 
data_PMA2
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          '2(Cl3 Pb), C5 H16 N2'
_chemical_formula_sum
 'C5 H16 Cl6 N2 Pb2' 
_chemical_formula_weight          731.30

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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Cl'  'Cl'   0.1484   0.1585
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            28
_space_group_name_H-M_alt         'P m a 2'
_space_group_name_Hall            'P 2 -2a'
 
_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, -y, z'
 'x+1/2, -y, z'
 '-x+1/2, y, z'
 
_cell_length_a                    14.9094(6)
_cell_length_b                    9.4872(4)
_cell_length_c                    5.8622(3)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      829.20(6)
_cell_formula_units_Z             2
_cell_measurement_temperature     393(2)
_cell_measurement_reflns_used     4715
_cell_measurement_theta_min       2.5300
_cell_measurement_theta_max       30.5890
 
_exptl_crystal_description        Block
_exptl_crystal_colour             Colourless
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.929          
_exptl_crystal_F_000              652
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.200
_exptl_crystal_size_mid           0.200
_exptl_crystal_size_min           0.190
_exptl_absorpt_coefficient_mu     21.219
_shelx_estimated_absorpt_T_min    0.101
_shelx_estimated_absorpt_T_max    0.107
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.018
_exptl_absorpt_correction_T_max   0.020
_exptl_absorpt_process_details    'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       393(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'Rotating-anode X-ray tube'
_diffrn_measurement_device_type   'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method        'four-circle diffractometer'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             5952
_diffrn_reflns_av_unetI/netI      0.0449
_diffrn_reflns_av_R_equivalents   0.0766
_diffrn_reflns_limit_h_min        -17
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -6
_diffrn_reflns_limit_l_max        6
_diffrn_reflns_theta_min          2.545
_diffrn_reflns_theta_max          24.996
_diffrn_reflns_theta_full         24.996
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              1478
_reflns_number_gt                 1326
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.808
_reflns_Friedel_fraction_max      0.999
_reflns_Friedel_fraction_full     0.999
 
_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        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_cell_refinement        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction         'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_solution     'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material   'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0645P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef        0.0031(6)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack    0.57(5)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1478
_refine_ls_number_parameters      86
_refine_ls_number_restraints      61
_refine_ls_R_factor_all           0.0388
_refine_ls_R_factor_gt            0.0358
_refine_ls_wR_factor_ref          0.0925
_refine_ls_wR_factor_gt           0.0910
_refine_ls_goodness_of_fit_ref    1.004
_refine_ls_restrained_S_all       0.999
_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 0.05883(2) 0.71184(4) 0.4830(10) 0.0374(3) Uani 1 1 d . . . . .
Cl1 Cl 0.0000 1.0000 0.490(6) 0.084(2) Uani 1 2 d S T P . .
Cl2 Cl 0.0643(4) 0.7049(4) 0.984(5) 0.0769(18) Uani 1 1 d . . . . .
Cl3 Cl 0.1140(2) 0.4189(3) 0.488(3) 0.0651(11) Uani 1 1 d . . . . .
Cl4 Cl 0.2500 0.7530(7) 0.482(6) 0.080(2) Uani 1 2 d S T P . .
N1 N 0.2500 0.5224(19) -0.069(7) 0.081(13) Uani 1 2 d DS T P . .
H1A H 0.2103 0.5871 -0.0204 0.121 Uiso 0.5 1 d R U P . .
H1B H 0.3038 0.5390 -0.0051 0.121 Uiso 0.5 1 d R U P . .
H1C H 0.2500 0.5278 -0.2222 0.121 Uiso 1 2 d R U P . .
N2 N 0.2500 0.1230(17) 0.008(5) 0.055(5) Uani 1 2 d DS TU P . .
C1 C 0.2195(18) 0.382(2) 0.005(10) 0.051(9) Uani 0.5 1 d D U P . .
H1D H 0.1614 0.3658 -0.0613 0.061 Uiso 0.5 1 d R U P . .
H1E H 0.2129 0.3776 0.1676 0.061 Uiso 0.5 1 d R U P . .
C2 C 0.279(2) 0.264(3) -0.081(6) 0.059(9) Uani 0.5 1 d D U P . .
H2A H 0.2811 0.2616 -0.2443 0.071 Uiso 0.5 1 d R U P . .
H2B H 0.3381 0.2831 -0.0252 0.071 Uiso 0.5 1 d R U P . .
C3 C 0.2500 0.116(3) 0.261(4) 0.095(10) Uani 1 2 d DS TU P . .
H3A H 0.3030 0.1609 0.3188 0.142 Uiso 1 1 d R U . . .
H3C H 0.2500 0.0182 0.3041 0.142 Uiso 1 2 d R U P . .
C4 C 0.1748(19) 0.047(4) -0.094(5) 0.150(14) Uani 1 1 d D U . . .
H4A H 0.1735 -0.0526 -0.0653 0.226 Uiso 1 1 d R U . . .
H4B H 0.1230 0.0905 -0.0264 0.226 Uiso 1 1 d R U . . .
H4C H 0.1744 0.0635 -0.2556 0.226 Uiso 1 1 d 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 Cl3 2.860(4) 2_565 ?
Pb1 Cl1 2.8714(6) . ?
Pb1 Cl4 2.8769(10) . ?
Pb1 Cl3 2.898(3) . ?
Pb1 Cl2 2.93(3) 1_554 ?
Pb1 Cl2 2.94(3) . ?
Cl1 Pb1 2.8714(6) 2_575 ?
Cl2 Pb1 2.93(3) 1_556 ?
Cl3 Pb1 2.860(4) 2_565 ?
Cl4 Pb1 2.8769(10) 4 ?
N1 C1 1.48(2) . ?
N1 C1 1.48(2) 4 ?
N2 C4 1.460(19) . ?
N2 C4 1.460(19) 4 ?
N2 C3 1.49(2) . ?
N2 C2 1.50(2) 4 ?
N2 C2 1.50(2) . ?
C1 C1 0.91(5) 4 ?
C1 C2 1.22(4) 4 ?
C1 C2 1.51(2) . ?
C2 C2 0.86(7) 4 ?
C2 C1 1.22(4) 4 ?
 
