 
data_(FMTMA)PbI3
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C14 H20 Fe N, I3 Pb'
_chemical_formula_sum
 'C14 H20 Fe I3 N Pb ' 
_chemical_formula_weight          846.06

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'
 'Fe'  'Fe'   0.3463   0.8444
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'I'  'I'  -0.4742   1.8119
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            5
_space_group_name_H-M_alt         'C 2'
_space_group_name_Hall            'C 2y'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 
_cell_length_a                    25.8959(16)
_cell_length_b                    10.0928(5)
_cell_length_c                    7.9440(4)
_cell_angle_alpha                 90
_cell_angle_beta                  93.798(5)
_cell_angle_gamma                 90
_cell_volume                      2071.70(19)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     5330
_cell_measurement_theta_min       2.4470
_cell_measurement_theta_max       30.6610
 
_exptl_crystal_description        Flake
_exptl_crystal_colour             brown
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.713          
_exptl_crystal_F_000              1512
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.3
_exptl_crystal_size_mid           0.28
_exptl_crystal_size_min           0.25
_exptl_absorpt_coefficient_mu     13.279
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.11321
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.40.60a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source 'Rotating-anode X-ray tube'
_diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method        'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             5717
_diffrn_reflns_av_unetI/netI      0.0649
_diffrn_reflns_av_R_equivalents   0.0599
_diffrn_reflns_limit_h_min        -30
_diffrn_reflns_limit_h_max        30
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        9
_diffrn_reflns_theta_min          2.570
_diffrn_reflns_theta_max          24.998
_diffrn_reflns_theta_full         24.998
_diffrn_measured_fraction_theta_max   0.999
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.999
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.999
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              3207
_reflns_number_gt                 3004
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.882
_reflns_Friedel_fraction_max      0.999
_reflns_Friedel_fraction_full     0.999
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_cell_refinement     'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction      'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1118P)²+31.8915P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.082(8)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          3207
_refine_ls_number_parameters      186
_refine_ls_number_restraints      128
_refine_ls_R_factor_all           0.0637
_refine_ls_R_factor_gt            0.0611
_refine_ls_wR_factor_ref          0.1764
_refine_ls_wR_factor_gt           0.1742
_refine_ls_goodness_of_fit_ref    1.099
_refine_ls_restrained_S_all       1.086
_refine_ls_shift/su_max           0.002
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
C1 C 0.3097(4) 0.6369(9) 0.1899(11) 0.034(2) Uani 1 1 d . U . . .
C2 C 0.2645(5) 0.5598(9) 0.2029(14) 0.052(3) Uani 1 1 d . U . . .
H2 H 0.2613 0.4874 0.2839 0.062 Uiso 1 1 calc R U . . .
C3 C 0.2232(7) 0.6055(16) 0.0901(19) 0.078(4) Uani 1 1 d . U . . .
H3 H 0.1879 0.5703 0.0751 0.094 Uiso 1 1 calc R U . . .
C4 C 0.2458(5) 0.7162(14) -0.0012(16) 0.063(3) Uani 1 1 d . U . . .
H4 H 0.2279 0.7712 -0.0885 0.076 Uiso 1 1 calc R U . . .
C5 C 0.2973(5) 0.7319(11) 0.0650(13) 0.050(3) Uani 1 1 d . U . . .
H5 H 0.3211 0.8006 0.0297 0.059 Uiso 1 1 calc R U . . .
C6 C 0.2753(6) 0.8754(16) 0.4441(18) 0.078(4) Uani 1 1 d . U . . .
H6 H 0.3113 0.8962 0.4812 0.094 Uiso 1 1 calc R U . . .
C7 C 0.2458(7) 0.7744(14) 0.4990(19) 0.067(3) Uani 1 1 d . U . . .
H7 H 0.2581 0.7089 0.5833 0.080 Uiso 1 1 calc R U . . .
C8 C 0.2003(5) 0.7784(16) 0.4330(18) 0.075(4) Uani 1 1 d . U . . .
