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#$Date: 2016-10-04 10:11:08 +0300 (Tue, 04 Oct 2016) $
#$Revision: 186902 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/26/4002679.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4002679
loop_
_publ_author_name
'Lermer, Claudia'
'Birkhold, Susanne T.'
'Moudrakovski, Igor L.'
'Mayer, Peter'
'Schoop, Leslie M.'
'Schmidt-Mende, Lukas'
'Lotsch, Bettina V.'
_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).
Acta Cryst. A64, 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/[σ²(Fo²)+(0.0211P)²+0.9657P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C -0.0044(14) 0.7057(5) 0.0313(4) 0.0439(14) Uani 1 1 d .
H1A H -0.0706 0.7133 0.1025 0.053 Uiso 1 1 calc R
H1B H -0.1642 0.6693 0.0051 0.053 Uiso 1 1 calc R
C2 C 0.0347(13) 0.8262(5) -0.0211(3) 0.0307(11) Uani 1 1 d .
H2A H 0.1912 0.8629 0.0066 0.037 Uiso 1 1 calc R
H2B H -0.1607 0.8784 -0.0105 0.037 Uiso 1 1 calc R
C3 C 0.3099(11) 0.3339(4) 0.2767(4) 0.0242(10) Uani 1 1 d .
H3 H 0.2230 0.2851 0.3317 0.029 Uiso 1 1 calc R
C4 C 0.5781(13) 0.5071(4) 0.2152(4) 0.0316(11) Uani 1 1 d .
H4A H 0.8002 0.5008 0.2148 0.047 Uiso 1 1 calc R
H4B H 0.4903 0.5895 0.2256 0.047 Uiso 1 1 calc R
H4C H 0.5334 0.4861 0.1520 0.047 Uiso 1 1 calc R
C5 C 0.4774(14) 0.4461(4) 0.3946(3) 0.0327(11) Uani 1 1 d .
H5A H 0.3800 0.3854 0.4411 0.049 Uiso 1 1 calc R
H5B H 0.3791 0.5261 0.4087 0.049 Uiso 1 1 calc R
H5C H 0.6952 0.4409 0.4013 0.049 Uiso 1 1 calc R
N1 N 0.1301(9) 0.8187(3) -0.1291(3) 0.0239(8) Uani 1 1 d .
H1C H 0.320(7) 0.774(3) -0.1393(5) 0.036 Uiso 1 1 calc R
H1D H 0.143(7) 0.896(2) -0.1604(11) 0.036 Uiso 1 1 calc R
H1E H -0.013(6) 0.782(3) -0.1547(9) 0.036 Uiso 1 1 calc R
N2 N 0.4448(9) 0.4250(3) 0.2948(3) 0.0229(8) Uani 1 1 d .
F1 F 0.2692(10) 0.6331(4) 0.0186(3) 0.0644(11) Uani 1 1 d .
Br2 Br 1.21328(11) -0.10049(4) 0.61507(3) 0.02077(9) Uani 1 1 d .
Br3 Br 0.56665(11) 0.05122(4) 0.83390(3) 0.02501(10) Uani 1 1 d .
Br1 Br 0.09070(11) 0.26946(4) 0.63125(4) 0.03074(11) Uani 1 1 d .
Pb1 Pb 0.65368(4) 0.091490(13) 0.626673(11) 0.01760(6) Uani 1 1 d .
O1 O 0.2867(8) 0.3066(3) 0.1936(2) 0.0286(7) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
F1 C1 C2 109.7(5) . .
F1 C1 H1A 109.7 . .
C2 C1 H1A 109.7 . .
F1 C1 H1B 109.7 . .
C2 C1 H1B 109.7 . .
H1A C1 H1B 108.2 . .
C1 C2 N1 111.3(4) . .
C1 C2 H2A 109.4 . .
N1 C2 H2A 109.4 . .
C1 C2 H2B 109.4 . .
N1 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
O1 C3 N2 125.3(4) . .
O1 C3 H3 117.4 . .
N2 C3 H3 117.4 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
N2 C5 H5A 109.5 . .
N2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
N2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C2 N1 H1C 109.5 . .
C2 N1 H1D 109.5 . .
H1C N1 H1D 109.5 . .
C2 N1 H1E 109.5 . .
H1C N1 H1E 109.5 . .
H1D N1 H1E 109.5 . .
C3 N2 C5 121.5(4) . .
C3 N2 C4 121.5(4) . .
C5 N2 C4 117.0(4) . .
Pb1 Br2 Pb1 91.405(12) . 1_655
Pb1 Br1 Pb1 96.070(13) 1_455 .
Br3 Pb1 Br1 91.759(15) . 1_655
Br3 Pb1 Br1 91.184(15) . .
Br1 Pb1 Br1 96.072(13) 1_655 .
Br3 Pb1 Br2 90.390(13) . .
Br1 Pb1 Br2 86.857(13) 1_655 .
Br1 Pb1 Br2 176.630(13) . .
Br3 Pb1 Br2 89.858(13) . 1_455
Br1 Pb1 Br2 177.633(13) 1_655 1_455
Br1 Pb1 Br2 85.620(13) . 1_455
Br2 Pb1 Br2 91.405(12) . 1_455
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 F1 1.381(7) .
C1 C2 1.485(7) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 N1 1.493(6) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O1 1.237(5) .
C3 N2 1.311(6) .
C3 H3 0.9500 .
C4 N2 1.459(6) .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 N2 1.449(6) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
N1 H1C 0.9306 .
N1 H1D 0.9307 .
N1 H1E 0.9307 .
Br2 Pb1 3.0917(5) .
Br2 Pb1 3.1165(5) 1_655
Br3 Pb1 2.8168(5) .
Br1 Pb1 2.9650(5) 1_455
Br1 Pb1 3.0108(5) .
Pb1 Br1 2.9649(5) 1_655
Pb1 Br2 3.1166(5) 1_455
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1C O1 0.93 1.95 2.865(5) 166.4 2_665
N1 H1D Br3 0.93 2.71 3.395(4) 131.1 1_564
N1 H1E O1 0.93 1.83 2.755(5) 172.8 2_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
F1 C1 C2 N1 60.3(6) . .
O1 C3 N2 C5 -176.2(5) . .
O1 C3 N2 C4 1.6(7) . .
Pb1 Br1 Pb1 Br3 -88.104(15) 1_455 .
Pb1 Br1 Pb1 Br1 180.0 1_455 1_655
Pb1 Br1 Pb1 Br2 1.663(14) 1_455 1_455
Pb1 Br2 Pb1 Br3 -90.133(13) 1_655 .
Pb1 Br2 Pb1 Br1 1.607(14) 1_655 1_655
Pb1 Br2 Pb1 Br2 179.999(2) 1_655 1_455
