data_4_pbi3
_audit_creation_date               2018-09-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2014/7'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790;
Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984;
Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45,
 575-580.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           '0.5(I6 Pb2), C5 H6 N'
_chemical_formula_sum              'C5 H6 I3 N Pb'
_chemical_formula_weight           668.00
_chemical_melting_point            ?
_chemical_oxdiff_formula           'C5 H6 N Pb I3'
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'
 'I' 'I' -0.4742 1.8119 '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'

_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.
;
_space_group_crystal_system        'orthorhombic'
_space_group_IT_number             62
_space_group_name_H-M_alt          'P n m a'
_space_group_name_Hall             '-P 2ac 2n'
loop_
  _space_group_symop_operation_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'

_cell_length_a                     14.9049(4)
_cell_length_b                     8.0660(2)
_cell_length_c                     9.5902(3)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       1152.96(6)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      2055
_cell_measurement_temperature      100(2)
_cell_measurement_theta_max        31.1740
_cell_measurement_theta_min        3.3200
_shelx_estimated_absorpt_T_max     0.133
_shelx_estimated_absorpt_T_min     0.093
_exptl_absorpt_coefficient_mu      22.610
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.25185
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              yellow
_exptl_crystal_colour_lustre       .
_exptl_crystal_colour_modifier     .
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      3.848
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         prism
_exptl_crystal_F_000               1136
_exptl_crystal_size_max            0.2
_exptl_crystal_size_mid            0.15
_exptl_crystal_size_min            0.15
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0347
_diffrn_reflns_av_unetI/netI       0.0311
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.999
_diffrn_reflns_limit_h_max         15
_diffrn_reflns_limit_h_min         -19
_diffrn_reflns_limit_k_max         10
_diffrn_reflns_limit_k_min         -10
_diffrn_reflns_limit_l_max         10
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              5028
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.999
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.495
_diffrn_reflns_theta_min           2.733
_diffrn_ambient_temperature        100(2)
_diffrn_detector_area_resol_mean   16.2096
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.999
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -94.00  -36.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.3621 -178.0000 -120.0000 58

#__ type_ start__ end____ width___ exp.time_
  2 omega  -91.00  -40.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.3621 -178.0000   90.0000 51

#__ type_ start__ end____ width___ exp.time_
  3 omega   17.00   76.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       24.2996   77.0000   90.0000 59

#__ type_ start__ end____ width___ exp.time_
  4 omega  -90.00  -46.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.3621 -178.0000  -30.0000 44

