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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/4/00/26/4002678.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_4002678
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         '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).
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 0.995
_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/[σ²(Fo²)+(0.0113P)²+0.4700P] where P=(Fo²+2Fc²)/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)
_iucr_refine_instructions_details
;
TITL sv191op in Pnma (62) sir97
CELL  0.71069    7.7059   18.4574    8.7525    90.000    90.000    90.000
ZERR        4    0.0003    0.0007    0.0003     0.000     0.000     0.000
LATT   1
SYMM     0.50000 - X ,            - Y ,    0.50000 + Z
SYMM     0.50000 + X ,    0.50000 - Y ,    0.50000 - Z
SYMM             - X ,    0.50000 + Y ,            - Z
SFAC  C  H Cl  F  N Pb
UNIT 16 56 16 8 8 4
OMIT     0   2   0
OMIT     0   1   1
OMIT     0   3   1
LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!!
MERG 2
L.S. 10
FMAP 2
PLAN -20
ACTA
EQIV  $1 -x+2, -y+1, -z+1
EQIV  $2 -x+1, -y+1, -z+1
EQIV  $3 x+1/2, y, -z+3/2
HTAB N1 Cl3
HTAB N1 F1_$1
HTAB N1 Cl3_$2
HTAB N1 Cl3_$3
 
BOND $H
CONF
TEMP  -100
REM #####
WGHT      0.0113      0.4699 
FVAR       0.19239
C1    1    0.863594    0.385656    0.530193    11.00000    0.01812    0.01509 =
         0.02083    0.00222    0.00067    0.00271
AFIX  23
H1A   2    0.824597    0.335078    0.545650    11.00000   -1.20000
H1B   2    0.984204    0.389677    0.568221    11.00000   -1.20000
AFIX   0
C2    1    0.859160    0.403428    0.363313    11.00000    0.02757    0.01579 =
         0.01782   -0.00293    0.00343   -0.00563
AFIX  23
H2A   2    0.919560    0.365128    0.304638    11.00000   -1.20000
H2B   2    0.737374    0.405767    0.327637    11.00000   -1.20000
AFIX   0
CL1   3    0.590907    0.250000    0.729971    10.50000    0.01608    0.02896 =
         0.01656    0.00000   -0.00477    0.00000
CL2   3    0.616648    0.250000    0.297464    10.50000    0.01738    0.02084 =
         0.02091    0.00000    0.00570    0.00000
CL3   3    0.352345    0.405955    0.531554    11.00000    0.01873    0.01444 =
         0.01667    0.00068    0.00021    0.00148
F1    4    0.941343    0.470774    0.338745    11.00000    0.02890    0.01893 =
         0.02188    0.00264    0.00132   -0.00578
N1    5    0.749892    0.435401    0.618301    11.00000    0.01663    0.02043 =
         0.01520    0.00196    0.00167   -0.00008
H1    2    0.633656    0.424979    0.597013    11.00000    0.03744
H2    2    0.773823    0.479685    0.595458    11.00000    0.03863
H3    2    0.773466    0.429084    0.720144    11.00000    0.03814
PB1   6    0.351053    0.250000    0.505081    10.50000    0.01074    0.01192 =
         0.01078    0.00000    0.00000    0.00000
HKLF 4 1  1.0000  0.0000  0.0000  0.0000  0.0000  1.0000  0.0000 -1.0000  0.0000
 
REM  sv191op in Pnma (62) sir97
REM R1 =  0.0115 for   1362 Fo > 4sig(Fo)  and  0.0184 for all   1597 data
REM     76 parameters refined using      0 restraints
 
