A two-dimensional lead-free hybrid perovskite semiconductor with reduced melting temperature.
Singh, Akash; Crace, Ethan; Xie, Yi; Mitzi, David B.; Chemical communications (Cambridge, England) 59 (2023) 8302–8305; doi:10.1039/d3cc01788e

data_7131799
_publ_section_title
;
 A two-dimensional lead-free hybrid perovskite semiconductor with reduced
 melting temperature.
;
_journal_issue                   53
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8302
_journal_page_last               8305
_journal_paper_doi               10.1039/d3cc01788e
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'I4 Sn, 2(C7 H18 N)'
_chemical_formula_sum            'C14 H36 I4 N2 Sn'
_chemical_formula_weight         858.74
_chemical_name_systematic
'catena-[bis(heptan-2-ammonium) bis(mu-iodo)-diiodo-tin]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-01-10
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-04-10 deposited with the CCDC.	2023-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.04641(16)
_cell_length_b                   8.47695(15)
_cell_length_c                   34.0759(7)
_cell_measurement_reflns_used    31503
_cell_measurement_temperature    80.0(8)
_cell_measurement_theta_max      30.9320
_cell_measurement_theta_min      2.3930
_cell_volume                     2613.14(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.95a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      80.0(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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     -8.00  78.40   0.80   50.00    --    4.40  19.00  60.00  108
  2  \w    -18.00  70.00   0.80   50.00    --   -5.65  25.00 -70.33  110
  3  \w    -24.00  42.40   0.80   50.00    --    4.40  90.00-139.00   83
  4  \w    -18.00  67.60   0.80   50.00    --   -5.65  37.00 120.00  107
  5  \w    -18.00  67.60   0.80   50.00    --   -5.65  37.00  30.00  107
  6  \w    -18.00  70.00   0.80   50.00    --   -5.65  19.00-120.00  110
  7  \w    -18.00  67.60   0.80   50.00    --   -5.65  31.00-172.29  107
  8  \w    -18.00  67.60   0.80   50.00    --   -5.65  37.00 -30.00  107
  9  \w    -18.00  68.40   0.80   50.00    --   -5.65  32.00  81.23  108
 10  \w    -18.00  67.60   0.80   50.00    --   -5.65  31.00-100.42  107
 11  \w    -23.00  27.40   0.80   50.00    --   -5.65 -99.00-120.00   63
 12  \w    -42.00  32.40   0.80   50.00    --    4.40 -90.00 106.00   93
 13  \w    -41.00  21.40   0.80   50.00    --   -5.65 -90.00 106.00   78
 14  \w    -34.00  42.00   0.80   50.00    --   -5.65  90.00-139.00   95
 15  \w    -46.00  -2.00   0.80   50.00    --   -5.65 111.00 -49.37   55
 16  \w    -47.00  -5.40   0.80   50.00    --   -5.65 113.00  44.20   52
 17  \w    -47.00  -5.40   0.80   50.00    --   -5.65 113.00-129.55   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0091980000
_diffrn_orient_matrix_UB_12      -0.0396032000
_diffrn_orient_matrix_UB_13      -0.0181712000
_diffrn_orient_matrix_UB_21      -0.0557731000
_diffrn_orient_matrix_UB_22      -0.0547124000
_diffrn_orient_matrix_UB_23      0.0053920000
_diffrn_orient_matrix_UB_31      -0.0543410000
_diffrn_orient_matrix_UB_32      0.0493718000
_diffrn_orient_matrix_UB_33      -0.0086097000
_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  0.0741
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            103955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.872
_diffrn_reflns_theta_min         2.391
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.702
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.441
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.95a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             1584
_exptl_crystal_preparation
'Crystals were grown by slow cooling tin (II) iodide and racemic 2-aminoheptane in hydroiodic acid with hypophosphorous acid as a stabilizer. Samples were left sealed until use.'
_exptl_crystal_recrystallization_method 'See preparation details.'
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.009
_exptl_crystal_size_rad          0.400
_refine_diff_density_max         1.434
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.478
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         3117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.478
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0470
_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^)+34.3898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2818
_reflns_number_total             3117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01788e2.cif
_cod_data_source_block           ec1-187_akash_1mehasni_80k
_cod_original_cell_volume        2613.15(9)
_cod_database_code               7131799
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N Sn I'
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.513
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C6(H6)
1.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C2(H2A,H2B)
1.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              64992
_shelx_hkl_checksum              61192
_olex2_exptl_crystal_mounting_method
'Samples, still in the mother liquor, were opened in air and crystals were coated in paratone oil and transfered to a glass slide. Crystals were mounted on a Mitegen loop using paratone oil and quickly placed under a stream of nitrogen for screening and collection. '
_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 1.277
_oxdiff_exptl_absorpt_empirical_full_min 0.710