#------------------------------------------------------------------------------
#$Date: 2021-09-06 08:33:38 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268488 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/34/7243479.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_7243479
loop_
_publ_author_name
'Yuan, Yaxuan'
'Xian, Yeming'
'Long, Yi'
'Zhang, Yangyi'
'Rahman, Naveed Ur'
'Zhang, Yongli'
'Fan, Jiandong'
'Li, Wenzhe'
_publ_section_title
;
 Terpyridine-derived perovskite single crystals with tunable structures
 and electronic dimensionality
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              24816
_journal_page_last               24821
_journal_paper_doi               10.1039/D1RA03957A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'I6 Pb, 2(C15 H14 N3)'
_chemical_formula_sum            'C30 H28 I6 N6 Pb'
_chemical_formula_weight         1441.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-03 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.854(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0069(3)
_cell_length_b                   14.6783(3)
_cell_length_c                   10.1587(3)
_cell_measurement_reflns_used    14265
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1020
_cell_measurement_theta_min      2.0960
_cell_volume                     1846.09(8)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  72.00   0.50    4.49    --    8.42  37.00  30.00  144
  2  ω     47.00  78.00   0.50    4.49    --    8.42  19.00 -60.00   62
  3  ω     22.00  77.00   0.50    4.49    --    8.42  19.00-180.00  110
  4  ω     16.00  62.00   0.50    4.49    --    8.42  37.00-180.00   92
  5  ω      3.00  62.00   0.50    4.49    --    8.42  77.00-120.00  118
  6  ω      0.00  44.00   0.50    4.49    --    8.42  19.00 -60.00   88
  7  ω     -7.00  44.00   0.50    4.49    --   -9.59  37.00 -60.00  102
  8  ω    -13.00  51.00   0.50    4.49    --    8.42  77.00-180.00  128
  9  ω    -33.00  -8.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 10  ω    -60.00 -13.00   0.50    4.49    --    8.42 -19.00   0.00   94
 11  ω    -46.00  26.00   0.50    4.49    --    8.42 -57.00  60.00  144
 12  ω      5.00  31.00   0.50    4.49    --    8.42 -99.00  30.00   52
 13  ω    -14.00  20.00   0.50    4.49    --   -9.59 -99.00 -30.00   68
 14  ω     16.00  41.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 15  ω    -12.00  13.00   0.50    4.49    --   -9.59 -99.00-180.00   50
 16  ω    -22.00   3.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 17  ω    -22.00   4.00   0.50    4.49    --   -9.59 -99.00 -60.00   52
 18  ω    -23.00  37.00   0.50    4.49    --    8.42 -99.00 -30.00  120
 19  ω    -21.00  17.00   0.50    4.49    --   -9.59 -99.00  30.00   76
 20  ω    -12.00  13.00   0.50    4.49    --    8.42 -99.00  90.00   50
 21  ω      4.00  30.00   0.50    4.49    --   -9.59  37.00 120.00   52
 22  ω    -16.00  10.00   0.50    4.49    --   -9.59 -99.00  90.00   52
 23  ω    -41.00  -2.00   0.50    4.49    --    8.42 -19.00 150.00   78
 24  ω    -61.00 -36.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 25  ω    -44.00 -19.00   0.50    4.49    --   -9.59 125.00 150.00   50
 26  ω    -37.00 -12.00   0.50    4.49    --   -9.59 125.00   0.00   50
 27  ω    -52.00 -26.00   0.50    4.49    --   -9.59 125.00 -60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0423740000
_diffrn_orient_matrix_UB_12      -0.0028939000
_diffrn_orient_matrix_UB_13      -0.0634380000
_diffrn_orient_matrix_UB_21      -0.0385229000
_diffrn_orient_matrix_UB_22      0.0054142000
_diffrn_orient_matrix_UB_23      0.0359732000
_diffrn_orient_matrix_UB_31      0.0017966000
_diffrn_orient_matrix_UB_32      0.0479282000
_diffrn_orient_matrix_UB_33      -0.0078788000
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18696
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.309
_diffrn_reflns_theta_min         2.106
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38545
_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_density_diffrn    2.593
_exptl_crystal_F_000             1300
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         2095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0295
_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)+(0.0342P)²+4.0489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0722
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1842
_reflns_number_total             2095
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ra03957a2.cif
_cod_data_source_block           exp_562_v-3pypbi-dark-hemi
_cod_database_code               7243479
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb I C N'
_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.
