# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_bpy4dca
_database_code_depnum_ccdc_archive 'CCDC 2151937'
loop_
_audit_author_name
_audit_author_address
'Lauren Hatcher'
;Cardiff University
United Kingdom
;
_audit_update_record             
;
2022-02-14 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        "dimethyl 2,2'-bipyridine-4,4'-dicarboxylate"
_chemical_name_common            bpy4dc
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N2 O4'
_chemical_formula_sum            'C14 H12 N2 O4'
_chemical_formula_weight         272.26

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   3.8010(2)
_cell_length_b                   5.8557(3)
_cell_length_c                   27.5948(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.720(4)
_cell_angle_gamma                90
_cell_volume                     612.90(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2159
_cell_measurement_theta_min      4.1330
_cell_measurement_theta_max      29.4780

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.110
_shelx_estimated_absorpt_T_min   0.947
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_T_min  0.79808
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            3721
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.557
_diffrn_reflns_theta_max         26.359
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             1251
_reflns_number_gt                1103
_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 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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)+(0.0502P)²+0.2853P] 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         1251
_refine_ls_number_parameters     92
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1066
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
O1 O 0.7895(3) 0.33378(19) 0.65943(4) 0.0291(3) Uani 1 1 d . . . . .
O2 O 0.6313(3) 0.6610(2) 0.69412(4) 0.0357(4) Uani 1 1 d . . . . .
N1 N 0.3024(3) 0.7664(2) 0.51599(4) 0.0212(3) Uani 1 1 d . . . . .
C1 C 0.2541(4) 0.8931(3) 0.55525(6) 0.0228(4) Uani 1 1 d . . . . .
H1 H 0.135722 1.035216 0.550945 0.027 Uiso 1 1 calc R U . . .
C2 C 0.3679(4) 0.8279(3) 0.60196(5) 0.0225(4) Uani 1 1 d . . . . .
H2 H 0.333807 0.924672 0.628898 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5329(4) 0.6177(3) 0.60834(5) 0.0198(3) Uani 1 1 d . . . . .
C4 C 0.5853(4) 0.4841(2) 0.56800(5) 0.0196(3) Uani 1 1 d . . . . .
H4 H 0.697250 0.339458 0.571404 0.024 Uiso 1 1 calc R U . . .
C5 C 0.4706(4) 0.5665(2) 0.52237(5) 0.0184(3) Uani 1 1 d . . . . .
C6 C 0.6544(4) 0.5445(3) 0.65868(5) 0.0228(4) Uani 1 1 d . . . . .
C7 C 0.9181(5) 0.2498(3) 0.70672(6) 0.0319(4) Uani 1 1 d . . . . .
H7A H 1.006872 0.093726 0.703530 0.048 Uiso 1 1 calc R U . . .
H7B H 0.725400 0.250192 0.728656 0.048 Uiso 1 1 calc R U . . .
H7C H 1.108998 0.348613 0.719959 0.048 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
O1 C6 1.3362(19) . ?
O1 C7 1.4497(18) . ?
O2 C6 1.2004(18) . ?
N1 C1 1.3354(19) . ?
N1 C5 1.3401(19) . ?
C1 C2 1.386(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.385(2) . ?
C3 C6 1.498(2) . ?
C4 C5 1.392(2) . ?
C4 H4 0.9500 . ?
C5 C5 1.489(3) 3_666 ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

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
C6 O1 C7 115.73(12) . . ?
C1 N1 C5 117.91(12) . . ?
N1 C1 C2 123.41(14) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.23(14) . . ?
C1 C2 H2 120.9 . . ?
C3 C2 H2 120.9 . . ?
C4 C3 C2 119.10(13) . . ?
C4 C3 C6 122.15(14) . . ?
C2 C3 C6 118.75(13) . . ?
C3 C4 C5 118.59(14) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 122.71(13) . . ?
N1 C5 C5 116.35(15) . 3_666 ?
C4 C5 C5 120.94(16) . 3_666 ?
O2 C6 O1 124.10(14) . . ?
O2 C6 C3 123.96(14) . . ?
O1 C6 C3 111.94(13) . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 C2 -0.2(2) . . . . ?
N1 C1 C2 C3 -1.6(2) . . . . ?
C1 C2 C3 C4 1.6(2) . . . . ?
C1 C2 C3 C6 -179.52(13) . . . . ?
C2 C3 C4 C5 0.1(2) . . . . ?
C6 C3 C4 C5 -178.75(13) . . . . ?
C1 N1 C5 C4 2.0(2) . . . . ?
C1 N1 C5 C5 -178.11(15) . . . 3_666 ?
C3 C4 C5 N1 -2.0(2) . . . . ?
C3 C4 C5 C5 178.16(15) . . . 3_666 ?
C7 O1 C6 O2 -1.1(2) . . . . ?
C7 O1 C6 C3 179.29(12) . . . . ?
C4 C3 C6 O2 175.66(15) . . . . ?
C2 C3 C6 O2 -3.2(2) . . . . ?
C4 C3 C6 O1 -4.7(2) . . . . ?
C2 C3 C6 O1 176.42(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1 N1 0.95 2.67 3.4315(19) 137.4 3_576 yes
C7 H7B O2 0.98 2.65 3.586(2) 159.7 2_646 yes

_refine_diff_density_max         0.214
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.048


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: dichloromethane'
####################################################################### 
# 
# 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_Poly1_2h-470nm_150K
_database_code_depnum_ccdc_archive 'CCDC 2151943'
loop_
_audit_author_name
_audit_author_address
'Lauren Hatcher'
;Cardiff University
United Kingdom
;
_audit_update_record             
;
2022-02-14 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT026_Poly1_2h-470nm_150K 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 32% Check
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
_vrf_PLAT084_Poly1_2h-470nm_150K 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.36 Report
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
_vrf_PLAT250_Poly1_2h-470nm_150K 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.6 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT342_Poly1_2h-470nm_150K 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.04 Ang.
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT910_Poly1_2h-470nm_150K 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 16 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
Dinitro-(dimethyl 2,2'-bipyridine-4,4'-dicarboxylate)palladium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N4 O8 Pd'
_chemical_formula_sum            'C14 H12 N4 O8 Pd'
_chemical_formula_weight         470.68

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.458(3)
_cell_length_b                   13.861(4)
_cell_length_c                   15.612(5)
_cell_angle_alpha                63.83(3)
_cell_angle_beta                 83.71(3)
_cell_angle_gamma                79.31(3)
_cell_volume                     1613.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    608
_cell_measurement_theta_min      3.7370
_cell_measurement_theta_max      30.9740

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.207
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.53335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6212
_diffrn_reflns_av_unetI/netI     0.4078
_diffrn_reflns_av_R_equivalents  0.1675
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.372
_diffrn_reflns_theta_max         25.396
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.982
_reflns_number_total             6212
_reflns_number_gt                2011
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1839P)²] 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         6212
_refine_ls_number_parameters     484
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.2688
_refine_ls_R_factor_gt           0.1242
_refine_ls_wR_factor_ref         0.3641
_refine_ls_wR_factor_gt          0.3002
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.871
_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
Pd1 Pd 0.5473(3) 0.4242(2) 0.26190(17) 0.0518(8) Uani 1 1 d . . . . .
O5 O 0.223(2) 0.0386(16) 0.6708(13) 0.051(4) Uani 1 1 d . . . . .
O6 O 0.181(3) 0.1761(16) 0.7110(14) 0.050(4) Uani 1 1 d . . . . .
O7 O 0.462(3) 0.0025(16) 0.1490(13) 0.055(5) Uani 1 1 d . . . . .
O8 O 0.395(2) -0.0656(15) 0.3040(13) 0.040(3) Uani 1 1 d . . . . .
N3 N 0.522(3) 0.293(2) 0.2445(17) 0.048(2) Uani 1 1 d . . . . .
N4 N 0.425(3) 0.3426(19) 0.3846(16) 0.039(2) Uani 1 1 d . . . . .
C1 C 0.389(3) 0.378(2) 0.4567(18) 0.033(4) Uani 1 1 d . . . . .
H1 H 0.404607 0.448844 0.444670 0.039 Uiso 1 1 calc R U . . .
C2 C 0.329(3) 0.311(2) 0.5458(19) 0.031(3) Uani 1 1 d . . . . .
H2 H 0.315208 0.332125 0.596400 0.037 Uiso 1 1 calc R U . . .
C3 C 0.290(3) 0.209(2) 0.5603(18) 0.028(3) Uani 1 1 d . . . . .
C4 C 0.333(3) 0.174(2) 0.4829(19) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.311597 0.106213 0.488627 0.046 Uiso 1 1 calc R U . . .
C5 C 0.405(3) 0.243(2) 0.403(2) 0.040(3) Uani 1 1 d . . . . .
C6 C 0.458(3) 0.218(2) 0.3158(19) 0.034(3) Uani 1 1 d . . . . .
C7 C 0.417(3) 0.121(2) 0.3161(18) 0.027(3) Uani 1 1 d . . . . .
H7 H 0.361619 0.071563 0.369073 0.033 Uiso 1 1 calc R U . . .
C8 C 0.461(3) 0.103(2) 0.2385(19) 0.033(3) Uani 1 1 d . . . . .
C9 C 0.537(3) 0.185(2) 0.1583(18) 0.031(3) Uani 1 1 d . . . . .
H9 H 0.569030 0.172967 0.102851 0.037 Uiso 1 1 calc R U . . .
C10 C 0.567(3) 0.284(2) 0.1608(17) 0.024(3) Uani 1 1 d . . . . .
H10 H 0.613287 0.339378 0.107905 0.028 Uiso 1 1 calc R U . . .
C11 C 0.228(3) 0.125(2) 0.6572(18) 0.030(3) Uani 1 1 d . . . . .
C12 C 0.117(3) 0.110(2) 0.8040(19) 0.038(5) Uani 1 1 d . . . . .
H12A H 0.011287 0.094513 0.797443 0.056 Uiso 1 1 calc R U . . .
H12B H 0.104740 0.149021 0.844151 0.056 Uiso 1 1 calc R U . . .
H12C H 0.190311 0.041487 0.833683 0.056 Uiso 1 1 calc R U . . .
C13 C 0.436(3) 0.006(2) 0.2255(19) 0.029(3) Uani 1 1 d . . . . .
C14 C 0.362(3) -0.172(2) 0.3030(19) 0.030(4) Uani 1 1 d . . . . .
H14A H 0.258024 -0.159029 0.274754 0.045 Uiso 1 1 calc R U . . .
H14B H 0.361196 -0.229508 0.368519 0.045 Uiso 1 1 calc R U . . .
H14C H 0.447548 -0.195444 0.265083 0.045 Uiso 1 1 calc R U . . .
O1 O 0.720(3) 0.558(3) 0.293(2) 0.0516(12) Uani 0.63(3) 1 d D . P A 1
O2 O 0.469(3) 0.603(2) 0.302(2) 0.0516(12) Uani 0.63(3) 1 d D . P A 1
N1 N 0.585(4) 0.5451(19) 0.2902(16) 0.0517(11) Uani 0.63(3) 1 d D . P A 1
O1A O 0.738(5) 0.570(4) 0.258(4) 0.0516(12) Uani 0.37(3) 1 d D . P A 2
O2A O 0.492(5) 0.554(4) 0.282(3) 0.0516(12) Uani 0.37(3) 1 d D . P A 2
N1A N 0.597(5) 0.611(3) 0.281(3) 0.0517(11) Uani 0.37(3) 1 d D . P A 2
O3 O 0.741(5) 0.472(3) 0.094(3) 0.0518(12) Uani 0.45(3) 1 d D . P A 3
O4 O 0.538(5) 0.593(3) 0.069(3) 0.0518(12) Uani 0.45(3) 1 d D . P A 3
N2 N 0.617(4) 0.510(3) 0.120(2) 0.0517(11) Uani 0.45(3) 1 d D . P A 3
O3A O 0.742(4) 0.463(3) 0.154(2) 0.0518(12) Uani 0.55(3) 1 d D . P A 4
O4A O 0.539(4) 0.553(3) 0.070(2) 0.0518(12) Uani 0.55(3) 1 d D . P A 4
N2A N 0.694(4) 0.528(3) 0.068(2) 0.0517(11) Uani 0.55(3) 1 d D . P A 4
Pd2 Pd 0.9266(3) 0.2928(2) 0.39908(17) 0.0504(8) Uani 1 1 d . . . . .
O13 O 1.104(2) 0.1145(14) 0.0372(12) 0.031(2) Uani 1 1 d . . . . .
O14 O 1.254(2) 0.2434(15) -0.0017(12) 0.036(2) Uani 1 1 d . . . . .
O15 O 1.215(2) 0.7161(15) 0.0078(12) 0.039(4) Uani 1 1 d . . . . .
O16 O 1.213(2) 0.7761(15) 0.1199(12) 0.035(3) Uani 1 1 d . . . . .
N7 N 0.977(3) 0.253(2) 0.2865(17) 0.047(2) Uani 1 1 d . . . . .
N8 N 1.040(2) 0.4198(18) 0.3125(15) 0.034(2) Uani 1 1 d . . . . .
C15 C 0.958(4) 0.163(2) 0.281(2) 0.048(3) Uani 1 1 d . . . . .
H15 H 0.910852 0.110697 0.335550 0.058 Uiso 1 1 calc R U . . .
C16 C 1.000(3) 0.137(2) 0.2043(19) 0.042(3) Uani 1 1 d . . . . .
H16 H 0.974077 0.074909 0.201628 0.050 Uiso 1 1 calc R U . . .
C17 C 1.084(4) 0.214(2) 0.131(2) 0.049(3) Uani 1 1 d . . . . .
C18 C 1.112(3) 0.311(2) 0.1314(18) 0.0236(19) Uani 1 1 d . . . . .
H18 H 1.167435 0.361397 0.079799 0.028 Uiso 1 1 calc R U . . .
C19 C 1.053(3) 0.329(2) 0.2130(18) 0.025(2) Uani 1 1 d . . . . .
C20 C 1.081(3) 0.425(2) 0.2234(18) 0.025(2) Uani 1 1 d . . . . .
C21 C 1.145(3) 0.514(2) 0.1525(18) 0.0236(19) Uani 1 1 d . . . . .
H21 H 1.181500 0.515691 0.092087 0.028 Uiso 1 1 calc R U . . .
C22 C 1.155(3) 0.600(2) 0.175(2) 0.037(3) Uani 1 1 d . . . . .
C23 C 1.127(3) 0.589(2) 0.2667(18) 0.033(3) Uani 1 1 d . . . . .
H23 H 1.156168 0.640411 0.284118 0.040 Uiso 1 1 calc R U . . .
C24 C 1.058(3) 0.503(2) 0.3328(17) 0.019(2) Uani 1 1 d . . . . .
H24 H 1.023182 0.501550 0.393277 0.023 Uiso 1 1 calc R U . . .
C25 C 1.140(3) 0.187(2) 0.047(2) 0.0405(18) Uani 1 1 d . . . . .
C26 C 1.327(3) 0.213(3) -0.073(2) 0.048(3) Uani 1 1 d . . . . .
H26A H 1.267743 0.255411 -0.131891 0.072 Uiso 1 1 calc R U . . .
H26B H 1.326532 0.135541 -0.052235 0.072 Uiso 1 1 calc R U . . .
H26C H 1.438376 0.227795 -0.084275 0.072 Uiso 1 1 calc R U . . .
C27 C 1.196(3) 0.698(2) 0.0925(19) 0.025(3) Uani 1 1 d . . . . .
C28 C 1.256(3) 0.884(2) 0.0437(18) 0.035(5) Uani 1 1 d . . . . .
H28A H 1.362528 0.872206 0.015525 0.053 Uiso 1 1 calc R U . . .
H28B H 1.255783 0.934119 0.072728 0.053 Uiso 1 1 calc R U . . .
H28C H 1.175708 0.916059 -0.006280 0.053 Uiso 1 1 calc R U . . .
O9 O 0.720(5) 0.439(4) 0.497(4) 0.0447(12) Uani 0.35(2) 1 d D . P B 5
O10 O 0.940(5) 0.342(4) 0.553(3) 0.0447(12) Uani 0.35(2) 1 d D . P B 5
N5 N 0.837(5) 0.375(3) 0.497(3) 0.0456(11) Uani 0.35(2) 1 d D . P B 5
O9A O 0.712(3) 0.406(2) 0.480(2) 0.0447(12) Uani 0.65(2) 1 d D . P B 6
O10A O 0.943(3) 0.314(2) 0.5183(19) 0.0447(12) Uani 0.65(2) 1 d D . P B 6
N5A N 0.825(3) 0.375(2) 0.5401(17) 0.0456(11) Uani 0.65(2) 1 d D . P B 6
O11 O 0.731(5) 0.130(4) 0.465(3) 0.0456(11) Uani 0.38(2) 1 d D . P B 7
O12 O 0.891(5) 0.092(4) 0.574(3) 0.0456(11) Uani 0.38(2) 1 d D . P B 7
N6 N 0.839(4) 0.150(3) 0.496(3) 0.0456(11) Uani 0.38(2) 1 d D . P B 7
O11A O 0.765(3) 0.186(2) 0.4577(19) 0.0456(11) Uani 0.62(2) 1 d D . P B 8
O12A O 0.964(3) 0.077(2) 0.532(2) 0.0456(11) Uani 0.62(2) 1 d D . P B 8
N6A N 0.810(3) 0.087(2) 0.5201(19) 0.0456(11) Uani 0.62(2) 1 d D . P B 8


