Toward Fluorinated Spacers for MAPI-Derived Hybrid Perovskites: Synthesis, Characterization, and Phase Transitions of (FC2H4NH3)2PbCl4
Lermer, Claudia; Birkhold, Susanne T.; Moudrakovski, Igor L.; Mayer, Peter; Schoop, Leslie M.; Schmidt-Mende, Lukas; Lotsch, Bettina V.; Chemistry of Materials 28 (2016) 6560–; doi:10.1021/acs.chemmater.6b02151

data_4002678
_publ_section_title
;
 Toward Fluorinated Spacers for MAPI-Derived Hybrid Perovskites:
 Synthesis, Characterization, and Phase Transitions of (FC2H4NH3)2PbCl4
;
_journal_issue                   18
_journal_name_full               'Chemistry of Materials'
_journal_page_first              6560
_journal_paper_doi               10.1021/acs.chemmater.6b02151
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'Cl4 Pb, 2(C2 H7 F N)'
_chemical_formula_sum            'C4 H14 Cl4 F2 N2 Pb'
_chemical_formula_weight         477.2
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                PbCl4_C2H7FN_sv191op_lotsch
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             04-Jul-14
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7059(3)
_cell_length_b                   18.4574(7)
_cell_length_c                   8.7525(3)
_cell_measurement_reflns_used    9983
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3299
_cell_measurement_theta_min      3.5226
_cell_volume                     1244.88(8)
_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
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    0.8_mm
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0119
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            38015
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         3.52
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    14.398
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.54604(16)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0115
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+0.4700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0232
_refine_ls_wR_factor_ref         0.0250
_reflns_number_gt                1362
_reflns_number_total             1597
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm6b02151_si_002.cif
_cod_data_source_block           sv191op
_cod_database_code               4002678