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_7243480
_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         'C30 H22 I6 N6 Pb3'
_chemical_formula_sum            'C30 H22 I6 N6 Pb3'
_chemical_formula_weight         1849.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-25
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4598(5)
_cell_length_b                   12.1864(2)
_cell_length_c                   14.4057(3)
_cell_measurement_reflns_used    14514
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.1960
_cell_measurement_theta_min      1.8170
_cell_volume                     3942.90(14)
_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 0.951
_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    -18.00   9.00   0.50    5.20    --   -9.59  19.00 -30.00   54
  2  \w     22.00  60.00   0.50    5.20    --   -9.59  19.00 -30.00   76
  3  \w     -3.00  23.00   0.50    5.20    --    8.42 -92.00 120.00   52
  4  \w    -23.00  16.00   0.50    5.20    --   -9.59 -99.00   0.00   78
  5  \w    -36.00  -8.00   0.50    5.20    --   -9.59 -30.00 -86.00   56
  6  \w    -59.00  -1.00   0.50    5.20    --    8.42 -19.00-150.00  116
  7  \w    -12.00  36.00   0.50    5.20    --    8.42 -99.00-120.00   96
  8  \w    -14.00  13.00   0.50    5.20    --   -9.59 -99.00-150.00   54
  9  \w    -40.00   2.00   0.50    5.20    --    8.42 -19.00 -60.00   84
 10  \w    -36.00 -11.00   0.50    5.20    --    8.42 -92.00 120.00   50
 11  \w    -55.00 -29.00   0.50    5.20    --   -9.59 125.00 120.00   52
 12  \w    -54.00 -29.00   0.50    5.20    --   -9.59 132.00 120.00   50
 13  \w    -44.00 -19.00   0.50    5.20    --    8.42 -19.00 150.00   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      -0.0289227000
_diffrn_orient_matrix_UB_12      0.0226428000
_diffrn_orient_matrix_UB_13      -0.0049344000
_diffrn_orient_matrix_UB_21      0.0029387000
_diffrn_orient_matrix_UB_22      -0.0021397000
_diffrn_orient_matrix_UB_23      -0.0489886000
_diffrn_orient_matrix_UB_31      -0.0123435000
_diffrn_orient_matrix_UB_32      -0.0535726000
_diffrn_orient_matrix_UB_33      -0.0001365000
_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  0.0457
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            30343
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.331
_diffrn_reflns_theta_min         1.813
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    17.506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42368
_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    3.116
_exptl_crystal_F_000             3232
_refine_diff_density_max         1.116
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.000465(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4243
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0181P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0489
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3312
_reflns_number_total             4243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra03957a2.cif
_cod_data_source_block           exp_566_3pypbi3-180c
_cod_original_cell_volume        3942.90(15)
_cod_database_code               7243480
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Pb I C N'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C9(H9), C16(H16), C8(H8), C13(H13), C15(H15), C20(H20), C21(H21),
 C1(H1), C2(H2)
;
_shelx_res_checksum              38873
_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 1.738
_oxdiff_exptl_absorpt_empirical_full_min 0.653