_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
Pd1 O2A 1.92(5) . ?
Pd1 N1 2.00(2) . ?
Pd1 N3 2.01(2) . ?
Pd1 N4 2.03(2) . ?
Pd1 N2 2.07(3) . ?
Pd1 O3A 2.18(3) . ?
O5 C11 1.13(3) . ?
O6 C11 1.31(3) . ?
O6 C12 1.44(3) . ?
O7 C13 1.21(3) . ?
O8 C13 1.25(3) . ?
O8 C14 1.56(3) . ?
N3 C6 1.29(3) . ?
N3 C10 1.37(3) . ?
N4 C5 1.32(3) . ?
N4 C1 1.40(3) . ?
C1 C2 1.39(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.43(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.48(3) . ?
C3 C11 1.55(4) . ?
C4 C5 1.35(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.55(3) . ?
C6 C7 1.45(3) . ?
C7 C8 1.34(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.45(3) . ?
C8 C13 1.51(3) . ?
C9 C10 1.47(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O1 N1 1.197(10) . ?
O2 N1 1.200(11) . ?
O1A N1A 1.303(11) . ?
O2A N1A 1.294(11) . ?
O3 N2 1.197(11) . ?
O4 N2 1.198(11) . ?
O3A N2A 1.294(11) . ?
O4A N2A 1.295(11) . ?
Pd2 N8 2.02(2) . ?
Pd2 O10A 2.03(3) . ?
Pd2 N7 2.04(2) . ?
Pd2 O11A 2.04(3) . ?
Pd2 N6 2.10(3) . ?
Pd2 N5 2.27(4) . ?
O13 C25 1.17(3) . ?
O14 C25 1.31(3) . ?
O14 C26 1.40(3) . ?
O15 C27 1.23(3) . ?
O16 C27 1.36(3) . ?
O16 C28 1.52(3) . ?
N7 C15 1.33(3) . ?
N7 C19 1.36(3) . ?
N8 C24 1.36(3) . ?
N8 C20 1.37(3) . ?
C15 C16 1.39(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.40(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.41(4) . ?
C17 C25 1.53(4) . ?
C18 C19 1.43(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.47(3) . ?
C20 C21 1.40(3) . ?
C21 C22 1.39(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.37(3) . ?
C22 C27 1.47(4) . ?
C23 C24 1.36(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O9 N5 1.194(11) . ?
O10 N5 1.198(11) . ?
O9A N5A 1.292(11) . ?
O10A N5A 1.297(11) . ?
O11 N6 1.196(11) . ?
O12 N6 1.201(11) . ?
O11A N6A 1.300(11) . ?
O12A N6A 1.305(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
O2A Pd1 N3 160.3(13) . . ?
N1 Pd1 N3 174.4(11) . . ?
O2A Pd1 N4 89.5(14) . . ?
N1 Pd1 N4 97.8(9) . . ?
N3 Pd1 N4 79.6(9) . . ?
N3 Pd1 N2 93.5(10) . . ?
N4 Pd1 N2 164.8(11) . . ?
N3 Pd1 O3A 92.1(10) . . ?
N4 Pd1 O3A 160.1(11) . . ?
C11 O6 C12 115(2) . . ?
C13 O8 C14 116.0(19) . . ?
C6 N3 C10 122(2) . . ?
C6 N3 Pd1 116.2(18) . . ?
C10 N3 Pd1 121.8(18) . . ?
C5 N4 C1 119(2) . . ?
C5 N4 Pd1 117.1(18) . . ?
C1 N4 Pd1 123.3(17) . . ?
C2 C1 N4 121(2) . . ?
C2 C1 H1 119.5 . . ?
N4 C1 H1 119.5 . . ?
C1 C2 C3 119(2) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 118(2) . . ?
C2 C3 C11 124(2) . . ?
C4 C3 C11 118(2) . . ?
C5 C4 C3 117(2) . . ?
C5 C4 H4 121.7 . . ?
C3 C4 H4 121.7 . . ?
N4 C5 C4 126(2) . . ?
N4 C5 C6 111(2) . . ?
C4 C5 C6 123(2) . . ?
N3 C6 C7 125(2) . . ?
N3 C6 C5 116(2) . . ?
C7 C6 C5 118(2) . . ?
C8 C7 C6 117(2) . . ?
C8 C7 H7 121.5 . . ?
C6 C7 H7 121.5 . . ?
C7 C8 C9 119(2) . . ?
C7 C8 C13 126(2) . . ?
C9 C8 C13 116(2) . . ?
C8 C9 C10 122(2) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
N3 C10 C9 115(2) . . ?
N3 C10 H10 122.3 . . ?
C9 C10 H10 122.3 . . ?
O5 C11 O6 130(3) . . ?
O5 C11 C3 122(2) . . ?
O6 C11 C3 108(2) . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O7 C13 O8 129(2) . . ?
O7 C13 C8 121(2) . . ?
O8 C13 C8 109(2) . . ?
O8 C14 H14A 109.5 . . ?
O8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 N1 O2 122.8(16) . . ?
O1 N1 Pd1 120(2) . . ?
O2 N1 Pd1 118(2) . . ?
N1A O2A Pd1 124(2) . . ?
O2A N1A O1A 108.3(12) . . ?
O3 N2 O4 122.4(16) . . ?
O3 N2 Pd1 116(3) . . ?
O4 N2 Pd1 121(3) . . ?
N2A O3A Pd1 114.4(17) . . ?
O3A N2A O4A 108.9(12) . . ?
N8 Pd2 O10A 94.4(9) . . ?
N8 Pd2 N7 81.9(9) . . ?
O10A Pd2 N7 163.8(10) . . ?
N8 Pd2 O11A 163.9(9) . . ?
N7 Pd2 O11A 91.9(10) . . ?
N8 Pd2 N6 172.5(13) . . ?
N7 Pd2 N6 97.6(11) . . ?
N8 Pd2 N5 90.5(10) . . ?
N7 Pd2 N5 165.7(14) . . ?
C25 O14 C26 113(2) . . ?
C27 O16 C28 118.5(19) . . ?
C15 N7 C19 120(2) . . ?
C15 N7 Pd2 128.8(19) . . ?
C19 N7 Pd2 111.4(17) . . ?
C24 N8 C20 120(2) . . ?
C24 N8 Pd2 124.9(16) . . ?
C20 N8 Pd2 114.3(16) . . ?
N7 C15 C16 127(3) . . ?
N7 C15 H15 116.4 . . ?
C16 C15 H15 116.4 . . ?
C15 C16 C17 112(2) . . ?
C15 C16 H16 123.8 . . ?
C17 C16 H16 123.8 . . ?
C16 C17 C18 124(2) . . ?
C16 C17 C25 115(2) . . ?
C18 C17 C25 121(2) . . ?
C17 C18 C19 117(2) . . ?
C17 C18 H18 121.7 . . ?
C19 C18 H18 121.7 . . ?
N7 C19 C18 120(2) . . ?
N7 C19 C20 118(2) . . ?
C18 C19 C20 122(2) . . ?
N8 C20 C21 121(2) . . ?
N8 C20 C19 114(2) . . ?
C21 C20 C19 126(2) . . ?
C22 C21 C20 117(2) . . ?
C22 C21 H21 121.6 . . ?
C20 C21 H21 121.6 . . ?
C23 C22 C21 121(3) . . ?
C23 C22 C27 125(2) . . ?
C21 C22 C27 114(2) . . ?
C24 C23 C22 120(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 N8 120(2) . . ?
C23 C24 H24 119.9 . . ?
N8 C24 H24 119.9 . . ?
O13 C25 O14 125(3) . . ?
O13 C25 C17 125(2) . . ?
O14 C25 C17 109(2) . . ?
O14 C26 H26A 109.5 . . ?
O14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O15 C27 O16 120(2) . . ?
O15 C27 C22 129(2) . . ?
O16 C27 C22 111(2) . . ?
O16 C28 H28A 109.5 . . ?
O16 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O16 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 N5 O10 123.0(17) . . ?
O9 N5 Pd2 134(3) . . ?
O10 N5 Pd2 103(3) . . ?
N5A O10A Pd2 118.5(15) . . ?
O9A N5A O10A 108.8(12) . . ?
O11 N6 O12 122.8(17) . . ?
O11 N6 Pd2 113(3) . . ?
O12 N6 Pd2 124(3) . . ?
N6A O11A Pd2 120.3(15) . . ?
O11A N6A O12A 107.3(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N4 C1 C2 -1(4) . . . . ?
Pd1 N4 C1 C2 -169.0(19) . . . . ?
N4 C1 C2 C3 -6(4) . . . . ?
C1 C2 C3 C4 7(4) . . . . ?
C1 C2 C3 C11 178(2) . . . . ?
C2 C3 C4 C5 -1(4) . . . . ?
C11 C3 C4 C5 -172(2) . . . . ?
C1 N4 C5 C4 8(5) . . . . ?
Pd1 N4 C5 C4 177(2) . . . . ?
C1 N4 C5 C6 -178(2) . . . . ?
Pd1 N4 C5 C6 -9(3) . . . . ?
C3 C4 C5 N4 -7(5) . . . . ?
C3 C4 C5 C6 180(3) . . . . ?
C10 N3 C6 C7 -3(5) . . . . ?
Pd1 N3 C6 C7 175(2) . . . . ?
C10 N3 C6 C5 -176(2) . . . . ?
Pd1 N3 C6 C5 2(4) . . . . ?
N4 C5 C6 N3 5(4) . . . . ?
C4 C5 C6 N3 179(3) . . . . ?
N4 C5 C6 C7 -169(2) . . . . ?
C4 C5 C6 C7 6(4) . . . . ?
N3 C6 C7 C8 5(5) . . . . ?
C5 C6 C7 C8 178(2) . . . . ?
C6 C7 C8 C9 -3(4) . . . . ?
C6 C7 C8 C13 177(3) . . . . ?
C7 C8 C9 C10 0(4) . . . . ?
C13 C8 C9 C10 179(2) . . . . ?
C6 N3 C10 C9 0(4) . . . . ?
Pd1 N3 C10 C9 -178.5(18) . . . . ?
C8 C9 C10 N3 2(4) . . . . ?
C12 O6 C11 O5 2(5) . . . . ?
C12 O6 C11 C3 179(2) . . . . ?
C2 C3 C11 O5 -167(3) . . . . ?
C4 C3 C11 O5 4(4) . . . . ?
C2 C3 C11 O6 16(4) . . . . ?
C4 C3 C11 O6 -173(2) . . . . ?
C14 O8 C13 O7 -3(4) . . . . ?
C14 O8 C13 C8 179(2) . . . . ?
C7 C8 C13 O7 171(3) . . . . ?
C9 C8 C13 O7 -9(4) . . . . ?
C7 C8 C13 O8 -11(4) . . . . ?
C9 C8 C13 O8 169(2) . . . . ?
Pd1 O2A N1A O1A 5(2) . . . . ?
Pd1 O3A N2A O4A -0.1(18) . . . . ?
C19 N7 C15 C16 -4(5) . . . . ?
Pd2 N7 C15 C16 -177(2) . . . . ?
N7 C15 C16 C17 6(5) . . . . ?
C15 C16 C17 C18 -5(5) . . . . ?
C15 C16 C17 C25 177(3) . . . . ?
C16 C17 C18 C19 1(5) . . . . ?
C25 C17 C18 C19 179(3) . . . . ?
C15 N7 C19 C18 -1(4) . . . . ?
Pd2 N7 C19 C18 174.0(19) . . . . ?
C15 N7 C19 C20 -176(3) . . . . ?
Pd2 N7 C19 C20 -2(3) . . . . ?
C17 C18 C19 N7 2(4) . . . . ?
C17 C18 C19 C20 177(3) . . . . ?
C24 N8 C20 C21 2(4) . . . . ?
Pd2 N8 C20 C21 173.7(18) . . . . ?
C24 N8 C20 C19 -180(2) . . . . ?
Pd2 N8 C20 C19 -8(3) . . . . ?
N7 C19 C20 N8 6(3) . . . . ?
C18 C19 C20 N8 -169(2) . . . . ?
N7 C19 C20 C21 -175(2) . . . . ?
C18 C19 C20 C21 9(4) . . . . ?
N8 C20 C21 C22 -5(4) . . . . ?
C19 C20 C21 C22 177(2) . . . . ?
C20 C21 C22 C23 11(4) . . . . ?
C20 C21 C22 C27 -170(2) . . . . ?
C21 C22 C23 C24 -14(4) . . . . ?
C27 C22 C23 C24 167(3) . . . . ?
C22 C23 C24 N8 10(4) . . . . ?
C20 N8 C24 C23 -4(4) . . . . ?
Pd2 N8 C24 C23 -175.5(18) . . . . ?
C26 O14 C25 O13 3(5) . . . . ?
C26 O14 C25 C17 172(2) . . . . ?
C16 C17 C25 O13 8(5) . . . . ?
C18 C17 C25 O13 -170(3) . . . . ?
C16 C17 C25 O14 -162(3) . . . . ?
C18 C17 C25 O14 20(4) . . . . ?
C28 O16 C27 O15 0(3) . . . . ?
C28 O16 C27 C22 -180(2) . . . . ?
C23 C22 C27 O15 -176(3) . . . . ?
C21 C22 C27 O15 4(4) . . . . ?
C23 C22 C27 O16 3(4) . . . . ?
C21 C22 C27 O16 -176(2) . . . . ?
Pd2 O10A N5A O9A 3.6(19) . . . . ?
Pd2 O11A N6A O12A -0.4(19) . . . . ?

