# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2024

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

data_l8414
_audit_block_doi                 10.5517/ccdc.csd.cc2dqm5y
_database_code_depnum_ccdc_archive 'CCDC 2226270'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-n18n2 2023
loop_
_audit_author_name
_audit_author_address
'Liviu Mirica'
;University of Illinois at Urbana Champaign
United States of America
;
_audit_update_record             
;
2022-12-13 deposited with the CCDC.	2024-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H22 N5 Pd, B F4'
_chemical_formula_sum            'C21 H22 B F4 N5 Pd'
_chemical_formula_weight         537.64

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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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                   8.2212(6)
_cell_length_b                   11.0718(9)
_cell_length_c                   12.3446(11)
_cell_angle_alpha                75.751(4)
_cell_angle_beta                 89.961(5)
_cell_angle_gamma                68.232(4)
_cell_volume                     1006.29(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9881
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      31.26

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_F_000             540
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.082
_exptl_absorpt_coefficient_mu    0.979
_shelx_estimated_absorpt_T_min   0.803
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7767
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_process_details   'sadabs v2012/1'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29820
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_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         2.054
_diffrn_reflns_theta_max         31.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6601
_reflns_number_gt                6435
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0172P)²+0.4877P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6601
_refine_ls_number_parameters     290
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0503
_refine_ls_wR_factor_gt          0.0497
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_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
Pd1 Pd 0.99433(2) 0.69370(2) 0.51389(2) 0.00974(3) Uani 1 1 d . . . . .
N1 N 1.0222(2) 0.58992(15) 0.68079(14) 0.0113(3) Uani 1 1 d . . . . .
N2 N 0.9132(2) 0.76897(17) 0.34367(15) 0.0126(3) Uani 1 1 d . . . . .
N3 N 0.8404(2) 0.88313(16) 0.60608(14) 0.0114(3) Uani 1 1 d . . . . .
N4 N 0.7293(2) 0.69693(19) 0.52078(17) 0.0111(3) Uani 1 1 d . . . . .
N5 N 1.2439(2) 0.74327(17) 0.63763(15) 0.0128(3) Uani 1 1 d . . . . .
C1 C 0.8899(3) 0.54602(17) 0.70618(15) 0.0120(3) Uani 1 1 d . . . . .
C2 C 0.8910(3) 0.4669(2) 0.81217(18) 0.0152(4) Uani 1 1 d . . . . .
H2 H 0.7982 0.4361 0.8298 0.018 Uiso 1 1 calc R U . . .
C3 C 1.0294(3) 0.4333(2) 0.89239(19) 0.0167(4) Uani 1 1 d . . . . .
H3 H 1.0358 0.3747 0.9643 0.020 Uiso 1 1 calc R U . . .
C4 C 1.1581(3) 0.4852(2) 0.86766(18) 0.0153(4) Uani 1 1 d . . . . .
H4 H 1.2511 0.4658 0.9229 0.018 Uiso 1 1 calc R U . . .
C5 C 1.1487(3) 0.5659(2) 0.76075(18) 0.0121(4) Uani 1 1 d . . . . .
C6 C 1.2885(3) 0.6254(2) 0.73171(18) 0.0150(4) Uani 1 1 d . . . . .
H6A H 1.3211 0.6485 0.7989 0.018 Uiso 1 1 calc R U . . .
H6B H 1.3946 0.5541 0.7167 0.018 Uiso 1 1 calc R U . . .
C7 C 1.2204(3) 0.7226(2) 0.52974(18) 0.0133(4) Uani 1 1 d . . . . .
H7A H 1.3210 0.6429 0.5209 0.016 Uiso 1 1 calc R U . . .
H7B H 1.2169 0.8021 0.4701 0.016 Uiso 1 1 calc R U . . .
C8 C 0.9838(3) 0.8315(2) 0.26143(19) 0.0152(4) Uani 1 1 d . . . . .
H8 H 1.0976 0.8303 0.2771 0.018 Uiso 1 1 calc R U . . .
C9 C 0.8976(3) 0.89764(19) 0.15457(17) 0.0166(4) Uani 1 1 d . . . . .
H9 H 0.9525 0.9397 0.0980 0.020 Uiso 1 1 calc R U . . .
C10 C 0.7310(3) 0.9018(2) 0.13119(18) 0.0183(4) Uani 1 1 d . . . . .
H10 H 0.6678 0.9495 0.0593 0.022 Uiso 1 1 calc R U . . .
C11 C 0.6579(3) 0.8353(2) 0.21428(19) 0.0172(4) Uani 1 1 d . . . . .
H11 H 0.5444 0.8353 0.1998 0.021 Uiso 1 1 calc R U . . .
C12 C 0.7520(3) 0.7688(2) 0.31888(17) 0.0130(4) Uani 1 1 d . . . . .
C13 C 0.6829(3) 0.6863(2) 0.40851(17) 0.0136(4) Uani 1 1 d . . . . .
H13A H 0.5534 0.7188 0.3940 0.016 Uiso 1 1 calc R U . . .
H13B H 0.7340 0.5907 0.4065 0.016 Uiso 1 1 calc R U . . .
C14 C 0.6099(3) 0.8277(2) 0.53962(18) 0.0132(4) Uani 1 1 d . . . . .
H14A H 0.4963 0.8221 0.5608 0.016 Uiso 1 1 calc R U . . .
H14B H 0.5863 0.9007 0.4694 0.016 Uiso 1 1 calc R U . . .
C15 C 0.6942(3) 0.8596(2) 0.63202(18) 0.0123(4) Uani 1 1 d . . . . .
C16 C 0.6404(3) 0.8474(2) 0.73892(18) 0.0147(4) Uani 1 1 d . . . . .
H16 H 0.5340 0.8344 0.7544 0.018 Uiso 1 1 calc R U . . .
C17 C 0.7459(3) 0.85476(19) 0.82353(17) 0.0169(4) Uani 1 1 d . . . . .
H17 H 0.7097 0.8511 0.8969 0.020 Uiso 1 1 calc R U . . .
