# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pb_(OCN)2
_database_code_depnum_ccdc_archive 'CCDC 2383820'
loop_
_audit_author_name
_audit_author_address
'Frank Tambornino'
;Philipps University Marburg
Germany
;
_audit_update_record             
;
2024-09-13 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2022-09-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Frank.Tambornino@chemie.uni-marburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 N2 O2 Pb'
_chemical_formula_sum            'C2 N2 O2 Pb'
_chemical_formula_weight         291.23
_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'
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'

_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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   8.5689(18)
_cell_length_b                   3.9410(9)
_cell_length_c                   11.660(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     393.74(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3543
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.10
_cell_measurement_theta_min      1.68
_shelx_estimated_absorpt_T_max   0.100
_shelx_estimated_absorpt_T_min   0.072
_exptl_absorpt_coefficient_mu    42.695
_exptl_absorpt_correction_T_max  0.0010
_exptl_absorpt_correction_T_min  0.0001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.913
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0993
_diffrn_reflns_av_unetI/netI     0.0643
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6464
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.906
_diffrn_reflns_theta_min         2.950
_diffrn_ambient_temperature      100
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
 291 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_diffrn_source_voltage           0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                517
_reflns_number_total             760
_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       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.81, Darmstadt 2018
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         4.712
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.482
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         760
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0415
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0970
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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 0.18174(7) 0.750000 0.40656(5) 0.02332(19) Uani 1 2 d S T P . .
O1 O 0.2333(13) 0.750000 0.7443(10) 0.028(2) Uani 1 2 d S T P . .
O2 O 0.4959(12) 0.250000 0.6678(10) 0.026(2) Uani 1 2 d S T P . .
N1 N 0.0308(14) 0.750000 0.6007(11) 0.022(2) Uani 1 2 d S T P . .
N2 N 0.3106(16) 0.250000 0.5151(12) 0.029(3) Uani 1 2 d S T P . .
C1 C 0.1290(18) 0.750000 0.6743(13) 0.019(3) Uani 1 2 d S T P . .
C2 C 0.4042(17) 0.250000 0.5906(15) 0.026(3) Uani 1 2 d S T P . .


_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 N1 2.607(13) . ?
Pb1 N1 2.685(8) 5_576 ?
Pb1 N1 2.685(8) 5_566 ?
Pb1 N2 2.589(9) . ?
Pb1 N2 2.589(9) 1_565 ?
O1 C1 1.210(18) . ?
O2 C2 1.195(19) . ?
N1 C1 1.203(19) . ?
N2 C2 1.19(2) . ?

