data_4ampPbBr4
_audit_creation_date              2018-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number            2013-4
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_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          'Br3.97 Pb, C6 H16 N2'
_chemical_formula_sum             'C6 H16 Br3.97 N2 Pb'
_chemical_formula_weight          640.64
_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'
 '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            29
_space_group_name_H-M_alt         'P c a 21'
_space_group_name_Hall            'P 2c -2ac'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z+1/2'
 '-x+1/2, y, z+1/2'
 'x+1/2, -y, z'

_cell_length_a                    17.745(4)
_cell_length_b                    10.235(2)
_cell_length_c                    7.8299(16)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1422.1(5)
_cell_formula_units_Z             4
_cell_measurement_reflns_used    10889
_cell_measurement_theta_min      1.99
_cell_measurement_theta_max      29.74
_cell_measurement_temperature     293(2)
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     22.986
_exptl_absorpt_process_details    ?
_exptl_crystal_density_diffrn     2.992
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.0435
_exptl_crystal_size_mid          0.0347
_exptl_crystal_size_min          0.0141
_exptl_crystal_F_000             1152
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.2403
_exptl_absorpt_correction_T_max  0.5298
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0417
_diffrn_reflns_av_unetI/netI      0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max        24
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_k_max        14
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_l_max        10
_diffrn_reflns_limit_l_min        -10
_diffrn_reflns_number             12316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full         26.000
_diffrn_reflns_theta_max          29.254
_diffrn_reflns_theta_min          1.990
_diffrn_ambient_temperature       293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device         '2-circle goniometer'
_diffrn_measurement_device_type    'STOE IPDS 2'
_diffrn_detector                   'image plate (34 cm diameter)'
_diffrn_detector_type              'STOE'
_diffrn_detector_area_resol_mean   6.67
_diffrn_source           'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage             50
_diffrn_source_current             40
_diffrn_source_power               2.00
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_radiation_monochromator    'plane graphite'
_diffrn_radiation_collimation      '0.5 mm diameter, monocapillary'
_diffrn_measurement_method         'rotation method'
_reflns_Friedel_coverage          0.861
_reflns_Friedel_fraction_full     0.997
_reflns_Friedel_fraction_max      0.989
_reflns_number_gt                 3221
_reflns_number_total              3840
_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        ?
_computing_data_collection        ?
_computing_data_reduction         ?
_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          1.636
_refine_diff_density_min          -1.850
_refine_diff_density_rms          0.226
_refine_ls_abs_structure_details
;
 Flack x determined using 1294 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack    -0.001(11)
_refine_ls_extinction_coef        0.0020(3)
_refine_ls_extinction_expression  'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method      SHELXL
_refine_ls_goodness_of_fit_ref    1.060
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      122
_refine_ls_number_reflns          3840
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0559
_refine_ls_R_factor_gt            0.0452
_refine_ls_restrained_S_all       1.060
_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)+(0.0790P)²+2.6940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1156
_refine_ls_wR_factor_ref          0.1284
_refine_special_details
;
 Refined as a 2-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.42(3) 0.58(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C4(H4)
3.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B)
3.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C)
;
_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 0.12266(3) 0.50729(4) 0.16153(19) 0.03669(19) Uani 1 1 d . . . . .
 Br2 Br 0.15211(9) 0.20689(14) 0.1413(3) 0.0476(4) Uani 1 1 d . . . . .
 Br3 Br 0.11301(10) 0.78570(15) 0.1859(3) 0.0497(5) Uani 1 1 d . . . . .
 Br4 Br 0.23299(10) 0.51957(16) 0.4639(3) 0.0472(4) Uani 1 1 d . . . . .
 Br5A Br -0.03714(11) 0.49730(16) 0.3355(3) 0.0512(7) Uani 0.969(10) 1 d . . .
 A 2
 N1 N 0.1178(7) 0.7632(12) 0.619(2) 0.045(3) Uani 1 1 d . . . . .
 H1A H 0.1291 0.7637 0.4979 0.054 Uiso 1 1 calc R . . . .
 H1B H 0.1148 0.6729 0.6561 0.054 Uiso 1 1 calc R . . . .