_refine_diff_density_max         1.616
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.289


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/water'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_Poly1_4h-470nm_150K
_database_code_depnum_ccdc_archive 'CCDC 2151944'
loop_
_audit_author_name
_audit_author_address
'Lauren Hatcher'
;Cardiff University
United Kingdom
;
_audit_update_record             
;
2022-02-14 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT026_Poly1_4h-470nm_150K 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 39% Check
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
_vrf_PLAT250_Poly1_4h-470nm_150K 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 6.2 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT342_Poly1_4h-470nm_150K 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03591 Ang.
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT369_Poly1_4h-470nm_150K 
;
PROBLEM: Long C(sp2)-C(sp2) Bond C5 - C6 . 1.58 Ang.
RESPONSE: As above - the structure solution suffers from weak diffraction data
and slightly reduced completeness for the reasons explained above. Possibly
this data (collected after 4 h illumination) would benefit from AFIX-66 
instructions to fix the benzene rings, however in an attempt to keep consistency
between models this was not attempted.
;
_vrf_PLAT413_Poly1_4h-470nm_150K 
;
PROBLEM: Short Inter XH3 .. XHn H9 ..H28A . 1.99 Ang.
RESPONSE: As above - the structure solution suffers from weak diffraction data
and slightly reduced completeness for the reasons explained above. Short H...H
contacts may also reflect the fact that the molecules are very flat and so pack
quite tightly together - this is seen in both polymorphs of this material.
;
_vrf_PLAT910_Poly1_4h-470nm_150K 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 16 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
Dinitro-(dimethyl 2,2'-bipyridine-4,4'-dicarboxylate)palladium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N4 O8 Pd'
_chemical_formula_sum            'C14 H12 N4 O8 Pd'
_chemical_formula_weight         470.68

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4584(18)
_cell_length_b                   13.867(3)
_cell_length_c                   15.643(4)
_cell_angle_alpha                63.83(2)
_cell_angle_beta                 83.510(18)
_cell_angle_gamma                79.336(16)
_cell_volume                     1617.2(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1088
_cell_measurement_theta_min      3.7360
_cell_measurement_theta_max      22.9560

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.204
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.59971
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6259
_diffrn_reflns_av_unetI/netI     0.2765
_diffrn_reflns_av_R_equivalents  0.1329
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.364
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             6259
_reflns_number_gt                2446
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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         6259
_refine_ls_number_parameters     484
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.2212
_refine_ls_R_factor_gt           0.1107
_refine_ls_wR_factor_ref         0.3512
_refine_ls_wR_factor_gt          0.2895
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_restrained_S_all      0.903
_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
Pd1 Pd 0.5476(3) 0.42443(18) 0.26149(14) 0.0535(7) Uani 1 1 d . . . . .
O5 O 0.224(2) 0.0390(13) 0.6713(11) 0.044(4) Uani 1 1 d . . . . .
O6 O 0.180(2) 0.1785(14) 0.7106(11) 0.044(3) Uani 1 1 d . . . . .
O7 O 0.463(2) 0.0038(15) 0.1480(12) 0.060(5) Uani 1 1 d . . . . .
O8 O 0.397(2) -0.0661(13) 0.3033(11) 0.037(3) Uani 1 1 d . . . . .
N3 N 0.522(3) 0.2911(17) 0.2451(14) 0.045(2) Uani 1 1 d . . . . .
N4 N 0.429(2) 0.3430(16) 0.3834(13) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.389(3) 0.3762(18) 0.4565(14) 0.027(3) Uani 1 1 d . . . . .
H1 H 0.405760 0.446788 0.444974 0.032 Uiso 1 1 calc R U . . .
C2 C 0.327(3) 0.3122(19) 0.5439(16) 0.033(3) Uani 1 1 d . . . . .
H2 H 0.307853 0.335597 0.593339 0.039 Uiso 1 1 calc R U . . .
C3 C 0.290(3) 0.2071(19) 0.5589(16) 0.030(3) Uani 1 1 d . . . . .
C4 C 0.334(3) 0.175(2) 0.4842(16) 0.039(3) Uani 1 1 d . . . . .
H4 H 0.315193 0.107151 0.490403 0.047 Uiso 1 1 calc R U . . .
C5 C 0.403(3) 0.244(2) 0.4041(17) 0.038(3) Uani 1 1 d . . . . .
C6 C 0.451(3) 0.2167(18) 0.3155(15) 0.028(3) Uani 1 1 d . . . . .
C7 C 0.424(3) 0.1175(19) 0.3159(16) 0.033(3) Uani 1 1 d . . . . .
H7 H 0.381756 0.062616 0.370928 0.040 Uiso 1 1 calc R U . . .
C8 C 0.461(3) 0.1056(18) 0.2373(16) 0.031(3) Uani 1 1 d . . . . .
C9 C 0.534(2) 0.1850(17) 0.1582(15) 0.026(3) Uani 1 1 d . . . . .
H9 H 0.565331 0.174235 0.102398 0.032 Uiso 1 1 calc R U . . .
C10 C 0.562(3) 0.2813(19) 0.1626(16) 0.037(3) Uani 1 1 d . . . . .
H10 H 0.606074 0.336876 0.109189 0.044 Uiso 1 1 calc R U . . .
C11 C 0.225(3) 0.1314(19) 0.6531(16) 0.030(3) Uani 1 1 d . . . . .
C12 C 0.111(3) 0.112(2) 0.8002(16) 0.040(5) Uani 1 1 d . . . . .
H12A H 0.011852 0.092270 0.790334 0.060 Uiso 1 1 calc R U . . .
H12B H 0.087341 0.152126 0.839574 0.060 Uiso 1 1 calc R U . . .
H12C H 0.187914 0.045942 0.832581 0.060 Uiso 1 1 calc R U . . .
C13 C 0.443(3) 0.0031(19) 0.2264(17) 0.036(3) Uani 1 1 d . . . . .
C14 C 0.365(3) -0.1694(18) 0.3026(16) 0.034(4) Uani 1 1 d . . . . .
H14A H 0.263889 -0.154909 0.270949 0.050 Uiso 1 1 calc R U . . .
H14B H 0.356666 -0.225050 0.368275 0.050 Uiso 1 1 calc R U . . .
H14C H 0.453517 -0.195216 0.268102 0.050 Uiso 1 1 calc R U . . .
O1 O 0.730(3) 0.567(2) 0.287(2) 0.0514(12) Uani 0.59(2) 1 d D . P A 1
O2 O 0.478(3) 0.600(2) 0.303(2) 0.0514(12) Uani 0.59(2) 1 d D . P A 1
N1 N 0.597(3) 0.5471(18) 0.2875(15) 0.0515(11) Uani 0.59(2) 1 d D . P A 1
O1A O 0.740(4) 0.567(3) 0.252(3) 0.0514(12) Uani 0.41(2) 1 d D . P A 2
O2A O 0.493(4) 0.558(3) 0.282(3) 0.0514(12) Uani 0.41(2) 1 d D . P A 2
N1A N 0.605(4) 0.612(3) 0.277(3) 0.0515(11) Uani 0.41(2) 1 d D . P A 2
O3 O 0.735(4) 0.473(3) 0.097(3) 0.0515(11) Uani 0.43(2) 1 d D . P A 3
O4 O 0.528(4) 0.591(3) 0.071(3) 0.0515(11) Uani 0.43(2) 1 d D . P A 3
N2 N 0.610(4) 0.510(3) 0.122(2) 0.0515(11) Uani 0.43(2) 1 d D . P A 3
O3A O 0.743(3) 0.465(2) 0.1522(19) 0.0515(11) Uani 0.57(2) 1 d D . P A 4
O4A O 0.545(4) 0.555(2) 0.066(2) 0.0515(11) Uani 0.57(2) 1 d D . P A 4
N2A N 0.700(4) 0.529(2) 0.0666(17) 0.0515(11) Uani 0.57(2) 1 d D . P A 4
Pd2 Pd 0.9284(3) 0.29139(18) 0.40068(15) 0.0517(7) Uani 1 1 d . . . . .
O13 O 1.1051(17) 0.1143(12) 0.0364(10) 0.0264(19) Uani 1 1 d . . . . .
O14 O 1.2497(19) 0.2436(13) -0.0009(11) 0.036(2) Uani 1 1 d . . . . .
O15 O 1.210(2) 0.7169(14) 0.0078(11) 0.048(4) Uani 1 1 d . . . . .
O16 O 1.2141(17) 0.7754(13) 0.1205(10) 0.030(3) Uani 1 1 d . . . . .
N7 N 0.980(3) 0.2526(18) 0.2892(15) 0.051(2) Uani 1 1 d . . . . .
N8 N 1.039(2) 0.4185(16) 0.3125(13) 0.037(2) Uani 1 1 d . . . . .
C15 C 0.960(3) 0.161(2) 0.2861(19) 0.054(3) Uani 1 1 d . . . . .
H15 H 0.919981 0.107013 0.342643 0.064 Uiso 1 1 calc R U . . .
C16 C 0.993(3) 0.138(2) 0.2074(17) 0.042(3) Uani 1 1 d . . . . .
H16 H 0.958349 0.078639 0.203519 0.051 Uiso 1 1 calc R U . . .
C17 C 1.085(3) 0.2126(19) 0.1324(16) 0.031(2) Uani 1 1 d . . . . .
C18 C 1.111(2) 0.3108(18) 0.1331(16) 0.0249(18) Uani 1 1 d . . . . .
H18 H 1.166003 0.361799 0.081119 0.030 Uiso 1 1 calc R U . . .
C19 C 1.054(2) 0.3300(18) 0.2131(15) 0.0210(18) Uani 1 1 d . . . . .
C20 C 1.082(2) 0.4218(18) 0.2248(15) 0.0210(18) Uani 1 1 d . . . . .
C21 C 1.143(2) 0.5122(18) 0.1535(16) 0.0249(18) Uani 1 1 d . . . . .
H21 H 1.177994 0.513407 0.093138 0.030 Uiso 1 1 calc R U . . .
C22 C 1.153(3) 0.603(2) 0.1727(17) 0.033(3) Uani 1 1 d . . . . .
C23 C 1.125(3) 0.590(2) 0.2660(16) 0.035(3) Uani 1 1 d . . . . .
H23 H 1.152014 0.642466 0.283513 0.042 Uiso 1 1 calc R U . . .
C24 C 1.057(2) 0.5031(18) 0.3336(16) 0.027(3) Uani 1 1 d . . . . .
H24 H 1.022786 0.500905 0.394302 0.033 Uiso 1 1 calc R U . . .
C25 C 1.144(3) 0.1813(19) 0.0524(16) 0.0278(18) Uani 1 1 d . . . . .
C26 C 1.326(3) 0.214(2) -0.0734(19) 0.050(4) Uani 1 1 d . . . . .
H26A H 1.266406 0.255445 -0.132091 0.074 Uiso 1 1 calc R U . . .
H26B H 1.328798 0.136288 -0.052996 0.074 Uiso 1 1 calc R U . . .
H26C H 1.436623 0.230869 -0.085314 0.074 Uiso 1 1 calc R U . . .
C27 C 1.199(3) 0.6975(19) 0.0930(16) 0.028(3) Uani 1 1 d . . . . .
C28 C 1.254(3) 0.883(2) 0.0432(17) 0.046(5) Uani 1 1 d . . . . .
H28A H 1.337662 0.869963 -0.000707 0.069 Uiso 1 1 calc R U . . .
H28B H 1.293415 0.923615 0.072603 0.069 Uiso 1 1 calc R U . . .
H28C H 1.157311 0.926217 0.008064 0.069 Uiso 1 1 calc R U . . .
O9 O 0.716(6) 0.439(5) 0.495(4) 0.0481(12) Uani 0.27(2) 1 d D . P B 5
O10 O 0.942(6) 0.354(5) 0.547(4) 0.0481(12) Uani 0.27(2) 1 d D . P B 5
N5 N 0.835(6) 0.379(4) 0.494(3) 0.0491(11) Uani 0.27(2) 1 d D . P B 5
O9A O 0.713(2) 0.4061(18) 0.4815(16) 0.0481(12) Uani 0.73(2) 1 d D . P B 6
O10A O 0.942(2) 0.3141(16) 0.5219(15) 0.0481(12) Uani 0.73(2) 1 d D . P B 6
N5A N 0.824(3) 0.3751(18) 0.5429(14) 0.0491(11) Uani 0.73(2) 1 d D . P B 6
O11 O 0.725(5) 0.126(4) 0.475(3) 0.0492(11) Uani 0.373(19) 1 d D . P B 7
O12 O 0.898(5) 0.099(4) 0.573(3) 0.0492(11) Uani 0.373(19) 1 d D . P B 7
N6 N 0.836(4) 0.152(2) 0.497(2) 0.0491(11) Uani 0.373(19) 1 d D . P B 7
O11A O 0.760(3) 0.1825(19) 0.4568(17) 0.0492(11) Uani 0.627(19) 1 d D . P B 8
O12A O 0.962(3) 0.082(2) 0.5328(18) 0.0492(11) Uani 0.627(19) 1 d D . P B 8
N6A N 0.812(3) 0.0852(18) 0.5205(17) 0.0491(11) Uani 0.627(19) 1 d D . P B 8


