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_7131798
_publ_section_title
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 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     dual
_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                   9.2171(4)
_cell_length_b                   8.5923(4)
_cell_length_c                   34.0460(18)
_cell_measurement_reflns_used    5429
_cell_measurement_temperature    299.97(10)
_cell_measurement_theta_max      27.4740
_cell_measurement_theta_min      2.4000
_cell_volume                     2696.3(2)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.97(10)
_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     -9.00  70.20   0.80  102.54    --    4.40  11.00 -20.00   99
  2  \w    -23.00  27.40   0.80  102.54    --   -5.65 -99.00 -60.00   63
  3  \w    -69.00  19.00   0.80  102.54    --    4.40 -11.00 166.00  110
  4  \w    -28.00  66.40   0.80  102.54    --   -5.65  77.00 -30.00  118
;
_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      0.0102617000
_diffrn_orient_matrix_UB_12      0.0041197000
_diffrn_orient_matrix_UB_13      0.0206232000
_diffrn_orient_matrix_UB_21      0.0754237000
_diffrn_orient_matrix_UB_22      0.0117787000
_diffrn_orient_matrix_UB_23      -0.0029018000
_diffrn_orient_matrix_UB_31      -0.0113736000
_diffrn_orient_matrix_UB_32      0.0815838000
_diffrn_orient_matrix_UB_33      -0.0006301000
_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     0.0353
_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       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            25770
_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         26.369
_diffrn_reflns_theta_min         2.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.526
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.727
_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    2.115
_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 stabilizer. Samples were left sealed until use.'
_exptl_crystal_recrystallization_method 'See preparation details.'
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.009
_refine_diff_density_max         1.258
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.357
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         2766
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.347
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+54.5525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2073
_reflns_number_total             2766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01788e2.cif
_cod_data_source_block           ortho_300k_103s_0p8
_cod_database_code               7131798
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C14 N2 Sn1 I4'
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.294
_olex2_refinement_description
;
1. Restrained distances
 C9-C1 = C5-C1
 1.54 with sigma of 0.02
2. Rigid bond restraints
 C1, N004, C005, C006, C007, C6, C5, C9
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N004 \\sim C005 \\sim C006 \\sim C007 \\sim C6 \\sim C5 \\sim C1 \\sim C9:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
4.a Ternary CH refined with riding coordinates:
 C005(H005)
4.b Secondary CH2 refined with riding coordinates:
 C007(H00G,H00H), C5(H5A,H5B), C6(H6A,H6B), C1(H1A,H1B)
4.c Idealised Me refined as rotating group:
 N004(H00A,H00B,H00C), C006(H00D,H00E,H00F), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              955
_shelx_hkl_checksum              84607
_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 Mitigen 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 1.223
_oxdiff_exptl_absorpt_empirical_full_min 0.851