 
data_IMM2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'I4 Pb, 2(C6 H12 F2 N) '
_chemical_formula_sum
 'C12 H24 F4 I4 N2 Pb ' 
_chemical_formula_weight          987.13

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'
 '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       orthorhombic
_space_group_IT_number            44
_space_group_name_H-M_alt         'I m m 2'
_space_group_name_Hall            'I 2 -2'
 
_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, -y, z'
 '-x, y, z'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 'x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, z+1/2'
 
_cell_length_a                    27.464(9)
_cell_length_b                    6.5518(10)
_cell_length_c                    6.5518(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1178.9(5)
_cell_formula_units_Z             2
_cell_measurement_temperature     423(2)
_cell_measurement_reflns_used   1164
_cell_measurement_theta_min     3.1670
_cell_measurement_theta_max     26.3660
 
_exptl_crystal_description        sheet
_exptl_crystal_colour             red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.781         
_exptl_crystal_F_000              880
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid           0.27
_exptl_crystal_size_min           0.25
_exptl_absorpt_coefficient_mu     12.421
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.034
_exptl_absorpt_correction_T_max   0.045
_exptl_absorpt_process_details    
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       423(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        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             3406
_diffrn_reflns_av_unetI/netI      0.1111
_diffrn_reflns_av_R_equivalents   0.1259
_diffrn_reflns_limit_h_min        -32
_diffrn_reflns_limit_h_max        28
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          2.967
_diffrn_reflns_theta_max          24.979
_diffrn_reflns_theta_full         24.979
_diffrn_measured_fraction_theta_max   0.995
_diffrn_measured_fraction_theta_full  0.995
_diffrn_reflns_Laue_measured_fraction_max    0.995
_diffrn_reflns_Laue_measured_fraction_full   0.995
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              1156
_reflns_number_gt                 591
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.830
_reflns_Friedel_fraction_max      0.998
_reflns_Friedel_fraction_full     0.998
 
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_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    0.52(3)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1156
_refine_ls_number_parameters      93
_refine_ls_number_restraints      160
_refine_ls_R_factor_all           0.2239
_refine_ls_R_factor_gt            0.1715
_refine_ls_wR_factor_ref          0.4769
_refine_ls_wR_factor_gt           0.4511
_refine_ls_goodness_of_fit_ref    1.585
_refine_ls_restrained_S_all       1.486
_refine_ls_shift/su_max           0.012
_refine_ls_shift/su_mean          0.003
 
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
N1 N 0.3776(4) 0.0000 0.6218(16) 0.127(4) Uani 1 2 d DS TU P . .
H1A H 0.3914 0.0000 0.4979 0.152 Uiso 1 2 d R U P . .
H1B H 0.3869 -0.1202 0.6756 0.152 Uiso 0.5 1 d R U P . .
C2 C 0.3225(3) 0.0000 0.5975(14) 0.130(4) Uani 1 2 d DS TU P . .
H2A H 0.3157 -0.1168 0.5137 0.156 Uiso 0.5 1 d R U P . .
H2B H 0.3157 0.1168 0.5137 0.156 Uiso 0.5 1 d R U P . .
C3 C 0.2831(3) 0.0000 0.7540(13) 0.127(3) Uani 1 2 d DS TU P . .
H3A H 0.2758 -0.1398 0.7852 0.152 Uiso 0.5 1 d R U P . .
H3B H 0.2546 0.0571 0.6916 0.152 Uiso 0.5 1 d R U P . .
C4 C 0.2908(3) 0.108(3) 0.9531(12) 0.129(3) Uani 0.5 1 d D U P . .
C5 C 0.3400(3) 0.068(2) 1.0472(9) 0.128(3) Uani 0.5 1 d D U P . .
H5A H 0.3528 -0.0658 1.0209 0.154 Uiso 0.5 1 d R U P . .
H5B H 0.3419 0.1016 1.1896 0.154 Uiso 0.5 1 d R U P . .
C6 C 0.3591(6) 0.230(2) 0.909(2) 0.128(4) Uani 0.5 1 d D U P . .
H6A H 0.3738 0.3340 0.9918 0.154 Uiso 0.5 1 d R U P . .
H6B H 0.3321 0.2915 0.8387 0.154 Uiso 0.5 1 d R U P . .
F1 F 0.2517(5) 0.082(4) 0.8272(15) 0.129(4) Uani 0.5 1 d D U P . .
F2 F 0.2734(8) 0.098(5) 1.1477(13) 0.130(4) Uani 0.5 1 d D U P . .
C1 C 0.3956(2) 0.1664(18) 0.7549(13) 0.128(4) Uani 0.5 1 d D U P . .
H1C H 0.4039 0.2815 0.6711 0.153 Uiso 0.5 1 d R U P . .
H1D H 0.4247 0.1223 0.8233 0.153 Uiso 0.5 1 d R U P . .
I1 I 0.5000 1.0000 0.3517(11) 0.1201(14) Uani 1 4 d S T P . .
I2 I 0.38566(16) 0.5000 0.2713(11) 0.200(3) Uani 1 2 d S T P . .
I3 I 0.5000 0.5000 -0.1476(14) 0.152(2) Uani 1 4 d S T P . .
Pb1 Pb 0.5000 0.5000 0.3441(5) 0.1044(7) Uani 1 4 d S T 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
N1 C1 1.481(12) 3 ?
N1 C1 1.481(12) . ?
N1 C2 1.521(13) . ?
C2 C3 1.490(12) . ?
C3 F1 1.125(19) 3 ?
C3 F1 1.125(19) . ?
C3 C4 1.499(13) 3 ?
C3 C4 1.499(13) . ?
C4 F2 1.364(13) . ?
C4 F1 1.365(14) . ?
C4 C4 1.41(4) 3 ?
C4 C5 1.506(12) . ?
C4 F1 1.84(3) 3 ?
C4 C5 1.879(18) 3 ?
C5 C5 0.89(3) 3 ?
C5 C6 1.493(16) . ?
C5 C4 1.879(18) 3 ?
C6 C1 1.481(15) . ?
F1 F1 1.08(5) 3 ?
F1 C4 1.84(3) 3 ?
F2 F2 1.29(6) 3 ?
I1 Pb1 3.2763(5) . ?
I1 Pb1 3.2763(5) 1_565 ?
I2 Pb1 3.176(5) . ?
I3 Pb1 3.222(10) . ?
I3 Pb1 3.330(10) 1_554 ?
Pb1 I2 3.176(5) 2_665 ?
Pb1 I1 3.2763(5) 1_545 ?
Pb1 I3 3.330(10) 1_556 ?
 