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
N1 Pb1 N1 72.0(3) . 5_576 ?
N1 Pb1 N1 94.4(4) 5_566 5_576 ?
N1 Pb1 N1 72.0(4) . 5_566 ?
N2 Pb1 N1 75.3(3) 1_565 5_576 ?
N2 Pb1 N1 75.3(3) . 5_566 ?
N2 Pb1 N1 77.7(3) . . ?
N2 Pb1 N1 77.7(3) 1_565 . ?
N2 Pb1 N1 149.7(4) 1_565 5_566 ?
N2 Pb1 N1 149.7(4) . 5_576 ?
N2 Pb1 N2 99.1(5) 1_565 . ?
Pb1 N1 Pb1 108.0(3) . 5_566 ?
Pb1 N1 Pb1 94.5(4) 5_566 5_576 ?
Pb1 N1 Pb1 108.0(3) . 5_576 ?
C1 N1 Pb1 105.8(10) . . ?
C1 N1 Pb1 119.8(6) . 5_566 ?
C1 N1 Pb1 119.8(6) . 5_576 ?
Pb1 N2 Pb1 99.1(5) 1_545 . ?
C2 N2 Pb1 130.4(2) . . ?
C2 N2 Pb1 130.4(2) . 1_545 ?
N1 C1 O1 176.8(17) . . ?
N2 C2 O2 178.8(17) . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT971_Pb_OCN2             
;
PROBLEM: Check Calcd Resid. Dens.  0.75Ang From Pb1             4.37 eA-3  
RESPONSE: The substance has a high absorption coefficient and the found residual
electron density can be treated as termination effects.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Pb_(SCN)2
_database_code_depnum_ccdc_archive 'CCDC 2383821'
loop_
_audit_author_name
_audit_author_address
'Frank Tambornino'
;Philipps University Marburg
Germany
;
_audit_update_record             
;
2024-09-13 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2022-09-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Frank.Tambornino@chemie.uni-marburg.de
_chemical_name_common            ?
_chemical_name_systematic        Pb(SCN)2
_chemical_formula_moiety         'C2 N2 Pb S2'
_chemical_formula_sum            'C2 N2 Pb S2'
_chemical_formula_weight         323.35
_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'
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'
S S 0.1246 0.1234 '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                   9.6128(9)
_cell_length_b                   6.5306(6)
_cell_length_c                   8.1913(7)
_cell_angle_alpha                90
_cell_angle_beta                 92.734(7)
_cell_angle_gamma                90
_cell_volume                     513.64(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14096
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.05
_shelx_estimated_absorpt_T_max   0.433
_shelx_estimated_absorpt_T_min   0.175
_exptl_absorpt_coefficient_mu    33.507
_exptl_absorpt_correction_T_max  0.0003
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             560
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0618
30 17 4 0.0728
16 13 30 0.0446
13 -14 30 0.0445
3 0 -5 0.0517
1 6 0 0.0995
1 1 30 0.0325
-4 -5 30 0.0407
-30 0 1 0.0526
-10 -6 1 0.0831
-16 -9 -30 0.0459
-17 11 -30 0.0449
-23 10 30 0.0688
-22 -5 30 0.0533
2 -30 1 0.0900
0 0 -1 0.0278

_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0084
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5951
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.488
_diffrn_reflns_theta_min         4.245
_diffrn_ambient_temperature      100
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
 540 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_diffrn_source_voltage           0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                763
_reflns_number_total             786
_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       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.81, Darmstadt 2018
;
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         1.026
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       0.00137(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         786
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0130
_refine_ls_R_factor_gt           0.0124
_refine_ls_restrained_S_all      1.168
_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)+(0.0219P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0303
_refine_ls_wR_factor_ref         0.0304
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_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 1.38980(2) 0.250000 0.01488(7) Uani 1 2 d S T P . .
S1 S 0.70778(7) 1.06024(11) 0.32902(9) 0.01913(13) Uani 1 1 d . . . . .
N1 N 0.5568(3) 0.7269(4) 0.4464(3) 0.0179(4) Uani 1 1 d . . . . .
C1 C 0.6186(3) 0.8666(4) 0.3988(3) 0.0163(5) 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
Pb1 S1 2.9862(7) . ?
Pb1 S1 3.1180(7) 3_455 ?
Pb1 S1 3.1180(7) 4_655 ?
Pb1 S1 2.9862(7) 2_655 ?
Pb1 N1 2.682(2) 6_575 ?
Pb1 N1 2.766(2) 1_565 ?
Pb1 N1 2.766(2) 2_665 ?
Pb1 N1 2.682(2) 5_676 ?
S1 C1 1.645(3) . ?
N1 C1 1.166(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
S1 Pb1 S1 87.77(3) 2_655 . ?
S1 Pb1 S1 72.686(12) . 4_655 ?
S1 Pb1 S1 144.31(2) 2_655 4_655 ?
S1 Pb1 S1 72.686(12) 2_655 3_455 ?
S1 Pb1 S1 138.17(3) 4_655 3_455 ?
S1 Pb1 S1 144.31(2) . 3_455 ?
N1 Pb1 S1 109.64(5) 1_565 . ?
N1 Pb1 S1 121.28(5) 6_575 3_455 ?
N1 Pb1 S1 75.99(5) 5_676 . ?
N1 Pb1 S1 144.22(5) 2_665 . ?
N1 Pb1 S1 75.52(5) 1_565 3_455 ?
N1 Pb1 S1 75.99(5) 6_575 2_655 ?
N1 Pb1 S1 80.36(5) 6_575 . ?
N1 Pb1 S1 80.36(5) 5_676 2_655 ?
N1 Pb1 S1 71.56(5) 5_676 3_455 ?
N1 Pb1 S1 144.22(5) 1_565 2_655 ?
N1 Pb1 S1 71.45(5) 2_665 3_455 ?
N1 Pb1 S1 75.52(5) 2_665 4_655 ?
N1 Pb1 S1 109.64(5) 2_665 2_655 ?
N1 Pb1 S1 71.56(5) 6_575 4_655 ?
N1 Pb1 S1 121.28(5) 5_676 4_655 ?
N1 Pb1 S1 71.45(5) 1_565 4_655 ?
N1 Pb1 N1 74.34(8) 6_575 2_665 ?
N1 Pb1 N1 74.34(8) 5_676 1_565 ?
N1 Pb1 N1 136.25(7) 6_575 1_565 ?
N1 Pb1 N1 136.25(7) 5_676 2_665 ?
N1 Pb1 N1 74.51(10) 1_565 2_665 ?
N1 Pb1 N1 146.98(11) 6_575 5_676 ?
Pb1 S1 Pb1 144.31(2) . 3_545 ?
C1 S1 Pb1 106.69(10) . 3_545 ?
C1 S1 Pb1 105.96(10) . . ?
Pb1 N1 Pb1 105.66(8) 5_676 1_545 ?
C1 N1 Pb1 131.5(2) . 5_676 ?
C1 N1 Pb1 121.2(2) . 1_545 ?
N1 C1 S1 178.7(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_asx021_180k_faces_pl
_database_code_depnum_ccdc_archive 'CCDC 2383823'
loop_
_audit_author_name
_audit_author_address
'Frank Tambornino'
;Philipps University Marburg
Germany
;
_audit_update_record             
;
2024-11-06 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2024-11-06
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
Frank.Tambornino@chemie.uni-marburg.de
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C2 H2 N2 O2 Pb2 Se2)'
_chemical_formula_sum            'C H N O Pb Se'
_chemical_formula_weight         329.18
_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'
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'
Se Se -0.0929 2.2259 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'