C18 C 0.9039(3) 0.86733(19) 0.79916(17) 0.0155(4) Uani 1 1 d . . . . .
H18 H 0.9809 0.8676 0.8563 0.019 Uiso 1 1 calc R U . . .
C19 C 0.9480(3) 0.87959(19) 0.68924(18) 0.0129(4) Uani 1 1 d . . . . .
C20 C 1.1304(3) 0.8722(2) 0.65893(19) 0.0144(4) Uani 1 1 d . . . . .
H20A H 1.1172 0.9461 0.5910 0.017 Uiso 1 1 calc R U . . .
H20B H 1.1899 0.8875 0.7210 0.017 Uiso 1 1 calc R U . . .
C21 C 0.7461(3) 0.5788(2) 0.61358(18) 0.0144(4) Uani 1 1 d . . . . .
H21A H 0.7716 0.4996 0.5832 0.017 Uiso 1 1 calc R U . . .
H21B H 0.6323 0.5959 0.6463 0.017 Uiso 1 1 calc R U . . .
F1 F 0.48588(19) 0.76636(15) -0.01236(14) 0.0340(4) Uani 1 1 d D . . . .
F2 F 0.42140(19) 0.65603(15) 0.15219(13) 0.0300(3) Uani 1 1 d D . . . .
F3 F 0.2735(2) 0.88011(14) 0.08249(13) 0.0287(3) Uani 1 1 d D . . . .
F4 F 0.2272(2) 0.73562(16) -0.00471(14) 0.0348(4) Uani 1 1 d D . . . .
B1 B 0.3525(3) 0.7586(2) 0.0531(2) 0.0192(5) Uani 1 1 d D . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C7 2.017(2) . ?
Pd1 N1 2.0633(17) . ?
Pd1 N2 2.0695(18) . ?
Pd1 N4 2.1677(16) . ?
Pd1 N3 2.5495(16) . ?
N1 C5 1.339(3) . ?
N1 C1 1.354(3) . ?
N2 C8 1.341(3) . ?
N2 C12 1.361(3) . ?
N3 C19 1.339(3) . ?
N3 C15 1.344(3) . ?
N4 C21 1.473(3) . ?
N4 C13 1.481(3) . ?
N4 C14 1.492(3) . ?
N5 C7 1.431(3) . ?
N5 C6 1.444(3) . ?
N5 C20 1.475(3) . ?
C1 C2 1.382(3) . ?
C1 C21 1.522(3) . ?
C2 C3 1.386(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.380(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.525(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.385(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.382(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.385(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.506(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.512(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.382(3) . ?
C16 C17 1.394(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.523(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
F1 B1 1.377(3) . ?
F2 B1 1.395(3) . ?
F3 B1 1.399(3) . ?
F4 B1 1.385(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Pd1 N1 92.67(8) . . ?
C7 Pd1 N2 104.11(8) . . ?
N1 Pd1 N2 162.35(6) . . ?
C7 Pd1 N4 166.28(7) . . ?
N1 Pd1 N4 82.85(7) . . ?
N2 Pd1 N4 81.99(7) . . ?
C7 Pd1 N3 89.68(7) . . ?
N1 Pd1 N3 77.90(6) . . ?
N2 Pd1 N3 107.19(6) . . ?
N4 Pd1 N3 76.72(6) . . ?
C5 N1 C1 120.19(17) . . ?
C5 N1 Pd1 127.94(14) . . ?
C1 N1 Pd1 111.86(13) . . ?
C8 N2 C12 117.82(19) . . ?
C8 N2 Pd1 129.46(15) . . ?
C12 N2 Pd1 112.04(14) . . ?
C19 N3 C15 118.61(18) . . ?
C19 N3 Pd1 110.44(12) . . ?
C15 N3 Pd1 100.38(12) . . ?
C21 N4 C13 114.22(17) . . ?
C21 N4 C14 113.59(17) . . ?
C13 N4 C14 110.68(17) . . ?
C21 N4 Pd1 104.31(12) . . ?
C13 N4 Pd1 104.17(12) . . ?
C14 N4 Pd1 109.12(12) . . ?
C7 N5 C6 115.65(17) . . ?
C7 N5 C20 118.36(17) . . ?
C6 N5 C20 115.93(17) . . ?
N1 C1 C2 120.6(2) . . ?
N1 C1 C21 118.49(17) . . ?
C2 C1 C21 120.8(2) . . ?
C1 C2 C3 119.0(2) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C4 C3 C2 119.86(19) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
N1 C5 C4 121.37(19) . . ?
N1 C5 C6 119.02(18) . . ?
C4 C5 C6 119.58(19) . . ?
N5 C6 C5 117.48(17) . . ?
N5 C6 H6A 107.9 . . ?
C5 C6 H6A 107.9 . . ?
N5 C6 H6B 107.9 . . ?
C5 C6 H6B 107.9 . . ?
H6A C6 H6B 107.2 . . ?
N5 C7 Pd1 110.08(13) . . ?
N5 C7 H7A 109.6 . . ?
Pd1 C7 H7A 109.6 . . ?
N5 C7 H7B 109.6 . . ?
Pd1 C7 H7B 109.6 . . ?
H7A C7 H7B 108.2 . . ?
N2 C8 C9 122.7(2) . . ?
N2 C8 H8 118.7 . . ?
C9 C8 H8 118.7 . . ?
C10 C9 C8 119.2(2) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 118.8(2) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 119.2(2) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N2 C12 C11 122.18(19) . . ?
N2 C12 C13 117.06(18) . . ?
C11 C12 C13 120.68(19) . . ?
N4 C13 C12 110.35(16) . . ?
N4 C13 H13A 109.6 . . ?
C12 C13 H13A 109.6 . . ?
N4 C13 H13B 109.6 . . ?
C12 C13 H13B 109.6 . . ?
H13A C13 H13B 108.1 . . ?
N4 C14 C15 109.83(16) . . ?
N4 C14 H14A 109.7 . . ?
C15 C14 H14A 109.7 . . ?
N4 C14 H14B 109.7 . . ?
C15 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
N3 C15 C16 122.40(19) . . ?
N3 C15 C14 114.12(18) . . ?
C16 C15 C14 122.92(18) . . ?
C15 C16 C17 118.49(19) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
C18 C17 C16 119.12(19) . . ?
C18 C17 H17 120.4 . . ?
C16 C17 H17 120.4 . . ?
C17 C18 C19 118.7(2) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N3 C19 C18 122.16(19) . . ?
N3 C19 C20 115.59(18) . . ?
C18 C19 C20 121.8(2) . . ?
N5 C20 C19 114.40(17) . . ?
N5 C20 H20A 108.7 . . ?
C19 C20 H20A 108.7 . . ?
N5 C20 H20B 108.7 . . ?
C19 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
N4 C21 C1 113.30(16) . . ?
N4 C21 H21A 108.9 . . ?
C1 C21 H21A 108.9 . . ?
N4 C21 H21B 108.9 . . ?
C1 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
F1 B1 F4 110.8(2) . . ?
F1 B1 F2 109.98(19) . . ?
F4 B1 F2 110.15(18) . . ?
F1 B1 F3 108.85(18) . . ?
F4 B1 F3 109.38(19) . . ?
F2 B1 F3 107.7(2) . . ?

