 
data_ba-pure-100k
 
_audit_creation_method            'SHELXL-2019/1'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety    'C4 H12 Br2 N Pb0.50'
_chemical_formula_sum
 'C4 H12 Br2 N Pb0.50' 
_chemical_formula_weight          337.56

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'
 'Pb'  'Pb'  -3.3944  10.1111
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            61
_space_group_name_H-M_alt         'P b c a'
_space_group_name_Hall            '-P 2ac 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, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    8.2490(8)
_cell_length_b                    8.1326(8)
_cell_length_c                    27.428(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1840.0(3)
_cell_formula_units_Z             8
_cell_measurement_temperature     100(2)
_cell_measurement_reflns_used     1526
_cell_measurement_theta_min       2.882
_cell_measurement_theta_max       30.503
 
_exptl_crystal_description        'prism frag'
_exptl_crystal_colour             'colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.437          
_exptl_crystal_F_000              1232
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.479
_exptl_crystal_size_mid           0.346
_exptl_crystal_size_min           0.202
_exptl_absorpt_coefficient_mu     17.836
_shelx_estimated_absorpt_T_min    0.043
_shelx_estimated_absorpt_T_max    0.123
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.043
_exptl_absorpt_correction_T_max   0.123
_exptl_absorpt_process_details    'Sadabs'
_diffrn_ambient_temperature       100(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Bruker AXS D8 Venture'
_diffrn_measurement_method        'profile data from θ/2θ scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             53118
_diffrn_reflns_av_unetI/netI      0.0335
_diffrn_reflns_av_R_equivalents   0.0736
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -37
_diffrn_reflns_limit_l_max        37
_diffrn_reflns_theta_min          2.882
_diffrn_reflns_theta_max          30.503
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.939
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.939
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.939
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              2636
_reflns_number_gt                 2255
_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.Subsequent electronic residual 
 Densities remained at the vicinity of the Pb atoms. All attempts
 to fit them in any reasonable chemically model failed.

;
 
_computing_data_collection 'APEX5 v2023.9.2'
_computing_cell_refinement 'APEX5 v2023.9.2'
_computing_data_reduction  'Saint, APEX5 v2023.9.2.'
_computing_structure_solution 'SHELXT'
_computing_structure_refinement 'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics  'Mercury 2022-3.0,POV-Ray v 3.7'
_computing_publication_material 'APEX5 v2023.9.2'
_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)+(0.1694P)²+9.4638P] 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          2636
_refine_ls_number_parameters      72
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0877
_refine_ls_R_factor_gt            0.0758
_refine_ls_wR_factor_ref          0.2503
_refine_ls_wR_factor_gt           0.2315
_refine_ls_goodness_of_fit_ref    1.201
_refine_ls_restrained_S_all       1.201
_refine_ls_shift/su_max           0.001
_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 0.500000 1.000000 0.500000 0.0108(3) Uani 1 2 d S . P . .
Br1 Br 0.30980(12) 0.68944(12) 0.50127(3) 0.0166(3) Uani 1 1 d . . . . .
Br2 Br 0.46923(17) 1.01738(12) 0.39071(4) 0.0170(3) Uani 1 1 d . . . . .
N1 N 0.5741(9) 0.5765(9) 0.5895(3) 0.0171(14) Uani 1 1 d . . . . .
H1A H 0.558279 0.681289 0.600083 0.026 Uiso 1 1 calc R U . . .
H1B H 0.558746 0.572103 0.556640 0.026 Uiso 1 1 calc R U . . .
H1C H 0.677066 0.544403 0.596661 0.026 Uiso 1 1 calc R U . . .
C1 C 0.4577(15) 0.4657(14) 0.6138(3) 0.022(2) Uani 1 1 d . . . . .
H1D H 0.476415 0.351033 0.603069 0.027 Uiso 1 1 calc R U . . .
H1E H 0.345627 0.496888 0.604894 0.027 Uiso 1 1 calc R U . . .
C2 C 0.4794(14) 0.4777(13) 0.6691(5) 0.020(2) Uani 1 1 d . . . . .
H2A H 0.460471 0.592620 0.679613 0.024 Uiso 1 1 calc R U . . .
H2B H 0.592181 0.448096 0.677730 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3621(13) 0.3638(13) 0.6962(3) 0.028(2) Uani 1 1 d . . . . .
H3A H 0.249591 0.392346 0.686939 0.034 Uiso 1 1 calc R U . . .
H3B H 0.382352 0.248962 0.685890 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3788(15) 0.3752(18) 0.7501(3) 0.041(3) Uani 1 1 d . . P . .
H4A H 0.492419 0.357957 0.759277 0.062 Uiso 1 1 calc R U . . .
H4B H 0.311230 0.290926 0.765588 0.062 Uiso 1 1 calc R U . . .
H4C H 0.343818 0.484314 0.761085 0.062 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 Br1 2.9735(10) 5_676 ?
Pb1 Br1 2.9736(10) . ?
Pb1 Br1 2.9842(10) 8_665 ?
Pb1 Br1 2.9842(10) 4_566 ?
Pb1 Br2 3.0115(11) 5_676 ?
Pb1 Br2 3.0116(11) . ?
N1 C1 1.477(13) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
C1 C2 1.529(15) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 C3 1.531(16) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.490(13) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
 
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_676 . ?
Br1 Pb1 Br1 90.773(11) 5_676 8_665 ?
Br1 Pb1 Br1 89.227(11) . 8_665 ?
Br1 Pb1 Br1 89.227(11) 5_676 4_566 ?
Br1 Pb1 Br1 90.773(11) . 4_566 ?
Br1 Pb1 Br1 180.0 8_665 4_566 ?
Br1 Pb1 Br2 90.40(2) 5_676 5_676 ?
Br1 Pb1 Br2 89.60(2) . 5_676 ?
Br1 Pb1 Br2 94.87(3) 8_665 5_676 ?
Br1 Pb1 Br2 85.13(3) 4_566 5_676 ?
Br1 Pb1 Br2 89.60(2) 5_676 . ?
Br1 Pb1 Br2 90.40(2) . . ?
Br1 Pb1 Br2 85.13(3) 8_665 . ?
Br1 Pb1 Br2 94.87(3) 4_566 . ?
Br2 Pb1 Br2 180.00(4) 5_676 . ?
Pb1 Br1 Pb1 152.90(4) . 4_466 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C2 109.5(9) . . ?
N1 C1 H1D 109.8 . . ?
C2 C1 H1D 109.8 . . ?
N1 C1 H1E 109.8 . . ?
C2 C1 H1E 109.8 . . ?
H1D C1 H1E 108.2 . . ?
C1 C2 C3 111.6(9) . . ?
C1 C2 H2A 109.3 . . ?
C3 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
C3 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C4 C3 C2 112.7(10) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
 
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 C1 C2 C3 -179.5(8) . . . . ?
C1 C2 C3 C4 -179.1(9) . . . . ?
 
_refine_diff_density_max    6.148
_refine_diff_density_min   -5.973
_refine_diff_density_rms    0.969