_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
Pd1 O2A 1.98(4) . ?
Pd1 N4 2.003(18) . ?
Pd1 N3 2.026(18) . ?
Pd1 N2 2.03(3) . ?
Pd1 N1 2.04(2) . ?
Pd1 O3A 2.20(3) . ?
O5 C11 1.19(3) . ?
O6 C11 1.32(3) . ?
O6 C12 1.42(3) . ?
O7 C13 1.21(2) . ?
O8 C13 1.24(3) . ?
O8 C14 1.51(2) . ?
N3 C6 1.31(3) . ?
N3 C10 1.35(3) . ?
N4 C5 1.32(3) . ?
N4 C1 1.40(2) . ?
C1 C2 1.37(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.46(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.41(3) . ?
C3 C11 1.50(3) . ?
C4 C5 1.35(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.58(3) . ?
C6 C7 1.43(3) . ?
C7 C8 1.31(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.42(3) . ?
C8 C13 1.54(3) . ?
C9 C10 1.43(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O1 N1 1.199(10) . ?
O2 N1 1.201(10) . ?
O1A N1A 1.304(11) . ?
O2A N1A 1.292(11) . ?
O3 N2 1.194(11) . ?
O4 N2 1.198(11) . ?
O3A N2A 1.289(11) . ?
O4A N2A 1.292(11) . ?
Pd2 N8 2.016(19) . ?
Pd2 N7 2.021(19) . ?
Pd2 O10A 2.07(2) . ?
Pd2 N6 2.09(3) . ?
Pd2 O11A 2.10(3) . ?
Pd2 N5 2.27(4) . ?
O13 C25 1.17(2) . ?
O14 C25 1.31(3) . ?
O14 C26 1.42(2) . ?
O15 C27 1.23(2) . ?
O16 C27 1.36(3) . ?
O16 C28 1.52(3) . ?
N7 C15 1.33(3) . ?
N7 C19 1.39(3) . ?
N8 C20 1.36(3) . ?
N8 C24 1.39(3) . ?
C15 C16 1.39(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.44(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.42(3) . ?
C17 C25 1.50(3) . ?
C18 C19 1.41(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.43(3) . ?
C20 C21 1.40(3) . ?
C21 C22 1.44(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.39(3) . ?
C22 C27 1.43(3) . ?
C23 C24 1.38(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O9 N5 1.197(11) . ?
O10 N5 1.198(11) . ?
O9A N5A 1.292(10) . ?
O10A N5A 1.296(10) . ?
O11 N6 1.198(11) . ?
O12 N6 1.201(11) . ?
O11A N6A 1.303(10) . ?
O12A N6A 1.297(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
O2A Pd1 N4 89.9(11) . . ?
O2A Pd1 N3 160.7(11) . . ?
N4 Pd1 N3 79.2(7) . . ?
N4 Pd1 N2 164.0(11) . . ?
N3 Pd1 N2 94.0(9) . . ?
N4 Pd1 N1 99.8(8) . . ?
N3 Pd1 N1 172.9(10) . . ?
N4 Pd1 O3A 159.9(9) . . ?
N3 Pd1 O3A 92.8(9) . . ?
C11 O6 C12 115.2(18) . . ?
C13 O8 C14 116.2(17) . . ?
C6 N3 C10 119.6(19) . . ?
C6 N3 Pd1 117.1(15) . . ?
C10 N3 Pd1 123.0(15) . . ?
C5 N4 C1 115.4(18) . . ?
C5 N4 Pd1 119.1(15) . . ?
C1 N4 Pd1 124.9(14) . . ?
C2 C1 N4 123.4(19) . . ?
C2 C1 H1 118.3 . . ?
N4 C1 H1 118.3 . . ?
C1 C2 C3 118.0(19) . . ?
C1 C2 H2 121.0 . . ?
C3 C2 H2 121.0 . . ?
C4 C3 C2 117.0(19) . . ?
C4 C3 C11 121(2) . . ?
C2 C3 C11 121.2(18) . . ?
C5 C4 C3 118(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
N4 C5 C4 127(2) . . ?
N4 C5 C6 110.6(19) . . ?
C4 C5 C6 122(2) . . ?
N3 C6 C7 124(2) . . ?
N3 C6 C5 113.2(18) . . ?
C7 C6 C5 122.4(19) . . ?
C8 C7 C6 117(2) . . ?
C8 C7 H7 121.4 . . ?
C6 C7 H7 121.4 . . ?
C7 C8 C9 121(2) . . ?
C7 C8 C13 124(2) . . ?
C9 C8 C13 115.6(18) . . ?
C8 C9 C10 119.8(19) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N3 C10 C9 118(2) . . ?
N3 C10 H10 120.9 . . ?
C9 C10 H10 120.9 . . ?
O5 C11 O6 126(2) . . ?
O5 C11 C3 121(2) . . ?
O6 C11 C3 112.4(19) . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O7 C13 O8 131(2) . . ?
O7 C13 C8 119(2) . . ?
O8 C13 C8 110.1(18) . . ?
O8 C14 H14A 109.5 . . ?
O8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 N1 O2 122.2(15) . . ?
O1 N1 Pd1 124.8(18) . . ?
O2 N1 Pd1 113.1(18) . . ?
N1A O2A Pd1 119.6(19) . . ?
O2A N1A O1A 108.6(12) . . ?
O3 N2 O4 122.9(16) . . ?
O3 N2 Pd1 115(2) . . ?
O4 N2 Pd1 123(2) . . ?
N2A O3A Pd1 115.7(14) . . ?
O3A N2A O4A 109.6(12) . . ?
N8 Pd2 N7 81.1(8) . . ?
N8 Pd2 O10A 95.5(8) . . ?
N7 Pd2 O10A 164.3(8) . . ?
N8 Pd2 N6 174.2(12) . . ?
N7 Pd2 N6 98.8(10) . . ?
N8 Pd2 O11A 161.4(8) . . ?
N7 Pd2 O11A 90.5(9) . . ?
N8 Pd2 N5 89.8(10) . . ?
N7 Pd2 N5 163.8(15) . . ?
C25 O14 C26 113.8(17) . . ?
C27 O16 C28 117.4(16) . . ?
C15 N7 C19 120(2) . . ?
C15 N7 Pd2 127.2(17) . . ?
C19 N7 Pd2 112.5(14) . . ?
C20 N8 C24 121.1(19) . . ?
C20 N8 Pd2 114.6(14) . . ?
C24 N8 Pd2 123.9(14) . . ?
N7 C15 C16 126(2) . . ?
N7 C15 H15 117.1 . . ?
C16 C15 H15 117.1 . . ?
C15 C16 C17 113(2) . . ?
C15 C16 H16 123.4 . . ?
C17 C16 H16 123.4 . . ?
C18 C17 C16 122(2) . . ?
C18 C17 C25 123.2(19) . . ?
C16 C17 C25 115.0(19) . . ?
C19 C18 C17 118.0(19) . . ?
C19 C18 H18 121.0 . . ?
C17 C18 H18 121.0 . . ?
N7 C19 C18 119.8(19) . . ?
N7 C19 C20 116.8(19) . . ?
C18 C19 C20 123.1(19) . . ?
N8 C20 C21 120.1(19) . . ?
N8 C20 C19 114.8(18) . . ?
C21 C20 C19 125(2) . . ?
C20 C21 C22 119.2(19) . . ?
C20 C21 H21 120.4 . . ?
C22 C21 H21 120.4 . . ?
C23 C22 C27 126(2) . . ?
C23 C22 C21 118(2) . . ?
C27 C22 C21 116(2) . . ?
C24 C23 C22 121(2) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 N8 120(2) . . ?
C23 C24 H24 120.2 . . ?
N8 C24 H24 120.2 . . ?
O13 C25 O14 123(2) . . ?
O13 C25 C17 128(2) . . ?
O14 C25 C17 108.6(18) . . ?
O14 C26 H26A 109.5 . . ?
O14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O15 C27 O16 120(2) . . ?
O15 C27 C22 129(2) . . ?
O16 C27 C22 110.7(19) . . ?
O16 C28 H28A 109.5 . . ?
O16 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O16 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 N5 O10 122.5(17) . . ?
O9 N5 Pd2 134(3) . . ?
O10 N5 Pd2 104(3) . . ?
N5A O10A Pd2 118.4(12) . . ?
O9A N5A O10A 108.6(11) . . ?
O11 N6 O12 122.7(17) . . ?
O11 N6 Pd2 119(3) . . ?
O12 N6 Pd2 118(3) . . ?
N6A O11A Pd2 116.5(13) . . ?
O12A N6A O11A 107.6(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N4 C1 C2 0(4) . . . . ?
Pd1 N4 C1 C2 -171.0(17) . . . . ?
N4 C1 C2 C3 -4(4) . . . . ?
C1 C2 C3 C4 5(4) . . . . ?
C1 C2 C3 C11 179(2) . . . . ?
C2 C3 C4 C5 -1(4) . . . . ?
C11 C3 C4 C5 -175(2) . . . . ?
C1 N4 C5 C4 5(4) . . . . ?
Pd1 N4 C5 C4 176(2) . . . . ?
C1 N4 C5 C6 179.2(19) . . . . ?
Pd1 N4 C5 C6 -10(3) . . . . ?
C3 C4 C5 N4 -4(4) . . . . ?
C3 C4 C5 C6 -178(2) . . . . ?
C10 N3 C6 C7 7(4) . . . . ?
Pd1 N3 C6 C7 -179.5(18) . . . . ?
C10 N3 C6 C5 -176(2) . . . . ?
Pd1 N3 C6 C5 -3(3) . . . . ?
N4 C5 C6 N3 8(3) . . . . ?
C4 C5 C6 N3 -178(2) . . . . ?
N4 C5 C6 C7 -175(2) . . . . ?
C4 C5 C6 C7 -1(4) . . . . ?
N3 C6 C7 C8 -7(4) . . . . ?
C5 C6 C7 C8 177(2) . . . . ?
C6 C7 C8 C9 4(4) . . . . ?
C6 C7 C8 C13 179(2) . . . . ?
C7 C8 C9 C10 -3(4) . . . . ?
C13 C8 C9 C10 -178(2) . . . . ?
C6 N3 C10 C9 -5(4) . . . . ?
Pd1 N3 C10 C9 -178.1(17) . . . . ?
C8 C9 C10 N3 3(3) . . . . ?
C12 O6 C11 O5 -5(4) . . . . ?
C12 O6 C11 C3 177.8(19) . . . . ?
C4 C3 C11 O5 8(4) . . . . ?
C2 C3 C11 O5 -166(2) . . . . ?
C4 C3 C11 O6 -175(2) . . . . ?
C2 C3 C11 O6 12(3) . . . . ?
C14 O8 C13 O7 2(4) . . . . ?
C14 O8 C13 C8 176.8(19) . . . . ?
C7 C8 C13 O7 172(3) . . . . ?
C9 C8 C13 O7 -13(4) . . . . ?
C7 C8 C13 O8 -3(4) . . . . ?
C9 C8 C13 O8 171(2) . . . . ?
Pd1 O2A N1A O1A 4(2) . . . . ?
Pd1 O3A N2A O4A 0.1(18) . . . . ?
C19 N7 C15 C16 -7(4) . . . . ?
Pd2 N7 C15 C16 178(2) . . . . ?
N7 C15 C16 C17 13(4) . . . . ?
C15 C16 C17 C18 -11(4) . . . . ?
C15 C16 C17 C25 172(2) . . . . ?
C16 C17 C18 C19 4(3) . . . . ?
C25 C17 C18 C19 -178(2) . . . . ?
C15 N7 C19 C18 -1(4) . . . . ?
Pd2 N7 C19 C18 174.1(16) . . . . ?
C15 N7 C19 C20 -175(2) . . . . ?
Pd2 N7 C19 C20 0(3) . . . . ?
C17 C18 C19 N7 2(3) . . . . ?
C17 C18 C19 C20 176(2) . . . . ?
C24 N8 C20 C21 -1(3) . . . . ?
Pd2 N8 C20 C21 172.7(15) . . . . ?
C24 N8 C20 C19 -178.8(19) . . . . ?
Pd2 N8 C20 C19 -5(2) . . . . ?
N7 C19 C20 N8 3(3) . . . . ?
C18 C19 C20 N8 -170.4(19) . . . . ?
N7 C19 C20 C21 -174(2) . . . . ?
C18 C19 C20 C21 12(3) . . . . ?
N8 C20 C21 C22 -3(3) . . . . ?
C19 C20 C21 C22 175(2) . . . . ?
C20 C21 C22 C23 10(3) . . . . ?
C20 C21 C22 C27 -173(2) . . . . ?
C27 C22 C23 C24 170(2) . . . . ?
C21 C22 C23 C24 -13(4) . . . . ?
C22 C23 C24 N8 10(4) . . . . ?
C20 N8 C24 C23 -2(3) . . . . ?
Pd2 N8 C24 C23 -175.4(17) . . . . ?
C26 O14 C25 O13 -7(3) . . . . ?
C26 O14 C25 C17 174(2) . . . . ?
C18 C17 C25 O13 -165(2) . . . . ?
C16 C17 C25 O13 12(4) . . . . ?
C18 C17 C25 O14 14(3) . . . . ?
C16 C17 C25 O14 -168(2) . . . . ?
C28 O16 C27 O15 -3(3) . . . . ?
C28 O16 C27 C22 -177(2) . . . . ?
C23 C22 C27 O15 -172(3) . . . . ?
C21 C22 C27 O15 11(4) . . . . ?
C23 C22 C27 O16 1(3) . . . . ?
C21 C22 C27 O16 -176.1(19) . . . . ?
Pd2 O10A N5A O9A 3.1(18) . . . . ?
Pd2 O11A N6A O12A -0.1(18) . . . . ?

