Dimensionally and Structurally Controllable Perovskite Single Crystals: Nickle(II)-Terpyridine-Complex (Ni-Tpy2) Based Perovskites
Zhang, Yongli; Zang, Meixiu; Yin, Hang; Liu, Peng; Xian, Yeming; Li, Wenzhe; CrystEngComm  (2020) –; doi:10.1039/C9CE02004G

data_7239960
_publ_section_title
;
 Dimensionally and Structurally Controllable Perovskite Single Crystals:
 Nickle(II)-Terpyridine-Complex (Ni-Tpy2) Based Perovskites
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE02004G
_journal_year                    2020
_chemical_formula_moiety         'I6 Pb2, I4 Pb, 2(C30 H22 N6 Ni)'
_chemical_formula_sum            'C60 H44 I10 N12 Ni2 Pb3'
_chemical_formula_weight         2941.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2019-11-29 deposited with the CCDC.	2020-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.3909(6)
_cell_length_b                   8.5089(2)
_cell_length_c                   39.5465(9)
_cell_measurement_reflns_used    12907
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5660
_cell_measurement_theta_min      1.8160
_cell_volume                     7534.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.51a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.51a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.51a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -44.00 -16.00   0.50   26.00    --   11.62 -60.00  19.00   56
  2  \w    -12.00  19.00   0.50   26.00    --   11.62 -60.00  19.00   62
  3  \w    -25.00   8.00   0.50   26.00    --  -13.11 -99.00 -30.00   66
  4  \w    -26.00  19.00   0.50   26.00    --  -13.11 -99.00 -90.00   90
  5  \w     10.00  63.00   0.50   26.00    --   11.62-125.00-150.00  106
  6  \w    -14.00  12.00   0.50   26.00    --  -13.11 -99.00-180.00   52
  7  \w     11.00  73.00   0.50   26.00    --   11.62  61.00  -3.00  124
  8  \w      4.00  29.00   0.50   26.00    --   11.62-115.00 143.00   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      -0.0180748000
_diffrn_orient_matrix_UB_12      0.0309213000
_diffrn_orient_matrix_UB_13      0.0001373000
_diffrn_orient_matrix_UB_21      0.0576116000
_diffrn_orient_matrix_UB_22      0.0046724000
_diffrn_orient_matrix_UB_23      0.0126974000
_diffrn_orient_matrix_UB_31      0.0574743000
_diffrn_orient_matrix_UB_32      0.0050294000
_diffrn_orient_matrix_UB_33      -0.0126696000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            31947
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.819
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.313
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.51a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.593
_exptl_crystal_F_000             5280
_refine_diff_density_max         1.245
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.142
_refine_ls_abs_structure_details
;
 Flack x determined using 2673 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.381(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         11161
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0440P)^2^+54.6590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1140
_reflns_Friedel_coverage         0.665
_reflns_Friedel_fraction_full    0.683
_reflns_Friedel_fraction_max     0.683
_reflns_number_gt                8032
_reflns_number_total             11161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02004g2.cif
_cod_data_source_block           exp_130_nipb3pyi-needle
_cod_database_code               7239960
_shelx_shelxl_version_number     2017/1
_diffrn_oxdiff_digest_frames
;
01f08097c621a4aa07d50acd7e3ed00795000253208
;
_diffrn_oxdiff_digest_hkl
;
019ff1dbb9f59d9351eb4d1bf47bbdd1643537
;
_reflns_odcompleteness_completeness 98.91
_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:
 C00W(H00W), C00Z(H00Z), C010(H010), C011(H011), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C01E(H01E), C01H(H01H),
 C01I(H01I), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N),
 C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01V(H01V),
 C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B), C17(H17), C19(H19), C29(H29),
 C45(H45)
;
_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 1.688
_oxdiff_exptl_absorpt_empirical_full_min 0.746