Temperature-responsive emission and elastic properties of a new 2D lead halide perovskite.
Fan, Jia-Hui; Qin, Yan; Azeem, Muhammad; Zhang, Zhuo-Zhen; Li, Zhi-Gang; Sun, Na; Yao, Zhao-Quan; Li, Wei; Dalton transactions (Cambridge, England : 2003) 50 (2021) 2648–2653; doi:10.1039/d0dt04165c

data_7706466
_publ_section_title
;
 Temperature-responsive emission and elastic properties of a new 2D lead
 halide perovskite.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2648
_journal_page_last               2653
_journal_paper_doi               10.1039/d0dt04165c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '0.25(I16 Pb4), 2(C9 H14 N O)'
_chemical_formula_sum            'C18 H28 I4 N2 O2 Pb'
_chemical_formula_weight         1019.21
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc25hpq3
_audit_creation_date             2017-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-21 deposited with the CCDC.	2021-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.4430(10)
_cell_angle_beta                 81.1380(10)
_cell_angle_gamma                89.9950(10)
_cell_formula_units_Z            4
_cell_length_a                   12.2659(2)
_cell_length_b                   12.3518(2)
_cell_length_c                   18.4045(2)
_cell_measurement_reflns_used    29294
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      73.7090
_cell_measurement_theta_min      4.8720
_cell_volume                     2715.94(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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      223.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.956
_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     57.00  87.00   0.50    1.00    --    0.00  38.00  90.00   60
  2  \w    -10.00  17.00   0.50    1.00    --    0.00  38.00  90.00   54
  3  \w    -16.00  79.00   0.50    1.00    --    0.00  38.00  30.00  190
  4  \w    -16.00  14.00   0.50    1.00    --    0.00 -38.00 150.00   60
  5  \w    -85.00 -60.00   0.50    1.00    --    0.00 -57.00   0.00   50
  6  \w     27.00  76.00   0.50    1.00    --    0.00  57.00-120.00   98
  7  \w    -42.00  -3.00   0.50    1.00    --    0.00 -57.00   0.00   78
  8  \w    -19.00   8.00   0.50    1.00    --    0.00  57.00 -60.00   54
  9  \w     36.00  89.00   0.50    1.00    --    0.00  38.00-180.00  106
 10  \w    -58.00 -20.00   0.50    1.00    --    0.00 -38.00 150.00   76
 11  \w    -28.00  31.00   0.50    1.00    --    0.00 -82.00  30.00  118
 12  \w    -16.00  25.00   0.50    1.00    --    0.00  38.00-180.00   82
 13  \w    -20.00  11.00   0.50    1.00    --    0.00  57.00-120.00   62
 14  \w     23.00  76.00   0.50    1.00    --    0.00  57.00 -60.00  106
 15  \w    -88.00 -61.00   0.50    1.00    --    0.00 -38.00 150.00   54
 16  \w     66.00 118.00   0.50    2.50    --   94.60  74.00  43.47  104
 17  \w    159.00 184.00   0.50    2.50    --   94.60  65.00 -88.11   50
 18  \w    101.00 184.00   0.50    2.50    --   94.60  74.00-128.40  166
 19  \w     71.00  97.00   0.50    2.50    --   94.60  65.00 -88.11   52
 20  \w     69.00 123.00   0.50    2.50    --   94.60  67.00-135.23  108
 21  \w     66.00  91.00   0.50    2.50    --   94.60  74.00-128.40   50
 22  \w     69.00 184.00   0.50    2.50    --   94.60  66.00-173.86  230
 23  \w    121.00 154.00   0.50    2.50    --   94.60  72.00  28.67   66
 24  \w     70.00 105.00   0.50    2.50    --   94.60  65.00 164.58   70
 25  \w     66.00  92.00   0.50    2.50    --   94.60  74.00-116.37   52
 26  \w      6.00 126.00   0.50    2.50    --   94.60 -82.00 -90.00  240
 27  \w      5.00 126.00   0.50    2.50    --   94.60 -82.00  90.00  242
 28  \w    120.00 145.00   0.50    2.50    --   94.60  61.00-150.00   50
 29  \w     67.00 118.00   0.50    2.50    --   94.60  72.00  28.67  102
 30  \w     42.00  70.00   0.50    2.50    --   94.60 -82.00   0.00   56
 31  \w     67.00  92.00   0.50    2.50    --   94.60  71.00-152.42   50
 32  \w     68.00 103.00   0.50    2.50    --   94.60  69.00 -28.75   70
 33  \w     69.00  95.00   0.50    2.50    --   94.60  69.00 120.64   52
 34  \w    148.00 174.00   0.50    2.50    --   94.60  69.00 -11.87   52
 35  \w     67.00  93.00   0.50    2.50    --   94.60  71.00  91.36   52
 36  \w    126.00 179.00   0.50    2.50    --   94.60  70.00 134.34  106
 37  \w      6.00 123.00   0.50    2.50    --   94.60 -77.00 120.00  234
