Low-Dimensional Hybrid Lead Iodide Perovskites Single Crystals via Bifunctional Amino Acid Cross-Linkage: Structural Diversity and Properties Controllability.
Xie, Guanying; Wang, Lei; Li, Peizhou; Song, Shuang; Yao, Changlin; Wang, Shanpeng; Liu, Yang; Wang, Zhen; Wang, Xinyuan; Tao, Xutang; ACS applied materials & interfaces 13 (2021) 3325–3335; doi:10.1021/acsami.0c16402

data_4518403
_publ_section_title
;
 Low-Dimensional Hybrid Lead Iodide Perovskites Single Crystals via
 Bifunctional Amino Acid Cross-Linkage: Structural Diversity and
 Properties Controllability.
;
_journal_issue                   2
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              3325
_journal_page_last               3335
_journal_paper_doi               10.1021/acsami.0c16402
_journal_volume                  13
_journal_year                    2021
_chemical_formula_moiety         'I6 Pb2, 2(C6 H14 N O2)'
_chemical_formula_sum            'C12 H28 I6 N2 O4 Pb2'
_chemical_formula_weight         1440.16
_space_group_crystal_system      orthorhombic
_space_group_IT_number           46
_space_group_name_Hall           'I 2 -2a'
_space_group_name_H-M_alt        'I m a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8547(3)
_cell_length_b                   20.5457(9)
_cell_length_c                   7.9790(3)
_cell_measurement_reflns_used    5537
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      31.19
_cell_measurement_theta_min      2.50
_cell_volume                     1451.59(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      250.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            11628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.198
_diffrn_reflns_theta_min         1.982
_exptl_absorpt_coefficient_mu    17.981
_exptl_crystal_density_diffrn    3.295
_exptl_crystal_description       yellow
_exptl_crystal_F_000             1256.0
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.268
_refine_diff_density_rms         0.332
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.0064(4)
_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   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         2882
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0504P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                2459
_reflns_number_total             2882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am0c16402_si_003.cif
_cod_data_source_block           c6(1)
_cod_depositor_comments
'Adding full bibliography for 4518400--4518404.cif.'
_cod_database_code               4518403
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Restrained distances
 C1-O2
 1.43 with sigma of 0.02
 C1-O1
 1.2 with sigma of 0.02
 C1-C2 = C2-C3 = C3-C4
 1.54 with sigma of 0.02
 C4-C5 = C5-C6
 1.54 with sigma of 0.02
 C6-N1
 1.48 with sigma of 0.02
 C5-N1
 2.5 with sigma of 0.02
 C2-O2
 2.5 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(N1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
5. Others
 Fixed Sof: O1(0.5) O2(0.5) H2(0.5) C1(0.5) C2(0.5) H2A(0.5) H2B(0.5) C3(0.5)
 H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5) C6(0.5)
 H6A(0.5) H6B(0.5) N1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
6.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
6.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              53589
_shelx_hkl_checksum              37879
_olex2_submission_special_instructions 'No special instructions were received'