data_shelx


_refine_ls_number_constraints   ?
#Added by publCIF



_diffrn_radiation_monochromator   'HELIOS optics'
#Added by publCIF



_audit_update_record
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2018-06-20 # Formatted by publCIF

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# publcif _publ_body_element loop start
loop_
_publ_body_element
_publ_body_title
_publ_body_contents

 section 
;
Introduction
; 
;

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 section 
;
Experimental
; 
;

;
 subsection 
;
Synthesis and crystallization
; 
;

;
 subsection 
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Refinement
;
;
Crystal data, data collection and structure refinement details are summarized
in Table 1.
;

 section 
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Results and discussion
; 
;

;
# publcif _publ_body_element loop end
 
_audit_creation_method            'SHELXL-2017/1'
_shelx_SHELXL_version_number      '2017/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C15 H26 I7 N3 Pb2' 
_chemical_formula_weight          1551.07

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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            60
_space_group_name_H-M_alt         'P b c n'
_space_group_name_Hall            '-P 2n 2ab'
 
_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+1/2, -y+1/2, z+1/2'
 '-x, y, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y-1/2, -z-1/2'
 'x, -y, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    41.4633(11)
_cell_length_b                    9.0279(3)
_cell_length_c                    8.7717(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      3283.48(16)
_cell_formula_units_Z             4
_cell_measurement_temperature     300(2)
_cell_measurement_reflns_used     6924
_cell_measurement_theta_min       2.95
_cell_measurement_theta_max       28.06
 
_exptl_crystal_description        Plate
_exptl_crystal_colour             Red
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     3.138          
_exptl_crystal_F_000              2688
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.092
_exptl_crystal_size_mid           0.065
_exptl_crystal_size_min           0.002
_exptl_absorpt_coefficient_mu     16.831
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.4388
_exptl_absorpt_correction_T_max   0.7461
_exptl_absorpt_process_details    'SADABS (2014)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       300(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'I\ms microfocus tube'
_diffrn_measurement_device_type   'Bruker D8 Quest ECO CMOS'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             61578
_diffrn_reflns_av_unetI/netI      0.0565
_diffrn_reflns_av_R_equivalents   0.1099
_diffrn_reflns_limit_h_min        -59
_diffrn_reflns_limit_h_max        59
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.309
_diffrn_reflns_theta_max          30.633
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.999
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.999
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.999
_reflns_number_total              5053
_reflns_number_gt                 2803
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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        'APEX3 (Bruker-AXS, 2015)'
_computing_cell_refinement        'Bruker SAINT'
_computing_data_reduction         'Bruker SAINT'
_computing_structure_solution     'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics     'VESTA (Momma and Izumi, 2017)'
_computing_publication_material   'publCIF (Westrip, 2010)'
_refine_special_details		?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+69.2290P] 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_number_reflns          5053
_refine_ls_number_parameters      120
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.1150
_refine_ls_R_factor_gt            0.0544
_refine_ls_wR_factor_ref          0.1310
_refine_ls_wR_factor_gt           0.1142
_refine_ls_goodness_of_fit_ref    1.170
_refine_ls_restrained_S_all       1.171
_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
Pb1 Pb 0.57831(2) 0.75113(5) 0.25421(5) 0.03684(12) Uani 1 1 d . . . . .
I1 I 0.57217(2) 0.45928(11) 0.46083(11) 0.0547(3) Uani 1 1 d . . . . .
I2 I 0.65300(2) 0.70529(12) 0.27447(12) 0.0575(3) Uani 1 1 d . . . . .
I3 I 0.500000 0.76589(18) 0.250000 0.0636(4) Uani 1 2 d S T P . .
I4 I 0.57971(3) 0.95864(12) 0.54620(12) 0.0646(3) Uani 1 1 d . . . . .
C1 C 0.500000 0.675(6) 0.750000 0.29(3) Uani 1 2 d DS T P . .
H1A H 0.516305 0.639446 0.681395 0.431 Uiso 0.5 1 calc R U P . .
H1B H 0.479278 0.639445 0.717556 0.431 Uiso 0.5 1 calc R U P . .
H1C H 0.504417 0.639446 0.851050 0.431 Uiso 0.5 1 calc R U P . .
N1 N 0.500000 0.825(5) 0.750000 0.29(3) Uani 1 2 d DS T P . .
H1D H 0.480221 0.857791 0.770242 0.431 Uiso 0.5 1 calc R U P . .
H1E H 0.506181 0.857791 0.658911 0.431 Uiso 0.5 1 calc R U P . .
H1F H 0.513598 0.857791 0.820847 0.431 Uiso 0.5 1 calc R U P . .
N2 N 0.6354(3) 0.3241(16) 0.1904(16) 0.070(4) Uani 1 1 d . . . . .
H2A H 0.614663 0.336997 0.213690 0.104 Uiso 1 1 calc R U . . .
H2B H 0.645504 0.410927 0.193466 0.104 Uiso 1 1 calc R U . . .
H2C H 0.636949 0.286037 0.097055 0.104 Uiso 1 1 calc R U . . .
C3 C 0.6850(4) 0.1949(18) 0.2693(15) 0.053(3) Uani 1 1 d . . . . .
C2 C 0.6503(5) 0.221(2) 0.302(2) 0.081(5) Uani 1 1 d . . . . .
H2D H 0.638866 0.127728 0.299241 0.097 Uiso 1 1 calc R U . . .
H2E H 0.648097 0.262479 0.403263 0.097 Uiso 1 1 calc R U . . .
C4 C 0.7086(5) 0.265(2) 0.332(3) 0.090(6) Uani 1 1 d . . . . .
H4 H 0.703725 0.341300 0.399690 0.108 Uiso 1 1 calc R U . . .
C7 C 0.7236(7) 0.054(2) 0.130(3) 0.101(7) Uani 1 1 d . . . . .
H7 H 0.728416 -0.019864 0.059810 0.122 Uiso 1 1 calc R U . . .
C5 C 0.7409(5) 0.235(2) 0.304(2) 0.086(6) Uani 1 1 d . . . . .
H5 H 0.757152 0.285218 0.355093 0.103 Uiso 1 1 calc R U . . .
C6 C 0.7481(5) 0.129(3) 0.200(2) 0.093(7) Uani 1 1 d . . . . .
H6 H 0.769505 0.107961 0.175643 0.111 Uiso 1 1 calc R U . . .
C8 C 0.6918(5) 0.086(2) 0.161(2) 0.079(5) Uani 1 1 d . . . . .
H8 H 0.675238 0.036032 0.111566 0.095 Uiso 1 1 calc R U . . .
 