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 -5.2(3) . . . . ?
Pd1 N1 C1 C2 175.85(14) . . . . ?
C5 N1 C1 C21 178.29(17) . . . . ?
Pd1 N1 C1 C21 -0.6(2) . . . . ?
N1 C1 C2 C3 0.1(3) . . . . ?
C21 C1 C2 C3 176.52(18) . . . . ?
C1 C2 C3 C4 3.7(3) . . . . ?
C2 C3 C4 C5 -2.5(3) . . . . ?
C1 N1 C5 C4 6.5(3) . . . . ?
Pd1 N1 C5 C4 -174.76(14) . . . . ?
C1 N1 C5 C6 -175.57(17) . . . . ?
Pd1 N1 C5 C6 3.2(3) . . . . ?
C3 C4 C5 N1 -2.6(3) . . . . ?
C3 C4 C5 C6 179.49(19) . . . . ?
C7 N5 C6 C5 -67.4(2) . . . . ?
C20 N5 C6 C5 77.7(2) . . . . ?
N1 C5 C6 N5 23.5(3) . . . . ?
C4 C5 C6 N5 -158.48(19) . . . . ?
C6 N5 C7 Pd1 71.87(18) . . . . ?
C20 N5 C7 Pd1 -72.28(19) . . . . ?
C12 N2 C8 C9 1.6(3) . . . . ?
Pd1 N2 C8 C9 -168.14(15) . . . . ?
N2 C8 C9 C10 1.0(3) . . . . ?
C8 C9 C10 C11 -2.4(3) . . . . ?
C9 C10 C11 C12 1.2(3) . . . . ?
C8 N2 C12 C11 -2.9(3) . . . . ?
Pd1 N2 C12 C11 168.62(15) . . . . ?
C8 N2 C12 C13 173.91(17) . . . . ?
Pd1 N2 C12 C13 -14.6(2) . . . . ?
C10 C11 C12 N2 1.5(3) . . . . ?
C10 C11 C12 C13 -175.18(18) . . . . ?
C21 N4 C13 C12 -152.45(17) . . . . ?
C14 N4 C13 C12 77.8(2) . . . . ?
Pd1 N4 C13 C12 -39.31(19) . . . . ?
N2 C12 C13 N4 38.5(2) . . . . ?
C11 C12 C13 N4 -144.68(19) . . . . ?
C21 N4 C14 C15 69.9(2) . . . . ?
C13 N4 C14 C15 -160.03(16) . . . . ?
Pd1 N4 C14 C15 -45.96(19) . . . . ?
C19 N3 C15 C16 7.7(3) . . . . ?
Pd1 N3 C15 C16 127.96(18) . . . . ?
C19 N3 C15 C14 -163.91(17) . . . . ?
Pd1 N3 C15 C14 -43.63(17) . . . . ?
N4 C14 C15 N3 65.9(2) . . . . ?
N4 C14 C15 C16 -105.6(2) . . . . ?
N3 C15 C16 C17 -2.5(3) . . . . ?
C14 C15 C16 C17 168.29(18) . . . . ?
C15 C16 C17 C18 -3.1(3) . . . . ?
C16 C17 C18 C19 3.4(3) . . . . ?
C15 N3 C19 C18 -7.3(3) . . . . ?
Pd1 N3 C19 C18 -122.25(17) . . . . ?
C15 N3 C19 C20 165.42(16) . . . . ?
Pd1 N3 C19 C20 50.45(19) . . . . ?
C17 C18 C19 N3 1.8(3) . . . . ?
C17 C18 C19 C20 -170.46(18) . . . . ?
C7 N5 C20 C19 80.9(2) . . . . ?
C6 N5 C20 C19 -63.1(2) . . . . ?
N3 C19 C20 N5 -69.0(2) . . . . ?
C18 C19 C20 N5 103.7(2) . . . . ?
C13 N4 C21 C1 144.50(17) . . . . ?
C14 N4 C21 C1 -87.3(2) . . . . ?
Pd1 N4 C21 C1 31.44(19) . . . . ?
N1 C1 C21 N4 -22.8(2) . . . . ?
C2 C1 C21 N4 160.74(17) . . . . ?

