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_7243481
_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         'I17 Pb5, I, 4(C15 H13 N3)'
_chemical_formula_sum            'C60 H52 I18 N12 Pb5'
_chemical_formula_weight         4261.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-03
_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                86.4469(11)
_cell_angle_beta                 70.5166(13)
_cell_angle_gamma                72.3962(13)
_cell_formula_units_Z            1
_cell_length_a                   12.8492(2)
_cell_length_b                   12.89296(18)
_cell_length_c                   15.7151(2)
_cell_measurement_reflns_used    23472
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.9030
_cell_measurement_theta_min      1.7560
_cell_volume                     2337.22(6)
_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  (Sheldrick, 2015)'
_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 0.948
_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    -36.00  22.00   0.50    2.51    --  -15.91  45.00 -60.00  116
  2  \w      8.00  49.00   0.50    2.51    --  -15.91  61.00 -30.00   82
  3  \w     -6.00  85.00   0.50    2.51    --   14.73  37.00-113.00  182
  4  \w     -7.00  84.00   0.50    2.51    --   14.73  61.00 -30.00  182
  5  \w     -2.00  42.00   0.50    2.51    --   14.73 -61.00  30.00   88
  6  \w     26.00  51.00   0.50    2.51    --   14.73 -94.00  60.00   50
  7  \w     12.00  59.00   0.50    2.51    --   14.73-125.00  30.00   94
  8  \w     15.00  69.00   0.50    2.51    --   14.73-125.00 150.00  108
  9  \w    -15.00  14.00   0.50    2.51    --   14.73 -30.00  90.00   58
 10  \w    -22.00   4.00   0.50    2.51    --  -15.91 -61.00  60.00   52
 11  \w    -35.00  30.00   0.50    2.51    --   14.73 -94.00  30.00  130
 12  \w    -23.00   2.00   0.50    2.51    --  -15.91 -15.00 -90.00   50
 13  \w    -33.00  54.00   0.50    2.51    --  -15.91  37.00-113.00  174
 14  \w    -16.00  81.00   0.50    2.51    --   14.73  77.00-120.00  194
 15  \w    -27.00  -2.00   0.50    2.51    --  -15.91  61.00 -30.00   50
 16  \w    -55.00   3.00   0.50    2.51    --   14.73 -15.00  30.00  116
 17  \w    -41.00 -16.00   0.50    2.51    --  -15.91 -37.00  90.00   50
 18  \w    -45.00  20.00   0.50    2.51    --   14.73 -37.00  90.00  130
 19  \w    -37.00   6.00   0.50    2.51    --   14.73 -30.00 -90.00   86
 20  \w    -30.00  -5.00   0.50    2.51    --  -15.91 -94.00-120.00   50
 21  \w     -7.00  21.00   0.50    2.51    --  -15.91 -94.00-150.00   56
 22  \w    -39.00 -13.00   0.50    2.51    --   14.73 -61.00  30.00   52
 23  \w     -7.00  19.00   0.50    2.51    --   14.73 -94.00  60.00   52
 24  \w    -28.00  11.00   0.50    2.51    --  -15.91 -94.00 150.00   78
 25  \w    -22.00   3.00   0.50    2.51    --  -15.91 -94.00  30.00   50
 26  \w    -70.00 -45.00   0.50    2.51    --  -15.91 -61.00  60.00   50
 27  \w    -72.00 -47.00   0.50    2.51    --  -15.91 -37.00  90.00   50
 28  \w     32.00  85.00   0.50    2.51    --   14.73  77.00 150.00  106
 29  \w    -44.00 -19.00   0.50    2.51    --   14.73 133.00 123.43   50
 30  \w    -70.00 -40.00   0.50    2.51    --  -15.91 125.00 -30.00   60
 31  \w    -59.00 -33.00   0.50    2.51    --  -15.91 125.00 -90.00   52
 32  \w    -81.00 -56.00   0.50    2.51    --  -15.91 -15.00 -90.00   50
;
_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      0.0409551000
_diffrn_orient_matrix_UB_12      -0.0039361000
_diffrn_orient_matrix_UB_13      0.0220634000
_diffrn_orient_matrix_UB_21      -0.0071164000
_diffrn_orient_matrix_UB_22      0.0565724000
_diffrn_orient_matrix_UB_23      -0.0045908000
_diffrn_orient_matrix_UB_31      -0.0451490000
_diffrn_orient_matrix_UB_32      0.0110282000
_diffrn_orient_matrix_UB_33      0.0422918000
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44481
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.203
_diffrn_reflns_theta_min         1.659
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.958
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50672
_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    3.028
_exptl_crystal_F_000             1860
_refine_diff_density_max         0.694
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         9900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0645
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7322
_reflns_number_total             9900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03957a2.cif
_cod_data_source_block           exp_567_vpbi3py
_cod_database_code               7243481
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'V Pb I C N'
_reflns_odcompleteness_completeness 99.90
_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:
 N00K(H00K), C00L(H00L), C00P(H00P), C00Q(H00Q), C00S(H00S), C00U(H00U),
 C00V(H00V), C00Y(H00Y), C5(H5), C7(H7), C13(H13), C14(H14), C15(H15), C17(H17),
  C18(H18), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C32(H32), C1(H1),
 C8(H8)
;
_shelx_res_checksum              80052
_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 1.831
_oxdiff_exptl_absorpt_empirical_full_min 0.687