# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_MOF
_database_code_depnum_ccdc_archive 'CCDC 1905924'
loop_
_audit_author_name
_audit_author_address
'Giannis Papaefstathiou'
;National and Kapodistrian University of Athens
Greece
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-28 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            'C9 H4 N O6 Pb'
_chemical_formula_weight         429.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   4.1673(2)
_cell_length_b                   25.707(2)
_cell_length_c                   18.2223(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1952.2(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    106.6(2)
_cell_measurement_reflns_used    1628
_cell_measurement_theta_min      4.1610
_cell_measurement_theta_max      72.5850

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.922
_exptl_crystal_F_000             1560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    33.853
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.44457
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      106.6(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            6617
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_av_R_equivalents  0.0603
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         4.209
_diffrn_reflns_theta_max         66.964
_diffrn_reflns_theta_full        66.964
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 0.987
_reflns_number_total             1708
_reflns_number_gt                1053
_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       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT, (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1820P)²+12.2758P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00063(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1708
_refine_ls_number_parameters     157
_refine_ls_number_restraints     75
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0870
_refine_ls_wR_factor_ref         0.3049
_refine_ls_wR_factor_gt          0.2808
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.129
_refine_ls_shift/su_max          0.000
_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
Pb2 Pb 0.000000 0.76032(4) 0.750000 0.0387(7) Uani 1 2 d S TU P . .
Pb1 Pb 1.000000 0.55704(8) 0.250000 0.0718(8) Uani 1 2 d S TU P . .
O4 O 0.557(4) 0.7445(6) 0.6601(9) 0.046(4) Uani 1 1 d . U . . .
O3 O -0.024(4) 0.5307(6) 0.5854(8) 0.056(4) Uani 1 1 d . . . . .
C6 C 0.693(4) 0.6980(9) 0.5262(9) 0.047(5) Uani 1 1 d D . . . .
H6 H 0.795295 0.729259 0.536800 0.057 Uiso 1 1 calc R U . . .
O2 O 0.492(5) 0.5612(7) 0.3434(11) 0.075(7) Uani 1 1 d . . . . .
C3 C 0.380(5) 0.6025(6) 0.4938(9) 0.043(5) Uani 1 1 d D . . . .
C7 C 0.736(5) 0.6741(8) 0.4565(9) 0.046(5) Uani 1 1 d D U . . .
H7 H 0.869766 0.689127 0.421591 0.056 Uiso 1 1 calc R U . . .
C9 C 0.054(5) 0.5208(9) 0.5181(15) 0.049(5) Uani 1 1 d . U . . .
N1 N 0.248(5) 0.5534(6) 0.4790(9) 0.049(4) Uani 1 1 d D U . . .
H1 H 0.300338 0.541370 0.436663 0.059 Uiso 1 1 calc R U . . .
C2 C 0.572(5) 0.6272(7) 0.4413(11) 0.053(6) Uani 1 1 d D U . . .
C4 C 0.350(5) 0.6264(6) 0.5618(10) 0.039(4) Uani 1 1 d D . . . .
H4 H 0.227854 0.609775 0.597541 0.047 Uiso 1 1 calc R U . . .
C5 C 0.493(4) 0.6742(7) 0.5798(9) 0.042(4) Uani 1 1 d D . . . .
C8 C 0.420(6) 0.7025(8) 0.6462(11) 0.050(5) Uani 1 1 d D U . . .
C1 C 0.604(9) 0.6077(12) 0.3679(13) 0.075(8) Uani 1 1 d D U . . .
O5 O 0.193(4) 0.6853(6) 0.6853(7) 0.049(3) Uani 1 1 d . U . . .
O1 O 0.842(7) 0.6285(8) 0.3215(11) 0.086(6) Uani 1 1 d . U . . .
O6 O 0.500000 0.5712(11) 0.750000 0.066(8) Uani 1 2 d S TU P A 1
O7 O 0.500000 0.5428(13) 0.750000 0.079(9) Uani 1 2 d S TU 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
Pb2 O5 2.399(13) . ?
Pb2 O5 2.399(14) 3_556 ?
Pb2 O4 2.500(14) 1_455 ?
Pb2 O4 2.500(14) 3_656 ?
Pb1 O1 2.35(2) . ?
Pb1 O1 2.35(2) 3_755 ?
Pb1 O2 2.67(2) 1_655 ?
Pb1 O2 2.67(2) 3_655 ?
Pb1 O2 2.72(2) 3_755 ?
Pb1 O2 2.72(2) . ?
O4 C8 1.25(3) . ?
O3 C9 1.29(3) . ?
C6 C5 1.421(17) . ?
C6 C7 1.422(17) . ?
C6 H6 0.9300 . ?
O2 C1 1.36(3) . ?
C3 C4 1.388(16) . ?
C3 C2 1.401(18) . ?
C3 N1 1.403(17) . ?
C7 C2 1.414(17) . ?
C7 H7 0.9300 . ?
C9 C9 1.33(5) 5_566 ?
C9 N1 1.37(3) . ?
N1 H1 0.8600 . ?
C2 C1 1.435(19) . ?
C4 C5 1.404(17) . ?
C4 H4 0.9300 . ?
C5 C8 1.445(17) . ?
C8 O5 1.26(3) . ?
C1 O1 1.41(3) . ?
O6 O7 0.73(3) . ?

