data_7175-8629_n2
_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(Br6 Pb2), C5 H6 N'
_chemical_formula_sum              'C5 H6 Br3 N Pb'
_chemical_formula_weight           527.03
_chemical_melting_point            ?
_chemical_oxdiff_formula           'Pb Br3 N C5 H6'
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'
 'Br' 'Br' -0.2901 2.4595
 '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                     14.0045(6)
_cell_length_b                     7.7690(4)
_cell_length_c                     9.1780(5)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       998.57(8)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      4429
_cell_measurement_temperature      100(2)
_cell_measurement_theta_max        30.5740
_cell_measurement_theta_min        3.4360
_shelx_estimated_absorpt_T_max     0.069
_shelx_estimated_absorpt_T_min     0.069
_exptl_absorpt_coefficient_mu      28.834
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.12170
_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      3.506
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         prism
_exptl_crystal_F_000               920
_exptl_crystal_size_max            0.2
_exptl_crystal_size_mid            0.2
_exptl_crystal_size_min            0.2
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.1080
_diffrn_reflns_av_unetI/netI       0.0406
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  1.000
_diffrn_reflns_limit_h_max         18
_diffrn_reflns_limit_h_min         -18
_diffrn_reflns_limit_k_max         10
_diffrn_reflns_limit_k_min         -10
_diffrn_reflns_limit_l_max         11
_diffrn_reflns_limit_l_min         -11
_diffrn_reflns_number              15722
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  1.000
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           27.497
_diffrn_reflns_theta_min           2.653
_diffrn_ambient_temperature        100(2)
_diffrn_detector_area_resol_mean   16.2096
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  1.000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -77.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  178.0000  -90.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega   40.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000 -180.0000 52

#__ type_ start__ end____ width___ exp.time_
  3 omega  -44.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -57.0000 -120.0000 57

#__ type_ start__ end____ width___ exp.time_
  4 omega  -90.00  -63.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241 -178.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  5 omega  -48.00   22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241  -19.0000   30.0000 70

#__ type_ start__ end____ width___ exp.time_
  6 omega   36.00   61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  178.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
  7 omega  -52.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -22.4241   77.0000  150.0000 99

#__ type_ start__ end____ width___ exp.time_
  8 omega   -4.00   40.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000 -180.0000 44

#__ type_ start__ end____ width___ exp.time_
  9 omega   67.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000 -180.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega  -25.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -99.0000   60.0000 90

#__ type_ start__ end____ width___ exp.time_
 11 omega   19.00   55.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   57.0000  120.0000 36

#__ type_ start__ end____ width___ exp.time_
 12 omega   -7.00   89.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000   30.0000 96

#__ type_ start__ end____ width___ exp.time_
 13 omega   -4.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616  -99.0000  -60.0000 69

#__ type_ start__ end____ width___ exp.time_
 14 omega   -2.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   38.0000  -30.0000 92

