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_7239958
_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         '0.17(I36 Pb12), C30 H22 N6 Ni'
_chemical_formula_sum            'C30 H22 I6 N6 Ni Pb2'
_chemical_formula_weight         1701.02
_space_group_crystal_system      cubic
_space_group_IT_number           220
_space_group_name_Hall           'I -4bd 2c 3'
_space_group_name_H-M_alt        'I -4 3 d'
_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            24
_cell_length_a                   29.1712(2)
_cell_length_b                   29.1712(2)
_cell_length_c                   29.1712(2)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.0370
_cell_measurement_theta_min      1.7040
_cell_volume                     24823.5(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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -4.00  46.00   0.50   57.74    --  -13.11  86.00 -61.00  100
  2  \w     16.00  44.00   0.50   57.74    --   11.62-125.00 150.00   56
;
_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      0.0189912000
_diffrn_orient_matrix_UB_12      -0.0108486000
_diffrn_orient_matrix_UB_13      0.0106139000
_diffrn_orient_matrix_UB_21      -0.0019521000
_diffrn_orient_matrix_UB_22      -0.0185274000
_diffrn_orient_matrix_UB_23      -0.0155712000
_diffrn_orient_matrix_UB_31      0.0151022000
_diffrn_orient_matrix_UB_32      0.0113056000
_diffrn_orient_matrix_UB_33      -0.0153808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            13778
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.710
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60771
_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    2.731
_exptl_crystal_F_000             18096
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 1098 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3185
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0080P)^2^+32.9860P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0279
_refine_ls_wR_factor_ref         0.0283
_reflns_Friedel_coverage         0.640
_reflns_Friedel_fraction_full    0.729
_reflns_Friedel_fraction_max     0.729
_reflns_number_gt                3005
_reflns_number_total             3185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce02004g2.cif
_cod_data_source_block           exp_122_ni-pb-3py-i
_cod_original_cell_volume        24823.5(5)
_cod_database_code               7239958
_shelx_shelxl_version_number     2017/1
_diffrn_oxdiff_digest_frames
;
011a931c357d7ad1c7d4e75d1b88f705ff000250a37
;
_diffrn_oxdiff_digest_hkl
;
01ba3b99ddd6a0a8c0c704065d05b03baab98c
;
_reflns_odcompleteness_completeness 99.63
_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:
 C00D(H00D), C00E(H00E), C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L),
 C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S)
;
_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 1.406
_oxdiff_exptl_absorpt_empirical_full_min 0.762