_cell_length_a                   8.6244(2)
_cell_length_b                   4.1674(4)
_cell_length_c                   11.5412(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     414.81(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    180.15
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.67
_shelx_estimated_absorpt_T_max   0.192
_shelx_estimated_absorpt_T_min   0.013
_exptl_absorpt_coefficient_mu    49.251
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_special_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    5.271
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11588
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.911
_diffrn_reflns_theta_min         2.949
_diffrn_ambient_temperature      180.15
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                719
_reflns_number_total             800
_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       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 1.72.0.0 (STOE, 2018)
X-Area LANA 1.71.6.0 (STOE, 2017)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         2.414
_refine_diff_density_min         -1.708
_refine_diff_density_rms         0.438
_refine_ls_extinction_coef       0.0183(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         800
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.084
_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)+(0.0387P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0555
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O1-H1
 0.9 with sigma of 0.02
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_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 0.37699(3) 0.750000 0.39124(2) 0.01653(11) Uani 1 2 d S T P . .
Se1 Se -0.09194(8) 0.750000 0.73560(6) 0.01793(17) Uani 1 2 d S T P . .
O1 O 0.6115(5) 0.750000 0.4966(5) 0.0175(9) Uani 1 2 d DS T P . .
N1 N 0.1520(7) 0.750000 0.5549(7) 0.0287(14) Uani 1 2 d S T P . .
C1 C 0.0541(8) 0.750000 0.6242(6) 0.0214(13) Uani 1 2 d S T P . .
H1 H 0.662(12) 0.750000 0.429(5) 0.05(3) Uiso 1 2 d DS . P . .


_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 O1 2.455(3) 5_676 ?
Pb1 O1 2.455(3) 5_666 ?
Pb1 N1 2.708(7) . ?
Se1 C1 1.800(7) . ?
O1 H1 0.90(2) . ?
N1 C1 1.163(10) . ?

