Completing the Picture of 2-(Aminomethylpyridinium) Lead Hybrid Perovskites: Insights into Structure, Conductivity Behavior, and Optical Properties
Lermer, Claudia; Senocrate, Alessandro; Moudrakovski, Igor; Seewald, Tobias; Hatz, Anna-Katharina; Mayer, Peter; Pielnhofer, Florian; Jaser, Julian A.; Schmidt-Mende, Lukas; Maier, Joachim; Lotsch, Bettina V.; Chemistry of Materials 30 (2018) 6289–; doi:10.1021/acs.chemmater.8b01840

data_4003367
_publ_section_title
;
 Completing the Picture of 2-(Aminomethylpyridinium) Lead Hybrid
 Perovskites: Insights into Structure, Conductivity Behavior, and Optical
 Properties
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6289
_journal_paper_doi               10.1021/acs.chemmater.8b01840
_journal_volume                  30
_journal_year                    2018
_chemical_formula_moiety         'Cl16 Pb4, 4(C6 H10 N2)'
_chemical_formula_sum            'C24 H40 Cl16 N8 Pb4'
_chemical_formula_weight         1836.60
_chemical_name_common            CLE13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_block_code                Pb4Cl16_4C6H10N2_tv308_lotsch
_audit_creation_method           SHELXL-2014
_audit_update_record             03-Sep-15
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.1050(8)
_cell_length_b                   15.7555(6)
_cell_length_c                   16.6214(6)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3941
_cell_measurement_theta_min      3.0748
_cell_volume                     4741.3(3)
_computing_cell_refinement       'APEX2 v2012.4-3 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.21'
_computing_data_reduction        'SAINT V8.18C (Bruker AXS Inc., 2011)'
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_computing_structure_solution
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'fixed-chi three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8Venture'
_diffrn_measurement_method       'mix of phi and omega scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45933
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         2.991
_diffrn_source                   'rotating anode (TXS)'
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    15.093
_exptl_absorpt_correction_T_max  0.5624
_exptl_absorpt_correction_T_min  0.3422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         2.076
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.534(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9700
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0196
_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^)+(0.0145P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0390
_refine_ls_wR_factor_ref         0.0402
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8927
_reflns_number_total             9700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b01840_si_002.cif
_cod_data_source_block           tv308
_cod_database_code               4003367
_shelxl_version_number           2014-3
_shelx_res_checksum              29218
_shelx_hkl_checksum              74783