data_a
_audit_creation_date               2018-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_acknowledgements
;
X-Ray services provided by SMoCC - The Small Molecule Crystallography
Center of ETH Zurich. 
;
_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. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'Br4 Pb, 2(C10 H22 N)'
_chemical_formula_sum              'C20 H44 Br4 N2 Pb'
_chemical_formula_weight           839.40
_chemical_melting_point            ?
_chemical_oxdiff_formula           C80H176B16N8Pb4
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        'monoclinic'
_space_group_IT_number             15
_space_group_name_H-M_alt          'C 1 2/c 1'
_space_group_name_Hall             '-C 2yc'
loop_
  _space_group_symop_operation_xyz
 '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, -y, -z'
 'x, -y, z-1/2'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                     20.3640(9)
_cell_length_b                     8.4235(2)
_cell_length_c                     18.8888(9)
_cell_angle_alpha                  90
_cell_angle_beta                   123.796(7)
_cell_angle_gamma                  90
_cell_volume                       2692.6(3)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      13211
_cell_measurement_temperature      100
_cell_measurement_theta_max        31.5670
_cell_measurement_theta_min        1.9810
_shelx_estimated_absorpt_T_max     0.205
_shelx_estimated_absorpt_T_min     0.205
_exptl_absorpt_coefficient_mu      12.211
_exptl_absorpt_correction_T_max    0.07156
_exptl_absorpt_correction_T_min    0.04269
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              colourless
_exptl_crystal_colour_primary      colourless
_exptl_crystal_density_diffrn      2.071
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               1600
_exptl_crystal_preparation         ?
_exptl_crystal_recrystallization_method 
 'crystallized from a dimethylformamide/diethylether mixture'
_exptl_crystal_size_max            0.19
_exptl_crystal_size_mid            0.19
_exptl_crystal_size_min            0.19
_exptl_special_details            
 'The data collection nominally covered a full sphere of reciprocal space by a combination of 4 sets of ω scans each set at different φ and/or 2θ angles and each scan (10 s exposure) covering -0.300° degrees in ω. The crystal to detector distance was 4.956 cm.'
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0161
_diffrn_reflns_av_unetI/netI       0.0123
_diffrn_reflns_Laue_measured_fraction_full  1.000
_diffrn_reflns_Laue_measured_fraction_max  0.920
_diffrn_reflns_limit_h_max         28
_diffrn_reflns_limit_h_min         -29
_diffrn_reflns_limit_k_max         12
_diffrn_reflns_limit_k_min         -11
_diffrn_reflns_limit_l_max         26
_diffrn_reflns_limit_l_min         -26
_diffrn_reflns_number              14568
_diffrn_reflns_point_group_measured_fraction_full  1.000
_diffrn_reflns_point_group_measured_fraction_max  0.920
_diffrn_reflns_theta_full          25.242
_diffrn_reflns_theta_max           31.474
_diffrn_reflns_theta_min           2.362
_diffrn_ambient_temperature        100
_diffrn_detector                   'Bruker Apex I'
_diffrn_detector_area_resol_mean   7.9
_diffrn_detector_type              'CCD area detector'
_diffrn_measured_fraction_theta_full  1.000
_diffrn_measured_fraction_theta_max  0.920
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      2.18 182.00   0.30   10.05    --   28.00  73.93 -25.82  600
  2  ω      2.18 182.00   0.30   10.06    --   28.00  73.93  94.18  600
  3  ω      2.18 182.00   0.30   10.07    --   28.00  73.93-145.82  600
;
_diffrn_measurement_device         'fixed chi three-circle diffractometer'
_diffrn_measurement_device_type   
 'Bruker SMART Platform with an Apex I-detector'
_diffrn_measurement_method         'ω scans'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        0.0119800000
_diffrn_orient_matrix_UB_12        -0.0553896000
_diffrn_orient_matrix_UB_13        0.0333182000
_diffrn_orient_matrix_UB_21        -0.0355897000
_diffrn_orient_matrix_UB_22        -0.0428917000
_diffrn_orient_matrix_UB_23        -0.0263222000
_diffrn_orient_matrix_UB_31        0.0185756000
_diffrn_orient_matrix_UB_32        -0.0467177000
_diffrn_orient_matrix_UB_33        -0.0153862000
_diffrn_radiation_monochromator    Parallel,graphite
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'sealed X-ray tube'
_diffrn_source_current             35.0
_diffrn_source_power               1.575
_diffrn_source_target              Mo
_diffrn_source_type                'Enhance (Mo) X-ray Source'
_diffrn_source_voltage             45.0
_diffrn_special_details            ?
