data_ea1
_audit_creation_date               2019-08-07
_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      'Department of Chemistry, Michigan State University, 578 S Shaw Ln, East Lansing, MI, 48824'
_audit_contact_author_email        'harelela@msu.edu'
_audit_contact_author_name         'Elad Harel'
_audit_contact_author_phone        '517-353-1078'
_publ_contact_author_id_orcid      ?
_publ_section_references           'Journal of the American Chemical Society'
_publ_contact_author_name          'Elad Harel'
_publ_contact_author_address       'Department of Chemistry, Michigan State University, 578 S Shaw Ln, East Lansing, MI, 48824'
_publ_contact_author_email         'harelela@msu.edu'
_publ_contact_author_fax           ?
_publ_contact_author_phone         '517-353-1078'
_publ_requested_journal                  
;
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          
 '0.5(I8 Pb2), I6 Pb2, 2(C2 H8 N), 2(C4 H12 N)'
_chemical_formula_sum              'C12 H40 I10 N4 Pb3'
_chemical_formula_weight           2131.05
_chemical_absolute_configuration   ?
_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'
 '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             36
_space_group_name_H-M_alt          'C m c 21'
_space_group_name_Hall             'C 2c -2'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x, y, z'
 'x, -y, z+1/2'
 'x+1/2, y+1/2, z'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, z'
 'x+1/2, -y+1/2, z+1/2'

_cell_length_a                     52.0158(16)
_cell_length_b                     8.9727(3)
_cell_length_c                     8.9745(3)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       4188.6(2)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      9793
_cell_measurement_temperature      298(2)
_cell_measurement_theta_max        30.06
_cell_measurement_theta_min        2.30
_shelx_estimated_absorpt_T_max     0.224
_shelx_estimated_absorpt_T_min     0.088
_exptl_absorpt_coefficient_mu      19.409
_exptl_absorpt_correction_T_max    0.7460
_exptl_absorpt_correction_T_min    0.5007
_exptl_absorpt_correction_type     'numerical'
_exptl_absorpt_process_details     'APEX-2'
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'red'
_exptl_crystal_density_diffrn      3.379
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         'square'
_exptl_crystal_F_000               3664
_exptl_crystal_size_max            0.244
_exptl_crystal_size_mid            0.224
_exptl_crystal_size_min            0.11
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0564
_diffrn_reflns_av_unetI/netI       0.0327
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.997
_diffrn_reflns_limit_h_max         73
_diffrn_reflns_limit_h_min         -73
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -12
_diffrn_reflns_limit_l_max         12
_diffrn_reflns_limit_l_min         -12
_diffrn_reflns_number              59074
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.997
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           30.176
_diffrn_reflns_theta_min           0.783
_diffrn_ambient_temperature        298.01
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.997
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     ?
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.884
_reflns_Friedel_fraction_full      1.000
_reflns_Friedel_fraction_max       0.997
_reflns_number_gt                  5176
_reflns_number_total               6246
_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         'APEX-2'
_computing_data_collection         'APEX-2'
_computing_data_reduction          'APEX-2'
_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           2.088
_refine_diff_density_min           -1.696
_refine_diff_density_rms           0.368
_refine_ls_abs_structure_details
;
 The structure can converge (shift<0.05)before adding hydrogens. However, it cannot converge after adding hydrogen. Since discussion of hydrogen bonding is not involved in this paper, the shift caused by the hydrogen will not influence the structure.