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
O1 Pb1 O1 116.2(2) 5_676 5_666 ?
O1 Pb1 N1 70.21(12) 5_676 . ?
O1 Pb1 N1 70.21(12) 5_666 . ?
Pb1 O1 Pb1 116.2(2) 5_676 5_666 ?
Pb1 O1 H1 116(3) 5_676 . ?
Pb1 O1 H1 116(3) 5_666 . ?
C1 N1 Pb1 179.2(6) . . ?
N1 C1 Se1 177.8(7) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ax001
_database_code_depnum_ccdc_archive 'CCDC 2383822'
loop_
_audit_author_name
_audit_author_address
'Frank Tambornino'
;Philipps University Marburg
Germany
;
_audit_update_record             
;
2024-11-07 deposited with the CCDC.	2024-11-14 downloaded from the CCDC.
;
_audit_creation_date             2024-11-07
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C4 N4 Pb2 Se4)'
_chemical_formula_sum            'C2 N2 Pb Se2'
_chemical_formula_weight         417.15
_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'
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'
Se Se -0.0929 2.2259 '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           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   12.479(2)
_cell_length_b                   4.2277(9)
_cell_length_c                   10.6523(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     562.00(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22989
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.27
_cell_measurement_theta_min      1.91
_shelx_estimated_absorpt_T_max   0.223
_shelx_estimated_absorpt_T_min   0.100
_exptl_absorpt_coefficient_mu    42.835
_exptl_absorpt_correction_T_max  0.0001
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.930
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-3 -1 0 0.0300
1 -4 0 0.2180
5 2 0 0.0400
-1 3 0 0.2290
1 1 -5 0.0100
-1 -1 5 0.0180
-5 -5 -4 0.0700
4 4 1 0.0910

_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_size_rad          0.100
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12950
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.514
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
 540 frames, detector distance = 80 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           0.000
_diffrn_source_power             0.000
_diffrn_source_voltage           0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                850
_reflns_number_total             912
_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       
;
X-Area Recipe 2.0.1 (STOE, 2023)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.29.0 (STOE, 2023)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.15.0 (STOE, 2023)
X-Area LANA 2.7.12 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         4.056
_refine_diff_density_min         -1.950
_refine_diff_density_rms         0.458
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         912
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.142
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0684P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0948
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     iterative
_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 0.31208(2) 0.750000 0.71155(3) 0.02365(16) Uani 1 2 d S T P . .
Se1 Se 0.70319(7) 0.750000 0.50644(8) 0.0226(2) Uani 1 2 d S T P . .
Se2 Se 0.41539(7) 0.250000 0.87630(8) 0.0236(2) Uani 1 2 d S T P . .
N2 N 0.6397(7) 0.250000 0.7922(7) 0.0265(15) Uani 1 2 d S T P . .
N1 N 0.4905(6) 0.750000 0.6228(7) 0.0273(15) Uani 1 2 d S T P . .
C2 C 0.5546(7) 0.250000 0.8213(9) 0.0258(16) Uani 1 2 d S T P . .
C1 C 0.5732(7) 0.750000 0.5760(7) 0.0220(15) Uani 1 2 d S T P . .


_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 Se1 3.1459(8) 5_676 ?
Pb1 Se1 3.1459(8) 5_666 ?
Pb1 Se2 3.0348(8) 1_565 ?
Pb1 Se2 3.0349(7) . ?
Pb1 N1 2.419(8) . ?
Se1 C1 1.784(8) . ?
Se2 C2 1.833(10) . ?
N2 C2 1.107(13) . ?
N1 C1 1.145(11) . ?