_refine_diff_density_max         1.963
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.313


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/water'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_Poly1_8h-470nm_150K
_database_code_depnum_ccdc_archive 'CCDC 2151945'
loop_
_audit_author_name
_audit_author_address
'Lauren Hatcher'
;Cardiff University
United Kingdom
;
_audit_update_record             
;
2022-02-14 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT026_Poly1_8h-470nm_150K 
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 39% Check
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
_vrf_PLAT250_Poly1_8h-470nm_150K 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 5.4 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT342_Poly1_8h-470nm_150K 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.03455 Ang.
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak leading 
to low overall resolution and so low precision on the final model structure.
;
_vrf_PLAT910_Poly1_8h-470nm_150K 
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 16 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Following irradiation of the sample with
470nm LED light, diffraction intensity was reduced further. Though twinning 
was dealt with using a HKLF-5 refinement, diffraction data remain weak with 
low overall completeness.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
Dinitro-(dimethyl 2,2'-bipyridine-4,4'-dicarboxylate)palladium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N4 O8 Pd'
_chemical_formula_sum            'C14 H12 N4 O8 Pd'
_chemical_formula_weight         470.68

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4570(17)
_cell_length_b                   13.863(2)
_cell_length_c                   15.648(4)
_cell_angle_alpha                63.84(2)
_cell_angle_beta                 83.505(18)
_cell_angle_gamma                79.366(16)
_cell_volume                     1617.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1081
_cell_measurement_theta_min      3.7350
_cell_measurement_theta_max      24.4750

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.933
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.204
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.62566
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6230
_diffrn_reflns_av_unetI/netI     0.2776
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.363
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             6230
_reflns_number_gt                2439
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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         6230
_refine_ls_number_parameters     484
_refine_ls_number_restraints     516
_refine_ls_R_factor_all          0.2209
_refine_ls_R_factor_gt           0.1072
_refine_ls_wR_factor_ref         0.3464
_refine_ls_wR_factor_gt          0.2855
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_restrained_S_all      0.887
_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
Pd1 Pd 0.5475(3) 0.42464(17) 0.26126(14) 0.0550(7) Uani 1 1 d . . . . .
O5 O 0.2230(19) 0.0395(13) 0.6708(11) 0.042(3) Uani 1 1 d . . . . .
O6 O 0.180(2) 0.1771(14) 0.7119(12) 0.050(4) Uani 1 1 d . . . . .
O7 O 0.460(2) 0.0043(14) 0.1487(12) 0.055(5) Uani 1 1 d . . . . .
O8 O 0.398(2) -0.0668(13) 0.3040(11) 0.043(3) Uani 1 1 d . . . . .
N3 N 0.521(3) 0.2927(17) 0.2433(14) 0.051(2) Uani 1 1 d . . . . .
N4 N 0.428(2) 0.3426(15) 0.3840(13) 0.038(2) Uani 1 1 d . . . . .
C1 C 0.394(3) 0.3792(19) 0.4551(15) 0.031(3) Uani 1 1 d . . . . .
H1 H 0.414791 0.448873 0.443737 0.037 Uiso 1 1 calc R U . . .
C2 C 0.328(3) 0.3125(19) 0.5430(16) 0.034(3) Uani 1 1 d . . . . .
H2 H 0.306725 0.336351 0.592029 0.041 Uiso 1 1 calc R U . . .
C3 C 0.294(3) 0.2088(19) 0.5595(16) 0.032(3) Uani 1 1 d . . . . .
C4 C 0.332(3) 0.1767(19) 0.4834(15) 0.036(3) Uani 1 1 d . . . . .
H4 H 0.309381 0.109316 0.489676 0.043 Uiso 1 1 calc R U . . .
C5 C 0.401(3) 0.2434(19) 0.4038(16) 0.035(3) Uani 1 1 d . . . . .
C6 C 0.451(2) 0.2141(17) 0.3184(15) 0.023(2) Uani 1 1 d . . . . .
C7 C 0.422(2) 0.1211(18) 0.3138(15) 0.026(3) Uani 1 1 d . . . . .
H7 H 0.369903 0.068847 0.366398 0.031 Uiso 1 1 calc R U . . .
C8 C 0.465(3) 0.1052(18) 0.2371(15) 0.031(3) Uani 1 1 d . . . . .
C9 C 0.537(3) 0.1847(18) 0.1576(16) 0.033(3) Uani 1 1 d . . . . .
H9 H 0.567588 0.174125 0.101655 0.040 Uiso 1 1 calc R U . . .
C10 C 0.562(3) 0.2828(18) 0.1629(15) 0.031(3) Uani 1 1 d . . . . .
H10 H 0.607282 0.338577 0.109882 0.037 Uiso 1 1 calc R U . . .
C11 C 0.228(2) 0.1317(18) 0.6526(15) 0.025(3) Uani 1 1 d . . . . .
C12 C 0.116(3) 0.1111(19) 0.8007(16) 0.038(5) Uani 1 1 d . . . . .
H12A H 0.009639 0.097728 0.792805 0.057 Uiso 1 1 calc R U . . .
H12B H 0.104718 0.147627 0.842775 0.057 Uiso 1 1 calc R U . . .
H12C H 0.187662 0.041791 0.828799 0.057 Uiso 1 1 calc R U . . .
C13 C 0.441(3) 0.0059(19) 0.2251(16) 0.033(3) Uani 1 1 d . . . . .
C14 C 0.367(3) -0.167(2) 0.3010(17) 0.044(4) Uani 1 1 d . . . . .
H14A H 0.276352 -0.149692 0.259929 0.066 Uiso 1 1 calc R U . . .
H14B H 0.340535 -0.220060 0.365482 0.066 Uiso 1 1 calc R U . . .
H14C H 0.463071 -0.198896 0.275484 0.066 Uiso 1 1 calc R U . . .
O1 O 0.730(3) 0.563(2) 0.290(2) 0.0547(12) Uani 0.58(2) 1 d D . P A 1
O2 O 0.479(3) 0.602(2) 0.301(2) 0.0547(12) Uani 0.58(2) 1 d D . P A 1
N1 N 0.598(3) 0.5463(18) 0.2882(15) 0.0551(11) Uani 0.58(2) 1 d D . P A 1
O1A O 0.738(4) 0.569(3) 0.253(3) 0.0547(12) Uani 0.42(2) 1 d D . P A 2
O2A O 0.490(4) 0.557(3) 0.282(3) 0.0547(12) Uani 0.42(2) 1 d D . P A 2
N1A N 0.601(4) 0.612(3) 0.279(3) 0.0551(11) Uani 0.42(2) 1 d D . P A 2
O3 O 0.732(5) 0.474(3) 0.094(3) 0.0551(11) Uani 0.38(2) 1 d D . P A 3
O4 O 0.526(5) 0.593(3) 0.069(3) 0.0551(11) Uani 0.38(2) 1 d D . P A 3
N2 N 0.607(5) 0.511(3) 0.120(2) 0.0551(11) Uani 0.38(2) 1 d D . P A 3
O3A O 0.742(3) 0.4648(19) 0.1498(18) 0.0551(11) Uani 0.62(2) 1 d D . P A 4
O4A O 0.540(3) 0.559(2) 0.0680(19) 0.0551(11) Uani 0.62(2) 1 d D . P A 4
N2A N 0.694(4) 0.531(2) 0.0656(16) 0.0551(11) Uani 0.62(2) 1 d D . P A 4
Pd2 Pd 0.9285(3) 0.29098(18) 0.40117(15) 0.0523(7) Uani 1 1 d . . . . .
O13 O 1.0987(17) 0.1131(12) 0.0384(10) 0.0279(19) Uani 1 1 d . . . . .
O14 O 1.2504(19) 0.2422(13) 0.0003(11) 0.039(2) Uani 1 1 d . . . . .
O15 O 1.210(2) 0.7151(13) 0.0080(11) 0.045(4) Uani 1 1 d . . . . .
O16 O 1.2159(18) 0.7745(13) 0.1200(11) 0.035(3) Uani 1 1 d . . . . .
N7 N 0.977(3) 0.2528(17) 0.2908(14) 0.048(2) Uani 1 1 d . . . . .
N8 N 1.038(2) 0.4183(16) 0.3118(13) 0.040(2) Uani 1 1 d . . . . .
C15 C 0.956(3) 0.164(2) 0.2852(17) 0.045(3) Uani 1 1 d . . . . .
H15 H 0.908240 0.111413 0.339657 0.054 Uiso 1 1 calc R U . . .
C16 C 0.997(3) 0.137(2) 0.2091(17) 0.047(3) Uani 1 1 d . . . . .
H16 H 0.969646 0.074989 0.207218 0.056 Uiso 1 1 calc R U . . .
C17 C 1.083(3) 0.213(2) 0.1343(18) 0.045(3) Uani 1 1 d . . . . .
C18 C 1.110(2) 0.3106(18) 0.1317(15) 0.0233(18) Uani 1 1 d . . . . .
H18 H 1.161884 0.362172 0.078803 0.028 Uiso 1 1 calc R U . . .
C19 C 1.054(2) 0.3275(18) 0.2136(15) 0.0225(18) Uani 1 1 d . . . . .
C20 C 1.081(2) 0.4207(18) 0.2242(15) 0.0225(18) Uani 1 1 d . . . . .
C21 C 1.142(2) 0.5133(17) 0.1514(15) 0.0233(18) Uani 1 1 d . . . . .
H21 H 1.172439 0.516853 0.089912 0.028 Uiso 1 1 calc R U . . .
C22 C 1.154(3) 0.6013(19) 0.1741(16) 0.032(3) Uani 1 1 d . . . . .
C23 C 1.128(2) 0.5914(18) 0.2652(15) 0.029(3) Uani 1 1 d . . . . .
H23 H 1.154234 0.644302 0.281904 0.035 Uiso 1 1 calc R U . . .
C24 C 1.059(2) 0.5002(17) 0.3346(15) 0.022(2) Uani 1 1 d . . . . .
H24 H 1.027683 0.496033 0.396221 0.027 Uiso 1 1 calc R U . . .
C25 C 1.143(3) 0.181(2) 0.0523(17) 0.0358(18) Uani 1 1 d . . . . .
C26 C 1.326(3) 0.214(2) -0.0748(17) 0.042(3) Uani 1 1 d . . . . .
H26A H 1.261899 0.253359 -0.131945 0.062 Uiso 1 1 calc R U . . .
H26B H 1.332564 0.135464 -0.054094 0.062 Uiso 1 1 calc R U . . .
H26C H 1.434503 0.233578 -0.089367 0.062 Uiso 1 1 calc R U . . .
C27 C 1.200(2) 0.6974(18) 0.0920(15) 0.024(3) Uani 1 1 d . . . . .
C28 C 1.251(3) 0.8821(19) 0.0449(16) 0.043(5) Uani 1 1 d . . . . .
H28A H 1.350323 0.871486 0.009196 0.065 Uiso 1 1 calc R U . . .
H28B H 1.264128 0.928901 0.074926 0.065 Uiso 1 1 calc R U . . .
H28C H 1.161596 0.916501 0.001383 0.065 Uiso 1 1 calc R U . . .
O9 O 0.687(6) 0.395(5) 0.509(4) 0.0500(11) Uani 0.26(2) 1 d D . P B 5
O10 O 0.931(6) 0.359(5) 0.542(4) 0.0500(11) Uani 0.26(2) 1 d D . P B 5
N5 N 0.824(6) 0.359(3) 0.498(3) 0.0502(10) Uani 0.26(2) 1 d D . P B 5
O9A O 0.721(2) 0.4147(17) 0.4804(15) 0.0500(11) Uani 0.74(2) 1 d D . P B 6
O10A O 0.942(2) 0.3117(16) 0.5237(15) 0.0500(11) Uani 0.74(2) 1 d D . P B 6
N5A N 0.829(3) 0.3764(17) 0.5437(14) 0.0502(10) Uani 0.74(2) 1 d D . P B 6
O11 O 0.735(5) 0.123(3) 0.475(3) 0.0502(11) Uani 0.394(19) 1 d D . P B 7
O12 O 0.908(4) 0.102(3) 0.571(3) 0.0502(11) Uani 0.394(19) 1 d D . P B 7
N6 N 0.844(4) 0.152(2) 0.496(2) 0.0502(10) Uani 0.394(19) 1 d D . P B 7
O11A O 0.760(3) 0.182(2) 0.4611(17) 0.0502(11) Uani 0.606(19) 1 d D . P B 8
O12A O 0.965(3) 0.079(2) 0.5319(18) 0.0502(11) Uani 0.606(19) 1 d D . P B 8
N6A N 0.813(3) 0.0842(19) 0.5230(17) 0.0502(10) Uani 0.606(19) 1 d D . P B 8