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
# C2 H2 F4  0.95 2.57 3.257(3) 129.7 2_666 
# C13 H13B N1  0.99 2.70 3.550(3) 144.7 2_766 
C2 H2 F2 0.95 2.37 3.307(2) 170.5 2_666
C6 H6B F2 0.99 2.42 3.122(3) 127.3 2_766
C9 H9 F3 0.95 2.49 3.164(3) 127.8 1_655
C11 H11 F3 0.95 2.48 3.366(3) 155.7 .
C14 H14A N5 0.99 2.63 3.594(3) 165.7 1_455
C18 H18 F4 0.95 2.40 3.232(3) 146.4 1_656

_refine_diff_density_max         0.684
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.089

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_l7317
_audit_block_doi                 10.5517/ccdc.csd.cc2dqm6z
_database_code_depnum_ccdc_archive 'CCDC 2226271'
loop_
_citation_id
_citation_doi
_citation_year
1 10.26434/chemrxiv-2023-n18n2 2023
loop_
_audit_author_name
_audit_author_address
'Liviu Mirica'
;University of Illinois at Urbana Champaign
United States of America
;
_audit_update_record             
;
2022-12-13 deposited with the CCDC.	2024-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C23 H26 N5 O2 Pd, C4 H8 O, C2 H3 O2, C2 H4 O2'
_chemical_formula_sum            'C31 H41 N5 O7 Pd'
_chemical_formula_weight         702.09

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

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

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

_cell_length_a                   7.9182(3)
_cell_length_b                   19.5779(9)
_cell_length_c                   20.2624(9)
_cell_angle_alpha                90
_cell_angle_beta                 94.348(2)
_cell_angle_gamma                90
_cell_volume                     3132.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    99(2)
_cell_measurement_reflns_used    9896
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      35.47

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_F_000             1456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.598
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.097
_exptl_absorpt_coefficient_mu    0.647
_shelx_estimated_absorpt_T_min   0.698
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6516
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker AXS Inc.)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      99(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            108458
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.448
_diffrn_reflns_theta_max         35.995
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14216
_reflns_number_gt                10395
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXT-2013 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
  
