data_4
_audit_creation_date               2019-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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.

Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122.
;
_chemical_name_common              ?
_chemical_name_systematic
;
 ? 
;
_chemical_formula_moiety           '2(I1.5 Pb0.5), C2 N1'
_chemical_formula_sum              'C2 I3 N Pb'
_chemical_formula_weight           625.92
_chemical_melting_point            ?
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'
 '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'

_space_group_crystal_system        'hexagonal'
_space_group_IT_number             194
_space_group_name_H-M_alt          'P 63/m m c'
_space_group_name_Hall             '-P 6c 2c'
loop_
  _space_group_symop_id
  _space_group_symop_operation_xyz
 1 'x, y, z'
 2 'x-y, x, z+1/2'
 3 '-y, x-y, z'
 4 '-x, -y, z+1/2'
 5 '-x+y, -x, z'
 6 'y, -x+y, z+1/2'
 7 'x-y, -y, -z'
 8 '-x, -x+y, -z'
 9 'y, x, -z'
 10 '-y, -x, -z+1/2'
 11 '-x+y, y, -z+1/2'
 12 'x, x-y, -z+1/2'
 13 '-x, -y, -z'
 14 '-x+y, -x, -z-1/2'
 15 'y, -x+y, -z'
 16 'x, y, -z-1/2'
 17 'x-y, x, -z'
 18 '-y, x-y, -z-1/2'
 19 '-x+y, y, z'
 20 'x, x-y, z'
 21 '-y, -x, z'
 22 'y, x, z-1/2'
 23 'x-y, -y, z-1/2'
 24 '-x, -x+y, z-1/2'

_cell_length_a                     8.7799(12)
_cell_length_b                     8.7799(12)
_cell_length_c                     8.193(2)
_cell_angle_alpha                  90.00
_cell_angle_beta                   90.00
_cell_angle_gamma                  120.00
_cell_volume                       546.94(19)
_cell_formula_units_Z              2
_cell_measurement_reflns_used      1106
_cell_measurement_temperature      273(2)
_cell_measurement_theta_max        25.363
_cell_measurement_theta_min        2.679
_exptl_absorpt_coefficient_mu      23.817
_exptl_absorpt_correction_T_max    0.7456
_exptl_absorpt_correction_T_min    0.2685
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details     ?
_exptl_crystal_colour              yellow
_exptl_crystal_colour_lustre       .
_exptl_crystal_colour_modifier     .
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      3.801
_exptl_crystal_density_meas        .
_exptl_crystal_density_method      'not measured'
_exptl_crystal_description         block
_exptl_crystal_F_000               520
_exptl_crystal_size_max            ?
_exptl_crystal_size_mid            ?
_exptl_crystal_size_min            ?
_exptl_special_details
;
 ? 
;
_diffrn_reflns_av_R_equivalents    0.0774
_diffrn_reflns_av_unetI/netI       0.0387
_diffrn_reflns_limit_h_max         10
_diffrn_reflns_limit_h_min         -11
_diffrn_reflns_limit_k_max         9
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         10
_diffrn_reflns_limit_l_min         -10
_diffrn_reflns_number              2678
_diffrn_reflns_theta_full          27.53
_diffrn_reflns_theta_max           27.53
_diffrn_reflns_theta_min           2.68
_diffrn_ambient_temperature        273.15
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.996
_diffrn_measured_fraction_theta_max  0.996
_diffrn_measurement_device_type    'CCD area detector'
_diffrn_measurement_method         'phi and omega scans'
_diffrn_radiation_monochromator    'graphite'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'fine-focus sealed tube'
_diffrn_standards_decay_%          ?
_diffrn_standards_interval_count   ?
_diffrn_standards_interval_time    ?
_diffrn_standards_number           ?
_reflns_number_gt                  217
_reflns_number_total               270
_reflns_threshold_expression       >2sigma(I)
_computing_cell_refinement         'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics      'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement    'XL (Sheldrick, 2008)'
_computing_structure_solution      'XS (Sheldrick, 2008)'
_refine_diff_density_max           1.130
_refine_diff_density_min           -0.808
_refine_diff_density_rms           0.191
_refine_ls_extinction_coef         ?
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.200
_refine_ls_hydrogen_treatment      undef
_refine_ls_matrix_type             full
_refine_ls_number_parameters       14
_refine_ls_number_reflns           270
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0573
_refine_ls_R_factor_gt             0.0413
_refine_ls_restrained_S_all        1.200
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'calc w=1/[σ²(Fo²)+(0.0492P)²+0.1299P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0946
_refine_ls_wR_factor_ref           0.1002
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: N2(0.08333)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       heavy
_atom_sites_solution_secondary     difmap
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_calc_flag
  _atom_site_disorder_assembly
  _atom_site_disorder_group
  _atom_site_site_symmetry_order
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
 Pb1 Pb 0.0000 0.0000 0.0000 0.0455(4) Uani 1 d . . 12 S T P
 I2 I -0.32843(14) -0.16421(7) -0.2500 0.0841(6) Uani 1 d . . 4 S T P
 C1 C -0.6667 -0.3333 0.115(5) 0.19(2) Uani 1 d . . 6 S T P
 N2 N -0.380(3) 0.240(7) -0.2500 0.13(3) Uani 0.33 d . . 4 S T P