 Flack x determined using 2124 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack     0.003(4)
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.077
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       95
_refine_ls_number_reflns           6246
_refine_ls_number_restraints       15
_refine_ls_R_factor_all            0.0599
_refine_ls_R_factor_gt             0.0444
_refine_ls_restrained_S_all        1.076
_refine_ls_shift/su_max            1.543
_refine_ls_shift/su_mean           0.040
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0714P)²+76.1417P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1257
_refine_ls_wR_factor_ref           0.1425
_refine_special_details
;
 Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-C1 = C1-C2
 1.5 with sigma of 0.02
 N2-C3
 1.5 with sigma of 0.02
 N2-C3 = C3-C4
 1.5 with sigma of 0.02
 C3-C4
 1.5 with sigma of 0.02
 C3-C4 = C4-C5
 1.5 with sigma of 0.02
 C4-C5 = C5-C6
 1.5 with sigma of 0.02
 N1-C2
 2.592 with sigma of 0.04
 N2-C4
 2.592 with sigma of 0.04
 C3-C5
 2.592 with sigma of 0.04
 C4-C6
 2.592 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(N1) = Uiso(C1) = Uiso(C2)
Uiso(N2) = Uiso(C3)
Uiso(N2) = Uiso(C3) = Uiso(C4)
Uiso(N2) = Uiso(C3) = Uiso(C4) = Uiso(C5) = Uiso(C6)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C3(H3A,H3B), C4(H4A,H4B), C5(H5B,H5A)
4.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), C2(H2D,H2E,H2F), C6(H6B,H6A,H6C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       direct
_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 0.0000 -0.25993(9) -0.32796(9) 0.03137(19) Uani 1 2 d S T P . .
 Pb2 Pb -0.12760(2) -0.24949(6) -0.30828(7) 0.03650(17) Uani 1 1 d . . . . .
 I3 I -0.12074(3) -0.0017(2) -0.0564(2) 0.0653(4) Uani 1 1 d . . . . .
 I4 I -0.06116(2) -0.23666(16) -0.3081(3) 0.0579(4) Uani 1 1 d . . . . .
 I5 I 0.0000 0.04471(18) -0.1228(2) 0.0466(4) Uani 1 2 d S T P . .
 I6 I -0.13440(4) -0.4946(2) -0.05235(19) 0.0687(4) Uani 1 1 d . . . . .
 I7 I 0.0000 -0.4403(2) -0.0213(3) 0.0558(5) Uani 1 2 d S T P . .
 I1 I -0.18453(3) -0.1902(2) -0.3153(4) 0.1005(8) Uani 1 1 d . . . . .
 N1 N -0.0537(6) -0.157(3) 0.085(3) 0.107(6) Uiso 1 1 d D . . . .
 H1A H -0.0493 -0.1714 -0.0100 0.129 Uiso 1 1 calc GR . . . .
 H1B H -0.0396 -0.1488 0.1401 0.129 Uiso 1 1 calc GR . . . .
 H1C H -0.0629 -0.0733 0.0922 0.129 Uiso 1 1 calc GR . . . .
 N2 N -0.1681(7) -0.213(5) 0.200(5) 0.182(10) Uiso 1 1 d D . . . .
 H2A H -0.1573 -0.1899 0.1261 0.218 Uiso 1 1 calc GR . . . .
 H2B H -0.1615 -0.2884 0.2523 0.218 Uiso 1 1 calc GR . . . .
 H2C H -0.1703 -0.1348 0.2586 0.218 Uiso 1 1 calc GR . . . .
 C1 C -0.0693(7) -0.284(4) 0.138(4) 0.107(6) Uiso 1 1 d D . . . .
 H1D H -0.0657 -0.3687 0.0737 0.129 Uiso 1 1 calc R . . . .
 H1E H -0.0873 -0.2589 0.1252 0.129 Uiso 1 1 calc R . . . .
 C2 C -0.0653(7) -0.333(4) 0.296(4) 0.107(6) Uiso 1 1 d D . . . .
 H2D H -0.0598 -0.4346 0.2981 0.161 Uiso 1 1 calc GR . . . .
 H2E H -0.0812 -0.3234 0.3500 0.161 Uiso 1 1 calc GR . . . .
 H2F H -0.0525 -0.2708 0.3421 0.161 Uiso 1 1 calc GR . . . .
 C3 C -0.1935(9) -0.260(7) 0.135(5) 0.182(10) Uiso 1 1 d D . . . .
 H3A H -0.2002 -0.1768 0.0776 0.218 Uiso 1 1 calc R . . . .
 H3B H -0.1904 -0.3411 0.0663 0.218 Uiso 1 1 calc R . . . .
 C4 C -0.2140(9) -0.308(7) 0.242(5) 0.182(10) Uiso 1 1 d D . . . .
 H4A H -0.2208 -0.2195 0.2901 0.218 Uiso 1 1 calc R . . . .