 38  \w     75.00 110.00   0.50    2.50    --   94.60  45.00  90.00   70
 39  \w     71.00  96.00   0.50    2.50    --   94.60  61.00  90.00   50
 40  \w     71.00  97.00   0.50    2.50    --   94.60  61.00  30.00   52
 41  \w     67.00  94.00   0.50    2.50    --   94.60  71.00 -86.34   54
 42  \w     71.00 151.00   0.50    2.50    --   94.60  61.00 -60.00  160
 43  \w     68.00 115.00   0.50    2.50    --   94.60  69.00 -11.87   94
 44  \w      7.00 125.00   0.50    2.50    --   94.60 -82.00 -60.00  236
 45  \w     72.00 124.00   0.50    2.50    --   94.60  61.00 -90.00  104
 46  \w     71.00  97.00   0.50    2.50    --   94.60  61.00 -30.00   52
 47  \w     71.00 180.00   0.50    2.50    --   94.60  61.00 120.00  218
 48  \w     68.00 182.00   0.50    2.50    --   94.60  69.00   6.47  228
 49  \w     72.00  98.00   0.50    2.50    --   94.60  57.00  18.91   52
 50  \w     71.00  97.00   0.50    2.50    --   94.60  61.00-120.00   52
 51  \w     76.00 102.00   0.50    2.50    --   94.60  55.00-153.36   52
 52  \w     69.00  95.00   0.50    2.50    --   94.60  67.00  47.74   52
 53  \w      7.00 111.00   0.50    2.50    --   94.60 -82.00-180.00  208
 54  \w     88.00 113.00   0.50    2.50    --   94.60 -82.00   0.00   50
 55  \w     71.00 142.00   0.50    2.50    --   94.60  61.00-180.00  142
 56  \w     71.00  97.00   0.50    2.50    --   94.60  61.00-150.00   52
 57  \w    158.00 184.00   0.50    2.50    --   94.60  74.00  43.47   52
 58  \w     69.00  96.00   0.50    2.50    --   94.60  68.00 151.07   54
 59  \w     68.00 105.00   0.50    2.50    --   94.60  70.00 134.34   74
 60  \w     71.00 175.00   0.50    2.50    --   94.60  59.00 -40.88  208
 61  \w     74.00 183.00   0.50    2.50    --   94.60  50.00  97.60  218
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0641906000
_diffrn_orient_matrix_UB_12      0.0809366000
_diffrn_orient_matrix_UB_13      0.0340853000
_diffrn_orient_matrix_UB_21      0.0328697000
_diffrn_orient_matrix_UB_22      0.0699627000
_diffrn_orient_matrix_UB_23      -0.0778609000
_diffrn_orient_matrix_UB_31      -0.1047243000
_diffrn_orient_matrix_UB_32      0.0675501000
_diffrn_orient_matrix_UB_33      0.0127473000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            52802
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.075
_diffrn_reflns_theta_min         2.465
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    47.894
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.08225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.493
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_refine_diff_density_max         5.595
_refine_diff_density_min         -2.818
_refine_diff_density_rms         0.349
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10732
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1395P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1746
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8731
_reflns_number_total             10732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04165c2.cif
_cod_data_source_block           20190620_4meopeai_223k
_cod_depositor_comments          'Adding full bibliography for 7706466.cif.'
_cod_database_code               7706466
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H18-H5AB
 2.45 with sigma of 0.01
 H0AA-H2AA
 2.45 with sigma of 0.01
 H16A-H1AA
 2.45 with sigma of 0.01
 H16B-H1AA
 2.5 with sigma of 0.02
 H2AC-H0AA
 2.5 with sigma of 0.02
3. Rigid bond restraints
 O1AA, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C0AA, C15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C00W, C19
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C00F(H00D,H00E), C00G(H00Z,HA), C00H(H00N,H00O), C00I(H00I,H00J), C00U(H00U,
 H00V), C00Z(H7AA,HB), C10(H10A,H10B), C11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C00K(H00P), C00M(H00R), C00N(H00), C00O(H00S), C00Q(H00Q), C00T(H00T),
 C00W(H1AA), C00X(H00X), C00Y(H6AA), C18(H18), C0AA(H0AA), C20(H20), C3AA(H3AA),
  C4AA(H4AA), C24(H24), C6AA(H6AB)
4.c Idealised Me refined as rotating group:
 N00B(H00A,H00B,H00C), N00C(H00F,H00G,H00H), N00D(H00K,H00L,H00M), N00E(H00W,
 H00Y,H), C17(H17A,H17B,H17C), C2AA(H2AA,H2AB,H2AC), C16(H16A,H16B,H16C),
 C5AA(H5AA,H5AB,H5AC)
;
_shelx_res_checksum              20125
_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 7.625
_oxdiff_exptl_absorpt_empirical_full_min 0.382