Tuning the luminescent properties of a three-dimensional perovskite ferroelectric (Me-Hdabco)CsI<sub>3</sub><i>via</i> Sn(II) doping.
Wang, Ze-Jie; Wu, Ling-Kun; Wang, Na; Hu, Qian-Qian; Li, Jian-Rong; Ye, Heng-Yun; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2799–2803; doi:10.1039/d2dt03939g

data_7712207
_publ_section_title
;
 Tuning the luminescent properties of a three-dimensional perovskite
 ferroelectric (Me-Hdabco)CsI<sub>3</sub><i>via</i> Sn(II) doping.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2799
_journal_page_last               2803
_journal_paper_doi               10.1039/d2dt03939g
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'Cs4 I12, 4(C7 H16 N2)'
_chemical_formula_sum            'C28 H64 Cs4 I12 N8'
_chemical_formula_weight         2567.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-11-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-07 deposited with the CCDC.	2023-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.481(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4211(9)
_cell_length_b                   21.4617(8)
_cell_length_c                   14.8276(6)
_cell_measurement_reflns_used    10977
_cell_measurement_temperature    273.00(10)
_cell_measurement_theta_max      29.2040
_cell_measurement_theta_min      1.9370
_cell_volume                     6498.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      273.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.771
_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  43.00   0.50    3.00    --    4.16  92.00 166.00   50
  2  \w    -16.00  65.00   0.50    3.00    --    4.16  40.00  50.00  162
  3  \w    -10.00  15.00   0.50    3.00    --    4.16  57.00 -90.00   50
  4  \w     22.00  69.00   0.50    3.00    --    4.16  57.00 -90.00   94
  5  \w    -21.00  22.00   0.50    3.00    --   -4.59 -99.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0289140000
_diffrn_orient_matrix_UB_12      0.0105662000
_diffrn_orient_matrix_UB_13      -0.0219986000
_diffrn_orient_matrix_UB_21      -0.0157664000
_diffrn_orient_matrix_UB_22      -0.0284729000
_diffrn_orient_matrix_UB_23      0.0106649000
_diffrn_orient_matrix_UB_31      -0.0110195000
_diffrn_orient_matrix_UB_32      0.0130550000
_diffrn_orient_matrix_UB_33      0.0411179000
_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  0.0603
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.771
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20564
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.359
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.953
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.624
_exptl_crystal_description       block
_exptl_crystal_F_000             4576
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.453
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.39(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         11047
_refine_ls_number_restraints     350
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0719P)^2^+100.2820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.771
_reflns_number_gt                9221
_reflns_number_total             11047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03939g2.cif
_cod_data_source_block           zj220909-1_rt2
_cod_depositor_comments
'Adding full bibliography for 7712206--7712207.cif.'
_cod_database_code               7712207
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.206
_shelx_estimated_absorpt_t_min   0.152
_reflns_odcompleteness_completeness 95.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.61(10)
 0.39(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N3-C12 = N3-C14 = N3-C8
 1.5 with sigma of 0.02
 C8-C9
 1.5 with sigma of 0.02
4. Rigid bond restraints
 N6, C15, C16
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim
C14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N6 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(N3) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C11) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(N4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Rigid body (RIGU) restrains
 N3, N4, C8, C9, C10, C11, C12, C13, C14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
7.a Ternary CH refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N8(H8)
7.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
7.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              57926
_shelx_hkl_checksum              82930
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.742