All  H atoms were positioned geometrically and refined using a 
riding model with C---H = 0.95--0.99 Å and with Uiso(H) 
= 1.2 (1.5 for methyl groups) times Ueq(C). 
  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0259P)²+2.0699P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14216
_refine_ls_number_parameters     402
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0351
_refine_ls_wR_factor_ref         0.0739
_refine_ls_wR_factor_gt          0.0655
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.003
_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 0.08143(2) 0.49682(2) 0.21885(2) 0.00935(3) Uani 1 1 d . . . . .
O1 O 0.13674(13) 0.56601(5) 0.29116(5) 0.0142(2) Uani 1 1 d . . . . .
O2 O -0.12205(16) 0.61100(7) 0.27187(7) 0.0284(3) Uani 1 1 d . . . . .
N1 N -0.13584(14) 0.45374(6) 0.24803(6) 0.0108(2) Uani 1 1 d . . . . .
N2 N 0.11820(15) 0.34947(6) 0.25788(6) 0.0121(2) Uani 1 1 d . . . . .
N3 N 0.27866(14) 0.52888(6) 0.17161(6) 0.0117(2) Uani 1 1 d . . . . .
N4 N 0.03137(14) 0.43852(6) 0.13734(6) 0.0098(2) Uani 1 1 d . . . . .
N5 N -0.01862(16) 0.39269(6) 0.40627(6) 0.0137(2) Uani 1 1 d . . . . .
C1 C -0.18549(17) 0.44190(7) 0.30911(7) 0.0123(2) Uani 1 1 d . . . . .
C2 C -0.34522(18) 0.41489(8) 0.31708(8) 0.0161(3) Uani 1 1 d . . . . .
H2 H -0.3815 0.4085 0.3603 0.019 Uiso 1 1 calc R U . . .
C3 C -0.45160(18) 0.39733(8) 0.26226(8) 0.0177(3) Uani 1 1 d . . . . .
H3 H -0.5630 0.3811 0.2673 0.021 Uiso 1 1 calc R U . . .
C4 C -0.39259(17) 0.40380(8) 0.19988(8) 0.0150(3) Uani 1 1 d . . . . .
H4 H -0.4601 0.3894 0.1616 0.018 Uiso 1 1 calc R U . . .
C5 C -0.23381(16) 0.43154(7) 0.19433(7) 0.0112(2) Uani 1 1 d . . . . .
C6 C -0.15931(16) 0.43934(8) 0.12854(7) 0.0125(2) Uani 1 1 d . . . . .
H6A H -0.1980 0.4829 0.1078 0.015 Uiso 1 1 calc R U . . .
H6B H -0.1992 0.4016 0.0988 0.015 Uiso 1 1 calc R U . . .
C7 C 0.10343(18) 0.36743(7) 0.13973(7) 0.0123(2) Uani 1 1 d . . . . .
H7A H 0.2286 0.3701 0.1418 0.015 Uiso 1 1 calc R U . . .
H7B H 0.0646 0.3429 0.0986 0.015 Uiso 1 1 calc R U . . .
C8 C 0.05118(17) 0.32770(7) 0.19847(7) 0.0117(2) Uani 1 1 d . . . . .
C9 C -0.06745(19) 0.27561(8) 0.19134(8) 0.0159(3) Uani 1 1 d . . . . .
H9 H -0.1117 0.2614 0.1486 0.019 Uiso 1 1 calc R U . . .
C10 C -0.1204(2) 0.24447(8) 0.24805(8) 0.0186(3) Uani 1 1 d . . . . .
H10 H -0.1979 0.2074 0.2448 0.022 Uiso 1 1 calc R U . . .
C11 C -0.0579(2) 0.26874(8) 0.30903(8) 0.0184(3) Uani 1 1 d . . . . .
H11 H -0.0940 0.2493 0.3485 0.022 Uiso 1 1 calc R U . . .
C12 C 0.05936(18) 0.32231(7) 0.31200(7) 0.0133(3) Uani 1 1 d . . . . .
C13 C 0.11803(19) 0.35457(8) 0.37734(7) 0.0151(3) Uani 1 1 d . . . . .
H13A H 0.1601 0.3185 0.4086 0.018 Uiso 1 1 calc R U . . .
H13B H 0.2133 0.3860 0.3707 0.018 Uiso 1 1 calc R U . . .
C14 C -0.06491(18) 0.45573(8) 0.36938(7) 0.0141(3) Uani 1 1 d . . . . .
H14A H 0.0391 0.4775 0.3551 0.017 Uiso 1 1 calc R U . . .
H14B H -0.1187 0.4880 0.3990 0.017 Uiso 1 1 calc R U . . .
C15 C 0.10632(17) 0.47599(8) 0.08158(7) 0.0125(2) Uani 1 1 d . . . . .
H15A H 0.1318 0.4432 0.0465 0.015 Uiso 1 1 calc R U . . .
H15B H 0.0235 0.5096 0.0621 0.015 Uiso 1 1 calc R U . . .
C16 C 0.26592(17) 0.51212(7) 0.10665(7) 0.0118(2) Uani 1 1 d . . . . .
C17 C 0.38884(18) 0.53215(8) 0.06572(8) 0.0147(3) Uani 1 1 d . . . . .
H17 H 0.3770 0.5217 0.0198 0.018 Uiso 1 1 calc R U . . .
C18 C 0.52953(18) 0.56759(8) 0.09235(8) 0.0165(3) Uani 1 1 d . . . . .
H18 H 0.6144 0.5821 0.0647 0.020 Uiso 1 1 calc R U . . .
C19 C 0.54550(18) 0.58172(8) 0.15956(8) 0.0168(3) Uani 1 1 d . . . . .
H19 H 0.6434 0.6042 0.1790 0.020 Uiso 1 1 calc R U . . .