 H4B H -0.2060 -0.3687 0.3180 0.218 Uiso 1 1 calc R . . . .
 C6 C -0.2407(11) -0.382(7) 0.014(5) 0.182(10) Uiso 1 1 d D . . . .
 H6C H -0.2388 -0.4779 -0.0312 0.272 Uiso 1 1 calc GR . . . .
 H6B H -0.2285 -0.3138 -0.0283 0.272 Uiso 1 1 calc GR . . . .
 H6A H -0.2578 -0.3452 -0.0039 0.272 Uiso 1 1 calc GR . . . .
 C5 C -0.2363(9) -0.394(6) 0.177(5) 0.182(10) Uiso 1 1 d D . . . .
 H5A H -0.2338 -0.4984 0.2007 0.218 Uiso 1 1 calc R . . . .
 H5B H -0.2518 -0.3617 0.2274 0.218 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 I4 3.1932(11) 3 ?
 Pb1 I4 3.1933(11) . ?
 Pb1 I5 3.276(2) 2_554 ?
 Pb1 I5 3.2958(18) . ?
 Pb1 I7 3.2004(19) 2_544 ?
 Pb1 I7 3.193(2) . ?
 Pb2 I3 3.1912(17) . ?
 Pb2 I3 3.1878(17) 4_554 ?
 Pb2 I6 3.1928(17) 4_544 ?
 Pb2 I6 3.1999(17) . ?
 Pb2 I1 3.0094(17) . ?
 I3 Pb2 3.1878(17) 4 ?
 I5 Pb1 3.276(2) 2 ?
 I6 Pb2 3.1928(17) 4_545 ?
 I7 Pb1 3.2004(19) 2_545 ?
 N1 C1 1.48(2) . ?
 N2 C3 1.504(19) . ?
 C1 C2 1.50(2) . ?
 C3 C4 1.493(16) . ?
 C4 C5 1.510(18) . ?
 C6 C5 1.48(3) . ?

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
 I4 Pb1 I4 170.14(7) 3 . ?
 I4 Pb1 I5 85.10(3) . . ?
 I4 Pb1 I5 90.37(4) 3 2_554 ?
 I4 Pb1 I5 85.10(3) 3 . ?
 I4 Pb1 I5 90.37(4) . 2_554 ?
 I4 Pb1 I7 89.14(4) 3 . ?
 I4 Pb1 I7 94.89(3) . 2_544 ?
 I4 Pb1 I7 89.14(4) . . ?
 I4 Pb1 I7 94.89(3) 3 2_544 ?
 I5 Pb1 I5 87.84(2) 2_554 . ?
 I7 Pb1 I5 178.86(7) 2_544 . ?
 I7 Pb1 I5 86.49(6) . . ?
 I7 Pb1 I5 174.33(6) . 2_554 ?
 I7 Pb1 I5 93.30(7) 2_544 2_554 ?
 I7 Pb1 I7 92.37(3) . 2_544 ?
 I3 Pb2 I3 89.409(15) 4_554 . ?
 I3 Pb2 I6 178.19(6) . 4_544 ?
 I3 Pb2 I6 89.02(6) . . ?
 I3 Pb2 I6 92.38(6) 4_554 4_544 ?
 I3 Pb2 I6 178.43(6) 4_554 . ?
 I6 Pb2 I6 89.191(15) 4_544 . ?
 I1 Pb2 I3 88.30(7) . 4_554 ?
 I1 Pb2 I3 90.10(7) . . ?
 I1 Pb2 I6 91.60(7) . . ?
 I1 Pb2 I6 90.21(7) . 4_544 ?
 Pb2 I3 Pb2 167.12(6) 4 . ?
 Pb1 I5 Pb1 160.09(7) 2 . ?
 Pb2 I6 Pb2 167.03(7) 4_545 . ?
 Pb1 I7 Pb1 153.28(9) . 2_545 ?
 N1 C1 C2 117(3) . . ?
 C4 C3 N2 118(3) . . ?
 C3 C4 C5 117(3) . . ?
 C6 C5 C4 117(3) . . ?


_olex2_submission_special_instructions  'No special instructions were received'
loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.896(14)
 2 0.104(14)