H8 H 0.1734 0.7142 0.4577 0.090 Uiso 1 1 calc R U . . .
C9 C 0.1925(4) 0.8810(16) 0.320(2) 0.103(5) Uani 1 1 d D U . . .
H9 H 0.1606 0.9055 0.2545 0.124 Uiso 1 1 calc R U . . .
C10 C 0.2431(4) 0.9438(12) 0.3197(17) 0.074(4) Uani 1 1 d D U . . .
H10 H 0.2523 1.0218 0.2546 0.089 Uiso 1 1 calc R U . . .
C11 C 0.3579(4) 0.6261(9) 0.3033(12) 0.039(2) Uani 1 1 d . U . . .
H11A H 0.3489 0.5911 0.4111 0.047 Uiso 1 1 calc R U . . .
H11B H 0.3719 0.7144 0.3230 0.047 Uiso 1 1 calc R U . . .
C12 C 0.4169(5) 0.5959(16) 0.0748(17) 0.073(4) Uani 1 1 d . U . . .
H12A H 0.4499 0.5583 0.0531 0.109 Uiso 1 1 calc R U . . .
H12B H 0.4201 0.6905 0.0838 0.109 Uiso 1 1 calc R U . . .
H12C H 0.3921 0.5741 -0.0161 0.109 Uiso 1 1 calc R U . . .
C13 C 0.4443(7) 0.535(2) 0.3680(17) 0.090(5) Uani 1 1 d . U . . .
H13A H 0.4648 0.4580 0.3489 0.135 Uiso 1 1 calc R U . . .
H13B H 0.4316 0.5306 0.4786 0.135 Uiso 1 1 calc R U . . .
H13C H 0.4652 0.6131 0.3593 0.135 Uiso 1 1 calc R U . . .
C14 C 0.3818(7) 0.4028(12) 0.207(2) 0.087(5) Uani 1 1 d . U . . .
H14A H 0.4103 0.3507 0.1721 0.131 Uiso 1 1 calc R U . . .
H14B H 0.3543 0.4015 0.1199 0.131 Uiso 1 1 calc R U . . .
H14C H 0.3697 0.3665 0.3088 0.131 Uiso 1 1 calc R U . . .
Fe1 Fe 0.25021(6) 0.75169(15) 0.25280(19) 0.0423(4) Uani 1 1 d . U . . .
I1 I 0.54514(3) 0.25935(7) 0.24567(9) 0.0530(2) Uani 1 1 d . U . . .
I2 I 0.40243(2) 0.02452(8) 0.22915(8) 0.04791(17) Uani 1 1 d . U . . .
I3 I 0.55588(4) -0.17452(7) 0.27432(9) 0.0611(2) Uani 1 1 d . U . . .
N1 N 0.3991(3) 0.5407(8) 0.2375(9) 0.0389(18) Uani 1 1 d . U . . .
Pb1 Pb 0.5000 0.03346(6) 0.0000 0.04271(12) Uani 1 2 d S TU P . .
Pb2 Pb 0.5000 0.03536(6) 0.5000 0.04121(12) Uani 1 2 d S TU P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
C1 C5 1.401(14) . ?
C1 C2 1.416(15) . ?
C1 C11 1.494(13) . ?
C1 Fe1 2.016(9) . ?
C2 C3 1.43(2) . ?
C2 Fe1 2.016(10) . ?
C3 C4 1.48(2) . ?
C3 Fe1 2.054(16) . ?
C4 C5 1.410(18) . ?
C4 Fe1 2.045(13) . ?
C5 Fe1 1.999(12) . ?
C6 C7 1.36(2) . ?
C6 C10 1.428(19) . ?
C6 Fe1 2.039(15) . ?
C7 C8 1.26(2) . ?
C7 Fe1 1.980(15) . ?
C8 C9 1.38(2) . ?
C8 Fe1 2.009(14) . ?