C20 C 0.41623(18) 0.56255(8) 0.19775(8) 0.0153(3) Uani 1 1 d . . . . .
H20 H 0.4245 0.5734 0.2436 0.018 Uiso 1 1 calc R U . . .
C21 C 0.02125(19) 0.61171(8) 0.29935(8) 0.0153(3) Uani 1 1 d D . . . .
C22 C 0.0789(2) 0.66758(9) 0.34743(10) 0.0286(4) Uani 1 1 d D . . . .
H22A H 0.1340 0.6471 0.3876 0.043 Uiso 1 1 calc R U . . .
H22B H -0.0192 0.6944 0.3588 0.043 Uiso 1 1 calc R U . . .
H22C H 0.1595 0.6974 0.3270 0.043 Uiso 1 1 calc R U . . .
C23 C 0.0373(2) 0.41074(9) 0.47488(8) 0.0181(3) Uani 1 1 d . . . . .
H23A H 0.0742 0.3694 0.4992 0.027 Uiso 1 1 calc R U . . .
H23B H -0.0568 0.4318 0.4962 0.027 Uiso 1 1 calc R U . . .
H23C H 0.1318 0.4431 0.4750 0.027 Uiso 1 1 calc R U . . .
O1S O 0.64086(16) 0.43189(7) 0.53465(7) 0.0282(3) Uani 1 1 d . . . . .
C1S C 0.5468(2) 0.37988(10) 0.49917(9) 0.0256(4) Uani 1 1 d . . . . .
H1SA H 0.6220 0.3518 0.4732 0.031 Uiso 1 1 calc R U . . .
H1SB H 0.4572 0.4002 0.4685 0.031 Uiso 1 1 calc R U . . .
C2S C 0.4691(2) 0.33666(9) 0.55139(9) 0.0227(3) Uani 1 1 d . . . . .
H2SA H 0.5428 0.2974 0.5646 0.027 Uiso 1 1 calc R U . . .
H2SB H 0.3560 0.3195 0.5351 0.027 Uiso 1 1 calc R U . . .
C3S C 0.4562(3) 0.38678(10) 0.60934(10) 0.0282(4) Uani 1 1 d . . . . .
H3SA H 0.3366 0.3945 0.6183 0.034 Uiso 1 1 calc R U . . .
H3SB H 0.5188 0.3693 0.6500 0.034 Uiso 1 1 calc R U . . .
C4S C 0.5364(2) 0.45191(9) 0.58573(9) 0.0249(3) Uani 1 1 d . . . . .
H4SA H 0.4480 0.4844 0.5683 0.030 Uiso 1 1 calc R U . . .
H4SB H 0.6052 0.4741 0.6225 0.030 Uiso 1 1 calc R U . . .
O3 O 0.60372(15) 0.11115(6) 0.42883(7) 0.0268(3) Uani 1 1 d . . . . .
O4 O 0.40089(15) 0.15058(7) 0.48779(6) 0.0239(3) Uani 1 1 d . . . . .
C24 C 0.48054(19) 0.14894(8) 0.43510(9) 0.0193(3) Uani 1 1 d D . . . .
C25 C 0.4198(3) 0.19564(11) 0.37876(10) 0.0317(4) Uani 1 1 d D . . . .
H25A H 0.4447 0.2432 0.3912 0.048 Uiso 1 1 calc R U . . .
H25B H 0.2973 0.1901 0.3693 0.048 Uiso 1 1 calc R U . . .
H25C H 0.4779 0.1840 0.3393 0.048 Uiso 1 1 calc R U . . .
O5 O 0.13957(15) 0.21887(6) 0.48241(7) 0.0262(3) Uani 1 1 d . . . . .
H5 H 0.2236 0.1927 0.4876 0.039 Uiso 1 1 calc R U . . .
O6 O 0.03046(17) 0.14648(8) 0.55310(7) 0.0318(3) Uani 1 1 d . . . . .
C26 C 0.0181(2) 0.19575(9) 0.51577(8) 0.0183(3) Uani 1 1 d D . . . .
C27 C -0.1470(2) 0.23307(9) 0.50275(9) 0.0212(3) Uani 1 1 d D . . . .
H27A H -0.2159 0.2100 0.4672 0.032 Uiso 1 1 calc R U . . .
H27B H -0.1247 0.2802 0.4895 0.032 Uiso 1 1 calc R U . . .
H27C H -0.2080 0.2333 0.5431 0.032 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 N3 1.9940(12) . ?
Pd1 O1 2.0191(10) . ?
Pd1 N4 2.0220(12) . ?
Pd1 N1 2.0432(12) . ?
O1 C21 1.2990(18) . ?
O2 C21 1.2256(19) . ?
N1 C1 1.3468(19) . ?
N1 C5 1.3589(18) . ?
N2 C12 1.3342(19) . ?
N2 C8 1.3474(19) . ?
N3 C20 1.3470(18) . ?
N3 C16 1.3529(19) . ?
N4 C7 1.5036(18) . ?
N4 C15 1.5060(18) . ?
N4 C6 1.5070(17) . ?
N5 C23 1.470(2) . ?
N5 C13 1.4723(19) . ?
N5 C14 1.4747(19) . ?
C1 C2 1.392(2) . ?
C1 C14 1.516(2) . ?
C2 C3 1.386(2) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(2) . ?
C3 H3 0.9500 . ?
C4 C5 1.3820(19) . ?
C4 H4 0.9500 . ?
C5 C6 1.506(2) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.506(2) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.386(2) . ?
C9 C10 1.393(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.508(2) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.5027(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.383(2) . ?
C17 C18 1.387(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(2) . ?
C18 H18 0.9500 . ?
C19 C20 1.381(2) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.512(2) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O1S C1S 1.424(2) . ?
