 
data_AIZ-Pb1
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C23 H15 N3 O7 Pb2 S'
_chemical_formula_sum
 'C23 H15 N3 O7 Pb2 S' 
_chemical_formula_weight          891.84

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'
 'O'  'O'   0.0106   0.0060
 '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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_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'
 
_cell_length_a                    6.7301(5)
_cell_length_b                    11.7798(10)
_cell_length_c                    16.9376(14)
_cell_angle_alpha                 102.469(3)
_cell_angle_beta                  93.546(3)
_cell_angle_gamma                 92.657(3)
_cell_volume                      1306.16(18)
_cell_formula_units_Z             2
_cell_measurement_temperature     273(2)
_cell_measurement_reflns_used     9874
_cell_measurement_theta_min        2.37
_cell_measurement_theta_max       27.13
 
_exptl_crystal_description        needle
_exptl_crystal_colour             brown
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     2.268          
_exptl_crystal_F_000              1440
_exptl_transmission_factor_min    0.763
_exptl_transmission_factor_max    0.836
_exptl_crystal_size_max           0.136
_exptl_crystal_size_mid           0.063
_exptl_crystal_size_min           0.031
_exptl_absorpt_coefficient_mu     12.999
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       273(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    Mo
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             36177
_diffrn_reflns_av_unetI/netI      0.0399
_diffrn_reflns_av_R_equivalents   0.0733
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -20
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          1.774
_diffrn_reflns_theta_max          24.996
_diffrn_reflns_theta_full         24.996
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              4574
_reflns_number_gt                 3817
_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.
;
 
