Phase transition, optical and dielectric properties regulated by anion-substitution in a homologous series of 2D hybrid organic‒inorganic perovskites
Wei, Wen-Juan; Li, Chao; Li, Lin-Sui; Tang, Yun-Zhi; Jiang, Xing-Xing; Lin, Zhe-Shuai; Journal of Materials Chemistry C 7 (2019) 11964–; doi:10.1039/C9TC04479E

data_7238000
_publ_section_title
;
 Phase transition, optical and dielectric properties regulated by
 anion-substitution in a homologous series of 2D hybrid organic--inorganic
 perovskites
;
_journal_issue                   38
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              11964
_journal_paper_doi               10.1039/C9TC04479E
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         '0.5(I8 Pb2), 2(C5.26 H9 N S0.74)'
_chemical_formula_sum            'C10.71 H24.71 I4 N2 Pb S1.29'
_chemical_formula_weight         937.65
_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     direct
_audit_creation_date             2019-05-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-24 deposited with the CCDC.	2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.810(2)
_cell_length_b                   8.6780(19)
_cell_length_c                   28.972(6)
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.547
_cell_measurement_theta_min      2.812
_cell_volume                     2215.0(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            22805
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.614
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    13.306
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.812
_exptl_crystal_description       block
_exptl_crystal_F_000             1670
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.916
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.282
_refine_ls_extinction_coef       0.00079(8)
_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   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         2566
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.225
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0346P)^2^+45.3005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1923
_reflns_number_total             2566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9tc04479e2.cif
_cod_data_source_block           t20180930lc_e16_0m
_cod_database_code               7238000
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.350
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
2. Shared sites
{C7, S7}
{C4, S4}
3. Rigid bond restraints
 S7, C0AA, C2AA, S4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C5 \\sim C1AA \\sim C7 \\sim C4 \\sim C0AA \\sim C2AA: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
S7 \\sim C0AA \\sim C2AA \\sim S4 \\sim C5: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C0AA) \\sim Ueq, Uanis(C2AA) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C7) = Uanis(S7)
Uanis(C4) = Uanis(S4)
5. Others
 Sof(H0AC)=Sof(H0AD)=Sof(S7)=1-FVAR(1)
 Sof(C7)=Sof(H0AA)=Sof(H0AB)=FVAR(1)
 Sof(H2AF)=Sof(H2AG)=Sof(S4)=1-FVAR(2)
 Sof(C4)=Sof(H2AD)=Sof(H2AE)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1AA(H1AA,H1AB), C0AA(H0AA,H0AB), C0AA(H0AC,H0AD), C2AA(H2AD,H2AE), C2AA(H2AF,
 H2AG)
6.b Idealised Me refined as rotating group:
 N2AA(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              40984
_olex2_submission_special_instructions 'No special instructions were received'