Terpyridine-derived perovskite single crystals with tunable structures and electronic dimensionality
Yuan, Yaxuan; Xian, Yeming; Long, Yi; Zhang, Yangyi; Rahman, Naveed Ur; Zhang, Yongli; Fan, Jiandong; Li, Wenzhe; RSC Advances 11 (2021) 24816–24821; doi:10.1039/D1RA03957A

data_7243479
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w      0.00  72.00   0.50    4.49    --    8.42  37.00  30.00  144
  2  \w     47.00  78.00   0.50    4.49    --    8.42  19.00 -60.00   62
  3  \w     22.00  77.00   0.50    4.49    --    8.42  19.00-180.00  110
  4  \w     16.00  62.00   0.50    4.49    --    8.42  37.00-180.00   92
  5  \w      3.00  62.00   0.50    4.49    --    8.42  77.00-120.00  118
  6  \w      0.00  44.00   0.50    4.49    --    8.42  19.00 -60.00   88
  7  \w     -7.00  44.00   0.50    4.49    --   -9.59  37.00 -60.00  102
  8  \w    -13.00  51.00   0.50    4.49    --    8.42  77.00-180.00  128
  9  \w    -33.00  -8.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 10  \w    -60.00 -13.00   0.50    4.49    --    8.42 -19.00   0.00   94
 11  \w    -46.00  26.00   0.50    4.49    --    8.42 -57.00  60.00  144
 12  \w      5.00  31.00   0.50    4.49    --    8.42 -99.00  30.00   52
 13  \w    -14.00  20.00   0.50    4.49    --   -9.59 -99.00 -30.00   68
 14  \w     16.00  41.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 15  \w    -12.00  13.00   0.50    4.49    --   -9.59 -99.00-180.00   50
 16  \w    -22.00   3.00   0.50    4.49    --    8.42 -99.00 -90.00   50
 17  \w    -22.00   4.00   0.50    4.49    --   -9.59 -99.00 -60.00   52
 18  \w    -23.00  37.00   0.50    4.49    --    8.42 -99.00 -30.00  120
 19  \w    -21.00  17.00   0.50    4.49    --   -9.59 -99.00  30.00   76
 20  \w    -12.00  13.00   0.50    4.49    --    8.42 -99.00  90.00   50
 21  \w      4.00  30.00   0.50    4.49    --   -9.59  37.00 120.00   52
 22  \w    -16.00  10.00   0.50    4.49    --   -9.59 -99.00  90.00   52
 23  \w    -41.00  -2.00   0.50    4.49    --    8.42 -19.00 150.00   78
 24  \w    -61.00 -36.00   0.50    4.49    --    8.42 -19.00 -60.00   50
 25  \w    -44.00 -19.00   0.50    4.49    --   -9.59 125.00 150.00   50
 26  \w    -37.00 -12.00   0.50    4.49    --   -9.59 125.00   0.00   50
 27  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0342P)^2^+4.0489P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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'
_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)
;
_shelx_res_checksum              94369
_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