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
C1 N1 C1 94.8(10) 3 . ?
C1 N1 C2 113.2(6) 3 . ?
C1 N1 C2 113.2(6) . . ?
C3 C2 N1 130.5(8) . . ?
F1 C3 F1 57(3) 3 . ?
F1 C3 C2 148.2(12) 3 . ?
F1 C3 C2 148.2(12) . . ?
F1 C3 C4 60.7(8) 3 3 ?
F1 C3 C4 88.0(11) . 3 ?
C2 C3 C4 119.7(7) . 3 ?
F1 C3 C4 88.0(11) 3 . ?
F1 C3 C4 60.7(8) . . ?
C2 C3 C4 119.7(7) . . ?
C4 C3 C4 56.3(15) 3 . ?
F2 C4 F1 106.4(12) . . ?
F2 C4 C4 87.4(16) . 3 ?
F1 C4 C4 83.0(14) . 3 ?
F2 C4 C3 137.9(17) . . ?
F1 C4 C3 46.0(9) . . ?
C4 C4 C3 61.8(8) 3 . ?
F2 C4 C5 85.7(11) . . ?
F1 C4 C5 158.6(17) . . ?
C4 C4 C5 80.0(10) 3 . ?
C3 C4 C5 113.7(10) . . ?
F2 C4 F1 100.5(14) . 3 ?
F1 C4 F1 35.6(18) . 3 ?
C4 C4 F1 47.4(8) 3 3 ?
C3 C4 F1 37.6(6) . 3 ?
C5 C4 F1 126.0(15) . 3 ?
F2 C4 C5 85.3(13) . 3 ?
F1 C4 C5 133.5(18) . 3 ?
C4 C4 C5 52.1(6) 3 3 ?
C3 C4 C5 95.6(10) . 3 ?
C5 C4 C5 27.8(9) . 3 ?
F1 C4 C5 98.7(13) 3 3 ?
C5 C5 C6 135.4(7) 3 . ?
C5 C5 C4 100.0(10) 3 . ?
C6 C5 C4 86.7(10) . . ?
C5 C5 C4 52.1(7) 3 3 ?
C6 C5 C4 119.3(8) . 3 ?
C4 C5 C4 47.9(13) . 3 ?
C1 C6 C5 116.9(12) . . ?
F1 F1 C3 61.3(13) 3 . ?
F1 F1 C4 97.0(14) 3 . ?
C3 F1 C4 73.3(10) . . ?
F1 F1 C4 47.4(8) 3 3 ?
C3 F1 C4 54.4(10) . 3 ?
C4 F1 C4 49.7(15) . 3 ?
F2 F2 C4 92.6(16) 3 . ?
C6 C1 N1 112.4(9) . . ?
Pb1 I1 Pb1 178.2(3) . 1_565 ?
Pb1 I3 Pb1 180.0 . 1_554 ?
I2 Pb1 I2 162.7(3) 2_665 . ?
I2 Pb1 I3 81.37(14) 2_665 . ?
I2 Pb1 I3 81.37(14) . . ?
I2 Pb1 I1 90.13(2) 2_665 . ?
I2 Pb1 I1 90.13(2) . . ?
I3 Pb1 I1 90.88(14) . . ?
I2 Pb1 I1 90.13(2) 2_665 1_545 ?
I2 Pb1 I1 90.13(2) . 1_545 ?
I3 Pb1 I1 90.88(14) . 1_545 ?
I1 Pb1 I1 178.2(3) . 1_545 ?
I2 Pb1 I3 98.63(14) 2_665 1_556 ?
I2 Pb1 I3 98.63(14) . 1_556 ?
I3 Pb1 I3 180.0 . 1_556 ?
I1 Pb1 I3 89.12(14) . 1_556 ?
I1 Pb1 I3 89.12(14) 1_545 1_556 ?
 
_refine_diff_density_max    4.553
_refine_diff_density_min   -2.534
_refine_diff_density_rms    0.603

# start Validation Reply Form

_vrf_PLAT084_IMM2
;

RESPONSE: The quality of crystal was effected by high temperature.          
;

_vrf_PLAT082_IMM2
;

RESPONSE: The quality of crystal was effected by high temperature.          
;

_vrf_PLAT242_IMM2
;

RESPONSE: The quality of crystal was effected by high temperature.          
;

# end Validation Reply Form