_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
Pd1 O2A 1.98(4) . ?
Pd1 N4 2.017(18) . ?
Pd1 N3 2.023(19) . ?
Pd1 N1 2.03(2) . ?
Pd1 N2 2.05(3) . ?
Pd1 O3A 2.21(3) . ?
O5 C11 1.19(2) . ?
O6 C11 1.33(3) . ?
O6 C12 1.40(3) . ?
O7 C13 1.20(2) . ?
O8 C13 1.27(3) . ?
O8 C14 1.49(3) . ?
N3 C10 1.33(3) . ?
N3 C6 1.37(3) . ?
N4 C5 1.33(3) . ?
N4 C1 1.40(3) . ?
C1 C2 1.39(3) . ?
C1 H1 0.9500 . ?
C2 C3 1.42(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.43(3) . ?
C3 C11 1.50(3) . ?
C4 C5 1.33(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.56(3) . ?
C6 C7 1.39(3) . ?
C7 C8 1.31(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.41(3) . ?
C8 C13 1.52(3) . ?
C9 C10 1.46(3) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O1 N1 1.195(10) . ?
O2 N1 1.201(10) . ?
O1A N1A 1.303(11) . ?
O2A N1A 1.295(11) . ?
O3 N2 1.195(11) . ?
O4 N2 1.199(11) . ?
O3A N2A 1.288(10) . ?
O4A N2A 1.287(10) . ?
Pd2 N7 1.999(18) . ?
Pd2 N8 2.017(18) . ?
Pd2 N6 2.05(3) . ?
Pd2 O10A 2.08(2) . ?
Pd2 O11A 2.11(3) . ?
Pd2 N5 2.15(4) . ?
O13 C25 1.18(2) . ?
O14 C25 1.31(3) . ?
O14 C26 1.44(2) . ?
O15 C27 1.22(2) . ?
O16 C27 1.36(2) . ?
O16 C28 1.49(3) . ?
N7 C15 1.32(3) . ?
N7 C19 1.39(3) . ?
N8 C20 1.37(3) . ?
N8 C24 1.37(3) . ?
C15 C16 1.38(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.41(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.40(3) . ?
C17 C25 1.54(3) . ?
C18 C19 1.42(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.43(3) . ?
C20 C21 1.42(3) . ?
C21 C22 1.44(3) . ?
C21 H21 0.9500 . ?
C22 C23 1.37(3) . ?
C22 C27 1.46(3) . ?
C23 C24 1.43(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
O9 N5 1.198(11) . ?
O10 N5 1.200(11) . ?
O9A N5A 1.287(10) . ?
O10A N5A 1.295(10) . ?
O11 N6 1.196(11) . ?
O12 N6 1.198(11) . ?
O11A N6A 1.301(10) . ?
O12A N6A 1.295(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
O2A Pd1 N4 89.4(11) . . ?
O2A Pd1 N3 159.8(11) . . ?
N4 Pd1 N3 79.7(7) . . ?
N4 Pd1 N1 99.6(8) . . ?
N3 Pd1 N1 173.2(10) . . ?
N4 Pd1 N2 163.3(11) . . ?
N3 Pd1 N2 93.3(10) . . ?
N4 Pd1 O3A 160.2(9) . . ?
N3 Pd1 O3A 91.8(8) . . ?
C11 O6 C12 116.6(18) . . ?
C13 O8 C14 115.5(17) . . ?
C10 N3 C6 120.7(19) . . ?
C10 N3 Pd1 123.2(15) . . ?
C6 N3 Pd1 116.1(14) . . ?
C5 N4 C1 118.3(18) . . ?
C5 N4 Pd1 118.8(15) . . ?
C1 N4 Pd1 122.2(14) . . ?
C2 C1 N4 119.4(19) . . ?
C2 C1 H1 120.3 . . ?
N4 C1 H1 120.3 . . ?
C1 C2 C3 120(2) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 117.1(19) . . ?
C2 C3 C11 123.3(19) . . ?
C4 C3 C11 119.5(19) . . ?
C5 C4 C3 118(2) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 N4 126(2) . . ?
C4 C5 C6 122(2) . . ?
N4 C5 C6 111.6(18) . . ?
N3 C6 C7 121.6(19) . . ?
N3 C6 C5 113.4(18) . . ?
C7 C6 C5 124.9(19) . . ?
C8 C7 C6 120(2) . . ?
C8 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C7 C8 C9 120(2) . . ?
C7 C8 C13 125(2) . . ?
C9 C8 C13 115.3(18) . . ?
C8 C9 C10 118.8(19) . . ?
C8 C9 H9 120.6 . . ?
C10 C9 H9 120.6 . . ?
N3 C10 C9 119(2) . . ?
N3 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
O5 C11 O6 125(2) . . ?
O5 C11 C3 123(2) . . ?
O6 C11 C3 112.6(18) . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O7 C13 O8 129(2) . . ?
O7 C13 C8 121(2) . . ?
O8 C13 C8 110.4(18) . . ?
O8 C14 H14A 109.5 . . ?
O8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O1 N1 O2 122.6(16) . . ?
O1 N1 Pd1 124.6(19) . . ?
O2 N1 Pd1 112.8(18) . . ?
N1A O2A Pd1 120.1(19) . . ?
O2A N1A O1A 108.5(12) . . ?
O3 N2 O4 122.7(17) . . ?
O3 N2 Pd1 114(3) . . ?
O4 N2 Pd1 123(3) . . ?
N2A O3A Pd1 114.6(14) . . ?
O4A N2A O3A 110.0(12) . . ?
N7 Pd2 N8 80.9(7) . . ?
N7 Pd2 N6 98.2(10) . . ?
N8 Pd2 N6 173.2(11) . . ?
N7 Pd2 O10A 164.7(8) . . ?
N8 Pd2 O10A 96.6(8) . . ?
N7 Pd2 O11A 91.7(8) . . ?
N8 Pd2 O11A 162.0(8) . . ?
N7 Pd2 N5 164.9(16) . . ?
N8 Pd2 N5 96.6(11) . . ?
C25 O14 C26 113.6(17) . . ?
C27 O16 C28 117.9(16) . . ?
C15 N7 C19 117.0(19) . . ?
C15 N7 Pd2 128.7(16) . . ?
C19 N7 Pd2 114.0(14) . . ?
C20 N8 C24 122.4(18) . . ?
C20 N8 Pd2 114.6(14) . . ?
C24 N8 Pd2 122.9(14) . . ?
N7 C15 C16 127(2) . . ?
N7 C15 H15 116.3 . . ?
C16 C15 H15 116.3 . . ?
C15 C16 C17 114(2) . . ?
C15 C16 H16 123.2 . . ?
C17 C16 H16 123.2 . . ?
C18 C17 C16 124(2) . . ?
C18 C17 C25 121.4(19) . . ?
C16 C17 C25 114.8(19) . . ?
C17 C18 C19 115.3(19) . . ?
C17 C18 H18 122.3 . . ?
C19 C18 H18 122.3 . . ?
N7 C19 C18 122.5(19) . . ?
N7 C19 C20 115.5(18) . . ?
C18 C19 C20 121.9(18) . . ?
N8 C20 C21 119.5(19) . . ?
N8 C20 C19 114.7(18) . . ?
C21 C20 C19 125.7(19) . . ?
C20 C21 C22 117.8(19) . . ?
C20 C21 H21 121.1 . . ?
C22 C21 H21 121.1 . . ?
C23 C22 C21 121(2) . . ?
C23 C22 C27 125(2) . . ?
C21 C22 C27 113.6(19) . . ?
C22 C23 C24 119(2) . . ?
C22 C23 H23 120.6 . . ?
C24 C23 H23 120.6 . . ?
N8 C24 C23 119.6(19) . . ?
N8 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
O13 C25 O14 126(2) . . ?
O13 C25 C17 126(2) . . ?
O14 C25 C17 108.2(18) . . ?
O14 C26 H26A 109.5 . . ?
O14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O15 C27 O16 122(2) . . ?
O15 C27 C22 128(2) . . ?
O16 C27 C22 109.9(18) . . ?
O16 C28 H28A 109.5 . . ?
O16 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O16 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O9 N5 O10 122.2(17) . . ?
O9 N5 Pd2 131(3) . . ?
O10 N5 Pd2 107(3) . . ?
N5A O10A Pd2 119.1(12) . . ?
O9A N5A O10A 109.4(12) . . ?
O11 N6 O12 123.4(17) . . ?
O11 N6 Pd2 119(2) . . ?
O12 N6 Pd2 117(2) . . ?
N6A O11A Pd2 116.7(13) . . ?
O12A N6A O11A 108.0(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N4 C1 C2 -2(3) . . . . ?
Pd1 N4 C1 C2 -172.0(16) . . . . ?
N4 C1 C2 C3 -1(3) . . . . ?
C1 C2 C3 C4 1(3) . . . . ?
C1 C2 C3 C11 179(2) . . . . ?
C2 C3 C4 C5 2(3) . . . . ?
C11 C3 C4 C5 -176(2) . . . . ?
C3 C4 C5 N4 -5(4) . . . . ?
C3 C4 C5 C6 178(2) . . . . ?
C1 N4 C5 C4 5(4) . . . . ?
Pd1 N4 C5 C4 176(2) . . . . ?
C1 N4 C5 C6 -177.8(19) . . . . ?
Pd1 N4 C5 C6 -7(3) . . . . ?
C10 N3 C6 C7 0(4) . . . . ?
Pd1 N3 C6 C7 177.9(16) . . . . ?
C10 N3 C6 C5 -176(2) . . . . ?
Pd1 N3 C6 C5 1(3) . . . . ?
C4 C5 C6 N3 -179(2) . . . . ?
N4 C5 C6 N3 4(3) . . . . ?
C4 C5 C6 C7 4(4) . . . . ?
N4 C5 C6 C7 -173(2) . . . . ?
N3 C6 C7 C8 2(3) . . . . ?
C5 C6 C7 C8 178(2) . . . . ?
C6 C7 C8 C9 -2(3) . . . . ?
C6 C7 C8 C13 179(2) . . . . ?
C7 C8 C9 C10 0(3) . . . . ?
C13 C8 C9 C10 179(2) . . . . ?
C6 N3 C10 C9 -2(4) . . . . ?
Pd1 N3 C10 C9 -179.5(16) . . . . ?
C8 C9 C10 N3 2(3) . . . . ?
C12 O6 C11 O5 -2(3) . . . . ?
C12 O6 C11 C3 180.0(19) . . . . ?
C2 C3 C11 O5 -168(2) . . . . ?
C4 C3 C11 O5 10(3) . . . . ?
C2 C3 C11 O6 10(3) . . . . ?
C4 C3 C11 O6 -172(2) . . . . ?
C14 O8 C13 O7 0(4) . . . . ?
C14 O8 C13 C8 178.5(19) . . . . ?
C7 C8 C13 O7 168(2) . . . . ?
C9 C8 C13 O7 -11(3) . . . . ?
C7 C8 C13 O8 -10(3) . . . . ?
C9 C8 C13 O8 171(2) . . . . ?
Pd1 O2A N1A O1A 5(2) . . . . ?
Pd1 O3A N2A O4A 1.7(18) . . . . ?
C19 N7 C15 C16 -3(4) . . . . ?
Pd2 N7 C15 C16 -177(2) . . . . ?
N7 C15 C16 C17 6(4) . . . . ?
C15 C16 C17 C18 -7(4) . . . . ?
C15 C16 C17 C25 175(2) . . . . ?
C16 C17 C18 C19 4(4) . . . . ?
C25 C17 C18 C19 -178(2) . . . . ?
C15 N7 C19 C18 0(3) . . . . ?
Pd2 N7 C19 C18 174.7(16) . . . . ?
C15 N7 C19 C20 -177(2) . . . . ?
Pd2 N7 C19 C20 -2(3) . . . . ?
C17 C18 C19 N7 0(3) . . . . ?
C17 C18 C19 C20 176(2) . . . . ?
C24 N8 C20 C21 -3(3) . . . . ?
Pd2 N8 C20 C21 172.4(15) . . . . ?
C24 N8 C20 C19 178.9(19) . . . . ?
Pd2 N8 C20 C19 -5(2) . . . . ?
N7 C19 C20 N8 5(3) . . . . ?
C18 C19 C20 N8 -172.0(19) . . . . ?
N7 C19 C20 C21 -173(2) . . . . ?
C18 C19 C20 C21 11(3) . . . . ?
N8 C20 C21 C22 0(3) . . . . ?
C19 C20 C21 C22 177(2) . . . . ?
C20 C21 C22 C23 8(3) . . . . ?
C20 C21 C22 C27 -173.3(19) . . . . ?
C21 C22 C23 C24 -11(3) . . . . ?
C27 C22 C23 C24 170(2) . . . . ?
C20 N8 C24 C23 0(3) . . . . ?
Pd2 N8 C24 C23 -175.6(15) . . . . ?
C22 C23 C24 N8 7(3) . . . . ?
C26 O14 C25 O13 -5(4) . . . . ?
C26 O14 C25 C17 175(2) . . . . ?
C18 C17 C25 O13 -163(3) . . . . ?
C16 C17 C25 O13 15(4) . . . . ?
C18 C17 C25 O14 16(3) . . . . ?
C16 C17 C25 O14 -165(2) . . . . ?
C28 O16 C27 O15 -1(3) . . . . ?
C28 O16 C27 C22 -175.9(19) . . . . ?
C23 C22 C27 O15 -172(2) . . . . ?
C21 C22 C27 O15 9(3) . . . . ?
C23 C22 C27 O16 2(3) . . . . ?
C21 C22 C27 O16 -177.3(18) . . . . ?
Pd2 O10A N5A O9A 2.1(18) . . . . ?
Pd2 O11A N6A O12A -0.4(18) . . . . ?

