# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_ZNZ2750_Ba_0m
_database_code_depnum_ccdc_archive 'CCDC 1964124'
loop_
_audit_author_name
_audit_author_address
'Wenjia Hao'
;SWUST
China
;
_audit_update_record             
;
2020-03-04 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H8 Ba N6 O7'
_chemical_formula_weight         377.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 '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'
Ba Ba -0.3132 6.7527 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.3803(3)
_cell_length_b                   15.7214(6)
_cell_length_c                   10.7123(4)
_cell_angle_alpha                90
_cell_angle_beta                 92.8860(10)
_cell_angle_gamma                90
_cell_volume                     1073.16(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    3217
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      50.17

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_F_000             720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    20.121
_shelx_estimated_absorpt_T_min   0.238
_shelx_estimated_absorpt_T_max   0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0240
_exptl_absorpt_correction_T_max  0.1417
_exptl_absorpt_process_details   
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     1.34139
_diffrn_radiation_type           GaK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12571
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.349
_diffrn_reflns_theta_max         52.976
_diffrn_reflns_theta_full        52.976
_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             1905
_reflns_number_gt                1828
_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-2018/3 (Sheldrick, 2018)'
_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)+(0.0595P)²+7.3031P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1905
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1202
_refine_ls_wR_factor_gt          0.1192
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_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
Ba1 Ba 0.60787(6) 0.51280(3) 0.81916(4) 0.0200(2) Uani 1 1 d . . . . .
O1 O 0.3689(9) 0.3255(3) 0.6022(5) 0.0312(13) Uani 1 1 d . . . . .
C1 C 0.6474(11) 0.2717(4) 0.6883(7) 0.0201(15) Uani 1 1 d . . . . .
O2 O 0.7645(10) 0.5415(4) 0.5870(5) 0.0361(14) Uani 1 1 d . . . . .
H2A H 0.734125 0.596054 0.558761 0.054 Uiso 1 1 d R U . . .
H2B H 0.698199 0.508041 0.525545 0.054 Uiso 1 1 d R U . . .
C2 C 0.8514(12) 0.2624(5) 0.7537(6) 0.0211(15) Uani 1 1 d . . . . .
N2 N 0.3500(10) 0.2389(4) 0.5832(6) 0.0248(14) Uani 1 1 d . . . . .
O3 O 0.5612(9) 0.1245(3) 0.6374(5) 0.0298(12) Uani 1 1 d . . . . .
C3 C 0.5232(11) 0.2051(4) 0.6362(6) 0.0176(14) Uani 1 1 d . . . . .
O4 O 0.9442(9) 0.4077(3) 0.7988(5) 0.0307(13) Uani 1 1 d . . . . .
N4 N 0.5518(10) 0.3445(4) 0.6686(6) 0.0285(15) Uani 1 1 d . . . . .
N5 N 0.9447(10) 0.1880(4) 0.7770(6) 0.0247(14) Uani 1 1 d . . . . .
O5 O 0.5102(8) 0.3663(3) 0.9798(5) 0.0270(12) Uani 1 1 d . . . . .
H5B H 0.392985 0.346279 0.952477 0.032 Uiso 1 1 d R U . . .
H5A H 0.605715 0.320039 0.988327 0.032 Uiso 1 1 d R U . . .
N6 N 1.1293(9) 0.2068(4) 0.8401(6) 0.0219(13) Uani 1 1 d . . . . .
O6 O 0.7796(9) 0.4955(3) 1.0626(5) 0.0216(11) Uani 1 1 d . . . . .
H6B H 0.683413 0.476143 1.106814 0.026 Uiso 1 1 d R U . . .
H6A H 0.900303 0.460993 1.078424 0.026 Uiso 1 1 d R U . . .
N7 N 1.1483(10) 0.2912(4) 0.8547(6) 0.0248(13) Uani 1 1 d . . . . .
O7 O 0.2391(10) 0.5322(5) 0.6506(6) 0.0418(15) Uani 1 1 d . . . . .
H7A H 0.123335 0.510749 0.685019 0.063 Uiso 1 1 d R U . . .
H7B H 0.206998 0.587928 0.639693 0.063 Uiso 1 1 d R U . . .
N8 N 0.9770(10) 0.3261(4) 0.8008(6) 0.0271(14) 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
Ba1 O4 2.726(5) . ?
Ba1 O2 2.763(6) . ?
Ba1 O3 2.767(5) 2_656 ?
Ba1 O6 2.790(5) . ?
Ba1 O6 2.837(6) 3_667 ?
Ba1 O7 2.909(6) . ?
Ba1 N5 2.953(6) 2_656 ?
Ba1 O5 2.960(5) . ?
Ba1 O5 2.997(5) 3_667 ?
Ba1 N4 3.110(6) . ?
Ba1 Ba1 4.1959(8) 3_667 ?
Ba1 H6B 2.064(6) 3_667 ?
O1 N4 1.369(8) . ?
O1 N2 1.380(8) . ?
C1 N4 1.309(10) . ?
C1 C3 1.411(10) . ?
C1 C2 1.453(10) . ?
O2 H2A 0.9270 . ?
O2 H2B 0.9278 . ?
C2 N5 1.331(10) . ?
C2 N8 1.364(10) . ?
N2 C3 1.328(9) . ?
O3 C3 1.291(9) . ?
O4 N8 1.300(8) . ?
N5 N6 1.360(8) . ?
O5 H5B 0.8500 . ?
O5 H5A 0.9501 . ?
N6 N7 1.341(9) . ?
O6 H6B 0.8500 . ?
O6 H6A 0.9500 . ?
N7 N8 1.328(9) . ?
O7 H7A 0.9070 . ?
O7 H7B 0.9067 . ?