#__ type_ start__ end____ width___ exp.time_
  5 omega  -44.00  -18.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.3621   77.0000  150.0000 26
;
_diffrn_measurement_device_type    'Xcalibur, Eos'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_UB_11        -0.0221747000
_diffrn_orient_matrix_UB_12        0.0157753000
_diffrn_orient_matrix_UB_13        0.0641593000
_diffrn_orient_matrix_UB_21        0.0057463000
_diffrn_orient_matrix_UB_22        0.0863472000
_diffrn_orient_matrix_UB_23        -0.0102769000
_diffrn_orient_matrix_UB_31        -0.0417074000
_diffrn_orient_matrix_UB_32        0.0035363000
_diffrn_orient_matrix_UB_33        -0.0355013000
_diffrn_radiation_monochromator    graphite
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1314
_reflns_number_total               1417
_reflns_odcompleteness_completeness  99.78
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       28.98
_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.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max           1.784
_refine_diff_density_min           -3.300
_refine_diff_density_rms           0.405
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.136
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       52
_refine_ls_number_reflns           1417
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0337
_refine_ls_R_factor_gt             0.0306
_refine_ls_restrained_S_all        1.136
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0265P)²+14.6456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0717
_refine_ls_wR_factor_ref           0.0732
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Shared sites
{C3, N4}
3. Uiso/Uaniso restraints and constraints
Uanis(C3) = Uanis(N4)
4. Others
 Fixed Sof: C3(0.5) H3(0.5) N4(0.5) H4(0.5) H1B(0.5) H1A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), N4(H4), C1(H1B), C1(H1A), C2(H2)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       iterative
_atom_sites_solution_secondary     ?
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
 Pb1 Pb 0.5000 0.5000 0.5000 0.01025(12) Uani 1 2 d S T P . .
 I1 I 0.60955(5) 0.7500 0.69658(7) 0.01855(18) Uani 1 2 d S T P . .
 I2 I 0.33529(5) 0.7500 0.54016(7) 0.01480(16) Uani 1 2 d S T P . .
 I3 I 0.44274(5) 0.2500 0.75326(8) 0.0324(2) Uani 1 2 d S T P . .
 C3 C 0.3945(5) 0.8333(9) 0.9238(7) 0.0208(16) Uani 0.5 1 d . . . A 2
 H3 H 0.4267 0.8912 0.8536 0.025 Uiso 0.5 1 calc R . . A 2
 N4 N 0.3945(5) 0.8333(9) 0.9238(7) 0.0208(16) Uani 0.5 1 d . . . A 1
 H4 H 0.4244 0.8869 0.8587 0.025 Uiso 0.5 1 calc R . . A 1
 C1 C 0.3497(6) 0.9192(11) 1.0214(8) 0.0196(17) Uani 1 1 d . . . . .
 H1B H 0.3508 1.0370 1.0203 0.024 Uiso 0.5 1 calc R . . A 2
 H1A H 0.3508 1.0370 1.0203 0.024 Uiso 0.5 1 calc R . . A 1
 C2 C 0.3022(5) 0.8368(11) 1.1228(8) 0.0200(17) Uani 1 1 d . . . . .
 H2 H 0.2699 0.8966 1.1918 0.024 Uiso 1 1 calc R . . . .


_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
 Pb1 I1 3.2073(5) 5_666 ?
 Pb1 I1 3.2073(5) . ?
 Pb1 I2 3.2002(5) . ?
 Pb1 I2 3.2002(5) 5_666 ?
 Pb1 I3 3.2701(6) . ?
 Pb1 I3 3.2701(6) 5_666 ?
 I1 Pb1 3.2073(5) 4_656 ?
 I2 Pb1 3.2002(5) 4_656 ?
 I3 Pb1 3.2701(6) 4_646 ?
 C3 C3 1.343(14) 8_575 ?
 C3 C1 1.343(11) . ?
 N4 N4 1.343(14) 8_575 ?
 N4 C1 1.343(11) . ?
 C1 C2 1.375(12) . ?
 C2 C2 1.400(18) 8_575 ?

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
 I1 Pb1 I1 180.0 5_666 . ?
 I1 Pb1 I3 94.820(15) 5_666 5_666 ?
 I1 Pb1 I3 94.819(15) . . ?
 I1 Pb1 I3 85.181(15) . 5_666 ?
 I1 Pb1 I3 85.180(15) 5_666 . ?
 I2 Pb1 I1 94.379(15) 5_666 . ?
 I2 Pb1 I1 85.621(15) . . ?
 I2 Pb1 I1 85.621(15) 5_666 5_666 ?
 I2 Pb1 I1 94.379(15) . 5_666 ?
 I2 Pb1 I2 180.0 . 5_666 ?
 I2 Pb1 I3 84.320(15) . 5_666 ?
 I2 Pb1 I3 84.321(15) 5_666 . ?
 I2 Pb1 I3 95.679(15) . . ?
 I2 Pb1 I3 95.679(15) 5_666 5_666 ?
 I3 Pb1 I3 180.0 5_666 . ?
 Pb1 I1 Pb1 77.912(16) . 4_656 ?
 Pb1 I2 Pb1 78.118(16) 4_656 . ?
 Pb1 I3 Pb1 76.143(16) 4_646 . ?
 C1 C3 C3 121.1(5) . 8_575 ?
 C1 N4 N4 121.1(5) . 8_575 ?
 C3 C1 C2 120.0(8) . . ?
 N4 C1 C2 120.0(8) . . ?
 C1 C2 C2 118.9(5) . 8_575 ?

_olex2_submission_special_instructions  'No special instructions were received'