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  3946
_reflns_number_total               4117
_reflns_odcompleteness_completeness  99.97
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       26.32
_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 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_collection         'SMART v5.630 (Bruker, 2003)'
_computing_data_reduction          'CrysAlisPro 1.171.39.28c (Rigaku OD, 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           0.744
_refine_diff_density_min           -0.599
_refine_diff_density_rms           0.111
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.079
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       125
_refine_ls_number_reflns           4117
_refine_ls_number_restraints       0
_refine_ls_R_factor_all            0.0229
_refine_ls_R_factor_gt             0.0213
_refine_ls_restrained_S_all        1.079
_refine_ls_shift/su_max            0.001
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.0254P)²+7.4614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.0501
_refine_ls_wR_factor_ref           0.0508
_refine_special_details            ?
_olex2_refinement_description
;
1. Others
 Fixed U12: Pb1(0)
 Fixed U23: Pb1(0)
 Fixed Uiso: H1A(0.026) H1B(0.026) H2A(0.029) H2B(0.029) H3A(0.032) H3B(0.032)
 H4A(0.027) H4B(0.027) H5A(0.026) H5B(0.026) H6A(0.024) H6B(0.024) H7A(0.027)
 H7B(0.027) H8A(0.026) H8B(0.026) H9A(0.044) H9B(0.044) H9C(0.044) H10A(0.039)
 H10B(0.039) H10C(0.039)
 Fixed X: Pb1(0.5) H1A(0.059648) H1B(0.054412) H2A(0.028195) H2B(-0.034771)
 H3A(0.017629) H3B(0.031974) H4A(0.150231) H4B(0.148372) H5A(0.238805)
 H5B(0.173238) H6A(0.239779) H6B(0.156869) H7A(0.189038) H7B(0.102518)
 H8A(0.148662) H8B(0.236642) H9A(0.108105) H9B(0.172132) H9C(0.198416)
 H10A(0.185297) H10B(0.258751) H10C(0.189946)
 Fixed Y: H1A(0.966926) H1B(0.835767) H2A(0.637405) H2B(0.777741)
 H3A(0.689624) H3B(0.875461) H4A(0.768795) H4B(0.630779) H5A(0.824905)
 H5B(0.960759) H6A(0.646327) H6B(0.580344) H7A(0.678916) H7B(0.628682)
 H8A(0.370599) H8B(0.41992) H9A(0.411655) H9B(0.272697) H9C(0.444656)
 H10A(0.932527) H10B(0.922658) H10C(1.049439)
 Fixed Z: Pb1(0.75) H1A(0.576607) H1B(0.512356) H2A(0.57989) H2B(0.551669)
 H3A(0.694502) H3B(0.690609) H4A(0.803378) H4B(0.743934) H5A(0.762132)
 H5B(0.730221) H6A(0.663225) H6B(0.641054) H7A(0.518585) H7B(0.493199)
 H8A(0.54849) H8B(0.579152) H9A(0.403425) H9B(0.44871) H9C(0.437216)
 H10A(0.554276) H10B(0.651503) H10C(0.623716)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       dual
_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 0.500000 0.78841(2) 0.750000 0.01899(4) Uani 1 2 d S T P . .
 Br1 Br 0.58730(2) 0.79025(3) 0.66360(2) 0.02200(6) Uani 1 1 d . . . . .
 Br2 Br 0.39055(2) 0.57918(3) 0.63434(2) 0.02443(6) Uani 1 1 d . . . . .
 N1 N 0.15829(12) 0.8234(2) 0.63149(13) 0.0191(4) Uani 1 1 d . . . . .
 C1 C 0.07051(14) 0.8543(3) 0.57171(15) 0.0214(4) Uani 1 1 d . . . . .
 H1A H 0.059648 0.966926 0.576607 0.026 Uiso 1 1 calc R . . . .
 H1B H 0.054412 0.835767 0.512356 0.026 Uiso 1 1 calc R . . . .
 C2 C 0.02176(15) 0.7496(3) 0.59052(16) 0.0241(5) Uani 1 1 d . . . . .
 H2A H 0.028195 0.637405 0.579890 0.029 Uiso 1 1 calc R . . . .
 H2B H -0.034771 0.777741 0.551669 0.029 Uiso 1 1 calc R . . . .
 C3 C 0.04648(16) 0.7680(4) 0.68253(18) 0.0270(5) Uani 1 1 d . . . . .
 H3A H 0.017629 0.689624 0.694502 0.032 Uiso 1 1 calc R . . . .
 H3B H 0.031974 0.875461 0.690609 0.032 Uiso 1 1 calc R . . . .