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N005(H005), N006(H006), C009(H009), C00A(H00A), C00B(H00B), C00C(H00C),
 C00D(H00D), C00E(H00E)
;
_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 1.759
_oxdiff_exptl_absorpt_empirical_full_min 0.668
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'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
Pb01 Pb 0.500000 0.500000 0.500000 0.03979(12) Uani 1 4 d S T P . .
I002 I 0.75978(4) 0.500000 0.52833(4) 0.04605(14) Uani 1 2 d S T P . .
I003 I 0.43368(4) 0.500000 0.17670(4) 0.05429(15) Uani 1 2 d S T P . .
I004 I 0.500000 0.72502(4) 0.500000 0.06300(17) Uani 1 2 d S T P . .
N005 N 0.8617(4) 0.500000 0.9655(5) 0.0386(13) Uani 1 2 d S T P . .
H005 H 0.841716 0.500001 0.876585 0.046 Uiso 1 2 calc R U P . .
N006 N 0.8164(3) 0.6495(3) 0.8115(4) 0.0497(10) Uani 1 1 d . . . . .
H006 H 0.802701 0.594679 0.781224 0.060 Uiso 1 1 calc R U . . .
C007 C 0.8773(3) 0.5789(4) 1.0355(5) 0.0422(11) Uani 1 1 d . . . . .
C008 C 0.8562(3) 0.6617(4) 0.9493(5) 0.0442(11) Uani 1 1 d . . . . .
C009 C 0.8769(4) 0.7498(4) 0.9954(6) 0.0564(15) Uani 1 1 d . . . . .
H009 H 0.903701 0.761451 1.089720 0.068 Uiso 1 1 calc R U . . .
C00A C 0.8581(4) 0.8211(4) 0.9022(7) 0.0633(16) Uani 1 1 d . . . . .
H00A H 0.872632 0.880484 0.934468 0.076 Uiso 1 1 calc R U . . .
C00B C 0.9277(7) 0.500000 1.2475(8) 0.068(3) Uani 1 2 d S T P . .
H00B H 0.950755 0.499999 1.343693 0.082 Uiso 1 2 calc R U P . .
C00C C 0.9112(4) 0.5816(5) 1.1785(5) 0.0578(14) Uani 1 1 d . . . . .
H00C H 0.922249 0.636694 1.226079 0.069 Uiso 1 1 calc R U . . .
C00D C 0.8181(5) 0.8052(4) 0.7624(7) 0.0652(16) Uani 1 1 d . . . . .
H00D H 0.805714 0.852905 0.699224 0.078 Uiso 1 1 calc R U . . .
C00E C 0.7969(5) 0.7169(4) 0.7191(6) 0.0632(15) Uani 1 1 d . . . . .
H00E H 0.769020 0.703977 0.625241 0.076 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'
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
I002 Pb01 I002 180.0 . 5_666 ?
I002 Pb01 I004 90.0 5_666 . ?
I002 Pb01 I004 90.0 . . ?
I002 Pb01 I004 90.0 . 5_666 ?
I002 Pb01 I004 90.0 5_666 5_666 ?
I003 Pb01 I002 92.116(12) 5_666 5_666 ?
I003 Pb01 I002 92.116(12) . . ?
I003 Pb01 I002 87.883(12) 5_666 . ?
I003 Pb01 I002 87.884(12) . 5_666 ?
I003 Pb01 I003 180.0 . 5_666 ?
I003 Pb01 I004 90.0 5_666 5_666 ?
I003 Pb01 I004 90.0 5_666 . ?
