Anomalous inclusion of chloride ions in ethylenediammonium lead iodide turns 1D non-perovskite into a 2D perovskite structure
Fazayeli, Monireh; Khatamian, Maasoumeh; Cruciani, Giuseppe; CrystEngComm 22 (2020) 8063–8071; doi:10.1039/D0CE00184H

data_7241764
_publ_section_title
;
 Anomalous inclusion of chloride ions in ethylenediammonium lead iodide
 turns 1D non-perovskite into a 2D perovskite structure
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8063
_journal_page_last               8071
_journal_paper_doi               10.1039/D0CE00184H
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'I4 Pb, 2(Cl), 2(C2 H10 N2)'
_chemical_formula_sum            'C16 H80 Cl8 I16 N16 Pb4'
_chemical_formula_weight         3639.72
_chemical_name_systematic        'ethylenediammonium lead iodide chloride'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Light-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-23
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-24 deposited with the CCDC.	2020-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   8.7590(4)
_cell_length_b                   9.4400(4)
_cell_length_c                   23.5450(8)
_cell_measurement_temperature    296(2)
_cell_volume                     1946.82(14)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.886
_diffrn_measured_fraction_theta_max 0.892
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.886
_diffrn_reflns_Laue_measured_fraction_max 0.892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            10927
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.603
_diffrn_reflns_theta_min         3.289
_exptl_absorpt_coefficient_mu    15.269
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'reddish orange'
_exptl_crystal_density_diffrn    3.104
_exptl_crystal_F_000             1600
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.394
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.271
_refine_ls_extinction_coef       0.00068(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         2071
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.831
_refine_ls_shift/su_mean         0.063
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+66.9166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1165
_reflns_number_total             2071
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00184h2.cif
_cod_data_source_block           96-8-2_ref
_cod_database_code               7241764
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.310
_shelx_estimated_absorpt_t_min   0.310
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 N0AA-H0AA = N0AA-H0AB = N0AA-H0AC
 0.85 with sigma of 0.02
 H0AA-H0AB = H0AA-H0AC = H0AB-H0AC
 1.4 with sigma of 0.02
 C02-H0AA = C02-H0AB = C02-H0AC
 1.9 with sigma of 0.02
 N03-H03A = N03-H03B = N03-H03C
 0.85 with sigma of 0.02
 H03A-H03B = H03A-H03C = H03B-H03C
 1.4 with sigma of 0.02
 C01-H03A = C01-H03B = C01-H03C
 1.9 with sigma of 0.02
3. Others
 Fixed Uiso: H0AA(0.19) H0AB(0.19) H0AC(0.19) H03A(0.19) H03B(0.19) H03C(0.19)
4.a Secondary CH2 refined with riding coordinates:
 C02(H02A,H02B), C01(H01A,H01B)
;
_shelx_res_checksum              26440
_olex2_submission_special_instructions 'No special instructions were received'