 
_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 3.1294(11) . ?
Pb1 I4 3.1738(10) . ?
Pb1 I4 3.1934(10) 7_575 ?
Pb1 I1 3.2081(10) . ?
Pb1 I1 3.2087(10) 7_565 ?
Pb1 I3 3.2498(5) . ?
C1 N1 1.35(4) . ?
N2 C2 1.48(2) . ?
C3 C4 1.29(2) . ?
C3 C8 1.39(2) . ?
C3 C2 1.48(2) . ?
C4 C5 1.39(3) . ?
C7 C6 1.37(3) . ?
C7 C8 1.38(3) . ?
C5 C6 1.35(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
I2 Pb1 I4 90.81(3) . . ?
I2 Pb1 I4 97.06(3) . 7_575 ?
I4 Pb1 I4 88.650(14) . 7_575 ?
I2 Pb1 I1 86.43(3) . . ?
I4 Pb1 I1 91.74(3) . . ?
I4 Pb1 I1 176.48(3) 7_575 . ?
I2 Pb1 I1 92.62(3) . 7_565 ?
I4 Pb1 I1 176.49(3) . 7_565 ?
I4 Pb1 I1 91.66(3) 7_575 7_565 ?
I1 Pb1 I1 87.742(14) . 7_565 ?
I2 Pb1 I3 174.13(4) . . ?
I4 Pb1 I3 90.19(3) . . ?
I4 Pb1 I3 88.74(3) 7_575 . ?
I1 Pb1 I3 87.76(3) . . ?
I1 Pb1 I3 86.32(3) 7_565 . ?
Pb1 I1 Pb1 158.91(4) . 7_566 ?
Pb1 I3 Pb1 175.30(6) . 3_655 ?
Pb1 I4 Pb1 160.92(4) . 7_576 ?
C4 C3 C8 118.8(18) . . ?
C4 C3 C2 125.1(18) . . ?
C8 C3 C2 116.1(16) . . ?
N2 C2 C3 112.3(15) . . ?
C3 C4 C5 124(2) . . ?
C6 C7 C8 121(2) . . ?
C6 C5 C4 118(2) . . ?
C5 C6 C7 119(2) . . ?
C7 C8 C3 118.6(18) . . ?
 
_refine_diff_density_max    2.256
_refine_diff_density_min   -2.075
_refine_diff_density_rms    0.237


loop_
_publcif_info_cif.paper_type
 ?



_publcif_funding_html
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