C9 C10 1.454(14) . ?
C9 Fe1 2.079(14) . ?
C10 Fe1 2.022(12) . ?
C11 N1 1.494(13) . ?
C12 N1 1.507(16) . ?
C13 N1 1.511(17) . ?
C14 N1 1.478(15) . ?
I1 Pb1 3.1735(8) . ?
I1 Pb2 3.2973(8) . ?
I2 Pb2 3.2102(6) . ?
I2 Pb1 3.2117(7) . ?
I3 Pb2 3.1842(9) . ?
I3 Pb1 3.2911(9) . ?
Pb1 I1 3.1735(8) 2_655 ?
Pb1 I2 3.2117(7) 2_655 ?
Pb1 I3 3.2911(9) 2_655 ?
Pb2 I3 3.1842(9) 2_656 ?
Pb2 I2 3.2101(6) 2_656 ?
Pb2 I1 3.2973(8) 2_656 ?
 
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
 _geom_angle_publ_flag
C5 C1 C2 106.1(9) . . ?
C5 C1 C11 128.3(9) . . ?
C2 C1 C11 125.3(9) . . ?
C5 C1 Fe1 68.9(6) . . ?
C2 C1 Fe1 69.4(6) . . ?
C11 C1 Fe1 120.9(6) . . ?
C1 C2 C3 111.4(10) . . ?
C1 C2 Fe1 69.5(5) . . ?
C3 C2 Fe1 70.9(8) . . ?
C2 C3 C4 104.4(12) . . ?
C2 C3 Fe1 68.1(7) . . ?
C4 C3 Fe1 68.6(8) . . ?
C5 C4 C3 107.4(11) . . ?
C5 C4 Fe1 67.8(7) . . ?
C3 C4 Fe1 69.2(8) . . ?
C1 C5 C4 110.7(10) . . ?
C1 C5 Fe1 70.2(6) . . ?
C4 C5 Fe1 71.4(7) . . ?
C7 C6 C10 105.5(13) . . ?
C7 C6 Fe1 67.8(9) . . ?
C10 C6 Fe1 68.8(8) . . ?
C8 C7 C6 111.9(15) . . ?
C8 C7 Fe1 72.9(10) . . ?
C6 C7 Fe1 72.5(9) . . ?
C7 C8 C9 112.8(14) . . ?
C7 C8 Fe1 70.4(10) . . ?
C9 C8 Fe1 73.1(9) . . ?
C8 C9 C10 103.7(11) . . ?
C8 C9 Fe1 67.6(8) . . ?
C10 C9 Fe1 67.1(7) . . ?
C6 C10 C9 105.9(12) . . ?
C6 C10 Fe1 70.1(8) . . ?
C9 C10 Fe1 71.4(8) . . ?
C1 C11 N1 114.8(8) . . ?
C7 Fe1 C5 145.8(6) . . ?
C7 Fe1 C8 36.7(7) . . ?
C5 Fe1 C8 176.7(5) . . ?
C7 Fe1 C1 114.0(6) . . ?
C5 Fe1 C1 40.8(4) . . ?
C8 Fe1 C1 142.3(5) . . ?
C7 Fe1 C2 109.2(5) . . ?
C5 Fe1 C2 68.2(5) . . ?
C8 Fe1 C2 113.8(6) . . ?
C1 Fe1 C2 41.1(4) . . ?
C7 Fe1 C10 67.5(6) . . ?
C5 Fe1 C10 111.3(5) . . ?
C8 Fe1 C10 67.0(6) . . ?
C1 Fe1 C10 134.5(4) . . ?
C2 Fe1 C10 173.7(5) . . ?
C7 Fe1 C6 39.6(6) . . ?
C5 Fe1 C6 115.9(5) . . ?
C8 Fe1 C6 64.9(6) . . ?
C1 Fe1 C6 109.0(5) . . ?
C2 Fe1 C6 132.9(6) . . ?