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0580P)²+25.6149P] 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          4574
_refine_ls_number_parameters      325
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0632
_refine_ls_R_factor_gt            0.0494
_refine_ls_wR_factor_ref          0.1392
_refine_ls_wR_factor_gt           0.1300
_refine_ls_goodness_of_fit_ref    1.062
_refine_ls_restrained_S_all       1.062
_refine_ls_shift/su_max           0.002
_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
Pb01 Pb 1.18087(7) 1.06932(4) 0.82096(3) 0.03545(16) Uani 1 1 d . . . . .
Pb02 Pb 0.30196(10) 0.70690(5) 0.21549(3) 0.0531(2) Uani 1 1 d . . . . .
O004 O 0.9616(13) 0.9656(9) 0.8943(6) 0.047(2) Uani 1 1 d . . . . .
O005 O 0.5621(14) 0.9057(8) 0.2960(5) 0.045(2) Uani 1 1 d . . . . .
O006 O 0.9692(14) 0.9752(9) 0.7137(6) 0.050(2) Uani 1 1 d . . . . .
O007 O 0.8715(16) 1.1442(10) 0.8983(7) 0.064(3) Uani 1 1 d . . . . .
O2 O 0.9413(14) 1.1549(8) 0.6971(6) 0.049(2) Uani 1 1 d . . . . .
O1 O 0.5019(16) 0.7423(8) 0.3360(6) 0.056(3) Uani 1 1 d . . . . .
N00A N 0.6730(16) 0.1285(10) 0.2025(7) 0.044(3) Uani 1 1 d . . . . .
C00B C 0.5374(19) 1.1078(13) 0.9854(8) 0.042(3) Uani 1 1 d . . . . .
H00B H 0.560985 1.181824 0.975798 0.051 Uiso 1 1 calc R U . . .
C00C C 0.6692(18) 1.0229(11) 0.9592(7) 0.035(3) Uani 1 1 d . . . . .
C00D C 0.6658(17) 0.8984(11) 0.4316(7) 0.033(3) Uani 1 1 d . . . . .
O3 O 0.459(2) 0.5258(9) 0.1946(8) 0.072(3) Uani 1 1 d . . . . .
C00F C 0.7949(16) 1.0668(11) 0.5331(7) 0.032(3) Uani 1 1 d . . . . .
H00F H 0.827644 1.146402 0.548343 0.039 Uiso 1 1 calc R U . . .
C00G C 0.9152(17) 1.0486(13) 0.6725(8) 0.038(3) Uani 1 1 d . . . . .
C00H C 0.7186(17) 1.0171(10) 0.4540(7) 0.031(3) Uani 1 1 d . . . . .
H00H H 0.703127 1.063405 0.416261 0.038 Uiso 1 1 calc R U . . .
C00I C 0.8221(17) 0.9960(11) 0.5896(8) 0.035(3) Uani 1 1 d . . . . .
C00J C 0.845(2) 1.0460(13) 0.9150(8) 0.043(3) Uani 1 1 d . . . . .
N1 N 0.144(2) 0.5625(12) 0.2798(10) 0.066(4) Uani 1 1 d . . . . .
C00L C 0.771(2) 0.8792(11) 0.5662(8) 0.040(3) Uani 1 1 d . . . . .
H00L H 0.790201 0.832161 0.603263 0.048 Uiso 1 1 calc R U . . .
C00M C 0.5735(19) 0.8454(11) 0.3483(8) 0.039(3) Uani 1 1 d . . . . .
C00N C 0.6279(19) 0.9145(12) 0.9745(7) 0.039(3) Uani 1 1 d . . . . .
H00N H 0.712673 0.855217 0.957669 0.047 Uiso 1 1 calc R U . . .
N2 N 0.228(2) 0.4593(10) 0.2750(9) 0.059(3) Uani 1 1 d . . . . .
H2A H 0.184482 0.405419 0.297887 0.071 Uiso 1 1 calc R U . . .
C00P C 0.483(2) 0.3345(12) 0.2191(9) 0.047(3) Uani 1 1 d . . . . .
C00Q C -0.106(2) 0.4940(13) 0.3639(11) 0.057(4) Uani 1 1 d . . . . .
C00R C 0.6904(19) 0.8296(11) 0.4886(8) 0.036(3) Uani 1 1 d . . . . .
H00R H 0.652923 0.750396 0.474409 0.043 Uiso 1 1 calc R U . . .
C00S C 0.756(2) 0.2193(13) 0.1798(10) 0.054(4) Uani 1 1 d . . . . .
H00S H 0.879541 0.212391 0.157770 0.065 Uiso 1 1 calc R U . . .
C00T C 0.389(3) 0.4511(14) 0.2291(10) 0.058(4) Uani 1 1 d . . . . .
C00U C 0.667(2) 0.3230(13) 0.1877(10) 0.059(4) Uani 1 1 d . . . . .
H00U H 0.730610 0.385468 0.171983 0.071 Uiso 1 1 calc R U . . .
C00V C 0.391(2) 0.2387(13) 0.2403(10) 0.057(4) Uani 1 1 d . . . . .
H00V H 0.265249 0.241641 0.259967 0.068 Uiso 1 1 calc R U . . .
C3 C -0.014(3) 0.5753(14) 0.3216(10) 0.060(4) Uani 1 1 d . . . . .
H3 H -0.075639 0.645037 0.324418 0.072 Uiso 1 1 calc R U . . .
C00X C 0.493(2) 0.1400(13) 0.2312(9) 0.049(3) Uani 1 1 d . . . . .
H00X H 0.433018 0.075906 0.246159 0.059 Uiso 1 1 calc R U . . .
C4 C -0.294(3) 0.5061(14) 0.3923(11) 0.065(5) Uani 1 1 d . . . . .
H4 H -0.371255 0.567960 0.387693 0.078 Uiso 1 1 calc R U . . .
C2 C -0.354(3) 0.4171(17) 0.4282(13) 0.083(6) Uani 1 1 d . . . . .
H2 H -0.478321 0.410291 0.448548 0.099 Uiso 1 1 calc R U . . .
C1 C -0.211(4) 0.3409(17) 0.4301(15) 0.102(8) Uani 1 1 d . . . . .
H1 H -0.222765 0.278421 0.455314 0.122 Uiso 1 1 calc R U . . .
S1 S -0.0068(9) 0.3706(4) 0.3821(4) 0.0873(16) Uani 1 1 d . . . . .
 