O1S C4S 1.428(2) . ?
C1S C2S 1.520(3) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
C2S C3S 1.540(3) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C4S 1.518(3) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9900 . ?
C4S H4SB 0.9900 . ?
O3 C24 1.2384(19) . ?
O4 C24 1.281(2) . ?
C24 C25 1.512(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
O5 C26 1.298(2) . ?
O5 H5 0.8400 . ?
O6 C26 1.225(2) . ?
C26 C27 1.503(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 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
N3 Pd1 O1 90.14(5) . . ?
N3 Pd1 N4 84.13(5) . . ?
O1 Pd1 N4 171.82(5) . . ?
N3 Pd1 N1 167.46(5) . . ?
O1 Pd1 N1 102.01(5) . . ?
N4 Pd1 N1 83.46(5) . . ?
C21 O1 Pd1 116.03(9) . . ?
C1 N1 C5 119.48(12) . . ?
C1 N1 Pd1 130.38(10) . . ?
C5 N1 Pd1 110.02(9) . . ?
C12 N2 C8 118.02(13) . . ?
C20 N3 C16 119.99(12) . . ?
C20 N3 Pd1 127.21(10) . . ?
C16 N3 Pd1 112.79(9) . . ?
C7 N4 C15 107.75(11) . . ?
C7 N4 C6 112.84(11) . . ?
C15 N4 C6 110.75(11) . . ?
C7 N4 Pd1 116.47(9) . . ?
C15 N4 Pd1 105.89(8) . . ?
C6 N4 Pd1 102.90(8) . . ?
C23 N5 C13 108.70(11) . . ?
C23 N5 C14 108.89(12) . . ?
C13 N5 C14 112.61(12) . . ?
N1 C1 C2 120.22(13) . . ?
N1 C1 C14 119.96(12) . . ?
C2 C1 C14 119.78(13) . . ?
C3 C2 C1 120.25(14) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 118.81(14) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 118.80(14) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
N1 C5 C4 121.88(13) . . ?
N1 C5 C6 115.99(12) . . ?
C4 C5 C6 122.13(13) . . ?
C5 C6 N4 110.51(11) . . ?
C5 C6 H6A 109.5 . . ?
N4 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
N4 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N4 C7 C8 112.17(11) . . ?
N4 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
N4 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
N2 C8 C9 122.93(14) . . ?
N2 C8 C7 115.43(12) . . ?
C9 C8 C7 121.47(13) . . ?
C8 C9 C10 118.68(14) . . ?
C8 C9 H9 120.7 . . ?
C10 C9 H9 120.7 . . ?
C11 C10 C9 118.52(14) . . ?
C11 C10 H10 120.7 . . ?
C9 C10 H10 120.7 . . ?
C10 C11 C12 119.25(15) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 H11 120.4 . . ?
N2 C12 C11 122.37(14) . . ?
N2 C12 C13 116.82(13) . . ?
C11 C12 C13 120.73(14) . . ?
N5 C13 C12 112.03(12) . . ?
N5 C13 H13A 109.2 . . ?
C12 C13 H13A 109.2 . . ?
N5 C13 H13B 109.2 . . ?
C12 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
N5 C14 C1 112.07(12) . . ?
N5 C14 H14A 109.2 . . ?
C1 C14 H14A 109.2 . . ?
N5 C14 H14B 109.2 . . ?
C1 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 N4 110.18(11) . . ?
C16 C15 H15A 109.6 . . ?
N4 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
N4 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
N3 C16 C17 120.72(13) . . ?
N3 C16 C15 116.21(12) . . ?
C17 C16 C15 122.90(13) . . ?
C16 C17 C18 119.33(14) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C19 C18 C17 119.55(14) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 118.69(14) . . ?
C20 C19 H19 120.7 . . ?
C18 C19 H19 120.7 . . ?
N3 C20 C19 121.61(14) . . ?
N3 C20 H20 119.2 . . ?
C19 C20 H20 119.2 . . ?
O2 C21 O1 124.79(14) . . ?
O2 C21 C22 121.68(14) . . ?
O1 C21 C22 113.53(13) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N5 C23 H23A 109.5 . . ?
N5 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N5 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C1S O1S C4S 104.62(13) . . ?
O1S C1S C2S 105.68(14) . . ?
O1S C1S H1SA 110.6 . . ?
C2S C1S H1SA 110.6 . . ?
O1S C1S H1SB 110.6 . . ?
C2S C1S H1SB 110.6 . . ?
H1SA C1S H1SB 108.7 . . ?
C1S C2S C3S 103.28(14) . . ?
C1S C2S H2SA 111.1 . . ?
C3S C2S H2SA 111.1 . . ?