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
O4 Ba1 O2 72.85(18) . . ?
O4 Ba1 O3 78.52(16) . 2_656 ?
O2 Ba1 O3 74.95(18) . 2_656 ?
O4 Ba1 O6 75.04(16) . . ?
O2 Ba1 O6 135.57(18) . . ?
O3 Ba1 O6 69.18(16) 2_656 . ?
O4 Ba1 O6 135.66(16) . 3_667 ?
O2 Ba1 O6 140.54(17) . 3_667 ?
O3 Ba1 O6 128.94(16) 2_656 3_667 ?
O6 Ba1 O6 83.58(17) . 3_667 ?
O4 Ba1 O7 128.99(17) . . ?
O2 Ba1 O7 75.05(19) . . ?
O3 Ba1 O7 128.64(19) 2_656 . ?
O6 Ba1 O7 149.05(18) . . ?
O6 Ba1 O7 65.56(18) 3_667 . ?
O4 Ba1 N5 127.84(18) . 2_656 ?
O2 Ba1 N5 64.78(18) . 2_656 ?
O3 Ba1 N5 62.58(16) 2_656 2_656 ?
O6 Ba1 N5 116.71(16) . 2_656 ?
O6 Ba1 N5 96.44(16) 3_667 2_656 ?
O7 Ba1 N5 67.16(19) . 2_656 ?
O4 Ba1 O5 76.37(16) . . ?
O2 Ba1 O5 138.28(16) . . ?
O3 Ba1 O5 125.24(15) 2_656 . ?
O6 Ba1 O5 57.64(14) . . ?
O6 Ba1 O5 59.41(14) 3_667 . ?
O7 Ba1 O5 104.78(18) . . ?
N5 Ba1 O5 154.78(16) 2_656 . ?
O4 Ba1 O5 132.02(15) . 3_667 ?
O2 Ba1 O5 131.19(16) . 3_667 ?
O3 Ba1 O5 72.19(15) 2_656 3_667 ?
O6 Ba1 O5 59.45(14) . 3_667 ?
O6 Ba1 O5 56.76(14) 3_667 3_667 ?
O7 Ba1 O5 98.91(16) . 3_667 ?
N5 Ba1 O5 68.34(16) 2_656 3_667 ?
O5 Ba1 O5 90.45(14) . 3_667 ?
O4 Ba1 N4 60.87(16) . . ?
O2 Ba1 N4 73.11(18) . . ?
O3 Ba1 N4 133.93(17) 2_656 . ?
O6 Ba1 N4 115.53(16) . . ?
O6 Ba1 N4 96.47(16) 3_667 . ?
O7 Ba1 N4 72.46(18) . . ?
N5 Ba1 N4 127.18(17) 2_656 . ?
O5 Ba1 N4 67.52(16) . . ?
O5 Ba1 N4 152.34(16) 3_667 . ?
O4 Ba1 Ba1 108.17(13) . 3_667 ?
O2 Ba1 Ba1 175.52(13) . 3_667 ?
O3 Ba1 Ba1 100.87(12) 2_656 3_667 ?
O6 Ba1 Ba1 42.21(11) . 3_667 ?
O6 Ba1 Ba1 41.36(11) 3_667 3_667 ?