END  
;
_cod_data_source_file            cm6b02151_si_002.cif
_cod_data_source_block           sv191op
_cod_database_code               4002678
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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 0.8636(3) 0.38566(11) 0.5302(2) 0.0180(4) Uani 1 1 d .
H1A H 0.8246 0.3351 0.5457 0.022 Uiso 1 1 calc R
H1B H 0.9842 0.3897 0.5682 0.022 Uiso 1 1 calc R
C2 C 0.8592(3) 0.40343(11) 0.3633(2) 0.0204(4) Uani 1 1 d .
H2A H 0.9196 0.3651 0.3046 0.024 Uiso 1 1 calc R
H2B H 0.7374 0.4058 0.3276 0.024 Uiso 1 1 calc R
Cl1 Cl 0.59091(9) 0.2500 0.72997(7) 0.02053(15) Uani 1 2 d S
Cl2 Cl 0.61665(9) 0.2500 0.29746(8) 0.01971(15) Uani 1 2 d S
Cl3 Cl 0.35234(6) 0.40596(3) 0.53155(5) 0.01661(10) Uani 1 1 d .
F1 F 0.94134(16) 0.47077(6) 0.33875(12) 0.0232(3) Uani 1 1 d .
N1 N 0.7499(2) 0.43540(10) 0.6183(2) 0.0174(4) Uani 1 1 d .
H1 H 0.634(3) 0.4250(14) 0.597(3) 0.037(7) Uiso 1 1 d .
H2 H 0.774(3) 0.4797(15) 0.595(3) 0.039(8) Uiso 1 1 d .
H3 H 0.773(3) 0.4291(12) 0.720(3) 0.038(7) Uiso 1 1 d .
Pb1 Pb 0.351053(11) 0.2500 0.505081(10) 0.01115(4) Uani 1 2 d S
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.0181(10) 0.0151(10) 0.0208(10) 0.0022(8) 0.0007(8) 0.0027(8)
C2 0.0276(11) 0.0158(10) 0.0178(10) -0.0029(8) 0.0034(8) -0.0056(9)
Cl1 0.0161(3) 0.0290(4) 0.0166(3) 0.000 -0.0048(3) 0.000
Cl2 0.0174(3) 0.0208(4) 0.0209(3) 0.000 0.0057(3) 0.000
Cl3 0.0187(2) 0.0144(2) 0.0167(2) 0.00068(17) 0.00021(17) 0.00148(18)
F1 0.0289(6) 0.0189(6) 0.0219(6) 0.0026(5) 0.0013(5) -0.0058(6)
N1 0.0166(9) 0.0204(10) 0.0152(9) 0.0020(7) 0.0017(7) -0.0001(8)
Pb1 0.01074(5) 0.01192(5) 0.01078(5) 0.000 0.00000(4) 0.000
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'
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
N1 C1 C2 110.95(16) . .
N1 C1 H1A 109.4 . .
C2 C1 H1A 109.4 . .
N1 C1 H1B 109.4 . .
C2 C1 H1B 109.4 . .
H1A C1 H1B 108.0 . .
F1 C2 C1 109.35(15) . .
F1 C2 H2A 109.8 . .
C1 C2 H2A 109.8 . .
F1 C2 H2B 109.8 . .
C1 C2 H2B 109.8 . .
H2A C2 H2B 108.3 . .
Pb1 Cl1 Pb1 177.64(3) . 6_657
C1 N1 H1 109.5(16) . .
C1 N1 H2 109.9(17) . .
H1 N1 H2 111(2) . .
C1 N1 H3 108.0(14) . .
H1 N1 H3 111(2) . .
H2 N1 H3 108(2) . .
Cl1 Pb1 Cl2 88.40(2) . .
Cl1 Pb1 Cl3 86.511(9) . 8_565
Cl2 Pb1 Cl3 92.906(9) . 8_565
Cl1 Pb1 Cl3 86.511(9) . .
Cl2 Pb1 Cl3 92.906(9) . .
Cl3 Pb1 Cl3 170.787(18) 8_565 .
Cl1 Pb1 Cl1 84.041(4) . 6_557
Cl2 Pb1 Cl1 172.44(2) . 6_557
Cl3 Pb1 Cl1 86.649(9) 8_565 6_557
Cl3 Pb1 Cl1 86.649(9) . 6_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.485(3) .
C1 C2 1.497(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 F1 1.412(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
Cl1 Pb1 2.7001(6) .
Cl1 Pb1 3.0653(6) 6_657
Cl2 Pb1 2.7369(6) .
Cl3 Pb1 2.8879(5) .
N1 H1 0.93(2) .
N1 H2 0.86(3) .
N1 H3 0.92(3) .
Pb1 Cl3 2.8878(5) 8_565
Pb1 Cl1 3.0653(6) 6_557
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 H1 Cl3 0.93(2) 2.27(3) 3.2026(19) 176(2) .
N1 H2 F1 0.86(3) 2.45(3) 2.967(2) 119(2) 5_766
N1 H2 Cl3 0.86(3) 2.58(3) 3.304(2) 143(2) 5_666
N1 H3 Cl3 0.92(3) 2.30(3) 3.2110(18) 175(2) 6_657
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
N1 C1 C2 F1 68.8(2)