_refine_diff_density_max         1.822
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.301


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/water'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
####################################################################### 
# 
# 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_Poly1_GS_150K
_database_code_depnum_ccdc_archive 'CCDC 2151942'
loop_
_audit_author_name
_audit_author_address
'Lauren Hatcher'
;Cardiff University
United Kingdom
;
_audit_update_record             
;
2022-02-14 deposited with the CCDC.	2022-03-25 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT342_Poly1_GS_150K       
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02682 Ang.
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Though twinning was dealt with using a
HKLF-5 refinement, diffraction data remain weak, leading to low overall
resolution and therefore low precision on the final model structure.
;
_vrf_PLAT910_Poly1_GS_150K       
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 14 Note
RESPONSE: All available crystals of polymorph 1 are small, thin needles
that are intrisically twinned. Though twinning was dealt with using a
HKLF-5 refinement, diffraction data remain weak with low overall completeness.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        
;
Dinitro-(dimethyl 2,2'-bipyridine-4,4'-dicarboxylate)palladium(II)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H12 N4 O8 Pd'
_chemical_formula_sum            'C14 H12 N4 O8 Pd'
_chemical_formula_weight         470.68

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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.4976(9)
_cell_length_b                   13.812(2)
_cell_length_c                   15.5449(19)
_cell_angle_alpha                63.761(14)
_cell_angle_beta                 82.994(9)
_cell_angle_gamma                78.512(11)
_cell_volume                     1602.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1440
_cell_measurement_theta_min      3.7230
_cell_measurement_theta_max      26.0080

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_F_000             936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    1.215
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_T_min  0.79110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.107a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            6168
_diffrn_reflns_av_unetI/netI     0.1884
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.334
_diffrn_reflns_theta_max         25.388
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             6168
_reflns_number_gt                3599
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1456P)²] 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         6168
_refine_ls_number_parameters     486
_refine_ls_number_restraints     414
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2454
_refine_ls_wR_factor_gt          0.2032
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_restrained_S_all      0.928
_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
Pd1 Pd 0.54608(15) 0.42440(11) 0.26343(9) 0.0180(4) Uani 1 1 d . . . . .
Pd2 Pd 0.93255(16) 0.28806(12) 0.39991(9) 0.0206(4) Uani 1 1 d . . . . .
O5 O 0.2129(14) 0.0381(10) 0.6727(8) 0.024(2) Uani 1 1 d . . . . .
O8 O 0.3950(15) -0.0698(10) 0.3053(8) 0.025(2) Uani 1 1 d . . . . .
O15 O 1.2148(14) 0.7182(10) 0.0062(8) 0.025(2) Uani 1 1 d . . . . .
N8 N 1.0421(16) 0.4179(12) 0.3122(10) 0.0218(18) Uani 1 1 d . . . . .
N4 N 0.4331(16) 0.3407(12) 0.3915(10) 0.0190(19) Uani 1 1 d . . . . .
O14 O 1.2699(15) 0.2463(12) -0.0088(9) 0.0307(18) Uani 1 1 d . . . . .
N2 N 0.6350(19) 0.5021(13) 0.1292(11) 0.0271(13) Uani 1 1 d . . . . .
O7 O 0.4444(17) 0.0062(11) 0.1464(9) 0.033(3) Uani 1 1 d . . . . .
N5 N 0.8671(17) 0.3343(13) 0.5027(10) 0.0230(13) Uani 1 1 d . . . . .
O16 O 1.2239(14) 0.7756(11) 0.1185(8) 0.026(2) Uani 1 1 d . . . . .
O6 O 0.1949(15) 0.1696(10) 0.7222(8) 0.026(2) Uani 1 1 d . . . . .
O12 O 0.9128(17) 0.0866(12) 0.5574(10) 0.049(4) Uani 1 1 d . . . . .
N3 N 0.5071(16) 0.2934(11) 0.2437(10) 0.0165(19) Uani 1 1 d . . . . .
O9 O 0.7362(15) 0.3971(13) 0.4962(10) 0.041(3) Uani 1 1 d . . . . .
O13 O 1.1093(15) 0.1246(11) 0.0227(9) 0.0285(17) Uani 1 1 d . . . . .
N6 N 0.8409(17) 0.1502(13) 0.4823(11) 0.0258(13) Uani 1 1 d . . . . .
O2 O 0.7188(15) 0.5655(12) 0.2855(11) 0.039(3) Uani 1 1 d . . . . .
O1 O 0.4682(15) 0.6032(11) 0.3112(10) 0.035(2) Uani 1 1 d . . . . .
C5 C 0.405(2) 0.2390(15) 0.4060(12) 0.020(2) Uani 1 1 d . . . . .
N1 N 0.5814(17) 0.5490(12) 0.2903(10) 0.0207(13) Uani 1 1 d . . . . .
N7 N 0.9953(17) 0.2533(13) 0.2854(10) 0.024(2) Uani 1 1 d . . . . .
O11 O 0.7294(16) 0.1221(12) 0.4635(9) 0.038(2) Uani 1 1 d . . . . .
O3 O 0.5457(17) 0.5676(12) 0.0677(10) 0.045(4) Uani 1 1 d . . . . .
C6 C 0.4435(19) 0.2189(14) 0.3202(12) 0.017(2) Uani 1 1 d . . . . .
O4 O 0.7772(17) 0.4832(13) 0.1069(10) 0.046(4) Uani 1 1 d . . . . .
C9 C 0.5234(19) 0.1875(14) 0.1578(12) 0.019(2) Uani 1 1 d . . . . .
H9 H 0.554649 0.178785 0.100501 0.023 Uiso 1 1 calc R U . . .
C20 C 1.0836(18) 0.4262(14) 0.2241(12) 0.0162(15) Uani 1 1 d . . . . .
C1 C 0.395(2) 0.3719(15) 0.4649(12) 0.028(3) Uani 1 1 d . . . . .
H1 H 0.416682 0.440796 0.455794 0.034 Uiso 1 1 calc R U . . .
C11 C 0.224(2) 0.1265(15) 0.6603(12) 0.019(2) Uani 1 1 d . . . . .
C25 C 1.1551(19) 0.1930(14) 0.0379(11) 0.0174(14) Uani 1 1 d . . . . .
C2 C 0.328(2) 0.3076(15) 0.5503(12) 0.023(2) Uani 1 1 d . . . . .
H2 H 0.304068 0.331296 0.600019 0.027 Uiso 1 1 calc R U . . .
C19 C 1.0736(18) 0.3290(14) 0.2068(12) 0.0162(15) Uani 1 1 d . . . . .
C3 C 0.294(2) 0.2072(15) 0.5643(12) 0.019(2) Uani 1 1 d . . . . .
C17 C 1.096(2) 0.2172(15) 0.1225(12) 0.0227(19) Uani 1 1 d . . . . .
C15 C 0.9671(19) 0.1556(15) 0.2798(12) 0.020(2) Uani 1 1 d . . . . .
H15 H 0.914542 0.101738 0.330640 0.024 Uiso 1 1 calc R U . . .
C8 C 0.4566(17) 0.1095(13) 0.2343(11) 0.0142(19) Uani 1 1 d . . . . .
C7 C 0.4183(19) 0.1195(14) 0.3215(12) 0.015(2) Uani 1 1 d . . . . .
H7 H 0.378443 0.063583 0.377157 0.018 Uiso 1 1 calc R U . . .
C24 C 1.054(2) 0.5047(15) 0.3283(13) 0.025(2) Uani 1 1 d . . . . .
H24 H 1.017781 0.504184 0.388757 0.030 Uiso 1 1 calc R U . . .
O10 O 0.9499(18) 0.3178(15) 0.5666(11) 0.060(3) Uani 1 1 d . . . . .
C27 C 1.206(2) 0.6951(16) 0.0911(13) 0.021(2) Uani 1 1 d . . . . .
C13 C 0.437(2) 0.0098(15) 0.2240(12) 0.022(2) Uani 1 1 d . . . . .
C4 C 0.3333(18) 0.1753(14) 0.4893(11) 0.017(2) Uani 1 1 d . . . . .
H4 H 0.309096 0.107583 0.497047 0.020 Uiso 1 1 calc R U . . .
C16 C 1.021(2) 0.1462(15) 0.1963(11) 0.022(2) Uani 1 1 d . . . . .
H16 H 1.003914 0.083162 0.191194 0.027 Uiso 1 1 calc R U . . .
C22 C 1.155(2) 0.5995(16) 0.1715(13) 0.022(2) Uani 1 1 d . . . . .
C12 C 0.115(2) 0.1014(16) 0.8108(13) 0.029(3) Uani 1 1 d . . . . .
H12A H 0.004965 0.100936 0.797612 0.044 Uiso 1 1 calc R U . . .
H12B H 0.110804 0.130791 0.858130 0.044 Uiso 1 1 calc R U . . .
H12C H 0.174196 0.026507 0.836212 0.044 Uiso 1 1 calc R U . . .
C18 C 1.116(2) 0.3109(16) 0.1322(13) 0.026(2) Uani 1 1 d . . . . .
H18 H 1.164683 0.365003 0.079347 0.032 Uiso 1 1 calc R U . . .
C21 C 1.1453(18) 0.5179(14) 0.1506(12) 0.018(2) Uani 1 1 d . . . . .
H21 H 1.177907 0.520449 0.089014 0.021 Uiso 1 1 calc R U . . .
C26 C 1.339(2) 0.2222(19) -0.0901(13) 0.033(3) Uani 1 1 d . . . . .
H26A H 1.262480 0.255048 -0.141655 0.049 Uiso 1 1 calc R U . . .
H26B H 1.362242 0.142773 -0.068954 0.049 Uiso 1 1 calc R U . . .
H26C H 1.438960 0.252633 -0.113921 0.049 Uiso 1 1 calc R U . . .
C10 C 0.545(2) 0.2807(15) 0.1656(13) 0.024(3) Uani 1 1 d . . . . .
H10 H 0.589188 0.336646 0.111904 0.029 Uiso 1 1 calc R U . . .
C28 C 1.244(2) 0.8860(16) 0.0487(13) 0.032(4) Uani 1 1 d . . . . .
H28A H 1.352191 0.884902 0.019086 0.049 Uiso 1 1 calc R U . . .
H28B H 1.227480 0.934267 0.081090 0.049 Uiso 1 1 calc R U . . .
H28C H 1.164444 0.913051 -0.000999 0.049 Uiso 1 1 calc R U . . .
C23 C 1.115(2) 0.5896(16) 0.2636(12) 0.024(2) Uani 1 1 d . . . . .
H23 H 1.131207 0.645135 0.280290 0.028 Uiso 1 1 calc R U . . .
C14 C 0.371(2) -0.1684(15) 0.3007(13) 0.028(3) Uani 1 1 d . . . . .
H14A H 0.255278 -0.168574 0.301188 0.042 Uiso 1 1 calc R U . . .
H14B H 0.418121 -0.232711 0.356182 0.042 Uiso 1 1 calc R U . . .
H14C H 0.422221 -0.170627 0.241468 0.042 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
Pd1 N2 2.009(15) . ?
Pd1 N1 2.024(15) . ?
Pd1 N4 2.040(14) . ?
Pd1 N3 2.057(14) . ?
Pd2 N5 1.953(15) . ?
Pd2 N6 2.016(15) . ?
Pd2 N7 2.026(15) . ?
Pd2 N8 2.033(14) . ?
O5 C11 1.17(2) . ?
O8 C13 1.32(2) . ?
O8 C14 1.45(2) . ?
O15 C27 1.209(19) . ?
N8 C20 1.33(2) . ?
N8 C24 1.35(2) . ?
N4 C1 1.37(2) . ?
N4 C5 1.39(2) . ?
O14 C25 1.29(2) . ?
O14 C26 1.47(2) . ?
N2 O3 1.204(19) . ?
N2 O4 1.225(19) . ?
O7 C13 1.22(2) . ?
N5 O10 1.200(18) . ?
N5 O9 1.252(19) . ?
O16 C27 1.39(2) . ?
O16 C28 1.46(2) . ?
O6 C11 1.32(2) . ?
O6 C12 1.46(2) . ?
O12 N6 1.249(19) . ?
N3 C10 1.30(2) . ?
N3 C6 1.32(2) . ?
O13 C25 1.21(2) . ?
N6 O11 1.203(18) . ?
O2 N1 1.221(17) . ?
O1 N1 1.202(18) . ?
C5 C4 1.35(2) . ?
C5 C6 1.47(2) . ?
N7 C19 1.41(2) . ?
N7 C15 1.46(2) . ?
C6 C7 1.42(2) . ?
C9 C8 1.36(2) . ?
C9 C10 1.39(2) . ?
C9 H9 0.9500 . ?
C20 C21 1.42(2) . ?
C20 C19 1.50(2) . ?
C1 C2 1.36(2) . ?
C1 H1 0.9500 . ?
C11 C3 1.55(2) . ?
C25 C17 1.50(2) . ?
C2 C3 1.39(2) . ?
C2 H2 0.9500 . ?
C19 C18 1.29(2) . ?
C3 C4 1.40(2) . ?
C17 C16 1.32(2) . ?
C17 C18 1.41(3) . ?
C15 C16 1.38(2) . ?
C15 H15 0.9500 . ?
C8 C7 1.42(2) . ?
C8 C13 1.50(2) . ?
C7 H7 0.9500 . ?
C24 C23 1.31(2) . ?
C24 H24 0.9500 . ?
C27 C22 1.46(2) . ?
C4 H4 0.9500 . ?
C16 H16 0.9500 . ?
C22 C21 1.33(3) . ?
C22 C23 1.38(2) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C18 H18 0.9500 . ?
C21 H21 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C10 H10 0.9500 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C23 H23 0.9500 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