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
O5 Pb2 O5 73.1(7) . 3_556 ?
O5 Pb2 O4 78.2(5) . 1_455 ?
O5 Pb2 O4 86.8(5) 3_556 1_455 ?
O5 Pb2 O4 86.8(5) . 3_656 ?
O5 Pb2 O4 78.2(5) 3_556 3_656 ?
O4 Pb2 O4 161.3(8) 1_455 3_656 ?
O1 Pb1 O1 77.0(10) . 3_755 ?
O1 Pb1 O2 80.2(8) . 1_655 ?
O1 Pb1 O2 96.1(8) 3_755 1_655 ?
O1 Pb1 O2 96.1(8) . 3_655 ?
O1 Pb1 O2 80.2(8) 3_755 3_655 ?
O2 Pb1 O2 175.4(8) 1_655 3_655 ?
O1 Pb1 O2 122.4(7) . 3_755 ?
O1 Pb1 O2 53.3(7) 3_755 3_755 ?
O2 Pb1 O2 78.4(7) 1_655 3_755 ?
O2 Pb1 O2 101.4(7) 3_655 3_755 ?
O1 Pb1 O2 53.3(7) . . ?
O1 Pb1 O2 122.4(7) 3_755 . ?
O2 Pb1 O2 101.4(7) 1_655 . ?
O2 Pb1 O2 78.4(7) 3_655 . ?
O2 Pb1 O2 175.4(8) 3_755 . ?
C8 O4 Pb2 127.8(15) . 1_655 ?
C5 C6 C7 120.1(19) . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C1 O2 Pb1 120.7(19) . 1_455 ?
C1 O2 Pb1 88.4(16) . . ?
Pb1 O2 Pb1 101.4(7) 1_455 . ?
C4 C3 C2 117.5(17) . . ?
C4 C3 N1 122.3(16) . . ?
C2 C3 N1 120.0(16) . . ?
C2 C7 C6 118.9(19) . . ?
C2 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
O3 C9 C9 123(3) . 5_566 ?
O3 C9 N1 121(2) . . ?
C9 C9 N1 116(3) 5_566 . ?
C9 N1 C3 133.2(18) . . ?
C9 N1 H1 113.4 . . ?
C3 N1 H1 113.4 . . ?
C3 C2 C7 121.9(18) . . ?
C3 C2 C1 122(2) . . ?
C7 C2 C1 115.9(19) . . ?
C3 C4 C5 123.8(18) . . ?
C3 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C4 C5 C6 117.8(17) . . ?
C4 C5 C8 123.1(17) . . ?
C6 C5 C8 118.7(17) . . ?
O4 C8 O5 122.0(18) . . ?
O4 C8 C5 121(2) . . ?
O5 C8 C5 117.0(19) . . ?
O2 C1 O1 112(2) . . ?
O2 C1 C2 126(2) . . ?
O1 C1 C2 119(2) . . ?
C8 O5 Pb2 104.4(12) . . ?
C1 O1 Pb1 103.5(15) . . ?