 
_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
Pb01 O006 2.285(9) . ?
Pb01 O004 2.435(9) . ?
Pb01 N00A 2.533(11) 2_766 ?
Pb01 O007 2.615(10) . ?
Pb02 O1 2.322(10) . ?
Pb02 O3 2.391(11) . ?
Pb02 N1 2.445(15) . ?
Pb02 O2 2.651(10) 2_676 ?
O004 C00J 1.263(16) . ?
O005 C00M 1.251(16) . ?
O006 C00G 1.275(16) . ?
O007 C00J 1.255(17) . ?
O2 C00G 1.232(16) . ?
O1 C00M 1.255(16) . ?
N00A C00S 1.325(19) . ?
N00A C00X 1.334(18) . ?
C00B C00N 1.382(18) 2_677 ?
C00B C00C 1.387(18) . ?
C00B H00B 0.9300 . ?
C00C C00N 1.376(18) . ?
C00C C00J 1.484(18) . ?
C00D C00H 1.390(17) . ?
C00D C00R 1.395(17) . ?
C00D C00M 1.497(17) . ?
O3 C00T 1.25(2) . ?
C00F C00H 1.395(17) . ?
C00F C00I 1.408(17) . ?
C00F H00F 0.9300 . ?
C00G C00I 1.492(18) . ?
C00H H00H 0.9300 . ?
C00I C00L 1.369(18) . ?
N1 C3 1.31(2) . ?
N1 N2 1.351(17) . ?
C00L C00R 1.383(18) . ?
C00L H00L 0.9300 . ?
C00N H00N 0.9300 . ?
N2 C00T 1.37(2) . ?
N2 H2A 0.8600 . ?
C00P C00U 1.38(2) . ?
C00P C00V 1.39(2) . ?
C00P C00T 1.52(2) . ?
C00Q C4 1.38(2) . ?
C00Q C3 1.45(2) . ?
C00Q S1 1.705(16) . ?
C00R H00R 0.9300 . ?
C00S C00U 1.37(2) . ?
C00S H00S 0.9300 . ?
C00U H00U 0.9300 . ?
C00V C00X 1.36(2) . ?
C00V H00V 0.9300 . ?
C3 H3 0.9300 . ?
C00X H00X 0.9300 . ?
C4 C2 1.38(2) . ?
C4 H4 0.9300 . ?
C2 C1 1.35(3) . ?
C2 H2 0.9300 . ?
C1 S1 1.70(3) . ?
C1 H1 0.9300 . ?
 
