Decreasing the electronic confinement in layered perovskites through intercalation.
Smith, Matthew D.; Pedesseau, Laurent; Kepenekian, Mikaël; Smith, Ian C.; Katan, Claudine; Even, Jacky; Karunadasa, Hemamala I.; Chemical science 8 (2017) 1960–1968; doi:10.1039/c6sc02848a

data_1544657
_publ_section_title
;
 Decreasing the electronic confinement in layered perovskites through
 intercalation.
;
_journal_issue                   3
_journal_name_full               'Chemical science'
_journal_page_first              1960
_journal_page_last               1968
_journal_paper_doi               10.1039/c6sc02848a
_journal_volume                  8
_journal_year                    2017
_chemical_formula_moiety         '0.5(I8 Pb2), 2(C6 H15 I N)'
_chemical_formula_sum            'C12 H30 I6 N2 Pb'
_chemical_formula_weight         1170.97
_chemical_name_common            'bis(6-iodohexylammonium) tetraiodoplumbate'
_chemical_name_systematic
'bis(6-iodohexan-1-aminium) tetraiodoplumbate'
_chemical_properties_physical    ', Moisture-sensitive,Light-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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-27 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.0651(11)
_cell_length_b                   8.8852(10)
_cell_length_c                   33.617(5)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.282
_cell_measurement_theta_min      2.424
_cell_volume                     2707.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            48334
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.358
_diffrn_reflns_theta_min         2.553
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.070
_exptl_absorpt_correction_T_max  0.3322
_exptl_absorpt_correction_T_min  0.2406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1084 before and 0.0574 after correction.
The Ratio of minimum to maximum transmission is 0.7243.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             2064
_exptl_crystal_preparation       ', Luminescent'
_exptl_crystal_recrystallization_method
'Vapor diffusion of ether into acetonitrile'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.922
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+12.7240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2025
_reflns_number_total             2479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc02848a2.cif
_cod_data_source_block           g1_ortho_p_0_83_a
_cod_depositor_comments
;Adding full bibliography for 1544657.cif.

 Adding full bibliography for 1544657.cif.
;
_cod_database_code               1544657
_shelxl_version_number           2014-3
_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,H,H,H) groups
2. Restrained distances
 C2-C3 = C3-C4
 1.55 with sigma of 0.02
 C2A-C3A = C3A-C4A
 1.55 with sigma of 0.02
 C2-C4
 2.539 with sigma of 0.04
 C2A-C4A
 2.539 with sigma of 0.04
 C5-C4 \\sim C5A-C4A
 with sigma of 0.02
 C6-C5 \\sim C6A-C5A
 with sigma of 0.02
 I3-C6 \\sim I3-C6A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 N1-C1 \\sim N1-C1A
 with sigma of 0.02
3. Restrained angles
 C2-C3-C4
 fixed at 109.5 with sigma of 0.02
 C2-C3-C4
 fixed at 109.5 with sigma of 0.02
 C2-C3-C4
 fixed at 110 with sigma of 0.02
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
6. Others
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(C1A)=Sof(H1AD)=Sof(H1AE)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C3A)=
 Sof(H3AA)=Sof(H3AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C1(H1A,H1B), C4(H4A,H4B), C5(H5A,H5B), C2(H2A,H2B), C6(H6A,H6B),
 C1A(H1AD,H1AE), C2A(H2AA,H2AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C3A(H3AA,H3AB),
  C6A(H6AA,H6AB)
7.b Me refined with riding coordinates:
 N1(H1AA,H1AB,H1AC), N1(H1BD,H1BE,H1BF)
;
_shelx_res_checksum              33951
_olex2_exptl_crystal_mounting_method 'Mitegen micromount loop'
_olex2_submission_original_sample_id MS10
_olex2_submission_special_instructions 'No special instructions were received'