 C4 C 0.13517(15) 0.7435(3) 0.74497(16) 0.0225(5) Uani 1 1 d . . . . .
 H4A H 0.150231 0.768795 0.803378 0.027 Uiso 1 1 calc R . . . .
 H4B H 0.148372 0.630779 0.743934 0.027 Uiso 1 1 calc R . . . .
 C5 C 0.18178(15) 0.8481(3) 0.72250(15) 0.0218(4) Uani 1 1 d . . . . .
 H5A H 0.238805 0.824905 0.762132 0.026 Uiso 1 1 calc R . . . .
 H5B H 0.173238 0.960759 0.730221 0.026 Uiso 1 1 calc R . . . .
 C7 C 0.18182(14) 0.6570(3) 0.62318(15) 0.0197(4) Uani 1 1 d . . . . .
 H6A H 0.239779 0.646327 0.663225 0.024 Uiso 1 1 calc R . . . .
 H6B H 0.156869 0.580344 0.641054 0.024 Uiso 1 1 calc R . . . .
 C8 C 0.15978(15) 0.6115(3) 0.53504(15) 0.0227(5) Uani 1 1 d . . . . .
 H7A H 0.189038 0.678916 0.518585 0.027 Uiso 1 1 calc R . . . .
 H7B H 0.102518 0.628682 0.493199 0.027 Uiso 1 1 calc R . . . .
 C9 C 0.18002(15) 0.4375(3) 0.53461(15) 0.0216(4) Uani 1 1 d . . . . .
 H8A H 0.148662 0.370599 0.548490 0.026 Uiso 1 1 calc R . . . .
 H8B H 0.236642 0.419920 0.579152 0.026 Uiso 1 1 calc R . . . .
 C10 C 0.16316(17) 0.3871(4) 0.44824(18) 0.0291(5) Uani 1 1 d . . . . .
 H9A H 0.108105 0.411655 0.403425 0.044 Uiso 1 1 calc GR . . . .
 H9B H 0.172132 0.272697 0.448710 0.044 Uiso 1 1 calc GR . . . .
 H9C H 0.198416 0.444656 0.437216 0.044 Uiso 1 1 calc GR . . . .
 C6 C 0.20181(16) 0.9422(3) 0.61372(17) 0.0260(5) Uani 1 1 d . . . . .
 H10A H 0.185297 0.932527 0.554276 0.039 Uiso 1 1 calc GR . . . .
 H10B H 0.258751 0.922658 0.651503 0.039 Uiso 1 1 calc GR . . . .
 H10C H 0.189946 1.049439 0.623716 0.039 Uiso 1 1 calc GR . . . .


_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 3.0087(3) . ?
 Pb1 Br1 3.0088(3) 2_656 ?
 Pb1 Br2 2.7258(3) . ?
 Pb1 Br2 2.7258(3) 2_656 ?
 N1 C1 1.514(3) . ?
 N1 C5 1.521(3) . ?
 N1 C7 1.518(3) . ?
 N1 C6 1.493(3) . ?
 C1 C2 1.511(4) . ?
 C2 C3 1.525(4) . ?
 C3 C4 1.525(4) . ?
 C4 C5 1.518(4) . ?
 C7 C8 1.513(3) . ?
 C8 C9 1.524(4) . ?
 C9 C10 1.528(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
 Br1 Pb1 Br1 179.409(10) . 2_656 ?
 Br2 Pb1 Br1 92.005(8) . . ?
 Br2 Pb1 Br1 88.377(8) 2_656 . ?
 Br2 Pb1 Br1 88.378(8) . 2_656 ?
 Br2 Pb1 Br1 92.005(8) 2_656 2_656 ?
 Br2 Pb1 Br2 99.429(13) . 2_656 ?
 C1 N1 C5 108.55(19) . . ?
 C1 N1 C7 113.03(18) . . ?
 C7 N1 C5 108.92(18) . . ?
 C6 N1 C1 108.63(19) . . ?
 C6 N1 C5 108.04(19) . . ?
 C6 N1 C7 109.5(2) . . ?
 C2 C1 N1 112.5(2) . . ?
 C1 C2 C3 111.4(2) . . ?
 C2 C3 C4 111.5(2) . . ?
 C5 C4 C3 111.1(2) . . ?
 C4 C5 N1 112.6(2) . . ?
 C8 C7 N1 115.49(19) . . ?
 C7 C8 C9 109.5(2) . . ?
 C8 C9 C10 111.8(2) . . ?

_olex2_exptl_crystal_mounting_method  tip-mounted
_olex2_submission_special_instructions  'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max  1.288
_oxdiff_exptl_absorpt_empirical_full_min  0.772
