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_4002679
_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         'Br3 Pb, C3 H7 N O, C2 H7 F N'
_chemical_formula_sum            'C5 H14 Br3 F N2 O Pb'
_chemical_formula_weight         584.1
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                PbBr3_C2H7FN_dmf_sv225_lotsch
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             22-Jul-14
_cell_angle_alpha                83.8913(14)
_cell_angle_beta                 81.4800(17)
_cell_angle_gamma                83.1354(17)
_cell_formula_units_Z            2
_cell_length_a                   4.4434(2)
_cell_length_b                   11.2688(6)
_cell_length_c                   13.7677(7)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3098
_cell_measurement_theta_min      3.0044
_cell_volume                     674.11(6)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0331
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8838
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         3.00
_diffrn_source_current           50
_diffrn_source_power             2.5
_diffrn_source_type              'Bruker TXS'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    21.388
_exptl_absorpt_correction_T_max  0.4920
_exptl_absorpt_correction_T_min  0.3248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.8776(3)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.036
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+0.9657P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                2932
_reflns_number_total             3330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm6b02151_si_002.cif
_cod_data_source_block           sv225
_cod_database_code               4002679