C1S C2S H2SB 111.1 . . ?
C3S C2S H2SB 111.1 . . ?
H2SA C2S H2SB 109.1 . . ?
C4S C3S C2S 103.97(14) . . ?
C4S C3S H3SA 111.0 . . ?
C2S C3S H3SA 111.0 . . ?
C4S C3S H3SB 111.0 . . ?
C2S C3S H3SB 111.0 . . ?
H3SA C3S H3SB 109.0 . . ?
O1S C4S C3S 106.07(15) . . ?
O1S C4S H4SA 110.5 . . ?
C3S C4S H4SA 110.5 . . ?
O1S C4S H4SB 110.5 . . ?
C3S C4S H4SB 110.5 . . ?
H4SA C4S H4SB 108.7 . . ?
O3 C24 O4 122.80(16) . . ?
O3 C24 C25 119.46(16) . . ?
O4 C24 C25 117.74(14) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 O5 H5 109.5 . . ?
O6 C26 O5 124.62(15) . . ?
O6 C26 C27 121.26(15) . . ?
O5 C26 C27 114.07(14) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 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 -8.0(2) . . . . ?
Pd1 N1 C1 C2 176.49(11) . . . . ?
C5 N1 C1 C14 169.92(12) . . . . ?
Pd1 N1 C1 C14 -5.6(2) . . . . ?
N1 C1 C2 C3 2.7(2) . . . . ?
C14 C1 C2 C3 -175.21(14) . . . . ?
C1 C2 C3 C4 3.4(2) . . . . ?
C2 C3 C4 C5 -4.0(2) . . . . ?
C1 N1 C5 C4 7.4(2) . . . . ?
Pd1 N1 C5 C4 -176.26(12) . . . . ?
C1 N1 C5 C6 -172.93(12) . . . . ?
Pd1 N1 C5 C6 3.45(15) . . . . ?
C3 C4 C5 N1 -1.3(2) . . . . ?
C3 C4 C5 C6 179.04(14) . . . . ?
N1 C5 C6 N4 26.88(17) . . . . ?
C4 C5 C6 N4 -153.42(13) . . . . ?
C7 N4 C6 C5 84.33(14) . . . . ?
C15 N4 C6 C5 -154.78(12) . . . . ?
Pd1 N4 C6 C5 -42.01(12) . . . . ?
C15 N4 C7 C8 173.88(11) . . . . ?
C6 N4 C7 C8 -63.54(15) . . . . ?
Pd1 N4 C7 C8 55.16(13) . . . . ?
C12 N2 C8 C9 -4.2(2) . . . . ?
C12 N2 C8 C7 171.20(12) . . . . ?
N4 C7 C8 N2 -68.74(15) . . . . ?
N4 C7 C8 C9 106.78(15) . . . . ?
N2 C8 C9 C10 0.2(2) . . . . ?
C7 C8 C9 C10 -174.93(13) . . . . ?
C8 C9 C10 C11 2.7(2) . . . . ?
C9 C10 C11 C12 -1.6(2) . . . . ?
C8 N2 C12 C11 5.4(2) . . . . ?
C8 N2 C12 C13 -171.46(12) . . . . ?
C10 C11 C12 N2 -2.5(2) . . . . ?
C10 C11 C12 C13 174.22(14) . . . . ?
C23 N5 C13 C12 168.84(13) . . . . ?
C14 N5 C13 C12 -70.42(16) . . . . ?
N2 C12 C13 N5 108.97(15) . . . . ?
C11 C12 C13 N5 -67.90(18) . . . . ?
C23 N5 C14 C1 -157.34(12) . . . . ?
C13 N5 C14 C1 82.02(15) . . . . ?
N1 C1 C14 N5 -115.33(14) . . . . ?
C2 C1 C14 N5 62.58(18) . . . . ?
C7 N4 C15 C16 -90.79(13) . . . . ?
C6 N4 C15 C16 145.36(12) . . . . ?
Pd1 N4 C15 C16 34.50(13) . . . . ?
C20 N3 C16 C17 -3.3(2) . . . . ?
Pd1 N3 C16 C17 177.94(11) . . . . ?
C20 N3 C16 C15 -178.71(13) . . . . ?
Pd1 N3 C16 C15 2.50(15) . . . . ?
N4 C15 C16 N3 -25.59(17) . . . . ?
N4 C15 C16 C17 159.08(13) . . . . ?
N3 C16 C17 C18 2.4(2) . . . . ?
C15 C16 C17 C18 177.55(13) . . . . ?
C16 C17 C18 C19 0.7(2) . . . . ?
C17 C18 C19 C20 -2.8(2) . . . . ?
C16 N3 C20 C19 1.0(2) . . . . ?
Pd1 N3 C20 C19 179.62(11) . . . . ?
C18 C19 C20 N3 2.0(2) . . . . ?
Pd1 O1 C21 O2 8.3(2) . . . . ?
Pd1 O1 C21 C22 -172.06(12) . . . . ?
C4S O1S C1S C2S -40.65(17) . . . . ?
O1S C1S C2S C3S 26.24(18) . . . . ?
C1S C2S C3S C4S -3.01(19) . . . . ?
C1S O1S C4S C3S 38.59(18) . . . . ?
C2S C3S C4S O1S -21.05(19) . . . . ?

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
#C6 H6B O4  0.99 2.65 3.4157(19) 134.7 4_565 
#C15 H15A O3  0.99 2.61 3.533(2) 156.1 4_565 
C4 H4 O6 0.95 2.30 3.148(2) 147.6 4_565
C6 H6B O6 0.99 2.45 3.2595(19) 138.1 4_565
C7 H7B O4 0.99 2.51 3.3803(19) 146.6 4_565
C13 H13A O5 0.99 2.47 3.401(2) 156.5 .
C14 H14A O1 0.99 2.33 3.1791(19) 143.3 .
C15 H15B O3 0.99 2.24 3.124(2) 147.8 2
C19 H19 O2 0.95 2.55 3.395(2) 149.0 1_655
C20 H20 O1 0.95 2.54 3.0198(19) 111.1 .
C23 H23B O1S 0.98 2.57 3.474(2) 152.9 1_455
O5 H5 O4 0.84 1.63 2.4590(17) 169.7 .
C27 H27A O3 0.98 2.49 3.375(2) 149.3 1_455

_refine_diff_density_max         0.660
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.099