_refine_diff_density_max         3.674
_refine_diff_density_min         -3.237
_refine_diff_density_rms         0.407


# start Validation Reply Form

_vrf_PLAT973_Pb_MOF              
;
RESPONSE: The alert was mainly due to the existence of electron density around
the metal centers that not assigned to any element. Thus, such residual 
density is likely not from unaccounted atom types.
;
_vrf_PLAT972_Pb_MOF              
;
RESPONSE: The alert was mainly due to the existence of electron density around
the metal centers and oxygen atoms that not assigned to any element. Thus, such residual
density is likely not from unaccounted atom types.
;
_vrf_PLAT971_Pb_MOF              
;
RESPONSE: The alert was mainly due to the existence of electron density around
the metal centers and oxygen atoms that not assigned to any element. Thus, such residual
density is likely not from unaccounted atom types.
;
_vrf_PLAT342_Pb_MOF              
;
RESPONSE: This alert is generated because of a large amount of disorder in 
the structure.
;
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1905925'
loop_
_audit_author_name
_audit_author_address
'Giannis Papaefstathiou'
;National and Kapodistrian University of Athens
Greece
;
_audit_update_record             
;
2019-03-27 deposited with the CCDC.	2019-05-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 N4 Ni O16'
_chemical_formula_sum            'C24 H20 N4 Ni O16'
_chemical_formula_weight         679.13

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   21.7280(9)
_cell_length_b                   10.3246(4)
_cell_length_c                   13.1378(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.983(4)
_cell_angle_gamma                90
_cell_volume                     2911.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3934
_cell_measurement_theta_min      4.6810
_cell_measurement_theta_max      73.2580

_exptl_crystal_description       polyhedra
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    1.716
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78204
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.436
_oxdiff_exptl_absorpt_empirical_full_max 2.406
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.4223
_diffrn_reflns_number            8800
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.120
_diffrn_reflns_theta_max         73.375
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2891
_reflns_number_gt                2494
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0955P)²+4.2718P] 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         2891
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1508
_refine_ls_wR_factor_gt          0.1426
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_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
NI1 Ni 0.500000 0.000000 1.000000 0.0160(2) Uani 1 2 d S . P . .
N1 N 0.46258(9) 0.40638(19) 0.89518(14) 0.0180(4) Uani 1 1 d . . . . .
N2 N 0.28219(11) 0.9961(2) 0.3432(2) 0.0314(6) Uani 1 1 d . . . . .
O1 O 0.42065(8) 0.04001(16) 0.76779(12) 0.0218(4) Uani 1 1 d . . . . .
O2 O 0.46831(8) 0.15295(15) 0.90199(12) 0.0184(4) Uani 1 1 d . . . . .
O3 O 0.47771(9) 0.62627(16) 0.91347(13) 0.0243(4) Uani 1 1 d . . . . .
O4 O 0.32761(9) 0.58393(18) 0.48120(13) 0.0266(4) Uani 1 1 d . . . . .
O5 O 0.36980(9) 0.71596(17) 0.60768(14) 0.0277(4) Uani 1 1 d . . . . .
O6 O 0.43580(8) -0.12548(16) 0.92279(12) 0.0218(4) Uani 1 1 d . . . . .
O7 O 0.43345(9) 0.05687(17) 1.08516(13) 0.0249(4) Uani 1 1 d . . . . .
O8 O 0.29724(9) 0.78117(19) 0.36868(14) 0.0310(4) Uani 1 1 d . . . . .
C1 C 0.43770(11) 0.1452(2) 0.81104(17) 0.0170(5) Uani 1 1 d . . . . .
C2 C 0.42036(10) 0.2691(2) 0.75171(16) 0.0168(5) Uani 1 1 d . . . . .
C3 C 0.43090(11) 0.3947(2) 0.79330(16) 0.0164(5) Uani 1 1 d . . . . .
C4 C 0.41051(11) 0.5027(2) 0.73438(18) 0.0176(5) Uani 1 1 d . . . . .
H4 H 0.417021 0.585098 0.762637 0.021 Uiso 1 1 calc R U . . .
C5 C 0.38037(11) 0.4885(2) 0.63329(18) 0.0181(5) Uani 1 1 d . . . . .
C6 C 0.37184(11) 0.3649(2) 0.58977(17) 0.0202(5) Uani 1 1 d . . . . .
H6 H 0.353229 0.354799 0.521526 0.024 Uiso 1 1 calc R U . . .
C7 C 0.39136(11) 0.2580(2) 0.64934(17) 0.0193(5) Uani 1 1 d . . . . .
H7 H 0.385017 0.175919 0.620417 0.023 Uiso 1 1 calc R U . . .
C8 C 0.35912(11) 0.6079(2) 0.57327(18) 0.0202(5) Uani 1 1 d . . . . .
C9 C 0.48285(11) 0.5144(2) 0.94504(17) 0.0186(5) Uani 1 1 d . . . . .
C10 C 0.29797(12) 0.8936(3) 0.4012(2) 0.0288(6) Uani 1 1 d . . . . .
H10 H 0.310501 0.906691 0.471396 0.035 Uiso 1 1 calc R U . . .
C11 C 0.28617(16) 1.1262(3) 0.3862(4) 0.0544(10) Uani 1 1 d . . . . .
H11A H 0.272823 1.187775 0.332539 0.082 Uiso 1 1 calc R U . . .
H11B H 0.259837 1.132475 0.438272 0.082 Uiso 1 1 calc R U . . .
H11C H 0.328471 1.144208 0.416209 0.082 Uiso 1 1 calc R U . . .
C12 C 0.26358(18) 0.9846(3) 0.2329(3) 0.0443(8) Uani 1 1 d . . . . .
H12A H 0.253870 1.068835 0.203855 0.066 Uiso 1 1 calc R U . . .
H12B H 0.297032 0.947313 0.202875 0.066 Uiso 1 1 calc R U . . .
H12C H 0.227496 0.929980 0.218831 0.066 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
NI1 O7 2.0476(17) 5_657 ?
NI1 O7 2.0476(17) . ?
NI1 O6 2.0520(17) 5_657 ?
NI1 O6 2.0521(17) . ?
NI1 O2 2.0854(15) . ?
NI1 O2 2.0854(15) 5_657 ?
N1 C9 1.333(3) . ?
N1 C3 1.411(3) . ?
N2 C10 1.318(4) . ?
N2 C12 1.447(4) . ?
N2 C11 1.454(4) . ?
O1 C1 1.255(3) . ?
O2 C1 1.276(3) . ?
O3 C9 1.227(3) . ?
O4 C8 1.317(3) . ?
O5 C8 1.212(3) . ?
O8 C10 1.236(4) . ?
C1 C2 1.515(3) . ?
C2 C7 1.398(3) . ?
C2 C3 1.412(3) . ?
C3 C4 1.390(3) . ?
C4 C5 1.394(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.399(3) . ?
C5 C8 1.497(3) . ?
C6 C7 1.381(3) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
C9 C9 1.547(4) 5_667 ?
C10 H10 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