#__ type_ start__ end____ width___ exp.time_
 15 omega   -2.00   46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       23.3616   77.0000  -90.0000 48
;
_diffrn_measurement_device_type    'Xcalibur, Eos'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_UB_11        -0.0346243000
_diffrn_orient_matrix_UB_12        0.0299991000
_diffrn_orient_matrix_UB_13        0.0504159000
_diffrn_orient_matrix_UB_21        0.0225740000
_diffrn_orient_matrix_UB_22        0.0816391000
_diffrn_orient_matrix_UB_23        0.0013214000
_diffrn_orient_matrix_UB_31        -0.0292332000
_diffrn_orient_matrix_UB_32        0.0276355000
_diffrn_orient_matrix_UB_33        -0.0586448000
_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                  1026
_reflns_number_total               1231
_reflns_odcompleteness_completeness  99.80
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       28.51
_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           4.557
_refine_diff_density_min           -2.695
_refine_diff_density_rms           0.429
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.171
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       52
_refine_ls_number_reflns           1231
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0696
_refine_ls_R_factor_gt             0.0579
_refine_ls_restrained_S_all        1.171
_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)+(0.0461P)²+56.6043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.1350
_refine_ls_wR_factor_ref           0.1420
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{C1, N25}
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(N25)
4. Others
 Fixed Sof: C1(0.5) N25(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C0AA(H0AA), 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 0.0000 0.0116(2) Uani 1 2 d S T P . .
 Br1 Br 0.33832(14) 0.7500 0.0442(2) 0.0267(5) Uani 1 2 d S T P . .
 Br2 Br 0.60842(15) 0.7500 0.1893(2) 0.0329(6) Uani 1 2 d S T P . .
 C1 C 0.3963(11) 0.8331(19) 0.4251(15) 0.027(3) Uani 0.5 1 d . . . A 1
 H1 H 0.4298 0.8930 0.3507 0.032 Uiso 1 1 calc R . . A 1
 C0AA C 0.3495(12) 0.924(2) 0.5291(17) 0.029(3) Uani 1 1 d . . . . .
 H0AA H 0.3504 1.0461 0.5291 0.035 Uiso 1 1 calc R . . A 1
 C2 C 0.3000(10) 0.833(2) 0.6357(17) 0.028(4) Uani 1 1 d . . . . .
 H2 H 0.2660 0.8941 0.7090 0.034 Uiso 1 1 calc R . . . .
 Br3 Br 0.44597(16) 0.2500 0.2458(3) 0.0599(11) Uani 1 2 d S T P . .
 N25 N 0.3963(11) 0.8331(19) 0.4251(15) 0.027(3) Uani 0.5 1 d . . . A -1


_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 Br1 3.0106(15) . ?
 Pb1 Br1 3.0106(15) 5_665 ?
 Pb1 Br2 3.0158(16) . ?
 Pb1 Br2 3.0159(16) 5_665 ?
 Pb1 Br3 3.0716(18) 5_665 ?
 Pb1 Br3 3.0716(18) . ?
 Br1 Pb1 3.0106(15) 4_655 ?
 Br2 Pb1 3.0158(16) 4_655 ?
 C1 C1 1.29(3) 8_575 ?
 C1 C0AA 1.36(2) . ?
 C0AA C2 1.39(2) . ?
 C0AA N25 1.36(2) . ?
 C2 C2 1.29(4) 8_575 ?
 Br3 Pb1 3.0716(18) 4_645 ?

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
 Br1 Pb1 Br1 180.0 . 5_665 ?
 Br1 Pb1 Br2 83.43(5) 5_665 5_665 ?
 Br1 Pb1 Br2 96.57(5) . 5_665 ?
 Br1 Pb1 Br2 96.57(5) 5_665 . ?
 Br1 Pb1 Br2 83.43(5) . . ?
 Br1 Pb1 Br3 82.90(5) . 5_665 ?
 Br1 Pb1 Br3 82.90(5) 5_665 . ?
 Br1 Pb1 Br3 97.10(5) 5_665 5_665 ?
 Br1 Pb1 Br3 97.10(5) . . ?
 Br2 Pb1 Br2 180.0 . 5_665 ?
 Br2 Pb1 Br3 83.79(5) . 5_665 ?
 Br2 Pb1 Br3 96.21(5) . . ?
 Br2 Pb1 Br3 83.79(5) 5_665 . ?
 Br2 Pb1 Br3 96.21(5) 5_665 5_665 ?
 Br3 Pb1 Br3 180.0 5_665 . ?
 Pb1 Br1 Pb1 80.35(5) 4_655 . ?
 Pb1 Br2 Pb1 80.18(5) . 4_655 ?
 C1 C1 C0AA 121.3(10) 8_575 . ?
 C1 C0AA C2 118.3(16) . . ?
 N25 C0AA C1 0.0 . . ?
 N25 C0AA C2 118.3(16) . . ?
 C2 C2 C0AA 120.4(10) 8_575 . ?
 Pb1 Br3 Pb1 78.44(5) 4_645 . ?

_olex2_submission_special_instructions  'No special instructions were received'