 N2 N 0.1671(8) 1.2628(12) 0.7217(19) 0.046(3) Uani 1 1 d . . . . .
 H2A H 0.2131 1.2405 0.6867 0.055 Uiso 1 1 calc GR . . . .
 H2B H 0.1632 1.2490 0.8335 0.055 Uiso 1 1 calc GR . . . .
 H2C H 0.1592 1.3470 0.6996 0.055 Uiso 1 1 calc GR . . . .
 C3 C 0.1840(8) 0.9730(15) 0.658(3) 0.052(4) Uani 1 1 d . . . . .
 H3A H 0.2238 1.0163 0.7213 0.062 Uiso 1 1 calc R . . . .
 H3B H 0.1966 0.9776 0.5374 0.062 Uiso 1 1 calc R . . . .
 C4 C 0.1098(9) 1.0431(16) 0.689(2) 0.042(3) Uani 1 1 d . . . . .
 H4 H 0.0989 1.0413 0.8116 0.051 Uiso 1 1 calc R . . . .
 C5 C 0.0443(8) 0.8278(16) 0.648(4) 0.064(5) Uani 1 1 d . . . . .
 H5A H 0.0309 0.8215 0.7682 0.077 Uiso 1 1 calc R . . . .
 H5B H 0.0056 0.7841 0.5823 0.077 Uiso 1 1 calc R . . . .
 C6 C 0.1102(10) 1.1828(16) 0.630(2) 0.048(4) Uani 1 1 d . . . . .
 H6A H 0.1206 1.1855 0.5087 0.057 Uiso 1 1 calc R . . . .
 H6B H 0.0606 1.2204 0.6486 0.057 Uiso 1 1 calc R . . . .
 C7 C 0.1793(11) 0.8297(17) 0.713(3) 0.060(5) Uani 1 1 d . . . . .
 H7A H 0.2269 0.7864 0.6897 0.072 Uiso 1 1 calc R . . . .
 H7B H 0.1699 0.8248 0.8349 0.072 Uiso 1 1 calc R . . . .
 C8 C 0.0486(10) 0.9700(16) 0.597(3) 0.057(5) Uani 1 1 d . . . . .
 H8A H 0.0576 0.9753 0.4746 0.068 Uiso 1 1 calc R . . . .
 H8B H 0.0005 1.0114 0.6200 0.068 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 Br2 3.1228(17) . ?
 Pb1 Br3 2.8611(17) . ?
 Pb1 Br4 3.074(2) . ?
 Pb1 Br4 2.995(2) 3_554 ?
 Pb1 Br5A 3.148(2) . ?
 Pb1 Br5A 2.970(2) 2_564 ?
 Br4 Pb1 2.995(2) 3 ?
 Br5A Pb1 2.970(2) 2_565 ?
 N1 H1A 0.9700 . ?
 N1 H1B 0.9700 . ?
 N1 C5 1.480(18) . ?
 N1 C7 1.48(2) . ?
 N2 H2A 0.8900 . ?
 N2 H2B 0.8900 . ?
 N2 H2C 0.8900 . ?
 N2 C6 1.48(2) . ?
 C3 H3A 0.9700 . ?
 C3 H3B 0.9700 . ?
 C3 C4 1.52(2) . ?
 C3 C7 1.53(2) . ?
 C4 H4 0.9800 . ?
 C4 C6 1.50(2) . ?
 C4 C8 1.50(2) . ?
 C5 H5A 0.9700 . ?
 C5 H5B 0.9700 . ?
 C5 C8 1.51(3) . ?
 C6 H6A 0.9700 . ?
 C6 H6B 0.9700 . ?
 C7 H7A 0.9700 . ?
 C7 H7B 0.9700 . ?
 C8 H8A 0.9700 . ?
 C8 H8B 0.9700 . ?

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
 Br2 Pb1 Br5A 98.09(5) . . ?
 Br3 Pb1 Br2 173.74(5) . . ?
 Br3 Pb1 Br4 86.91(6) . . ?
 Br3 Pb1 Br4 92.51(6) . 3_554 ?