C10 Fe1 C6 41.2(6) . . ?
C7 Fe1 C4 172.7(7) . . ?
C5 Fe1 C4 40.8(5) . . ?
C8 Fe1 C4 136.9(6) . . ?
C1 Fe1 C4 69.4(5) . . ?
C2 Fe1 C4 68.7(5) . . ?
C10 Fe1 C4 115.3(6) . . ?
C6 Fe1 C4 146.7(6) . . ?
C7 Fe1 C3 131.7(6) . . ?
C5 Fe1 C3 70.0(6) . . ?
C8 Fe1 C3 109.6(6) . . ?
C1 Fe1 C3 70.5(5) . . ?
C2 Fe1 C3 41.0(6) . . ?
C10 Fe1 C3 145.2(6) . . ?
C6 Fe1 C3 170.8(6) . . ?
C4 Fe1 C3 42.2(6) . . ?
C7 Fe1 C9 65.4(7) . . ?
C5 Fe1 C9 137.6(6) . . ?
C8 Fe1 C9 39.3(7) . . ?
C1 Fe1 C9 176.0(5) . . ?
C2 Fe1 C9 142.9(5) . . ?
C10 Fe1 C9 41.5(4) . . ?
C6 Fe1 C9 67.9(6) . . ?
C4 Fe1 C9 111.7(6) . . ?
C3 Fe1 C9 113.1(6) . . ?
Pb1 I1 Pb2 75.710(18) . . ?
Pb2 I2 Pb1 76.415(14) . . ?
Pb2 I3 Pb1 75.654(19) . . ?
C14 N1 C11 112.7(9) . . ?
C14 N1 C12 108.3(10) . . ?
C11 N1 C12 110.7(9) . . ?
C14 N1 C13 106.8(12) . . ?
C11 N1 C13 108.7(9) . . ?
C12 N1 C13 109.6(10) . . ?
I1 Pb1 I1 88.15(3) . 2_655 ?
I1 Pb1 I2 95.58(2) . 2_655 ?
I1 Pb1 I2 86.74(2) 2_655 2_655 ?
I1 Pb1 I2 86.74(2) . . ?
I1 Pb1 I2 95.58(2) 2_655 . ?
I2 Pb1 I2 176.78(3) 2_655 . ?
I1 Pb1 I3 85.590(19) . . ?
I1 Pb1 I3 173.37(2) 2_655 . ?
I2 Pb1 I3 91.69(2) 2_655 . ?
I2 Pb1 I3 86.25(2) . . ?
I1 Pb1 I3 173.37(2) . 2_655 ?
I1 Pb1 I3 85.590(19) 2_655 2_655 ?
I2 Pb1 I3 86.26(2) 2_655 2_655 ?
I2 Pb1 I3 91.69(2) . 2_655 ?
I3 Pb1 I3 100.74(3) . 2_655 ?
I3 Pb2 I3 96.59(3) . 2_656 ?
I3 Pb2 I2 89.30(2) . 2_656 ?
I3 Pb2 I2 88.10(2) 2_656 2_656 ?
I3 Pb2 I2 88.10(2) . . ?
I3 Pb2 I2 89.30(2) 2_656 . ?
I2 Pb2 I2 176.09(3) 2_656 . ?
I3 Pb2 I1 85.315(19) . . ?
I3 Pb2 I1 173.66(2) 2_656 . ?
I2 Pb2 I1 97.98(2) 2_656 . ?
I2 Pb2 I1 84.718(19) . . ?
I3 Pb2 I1 173.67(2) . 2_656 ?
I3 Pb2 I1 85.315(19) 2_656 2_656 ?
I2 Pb2 I1 84.718(19) 2_656 2_656 ?
I2 Pb2 I1 97.98(2) . 2_656 ?
I1 Pb2 I1 93.43(3) . 2_656 ?
 
_refine_diff_density_max    3.130
_refine_diff_density_min   -2.724
_refine_diff_density_rms    0.353



