0.86136(19) 0.0224(8) Uani 1 1 d . . . . .
H5 H 0.704714 0.499202 0.868372 0.027 Uiso 1 1 calc R U . . .
C2 C 0.8883(4) 0.73585(18) 0.8966(2) 0.0224(8) Uani 1 1 d . . . . .
H6 H 0.796183 0.741390 0.909849 0.027 Uiso 1 1 calc R U . . .
O1 O 0.750000 0.64436(17) 0.750000 0.0214(8) Uani 1 2 d S T P . .
H7 H 0.693600 0.622487 0.772600 0.59(17) Uiso 1 1 d R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 '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'
C C 0.0033 0.0016 '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'
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
_geom_angle_publ_flag
I2 Pb1 I2 180.0 . 9_666 ?
I2 Pb1 I3 91.107(6) . . ?
I2 Pb1 I3 88.892(6) 9_666 . ?
I2 Pb1 I3 88.894(7) . 9_666 ?
I2 Pb1 I3 91.107(7) 9_666 9_666 ?
I3 Pb1 I3 180.0 . 9_666 ?
I2 Pb1 I3 91.106(7) . 12_655 ?
I2 Pb1 I3 88.893(7) 9_666 12_655 ?
I3 Pb1 I3 86.522(11) . 12_655 ?
I3 Pb1 I3 93.478(11) 9_666 12_655 ?
I2 Pb1 I3 88.894(7) . 4_566 ?
I2 Pb1 I3 91.107(7) 9_666 4_566 ?
I3 Pb1 I3 93.478(11) . 4_566 ?
I3 Pb1 I3 86.522(12) 9_666 4_566 ?
I3 Pb1 I3 180.0 12_655 4_566 ?
I1 Pb2 I4 95.210(9) . . ?
I1 Pb2 I4 95.209(9) . 14_556 ?
I4 Pb2 I4 98.389(12) . 14_556 ?
I1 Pb2 I3 89.508(7) . . ?
I4 Pb2 I3 171.235(8) . . ?
I4 Pb2 I3 88.508(12) 14_556 . ?
I1 Pb2 I3 89.507(7) . 12_655 ?
I4 Pb2 I3 88.508(12) . 12_655 ?
I4 Pb2 I3 171.235(8) 14_556 12_655 ?
I3 Pb2 I3 84.141(14) . 12_655 ?
I1 Pb2 I2 172.099(10) . 9_666 ?
I4 Pb2 I2 89.944(9) . 9_666 ?
I4 Pb2 I2 89.944(9) 14_556 9_666 ?
I3 Pb2 I2 84.633(7) . 9_666 ?
I3 Pb2 I2 84.634(7) 12_655 9_666 ?
Pb1 I2 Pb2 76.063(7) . 9_666 ?
Pb1 I3 Pb2 75.487(8) . . ?
Pb2 I4 Pb2 174.919(15) 14_456 . ?
C1 N1 N1 107.7(2) . 12_655 ?
C1 N2 C1 107.4(5) 12_655 . ?
C2 N3 N3 107.6(2) . 12_755 ?
C2 N4 C2 107.0(4) 12_755 . ?
N1 C1 N2 108.6(3) . . ?
N3 C2 N4 108.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 I2 3.1550(6) . ?
Pb1 I2 3.1551(6) 9_666 ?
Pb1 I3 3.2326(3) . ?
Pb1 I3 3.2326(3) 9_666 ?
Pb1 I3 3.2326(3) 12_655 ?
Pb1 I3 3.2326(3) 4_566 ?
Pb2 I1 3.0699(5) . ?
Pb2 I4 3.1716(3) . ?
Pb2 I4 3.1716(3) 14_556 ?
Pb2 I3 3.3062(4) . ?
Pb2 I3 3.3063(4) 12_655 ?
Pb2 I2 3.3381(5) 9_666 ?
N1 C1 1.303(5) . ?
N1 N1 1.372(6) 12_655 ?
N2 C1 1.342(5) 12_655 ?
N2 C1 1.342(5) . ?
N3 C2 1.303(5) . ?
N3 N3 1.355(6) 12_755 ?
N4 C2 1.334(4) 12_755 ?
N4 C2 1.334(4) . ?