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
 Pb1 0.0459(5) 0.0459(5) 0.0446(7) 0.000 0.000 0.0230(3)
 I2 0.0409(7) 0.1003(10) 0.0914(12) 0.000 0.000 0.0204(4)
 C1 0.25(4) 0.25(4) 0.07(3) 0.000 0.000 0.13(2)
 N2 0.12(4) 0.02(2) 0.22(9) 0.000 0.000 0.012(12)

_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 I2 3.2297(10) 13 ?
 Pb1 I2 3.2297(10) 15 ?
 Pb1 I2 3.2297(10) 2 ?
 Pb1 I2 3.2297(10) . ?
 Pb1 I2 3.2297(10) 14 ?
 Pb1 I2 3.2297(10) 3 ?
 I2 Pb1 3.2297(10) 2_554 ?
 C1 N2 1.31(4) 13_455 ?
 C1 N2 1.31(4) 15_445 ?
 C1 N2 1.31(4) 2 ?
 N2 C1 1.31(4) 2_564 ?
 N2 C1 1.31(4) 13_455 ?
 N2 N2 1.23(9) 14_455 ?
 N2 N2 1.23(9) 3_565 ?

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
 I2 Pb1 I2 180.00(3) 13 . ?
 I2 Pb1 I2 180.000(16) 3 15 ?
 I2 Pb1 I2 180.0 2 14 ?
 I2 Pb1 I2 95.93(2) 13 3 ?
 I2 Pb1 I2 95.93(2) 13 14 ?
 I2 Pb1 I2 84.07(2) . 3 ?
 I2 Pb1 I2 95.93(2) . 15 ?
 I2 Pb1 I2 84.07(2) 13 2 ?
 I2 Pb1 I2 84.07(2) 2 15 ?
 I2 Pb1 I2 95.93(2) . 2 ?
 I2 Pb1 I2 84.07(2) . 14 ?
 I2 Pb1 I2 95.93(2) 3 2 ?
 I2 Pb1 I2 95.93(2) 15 14 ?
 I2 Pb1 I2 84.07(2) 13 15 ?
 I2 Pb1 I2 84.07(2) 3 14 ?
 Pb1 I2 Pb1 78.72(3) . 2_554 ?
 N2 C1 N2 56(4) 13_455 2 ?
 N2 C1 N2 56(4) 15_445 2 ?
 N2 C1 N2 56(4) 13_455 15_445 ?
 C1 N2 C1 115(4) 13_455 2_564 ?
 N2 N2 C1 62.1(18) 3_565 13_455 ?
 N2 N2 C1 62.1(18) 3_565 2_564 ?
 N2 N2 C1 62.1(18) 14_455 2_564 ?
 N2 N2 C1 62.1(18) 14_455 13_455 ?
 N2 N2 N2 60.000(3) 3_565 14_455 ?

_olex2_submission_special_instructions  'No special instructions were received'
