Layered Hybrid Lead Perovskite Single Crystals: Phase Transformations and Tunable Optical Properties
Song, Jiewu; Dang, Yangyang; Liu, Xiaolong; Tao, Xutang; CrystEngComm  (2020) –; doi:10.1039/D0CE00753F

data_7241117
_publ_section_title
;
 Layered Hybrid Lead Perovskite Single Crystals: Phase Transformations and
 Tunable Optical Properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00753F
_journal_year                    2020
_chemical_formula_moiety         'I7 Pb2, C4 N, 1.5(C2), N'
_chemical_formula_sum            'C17 H30 I7 N3 Pb2'
_chemical_formula_weight         1579.12
_chemical_name_systematic        C17H30N3I7Pb2
_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_primary     direct
_audit_creation_date             2018-01-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-01-10 deposited with the CCDC.	2020-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                97.072(4)
_cell_angle_beta                 93.983(4)
_cell_angle_gamma                90.199(4)
_cell_formula_units_Z            2
_cell_length_a                   8.8092(5)
_cell_length_b                   8.8168(4)
_cell_length_c                   22.8196(12)
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    296.00(10)
_cell_measurement_theta_max      28.8120
_cell_measurement_theta_min      4.1300
_cell_volume                     1754.51(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (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      air
_diffrn_ambient_temperature      296.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1975
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.860
_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    -63.00  35.00   1.00    6.00    --   10.97 -37.00  60.00   98
  2  \w    -61.00  39.00   1.00    6.00    --   10.97 -57.00-180.00  100
  3  \w     34.00  98.00   1.00    6.00    --   10.97-178.00  90.00   64
  4  \w    -13.00  85.00   1.00    6.00    --   10.97  37.00-150.00   98
  5  \w    -20.00  29.00   1.00    6.00    --  -11.59 -99.00-150.00   49
  6  \w    -44.00  35.00   1.00    6.00    --  -11.59  77.00 -30.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0612121000
_diffrn_orient_matrix_UB_12      -0.0462145000
_diffrn_orient_matrix_UB_13      0.0064849000
_diffrn_orient_matrix_UB_21      0.0035839000
_diffrn_orient_matrix_UB_22      -0.0447712000
_diffrn_orient_matrix_UB_23      -0.0278980000
_diffrn_orient_matrix_UB_31      0.0524954000
_diffrn_orient_matrix_UB_32      -0.0493185000
_diffrn_orient_matrix_UB_33      0.0128667000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.860
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23284
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.860
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_min         3.266
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.752
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.989
_exptl_crystal_description       plate
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.705
_refine_diff_density_min         -1.896
_refine_diff_density_rms         0.315
_refine_ls_extinction_coef       0.00075(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         8472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+12.8276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6355
_reflns_number_total             8472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00753f2.cif
_cod_data_source_block           x1_CCDC2
_cod_original_cell_volume        1754.52(15)
_cod_database_code               7241117
_chemical_oxdiff_formula         'C1 H1 N1 Pb1 I1'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
;
_shelx_res_checksum              22757
_shelx_shelxl_version_number     2014/7
_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 3.025
_oxdiff_exptl_absorpt_empirical_full_min 0.559