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
Se1 Pb1 Se1 84.43(3) 5_666 5_676 ?
Se2 Pb1 Se1 157.01(3) 1_565 5_666 ?
Se2 Pb1 Se1 89.11(2) . 5_666 ?
Se2 Pb1 Se1 157.01(3) . 5_676 ?
Se2 Pb1 Se1 89.11(2) 1_565 5_676 ?
Se2 Pb1 Se2 88.30(3) 1_565 . ?
N1 Pb1 Se1 76.54(13) . 5_666 ?
N1 Pb1 Se1 76.54(13) . 5_676 ?
N1 Pb1 Se2 80.51(13) . . ?
N1 Pb1 Se2 80.51(13) . 1_565 ?
Pb1 Se1 Pb1 84.43(3) 5_666 5_676 ?
C1 Se1 Pb1 104.56(19) . 5_666 ?
C1 Se1 Pb1 104.56(18) . 5_676 ?
Pb1 Se2 Pb1 88.30(3) . 1_545 ?
C2 Se2 Pb1 102.6(2) . . ?
C2 Se2 Pb1 102.6(2) . 1_545 ?
C1 N1 Pb1 177.2(7) . . ?
N2 C2 Se2 177.7(9) . . ?
N1 C1 Se1 178.8(8) . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_STOE_detector_distance          '80.0 mm'
_STOE_detector_pixelsize_x       '0.150 mm'
_STOE_detector_pixelsize_y       '0.150 mm'
_STOE_detector_size_x            '34.0 cm'
_STOE_detector_size_y            '34.0 cm'
_STOE_evaluation_integration_A   21.4
_STOE_evaluation_integration_B   10.0
_STOE_evaluation_integration_EMS 0.020
_STOE_evaluation_LANA_BIS_l_even_max -
_STOE_evaluation_LANA_BIS_l_odd_max -
_STOE_evaluation_LANA_BOS_l_even_max 8
_STOE_evaluation_LANA_BOS_l_odd_max 5
_STOE_evaluation_LANA_completeness 99.8
_STOE_evaluation_LANA_DXS_max_order -
_STOE_evaluation_LANA_DYS_max_order -
_STOE_evaluation_LANA_FS_max_order 4
_STOE_evaluation_LANA_max_2theta_available 63.8
_STOE_evaluation_LANA_max_2theta_desired 63.8
_STOE_evaluation_LANA_mean_redundancy 14.1
_STOE_evaluation_LANA_number_refls_after_OR 15230
_STOE_evaluation_LANA_number_refls_outliers 4266
_STOE_evaluation_LANA_number_refls_total 19496
_STOE_evaluation_LANA_number_refls_unique 1081
_STOE_evaluation_LANA_number_refls_written 15230
_STOE_evaluation_LANA_OR_c1      0.035
_STOE_evaluation_LANA_OR_c2      0
_STOE_evaluation_LANA_OR_c3      0
_STOE_evaluation_LANA_OR_c4      0.7
_STOE_evaluation_LANA_point_group mmm
_STOE_evaluation_LANA_table      
;
#----------------------------------------------------------------------------
2Theta           8.0   14.6   21.2   27.8   34.4   41.0   47.6   54.2   60.8
#----------------------------------------------------------------------------
<Resolution>    4.55   2.79   1.92   1.47   1.20   1.01   0.88   0.78   0.70
N(total)         104    351    820   1378   1993   2746   3478   4239   4387
<Redundancy>     8.6   10.0   12.5   13.2   13.6   14.3   14.7   14.6   14.3
Complet. [%%]   100.0  100.0  100.0  100.0  100.0  100.0  100.0  100.0   99.2
<I/sigma>      232.5  318.9  136.6  105.9   56.1   38.3   20.7   11.9    6.6
R(int)         0.103  0.056  0.071  0.073  0.071  0.094  0.099  0.126  0.148
#----------------------------------------------------------------------------
;
_STOE_measurement_identifier     ax001
_STOE_measurement_max_exposure_per_frame '180.0 s'
_STOE_measurement_mean_exposure_per_frame '180.0 s'
_STOE_measurement_min_exposure_per_frame '180.0 s'
_STOE_measurement_total_exposure_time '27.0 h'
_STOE_measurement_total_frame_number 540
_STOE_measurement_total_run_number 3
_STOE_measurement_tube_power     '0.0 W'
# start Validation Reply Form
_vrf_PLAT971_ax001               
;
PROBLEM: Check Calcd Resid. Dens.  0.86Ang From Pb1             4.20 eA-3  
RESPONSE: The substance has a high absorption coefficient and the found residual
electron density can be treated as termination effects.
;