O7 Ba1 Ba1 106.89(14) . 3_667 ?
N5 Ba1 Ba1 112.01(12) 2_656 3_667 ?
O5 Ba1 Ba1 45.58(10) . 3_667 ?
O5 Ba1 Ba1 44.87(10) 3_667 3_667 ?
N4 Ba1 Ba1 111.27(13) . 3_667 ?
O4 Ba1 H6B 144.03(18) . 3_667 ?
O2 Ba1 H6B 134.9(2) . 3_667 ?
O3 Ba1 H6B 125.18(18) 2_656 3_667 ?
O6 Ba1 H6B 88.16(19) . 3_667 ?
O6 Ba1 H6B 8.40(4) 3_667 3_667 ?
O7 Ba1 H6B 60.9(2) . 3_667 ?
N5 Ba1 H6B 88.10(18) 2_656 3_667 ?
O5 Ba1 H6B 67.81(17) . 3_667 ?
O5 Ba1 H6B 53.61(17) 3_667 3_667 ?
N4 Ba1 H6B 100.87(19) . 3_667 ?
Ba1 Ba1 H6B 46.35(15) 3_667 3_667 ?
N4 O1 N2 111.0(5) . . ?
N4 C1 C3 109.7(6) . . ?
N4 C1 C2 124.3(7) . . ?
C3 C1 C2 126.0(7) . . ?
Ba1 O2 H2A 111.5 . . ?
Ba1 O2 H2B 111.9 . . ?
H2A O2 H2B 102.3 . . ?
N5 C2 N8 109.1(6) . . ?
N5 C2 C1 124.0(7) . . ?
N8 C2 C1 126.9(7) . . ?
C3 N2 O1 105.5(6) . . ?
C3 O3 Ba1 140.0(5) . 2_646 ?
O3 C3 N2 123.3(6) . . ?
O3 C3 C1 128.5(7) . . ?
N2 C3 C1 108.1(6) . . ?
N8 O4 Ba1 136.4(5) . . ?
C1 N4 O1 105.7(6) . . ?
C1 N4 Ba1 128.3(5) . . ?
O1 N4 Ba1 121.9(4) . . ?
C2 N5 N6 105.6(6) . . ?
C2 N5 Ba1 135.4(5) . 2_646 ?
N6 N5 Ba1 117.2(4) . 2_646 ?
Ba1 O5 Ba1 89.55(14) . 3_667 ?
Ba1 O5 H5B 107.2 . . ?
Ba1 O5 H5B 103.5 3_667 . ?
Ba1 O5 H5A 119.9 . . ?
Ba1 O5 H5A 126.9 3_667 . ?
H5B O5 H5A 107.4 . . ?
N7 N6 N5 110.2(6) . . ?
Ba1 O6 Ba1 96.42(17) . 3_667 ?
Ba1 O6 H6B 107.2 . . ?
Ba1 O6 H6B 20.8 3_667 . ?
Ba1 O6 H6A 120.0 . . ?
Ba1 O6 H6A 127.7 3_667 . ?
H6B O6 H6A 107.3 . . ?
N8 N7 N6 106.9(6) . . ?
Ba1 O7 H7A 111.0 . . ?
Ba1 O7 H7B 110.6 . . ?
H7A O7 H7B 103.2 . . ?
O4 N8 N7 122.9(6) . . ?
O4 N8 C2 128.8(7) . . ?
N7 N8 C2 108.3(6) . . ?