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
O006 Pb01 O004 81.7(3) . . ?
O006 Pb01 N00A 81.4(4) . 2_766 ?
O004 Pb01 N00A 78.7(3) . 2_766 ?
O006 Pb01 O007 89.0(4) . . ?
O004 Pb01 O007 51.6(3) . . ?
N00A Pb01 O007 130.3(4) 2_766 . ?
O1 Pb02 O3 81.8(4) . . ?
O1 Pb02 N1 80.8(4) . . ?
O3 Pb02 N1 66.0(4) . . ?
O1 Pb02 O2 83.9(3) . 2_676 ?
O3 Pb02 O2 146.6(4) . 2_676 ?
N1 Pb02 O2 82.0(4) . 2_676 ?
C00J O004 Pb01 97.3(9) . . ?
C00G O006 Pb01 108.7(8) . . ?
C00J O007 Pb01 89.0(8) . . ?
C00G O2 Pb02 126.2(8) . 2_676 ?
C00M O1 Pb02 107.2(8) . . ?
C00S N00A C00X 117.3(12) . . ?
C00S N00A Pb01 123.3(9) . 2_766 ?
C00X N00A Pb01 119.0(9) . 2_766 ?
C00N C00B C00C 121.9(13) 2_677 . ?
C00N C00B H00B 119.0 2_677 . ?
C00C C00B H00B 119.0 . . ?
C00N C00C C00B 117.0(12) . . ?
C00N C00C C00J 121.0(12) . . ?
C00B C00C C00J 122.0(12) . . ?
C00H C00D C00R 119.5(11) . . ?
C00H C00D C00M 120.5(11) . . ?
C00R C00D C00M 119.9(11) . . ?
C00T O3 Pb02 116.4(11) . . ?
C00H C00F C00I 119.9(11) . . ?
C00H C00F H00F 120.1 . . ?
C00I C00F H00F 120.1 . . ?
O2 C00G O006 123.6(12) . . ?
O2 C00G C00I 121.6(12) . . ?
O006 C00G C00I 114.8(12) . . ?
C00D C00H C00F 120.0(11) . . ?
C00D C00H H00H 120.0 . . ?
C00F C00H H00H 120.0 . . ?
C00L C00I C00F 119.2(12) . . ?
C00L C00I C00G 121.3(12) . . ?
C00F C00I C00G 119.5(12) . . ?
O007 C00J O004 122.1(13) . . ?
O007 C00J C00C 119.1(12) . . ?
O004 C00J C00C 118.8(13) . . ?
C3 N1 N2 114.7(14) . . ?
C3 N1 Pb02 126.6(11) . . ?
N2 N1 Pb02 118.7(11) . . ?
C00I C00L C00R 121.4(12) . . ?
C00I C00L H00L 119.3 . . ?
C00R C00L H00L 119.3 . . ?
O005 C00M O1 123.1(12) . . ?
O005 C00M C00D 119.7(12) . . ?
O1 C00M C00D 117.1(12) . . ?
C00B C00N C00C 121.1(12) 2_677 . ?
C00B C00N H00N 119.5 2_677 . ?
C00C C00N H00N 119.5 . . ?
N1 N2 C00T 111.5(13) . . ?
N1 N2 H2A 124.3 . . ?
C00T N2 H2A 124.3 . . ?
C00U C00P C00V 118.4(13) . . ?
C00U C00P C00T 119.0(14) . . ?
C00V C00P C00T 122.6(14) . . ?
C4 C00Q C3 122.7(15) . . ?
C4 C00Q S1 110.9(13) . . ?
C3 C00Q S1 126.3(13) . . ?
C00L C00R C00D 119.9(11) . . ?
C00L C00R H00R 120.0 . . ?
C00D C00R H00R 120.0 . . ?
N00A C00S C00U 122.2(14) . . ?
N00A C00S H00S 118.9 . . ?
C00U C00S H00S 118.9 . . ?
O3 C00T N2 127.3(15) . . ?
O3 C00T C00P 119.1(15) . . ?
N2 C00T C00P 113.6(14) . . ?
C00S C00U C00P 119.8(15) . . ?
C00S C00U H00U 120.1 . . ?
C00P C00U H00U 120.1 . . ?
C00X C00V C00P 117.3(15) . . ?
C00X C00V H00V 121.3 . . ?
C00P C00V H00V 121.3 . . ?
N1 C3 C00Q 128.0(15) . . ?
N1 C3 H3 116.0 . . ?
C00Q C3 H3 116.0 . . ?
N00A C00X C00V 124.8(14) . . ?
N00A C00X H00X 117.6 . . ?
C00V C00X H00X 117.6 . . ?
C00Q C4 C2 113.1(16) . . ?
C00Q C4 H4 123.4 . . ?
C2 C4 H4 123.4 . . ?
C1 C2 C4 111.7(19) . . ?
C1 C2 H2 124.2 . . ?
C4 C2 H2 124.2 . . ?
C2 C1 S1 113.4(14) . . ?
C2 C1 H1 123.3 . . ?
S1 C1 H1 123.3 . . ?
C1 S1 C00Q 90.7(10) . . ?
 
_refine_diff_density_max    3.006
_refine_diff_density_min   -2.885
_refine_diff_density_rms    0.253