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
N2 Pd1 N1 88.6(6) . . ?
N2 Pd1 N4 172.2(6) . . ?
N1 Pd1 N4 97.2(6) . . ?
N2 Pd1 N3 94.4(6) . . ?
N1 Pd1 N3 177.0(6) . . ?
N4 Pd1 N3 79.8(5) . . ?
N5 Pd2 N6 87.8(6) . . ?
N5 Pd2 N7 175.2(6) . . ?
N6 Pd2 N7 96.0(6) . . ?
N5 Pd2 N8 96.9(6) . . ?
N6 Pd2 N8 174.3(6) . . ?
N7 Pd2 N8 79.5(6) . . ?
C13 O8 C14 116.8(13) . . ?
C20 N8 C24 116.4(15) . . ?
C20 N8 Pd2 115.8(12) . . ?
C24 N8 Pd2 126.9(12) . . ?
C1 N4 C5 118.5(14) . . ?
C1 N4 Pd1 126.4(11) . . ?
C5 N4 Pd1 115.0(11) . . ?
C25 O14 C26 113.7(14) . . ?
O3 N2 O4 118.4(15) . . ?
O3 N2 Pd1 119.3(12) . . ?
O4 N2 Pd1 122.2(13) . . ?
O10 N5 O9 116.1(16) . . ?
O10 N5 Pd2 125.3(13) . . ?
O9 N5 Pd2 118.1(11) . . ?
C27 O16 C28 122.3(13) . . ?
C11 O6 C12 112.6(14) . . ?
C10 N3 C6 121.6(15) . . ?
C10 N3 Pd1 124.5(11) . . ?
C6 N3 Pd1 113.8(11) . . ?
O11 N6 O12 117.9(15) . . ?
O11 N6 Pd2 126.1(12) . . ?
O12 N6 Pd2 115.9(11) . . ?
C4 C5 N4 120.1(16) . . ?
C4 C5 C6 127.1(16) . . ?
N4 C5 C6 112.5(14) . . ?
O1 N1 O2 122.2(15) . . ?
O1 N1 Pd1 119.6(11) . . ?
O2 N1 Pd1 118.2(12) . . ?
C19 N7 C15 118.4(14) . . ?
C19 N7 Pd2 116.9(12) . . ?
C15 N7 Pd2 124.7(11) . . ?
N3 C6 C7 121.4(15) . . ?
N3 C6 C5 118.3(15) . . ?
C7 C6 C5 120.2(15) . . ?
C8 C9 C10 118.3(16) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
N8 C20 C21 123.1(16) . . ?
N8 C20 C19 116.4(15) . . ?
C21 C20 C19 120.3(15) . . ?
C2 C1 N4 122.3(16) . . ?
C2 C1 H1 118.8 . . ?
N4 C1 H1 118.8 . . ?
O5 C11 O6 128.3(16) . . ?
O5 C11 C3 121.2(16) . . ?
O6 C11 C3 110.2(15) . . ?
O13 C25 O14 125.7(16) . . ?
O13 C25 C17 123.1(15) . . ?
O14 C25 C17 110.9(15) . . ?
C1 C2 C3 119.4(17) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
C18 C19 N7 119.4(17) . . ?
C18 C19 C20 130.1(16) . . ?
N7 C19 C20 110.4(14) . . ?
C2 C3 C4 118.2(16) . . ?
C2 C3 C11 123.2(16) . . ?
C4 C3 C11 118.5(15) . . ?
C16 C17 C18 115.3(16) . . ?
C16 C17 C25 119.7(16) . . ?
C18 C17 C25 125.0(15) . . ?
C16 C15 N7 115.7(15) . . ?
C16 C15 H15 122.1 . . ?
N7 C15 H15 122.1 . . ?
C9 C8 C7 120.9(15) . . ?
C9 C8 C13 116.9(15) . . ?
C7 C8 C13 122.0(14) . . ?
C8 C7 C6 115.6(14) . . ?
C8 C7 H7 122.2 . . ?
C6 C7 H7 122.2 . . ?
C23 C24 N8 122.5(17) . . ?
C23 C24 H24 118.8 . . ?
N8 C24 H24 118.8 . . ?
O15 C27 O16 117.6(16) . . ?
O15 C27 C22 129.4(18) . . ?
O16 C27 C22 112.2(15) . . ?
O7 C13 O8 123.1(16) . . ?
O7 C13 C8 122.9(15) . . ?
O8 C13 C8 113.6(15) . . ?
C5 C4 C3 121.4(16) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C17 C16 C15 125.8(18) . . ?
C17 C16 H16 117.1 . . ?
C15 C16 H16 117.1 . . ?
C21 C22 C23 119.3(17) . . ?
C21 C22 C27 114.7(17) . . ?
C23 C22 C27 125.9(18) . . ?
O6 C12 H12A 109.5 . . ?
O6 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O6 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C19 C18 C17 125.3(17) . . ?
C19 C18 H18 117.4 . . ?
C17 C18 H18 117.4 . . ?
C22 C21 C20 117.2(16) . . ?
C22 C21 H21 121.4 . . ?
C20 C21 H21 121.4 . . ?
O14 C26 H26A 109.5 . . ?
O14 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
O14 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C10 C9 122.1(16) . . ?
N3 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
O16 C28 H28A 109.5 . . ?
O16 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O16 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C24 C23 C22 121.1(19) . . ?
C24 C23 H23 119.4 . . ?
C22 C23 H23 119.4 . . ?
O8 C14 H14A 109.5 . . ?
O8 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O8 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N4 C5 C4 3(2) . . . . ?
Pd1 N4 C5 C4 178.7(12) . . . . ?
C1 N4 C5 C6 177.2(15) . . . . ?
Pd1 N4 C5 C6 -7.5(18) . . . . ?
C10 N3 C6 C7 2(2) . . . . ?
Pd1 N3 C6 C7 -175.8(12) . . . . ?
C10 N3 C6 C5 179.6(16) . . . . ?
Pd1 N3 C6 C5 1.9(18) . . . . ?
C4 C5 C6 N3 177.0(16) . . . . ?
N4 C5 C6 N3 4(2) . . . . ?
C4 C5 C6 C7 -5(3) . . . . ?
N4 C5 C6 C7 -178.6(14) . . . . ?
C24 N8 C20 C21 3(2) . . . . ?
Pd2 N8 C20 C21 173.0(11) . . . . ?
C24 N8 C20 C19 178.6(14) . . . . ?
Pd2 N8 C20 C19 -11.3(18) . . . . ?
C5 N4 C1 C2 -1(3) . . . . ?
Pd1 N4 C1 C2 -176.1(13) . . . . ?
C12 O6 C11 O5 -11(3) . . . . ?
C12 O6 C11 C3 174.7(14) . . . . ?
C26 O14 C25 O13 4(3) . . . . ?
C26 O14 C25 C17 177.2(14) . . . . ?
N4 C1 C2 C3 -1(3) . . . . ?
C15 N7 C19 C18 1(2) . . . . ?
Pd2 N7 C19 C18 -179.9(14) . . . . ?
C15 N7 C19 C20 177.0(13) . . . . ?
Pd2 N7 C19 C20 -3.8(16) . . . . ?
N8 C20 C19 C18 -174.6(17) . . . . ?
C21 C20 C19 C18 1(3) . . . . ?
N8 C20 C19 N7 9.8(19) . . . . ?
C21 C20 C19 N7 -174.4(13) . . . . ?
C1 C2 C3 C4 1(3) . . . . ?
C1 C2 C3 C11 177.6(16) . . . . ?
O5 C11 C3 C2 -171.8(17) . . . . ?
O6 C11 C3 C2 3(2) . . . . ?
O5 C11 C3 C4 5(2) . . . . ?
O6 C11 C3 C4 179.8(15) . . . . ?
O13 C25 C17 C16 17(3) . . . . ?
O14 C25 C17 C16 -156.8(16) . . . . ?
O13 C25 C17 C18 -164.8(18) . . . . ?
O14 C25 C17 C18 22(2) . . . . ?
C19 N7 C15 C16 0(2) . . . . ?
Pd2 N7 C15 C16 -178.9(11) . . . . ?
C10 C9 C8 C7 -4(2) . . . . ?
C10 C9 C8 C13 -179.4(15) . . . . ?
C9 C8 C7 C6 4(2) . . . . ?
C13 C8 C7 C6 -180.0(14) . . . . ?
N3 C6 C7 C8 -4(2) . . . . ?
C5 C6 C7 C8 178.7(14) . . . . ?
C20 N8 C24 C23 -5(3) . . . . ?
Pd2 N8 C24 C23 -173.7(13) . . . . ?
C28 O16 C27 O15 3(2) . . . . ?
C28 O16 C27 C22 -168.0(15) . . . . ?
C14 O8 C13 O7 5(3) . . . . ?
C14 O8 C13 C8 179.0(14) . . . . ?
C9 C8 C13 O7 -16(2) . . . . ?
C7 C8 C13 O7 168.2(16) . . . . ?
C9 C8 C13 O8 169.9(14) . . . . ?
C7 C8 C13 O8 -6(2) . . . . ?
N4 C5 C4 C3 -3(2) . . . . ?
C6 C5 C4 C3 -176.2(16) . . . . ?
C2 C3 C4 C5 1(2) . . . . ?
C11 C3 C4 C5 -175.7(15) . . . . ?
C18 C17 C16 C15 -1(3) . . . . ?
C25 C17 C16 C15 177.1(16) . . . . ?
N7 C15 C16 C17 0(2) . . . . ?
O15 C27 C22 C21 14(3) . . . . ?
O16 C27 C22 C21 -176.5(15) . . . . ?
O15 C27 C22 C23 -164.7(19) . . . . ?
O16 C27 C22 C23 5(3) . . . . ?
N7 C19 C18 C17 -2(3) . . . . ?
C20 C19 C18 C17 -177.7(17) . . . . ?
C16 C17 C18 C19 3(3) . . . . ?
C25 C17 C18 C19 -175.7(17) . . . . ?
C23 C22 C21 C20 4(2) . . . . ?
C27 C22 C21 C20 -175.0(14) . . . . ?
N8 C20 C21 C22 -2(2) . . . . ?
C19 C20 C21 C22 -178.0(15) . . . . ?
C6 N3 C10 C9 -1(3) . . . . ?
Pd1 N3 C10 C9 176.6(12) . . . . ?
C8 C9 C10 N3 2(3) . . . . ?
N8 C24 C23 C22 6(3) . . . . ?
C21 C22 C23 C24 -6(3) . . . . ?
C27 C22 C23 C24 172.8(17) . . . . ?

_refine_diff_density_max         1.805
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.275


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile/water'
_chemical_properties_physical    Light-sensitive,Photo-sensitive