_refine_diff_density_max         1.772
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.223

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1974773'
loop_
_audit_author_name
_audit_author_address
HaoWenjia
;Southwest University of Science and Technology
China
;
_audit_update_record             
;
2019-12-30 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;
_audit_creation_date             2019-12-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.5(C6 H8 N12 O10 Pb2)'
_chemical_formula_sum            'C3 H4 N6 O5 Pb'
_chemical_formula_weight         411.31
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
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'

_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                   12.7154(7)
_cell_length_b                   4.4053(2)
_cell_length_c                   14.5814(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.481(5)
_cell_angle_gamma                90
_cell_volume                     807.85(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1622
_cell_measurement_temperature    200.01(10)
_cell_measurement_theta_max      30.4790
_cell_measurement_theta_min      4.5910
_shelx_estimated_absorpt_T_max   0.188
_shelx_estimated_absorpt_T_min   0.117
_exptl_absorpt_coefficient_mu    20.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            1416
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.973
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00   0.00   1.00    5.00    --  -16.11 -38.00 -60.00   87
  2  ω    -75.00  12.00   1.00    5.00    --  -16.11 -57.00-150.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0476093000
_diffrn_orient_matrix_UB_12      -0.0100982000
_diffrn_orient_matrix_UB_13      -0.0198037000
_diffrn_orient_matrix_UB_21      0.0291212000
_diffrn_orient_matrix_UB_22      -0.0280087000
_diffrn_orient_matrix_UB_23      0.0445088000
_diffrn_orient_matrix_UB_31      -0.0081812000
_diffrn_orient_matrix_UB_32      -0.1582619000
_diffrn_orient_matrix_UB_33      -0.0066246000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                732
_reflns_number_total             737
_reflns_odcompleteness_completeness 98.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.135
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         737
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0174
_refine_ls_restrained_S_all      0.959
_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)+(0.0269P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0419
_refine_ls_wR_factor_ref         0.0421
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Shared sites
{N1, C33}
{N3, O4}
2. Restrained distances
 O1W-H1WA
 0.86 with sigma of 0.02
 O1W-H1WB
 0.86 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(C33)
Uanis(N3) = Uanis(O4)
4. Others
 Fixed Sof: N1(0.5) N3(0.5) C33(0.5) O4(0.5)
;
_atom_sites_solution_hydrogens   difmap
_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 0.5000 0.22306(5) 0.2500 0.01200(11) Uani 1 2 d S T P A .
O1 O 0.5482(3) 0.7247(6) 0.3412(3) 0.0172(8) Uani 1 1 d . . . . .
O1W O 0.2898(3) 0.2097(8) 0.2133(3) 0.0216(9) Uani 1 1 d D . . . .
H1WA H 0.256(5) 0.350(13) 0.239(5) 0.06(2) Uiso 1 1 d D . . . .
H1WB H 0.273(7) 0.219(11) 0.1539(16) 0.05(3) Uiso 1 1 d D . . . .
N1 N 0.5787(4) 0.7614(7) 0.4300(4) 0.0117(10) Uani 0.5 1 d . . . A 1
N2 N 0.6503(3) 0.9667(8) 0.4644(2) 0.0152(8) Uani 1 1 d . . . . .
N3 N 0.6565(2) 0.9469(8) 0.5583(2) 0.0174(7) Uani 0.5 1 d . . . A 3
N4 N 0.5887(4) 0.7306(7) 0.5825(4) 0.0171(10) Uani 1 1 d . . . . .
C1 C 0.5408(3) 0.6162(10) 0.5038(3) 0.0119(8) Uani 1 1 d . . . . .
C33 C 0.5787(4) 0.7614(7) 0.4300(4) 0.0117(10) Uani 0.5 1 d . . . A 2
O4 O 0.6565(2) 0.9469(8) 0.5583(2) 0.0174(7) Uani 0.5 1 d . . . A 4


_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 2.593(3) 2_645 ?
Pb1 O1 2.593(3) 1_545 ?
Pb1 O1 2.605(3) . ?
Pb1 O1 2.605(3) 2_655 ?
Pb1 O1W 2.647(4) . ?
Pb1 O1W 2.647(4) 2_655 ?
O1 Pb1 2.593(3) 1_565 ?
O1 N1 1.305(7) . ?
O1W H1WA 0.87(2) . ?
O1W H1WB 0.86(2) . ?
N1 N2 1.329(6) . ?
N1 C1 1.398(6) . ?
N2 N3 1.362(5) . ?
N3 N4 1.367(5) . ?
N4 C1 1.317(6) . ?
C1 C1 1.450(8) 5_666 ?

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 64.29(16) 2_645 1_545 ?
O1 Pb1 O1 179.83(6) 1_545 2_655 ?
O1 Pb1 O1 115.88(15) 2_645 2_655 ?
O1 Pb1 O1 115.88(15) 1_545 . ?
O1 Pb1 O1 179.83(6) 2_645 . ?
O1 Pb1 O1 63.95(16) 2_655 . ?
O1 Pb1 O1W 76.20(12) . 2_655 ?
O1 Pb1 O1W 73.90(12) 1_545 2_655 ?
O1 Pb1 O1W 103.88(12) 1_545 . ?
O1 Pb1 O1W 103.88(12) 2_645 2_655 ?
O1 Pb1 O1W 76.20(12) 2_655 . ?
O1 Pb1 O1W 106.03(12) . . ?
O1 Pb1 O1W 73.90(12) 2_645 . ?
O1 Pb1 O1W 106.03(12) 2_655 2_655 ?
O1W Pb1 O1W 177.46(15) . 2_655 ?
Pb1 O1 Pb1 115.88(15) 1_565 . ?
N1 O1 Pb1 128.6(2) . . ?
N1 O1 Pb1 114.6(2) . 1_565 ?
Pb1 O1W H1WA 117(5) . . ?
Pb1 O1W H1WB 107(6) . . ?
H1WA O1W H1WB 109(6) . . ?
O1 N1 N2 123.1(4) . . ?
O1 N1 C1 128.4(4) . . ?
N2 N1 C1 108.4(4) . . ?
N2 N3 N4 111.1(3) . . ?
C1 N4 N3 105.6(4) . . ?
N1 C1 C1 126.0(5) . 5_666 ?
N4 C1 N1 109.2(4) . . ?
N4 C1 C1 124.8(5) . 5_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.979
_oxdiff_exptl_absorpt_empirical_full_min 0.576
