#------------------------------------------------------------------------------
#$Date: 2024-08-05 20:53:54 +0300 (Mon, 05 Aug 2024) $
#$Revision: 293732 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571900.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_1571900
loop_
_publ_author_name
'Fan, Chang-Chun'
'Liu, Cheng-Dong'
'Liang, Bei-Dou'
'Ju, Tong-Yu'
'Wang, Wei'
'Jin, Ming-Liang'
'Chai, Chao-Yang'
'Zhang, Wen'
_publ_section_title
;
 Chiral three-dimensional organic-inorganic lead iodide hybrid
 semiconductors.
;
_journal_issue                   29
_journal_name_full               'Chemical science'
_journal_page_first              11374
_journal_page_last               11381
_journal_paper_doi               10.1039/d4sc00954a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'I6 Pb2, 0.5(C14 H16 N4)'
_chemical_formula_sum            'C7 H8 I6 N2 Pb2'
_chemical_formula_weight         1295.93
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-01-05 deposited with the CCDC.	2024-06-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.9279(4)
_cell_length_b                   18.7521(6)
_cell_length_c                   17.6600(5)
_cell_measurement_reflns_used    7853
_cell_measurement_temperature    239.97(10)
_cell_measurement_theta_max      30.2530
_cell_measurement_theta_min      2.2780
_cell_volume                     4281.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      239.97(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  67.00   0.50    1.50    --    5.69  38.00 -30.00  152
  2  ω     -9.00  28.00   0.50    1.50    --   -6.24 -99.00-150.00   74
  3  ω    -22.00  10.00   0.50    1.50    --   -6.24 -94.00  39.00   64
  4  ω    -74.00  -4.00   0.50    1.50    --   -6.24 -42.00 149.00  140
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0147940000
_diffrn_orient_matrix_UB_12      -0.0508550000
_diffrn_orient_matrix_UB_13      -0.0029482000
_diffrn_orient_matrix_UB_21      -0.0152481000
_diffrn_orient_matrix_UB_22      0.0039783000
_diffrn_orient_matrix_UB_23      0.0348684000
_diffrn_orient_matrix_UB_31      -0.0340868000
_diffrn_orient_matrix_UB_32      0.0202628000
_diffrn_orient_matrix_UB_33      -0.0143184000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.832
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.832
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.618
_diffrn_reflns_theta_min         2.172
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    24.349
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    4.021
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.238
_refine_diff_density_min         -2.918
_refine_diff_density_rms         0.471
_refine_ls_extinction_coef       0.000063(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0561
_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)+(0.0848P)²+77.6044P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2333
_reflns_number_total             2864
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc00954a2.cif
_cod_data_source_block           3Rac-240K
_cod_depositor_comments
'Adding full bibliography for 1571897--1571906.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               1571900
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N I Pb'
_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_max   0.085
_shelx_estimated_absorpt_t_min   0.085
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Shared sites
{N1, C1}
2. Restrained distances
 C4-C6 = C4-C7
 2.38 with sigma of 0.01
 C3-C6
 2.74 with sigma of 0.01
 C5-C7
 2.72 with sigma of 0.01
 C6-N2
 1.34 with sigma of 0.01
 C7-N2
 1.34 with sigma of 0.01
 C3-C4 = C5-C4 = C3-C7 = C5-C6
 1.37 with sigma of 0.01
 C2-C3
 1.49 with sigma of 0.01
 C4-N2
 2.74 with sigma of 0.01
 C6-C7
 2.33 with sigma of 0.01
 C3-C5
 2.36 with sigma of 0.01
 N2-C3 = N2-C5
 2.34 with sigma of 0.01
 C2-C6
 4.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(N1) = Uiso(C1)
4. Rigid body (RIGU) restrains
 C5, C6, C7, N2, C3, C4, C2, N1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C1(0.5)
6.a Riding coordinates:
 N1(H1A,H1B,H1C)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C4(H4), C5(H5), C6(H6), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.921
_oxdiff_exptl_absorpt_empirical_full_min 0.394
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.25134(2) 0.12491(2) 0.12078(2) 0.02295(19) Uani 1 1 d . . . . .
I1 I 0.27781(10) 0.000000 0.000000 0.0447(3) Uani 1 2 d S T P . .
I2 I 0.500000 0.13472(4) 0.12780(5) 0.0307(2) Uani 1 2 d S T P . .
I3 I 0.250000 0.250000 0.000000 0.0739(5) Uani 1 2 d S . P . .
I4 I 0.250000 0.00565(5) 0.250000 0.0254(2) Uani 1 2 d S T P . .
I5 I 0.250000 0.24356(5) 0.250000 0.0248(2) Uani 1 2 d S T P . .
I6 I 0.000000 0.10775(7) 0.10978(6) 0.0426(3) Uani 1 2 d S T P . .
N1 N 0.0954(14) 0.3781(6) 0.3795(8) 0.081(5) Uiso 0.5 1 d . . P . .
H1A H 0.143869 0.383244 0.344113 0.098 Uiso 0.5 1 d R U P . .
H1B H 0.093309 0.417124 0.408203 0.098 Uiso 0.5 1 d R U P . .