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
O7 NI1 O7 180.00(6) 5_657 . ?
O7 NI1 O6 88.14(7) 5_657 5_657 ?
O7 NI1 O6 91.86(7) . 5_657 ?
O7 NI1 O6 91.86(7) 5_657 . ?
O7 NI1 O6 88.14(7) . . ?
O6 NI1 O6 180.0 5_657 . ?
O7 NI1 O2 94.19(7) 5_657 . ?
O7 NI1 O2 85.81(7) . . ?
O6 NI1 O2 87.74(6) 5_657 . ?
O6 NI1 O2 92.26(6) . . ?
O7 NI1 O2 85.81(7) 5_657 5_657 ?
O7 NI1 O2 94.19(7) . 5_657 ?
O6 NI1 O2 92.26(6) 5_657 5_657 ?
O6 NI1 O2 87.74(6) . 5_657 ?
O2 NI1 O2 180.0 . 5_657 ?
C9 N1 C3 127.8(2) . . ?
C10 N2 C12 121.3(3) . . ?
C10 N2 C11 121.5(3) . . ?
C12 N2 C11 117.1(3) . . ?
C1 O2 NI1 127.18(14) . . ?
O1 C1 O2 123.5(2) . . ?
O1 C1 C2 117.8(2) . . ?
O2 C1 C2 118.71(19) . . ?
C7 C2 C3 118.0(2) . . ?
C7 C2 C1 117.7(2) . . ?
C3 C2 C1 124.3(2) . . ?
C4 C3 N1 121.7(2) . . ?
C4 C3 C2 120.2(2) . . ?
N1 C3 C2 118.1(2) . . ?
C3 C4 C5 120.5(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 C8 118.4(2) . . ?
C6 C5 C8 121.7(2) . . ?
C7 C6 C5 119.2(2) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
C6 C7 C2 122.1(2) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
O5 C8 O4 123.9(2) . . ?
O5 C8 C5 122.4(2) . . ?
O4 C8 C5 113.7(2) . . ?
O3 C9 N1 128.0(2) . . ?
O3 C9 C9 120.1(3) . 5_667 ?
N1 C9 C9 111.9(2) . 5_667 ?
O8 C10 N2 124.5(3) . . ?
O8 C10 H10 117.8 . . ?
N2 C10 H10 117.8 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

_refine_diff_density_max         0.949
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.087


# start Validation Reply Form

_vrf_PLAT430_shelx               
;
RESPONSE: This alert is generated because there is a large amount of disorder 
in the structure.
;
# end Validation Reply Form