I003 Pb01 I004 90.0 . . ?
I003 Pb01 I004 90.0 . 5_666 ?
I004 Pb01 I004 180.0 . 5_666 ?
C007 N005 H005 120.3 . . ?
C007 N005 H005 120.3 6_565 . ?
C007 N005 C007 119.4(6) . 6_565 ?
C008 N006 H006 117.9 . . ?
C00E N006 H006 117.9 . . ?
C00E N006 C008 124.2(5) . . ?
N005 C007 C008 115.3(4) . . ?
N005 C007 C00C 121.9(5) . . ?
C00C C007 C008 122.8(5) . . ?
N006 C008 C007 116.7(4) . . ?
N006 C008 C009 116.9(5) . . ?
C009 C008 C007 126.3(5) . . ?
C008 C009 H009 119.8 . . ?
C008 C009 C00A 120.3(5) . . ?
C00A C009 H009 119.8 . . ?
C009 C00A H00A 119.7 . . ?
C00D C00A C009 120.7(5) . . ?
C00D C00A H00A 119.7 . . ?
C00C C00B H00B 119.1 6_565 . ?
C00C C00B H00B 119.1 . . ?
C00C C00B C00C 121.8(7) 6_565 . ?
C007 C00C H00C 121.3 . . ?
C00B C00C C007 117.5(6) . . ?
C00B C00C H00C 121.3 . . ?
C00A C00D H00D 121.0 . . ?
C00E C00D C00A 117.9(6) . . ?
C00E C00D H00D 121.0 . . ?
N006 C00E C00D 120.0(6) . . ?
N006 C00E H00E 120.0 . . ?
C00D C00E H00E 120.0 . . ?
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
Pb01 I002 3.3021(5) . ?
Pb01 I002 3.3021(5) 5_666 ?
Pb01 I003 3.1294(4) . ?
Pb01 I003 3.1295(4) 5_666 ?
Pb01 I004 3.3030(5) 5_666 ?
Pb01 I004 3.3029(5) . ?
N005 H005 0.8600 . ?
N005 C007 1.342(6) 6_565 ?
N005 C007 1.342(6) . ?
N006 H006 0.8600 . ?
N006 C008 1.347(6) . ?
N006 C00E 1.334(7) . ?
C007 C008 1.473(8) . ?
C007 C00C 1.384(7) . ?
C008 C009 1.373(7) . ?
C009 H009 0.9300 . ?
C009 C00A 1.382(8) . ?
C00A H00A 0.9300 . ?
C00A C00D 1.375(9) . ?
C00B H00B 0.9300 . ?
C00B C00C 1.371(7) . ?
C00B C00C 1.371(7) 6_565 ?
C00C H00C 0.9300 . ?
C00D H00D 0.9300 . ?
C00D C00E 1.369(8) . ?
C00E H00E 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
N005 C007 C008 N006 4.6(6) . . . . ?
N005 C007 C008 C009 -172.8(5) . . . . ?
N005 C007 C00C C00B -0.4(8) . . . . ?
N006 C008 C009 C00A -0.7(7) . . . . ?
C007 N005 C007 C008 -179.0(3) 6_565 . . . ?
C007 N005 C007 C00C 1.1(8) 6_565 . . . ?
C007 C008 C009 C00A 176.7(4) . . . . ?
C008 N006 C00E C00D 0.3(9) . . . . ?
C008 C007 C00C C00B 179.7(5) . . . . ?
C008 C009 C00A C00D 0.3(8) . . . . ?
C009 C00A C00D C00E 0.5(9) . . . . ?
C00A C00D C00E N006 -0.8(9) . . . . ?
C00C C007 C008 N006 -175.5(4) . . . . ?
C00C C007 C008 C009 7.1(7) . . . . ?
C00C C00B C00C C007 -0.3(11) 6_565 . . . ?
C00E N006 C008 C007 -177.3(5) . . . . ?
C00E N006 C008 C009 0.4(7) . . . . ?