H1C H 0.110249 0.340504 0.408203 0.098 Uiso 0.5 1 d R U P . .
N2 N 0.000000 0.4374(5) 0.1429(6) 0.066(4) Uani 1 2 d DS T P . .
H2 H 0.000000 0.477823 0.119831 0.079 Uiso 1 2 calc R U P . .
C1 C 0.0954(14) 0.3781(6) 0.3795(8) 0.081(5) Uiso 0.5 1 d . . P . .
C2 C 0.000000 0.3671(12) 0.3419(6) 0.083(6) Uani 1 2 d DS TU P . .
C3 C 0.000000 0.3724(5) 0.2568(5) 0.040(3) Uani 1 2 d DS T P . .
C4 C 0.000000 0.3094(4) 0.2164(6) 0.051(3) Uani 1 2 d DS T P . .
H4 H 0.000000 0.265700 0.241312 0.061 Uiso 1 2 calc R U P . .
C5 C 0.000000 0.3126(5) 0.1387(6) 0.059(4) Uani 1 2 d DS TU P . .
H5 H 0.000000 0.270595 0.110616 0.071 Uiso 1 2 calc R U P . .
C6 C 0.000000 0.3769(6) 0.1021(5) 0.061(4) Uani 1 2 d DS T P . .
H6 H 0.000000 0.378743 0.049493 0.073 Uiso 1 2 calc R U P . .
C7 C 0.000000 0.4362(4) 0.2187(6) 0.049(3) Uani 1 2 d DS T P . .
H7 H 0.000000 0.478759 0.245657 0.059 Uiso 1 2 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
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'
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
_geom_angle_publ_flag
I1 Pb1 I2 87.74(3) . . ?
I1 Pb1 I4 87.946(13) . . ?
I1 Pb1 I5 173.23(2) . . ?
I1 Pb1 I6 89.69(3) . . ?
I2 Pb1 I6 177.33(2) . . ?
I3 Pb1 I1 95.402(10) . . ?
I3 Pb1 I2 89.377(17) . . ?
I3 Pb1 I4 176.642(15) . . ?
I3 Pb1 I5 88.005(13) . . ?
I3 Pb1 I6 91.57(2) . . ?
I4 Pb1 I2 91.024(17) . . ?
I4 Pb1 I6 88.17(2) . . ?
I5 Pb1 I2 86.448(17) . . ?
I5 Pb1 I4 88.69(2) . . ?
I5 Pb1 I6 96.07(2) . . ?
Pb1 I1 Pb1 167.67(5) 3 . ?
Pb1 I2 Pb1 172.11(3) 11_655 . ?
Pb1 I3 Pb1 180.0 . 13 ?
Pb1 I4 Pb1 91.16(2) 8_545 . ?
Pb1 I5 Pb1 91.45(2) . 8_545 ?
Pb1 I6 Pb1 166.80(5) . 11 ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 107.4 . . ?
C2 N1 H1B 111.1 . . ?
C2 N1 H1C 109.9 . . ?
C6 N2 H2 119.3 . . ?
C7 N2 H2 119.3 . . ?
C7 N2 C6 121.4(5) . . ?
N1 C2 N1 121.2(16) 11 . ?
N1 C2 C3 117.3(8) 11 . ?
N1 C2 C3 117.3(8) . . ?
C4 C3 C2 117.4(11) . . ?
C7 C3 C2 123.1(11) . . ?
C7 C3 C4 119.6(5) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 H4 120.7 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(5) . . ?
C6 C5 H5 119.7 . . ?
N2 C6 C5 119.5(5) . . ?
N2 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
N2 C7 C3 120.4(5) . . ?
N2 C7 H7 119.8 . . ?
C3 C7 H7 119.8 . . ?
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 I1 3.1864(3) . ?
Pb1 I2 3.2223(3) . ?
Pb1 I3 3.1704(3) . ?
Pb1 I4 3.1952(7) . ?
Pb1 I5 3.1873(7) . ?
Pb1 I6 3.2710(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.416(18) . ?
N2 H2 0.8600 . ?
N2 C6 1.345(8) . ?
N2 C7 1.338(7) . ?
C2 C3 1.507(8) . ?
C3 C4 1.379(7) . ?
C3 C7 1.372(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.375(8) . ?
C5 H5 0.9300 . ?
C5 C6 1.368(8) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C2 C3 C4 -101.4(16) 11 . . . ?
N1 C2 C3 C4 101.4(16) . . . . ?
N1 C2 C3 C7 -78.6(16) . . . . ?
N1 C2 C3 C7 78.6(16) 11 . . . ?
C2 C3 C4 C5 180.000(2) . . . . ?
C2 C3 C7 N2 180.000(2) . . . . ?
C3 C4 C5 C6 0.000(2) . . . . ?
C4 C3 C7 N2 0.000(1) . . . . ?
C4 C5 C6 N2 0.000(2) . . . . ?
C6 N2 C7 C3 0.000(2) . . . . ?
C7 N2 C6 C5 0.000(2) . . . . ?
C7 C3 C4 C5 0.000(1) . . . . ?