 Br3 Pb1 Br5A 87.11(6) . . ?
 Br3 Pb1 Br5A 92.43(7) . 2_564 ?
 Br4 Pb1 Br2 82.65(5) 3_554 . ?
 Br4 Pb1 Br2 88.44(5) . . ?
 Br4 Pb1 Br4 81.46(2) 3_554 . ?
 Br4 Pb1 Br5A 103.99(7) . . ?
 Br4 Pb1 Br5A 174.50(8) 3_554 . ?
 Br5A Pb1 Br2 91.51(6) 2_564 . ?
 Br5A Pb1 Br4 89.63(7) 2_564 3_554 ?
 Br5A Pb1 Br4 171.02(7) 2_564 . ?
 Br5A Pb1 Br5A 84.90(3) 2_564 . ?
 Pb1 Br4 Pb1 160.16(9) 3 . ?
 Pb1 Br5A Pb1 146.39(9) 2_565 . ?
 H1A N1 H1B 108.0 . . ?
 C5 N1 H1A 109.3 . . ?
 C5 N1 H1B 109.3 . . ?
 C5 N1 C7 111.5(14) . . ?
 C7 N1 H1A 109.3 . . ?
 C7 N1 H1B 109.3 . . ?
 H2A N2 H2B 109.5 . . ?
 H2A N2 H2C 109.5 . . ?
 H2B N2 H2C 109.5 . . ?
 C6 N2 H2A 109.5 . . ?
 C6 N2 H2B 109.5 . . ?
 C6 N2 H2C 109.5 . . ?
 H3A C3 H3B 108.0 . . ?
 C4 C3 H3A 109.4 . . ?
 C4 C3 H3B 109.4 . . ?
 C4 C3 C7 111.1(14) . . ?
 C7 C3 H3A 109.4 . . ?
 C7 C3 H3B 109.4 . . ?
 C3 C4 H4 108.6 . . ?
 C6 C4 C3 113.4(13) . . ?
 C6 C4 H4 108.6 . . ?
 C6 C4 C8 109.3(16) . . ?
 C8 C4 C3 108.3(14) . . ?
 C8 C4 H4 108.6 . . ?
 N1 C5 H5A 109.6 . . ?
 N1 C5 H5B 109.6 . . ?
 N1 C5 C8 110.1(14) . . ?
 H5A C5 H5B 108.1 . . ?
 C8 C5 H5A 109.6 . . ?
 C8 C5 H5B 109.6 . . ?
 N2 C6 C4 112.4(14) . . ?
 N2 C6 H6A 109.1 . . ?
 N2 C6 H6B 109.1 . . ?
 C4 C6 H6A 109.1 . . ?
 C4 C6 H6B 109.1 . . ?
 H6A C6 H6B 107.9 . . ?
 N1 C7 C3 109.9(16) . . ?
 N1 C7 H7A 109.7 . . ?
 N1 C7 H7B 109.7 . . ?
 C3 C7 H7A 109.7 . . ?
 C3 C7 H7B 109.7 . . ?
 H7A C7 H7B 108.2 . . ?
 C4 C8 C5 112.7(17) . . ?
 C4 C8 H8A 109.0 . . ?
 C4 C8 H8B 109.0 . . ?
 C5 C8 H8A 109.0 . . ?
 C5 C8 H8B 109.0 . . ?
 H8A C8 H8B 107.8 . . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 N1 C5 C8 C4 -57(2) . . . . ?
 C3 C4 C6 N2 -62(2) . . . . ?
 C3 C4 C8 C5 56(2) . . . . ?
 C4 C3 C7 N1 58(2) . . . . ?
 C5 N1 C7 C3 -58(2) . . . . ?
 C6 C4 C8 C5 180.0(16) . . . . ?
 C7 N1 C5 C8 57(3) . . . . ?
 C7 C3 C4 C6 -177.6(17) . . . . ?
 C7 C3 C4 C8 -56(2) . . . . ?
 C8 C4 C6 N2 177.5(14) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

loop_
  _twin_individual_id
  _twin_individual_mass_fraction_refined
 1 0.42(3)
 2 0.58(3)