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
Cl3 Pb1 Cl1 97.91(7) 2_565 . ?
Cl3 Pb1 Cl4 162.09(14) 2_565 . ?
Cl1 Pb1 Cl4 99.99(14) . . ?
Cl3 Pb1 Cl3 80.78(11) 2_565 . ?
Cl1 Pb1 Cl3 178.1(6) . . ?
Cl4 Pb1 Cl3 81.32(15) . . ?
Cl3 Pb1 Cl2 91.5(4) 2_565 1_554 ?
Cl1 Pb1 Cl2 92.6(7) . 1_554 ?
Cl4 Pb1 Cl2 88.5(7) . 1_554 ?
Cl3 Pb1 Cl2 88.9(3) . 1_554 ?
Cl3 Pb1 Cl2 90.3(3) 2_565 . ?
Cl1 Pb1 Cl2 90.9(7) . . ?
Cl4 Pb1 Cl2 88.7(7) . . ?
Cl3 Pb1 Cl2 87.7(3) . . ?
Cl2 Pb1 Cl2 175.9(2) 1_554 . ?
Pb1 Cl1 Pb1 178.3(14) . 2_575 ?
Pb1 Cl2 Pb1 175.9(2) 1_556 . ?
Pb1 Cl3 Pb1 99.21(10) 2_565 . ?
Pb1 Cl4 Pb1 164.4(3) 4 . ?
C1 N1 C1 36(2) . 4 ?
C4 N2 C4 100(3) . 4 ?
C4 N2 C3 112.6(17) . . ?
C4 N2 C3 112.6(17) 4 . ?
C4 N2 C2 95(2) . 4 ?
C4 N2 C2 121(3) 4 4 ?
C3 N2 C2 113(2) . 4 ?
C4 N2 C2 121(3) . . ?
C4 N2 C2 95(2) 4 . ?
C3 N2 C2 113(2) . . ?
C2 N2 C2 33(3) 4 . ?
C1 C1 C2 89(2) 4 4 ?
C1 C1 N1 72.1(11) 4 . ?
C2 C1 N1 134(5) 4 . ?
C1 C1 C2 54.1(18) 4 . ?
C2 C1 C2 35(3) 4 . ?
N1 C1 C2 113(2) . . ?
C2 C2 C1 91(2) 4 4 ?
C2 C2 N2 73.4(13) 4 . ?
C1 C2 N2 133(3) 4 . ?
C2 C2 C1 54.1(18) 4 . ?
C1 C2 C1 37(3) 4 . ?
N2 C2 C1 112.2(19) . . ?
 
_refine_diff_density_max    0.983
_refine_diff_density_min   -1.129
_refine_diff_density_rms    0.236



