# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2018

####################################################################### 
# 
# 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_DATA2a
_database_code_depnum_ccdc_archive 'CCDC 1833099'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_DATA2a              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Due to the poor crystal quality, a lower theta max of diffraction was obtained, even if all possible steps were undertaken to ensure that the experiment was able to extract the best diffracting power from the sample. However, since the solution and refinement parameters are reasonable, we are confident that the crystal structure found is consistent. 
;
_vrf_PLAT213_DATA2a              
;
PROBLEM: Atom Pd1             has ADP max/min Ratio .....        4.3 oblate
RESPONSE: A bit of unavoidable disorder
;
_vrf_PLAT250_DATA2a              
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        5.6 Note
RESPONSE: unavoidable disorder
;
_vrf_PLAT411_DATA2a              
;
PROBLEM: Short Inter H...H Contact  H1E1     ..H1E1             1.94 Ang.
RESPONSE: Usual in similar compounds
;
_vrf_PLAT417_DATA2a              
;
PROBLEM: Short Inter D-H..H-D       H1M      ..H2M              1.97 Ang.
RESPONSE: Disorder is at the origin of that
;
# Added during the CSD deposition process: Monday 28 May 2018 02:36 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C114 H208 N8 O20 Pd2'
_chemical_formula_weight         2223.67

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                   12.0326(5)
_cell_length_b                   14.1370(6)
_cell_length_c                   20.7121(9)
_cell_angle_alpha                70.239(2)
_cell_angle_beta                 76.719(2)
_cell_angle_gamma                70.278(2)
_cell_volume                     3094.6(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      20.2

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             1200
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.354
_shelx_estimated_absorpt_T_min   0.932
_shelx_estimated_absorpt_T_max   0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25226
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.962
_diffrn_reflns_theta_max         21.752
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.650
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.650
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.650
_reflns_number_total             7274
_reflns_number_gt                6261
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1575P)²+5.7060P] 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         7274
_refine_ls_number_parameters     655
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0743
_refine_ls_wR_factor_ref         0.2164
_refine_ls_wR_factor_gt          0.2052
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.068
_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 0.77692(4) 0.88044(3) -0.31857(2) 0.0263(3) Uani 1 1 d . U . . .
N1 N 0.8900(4) 0.8988(4) -0.2681(2) 0.0263(11) Uani 1 1 d . U . . .
O1 O 0.7867(4) 1.0241(3) -0.3772(2) 0.0344(10) Uani 1 1 d . U . . .
O2 O 0.8813(4) 1.1428(3) -0.3936(2) 0.0351(10) Uani 1 1 d . U . . .
O3 O 0.9859(4) 1.0198(3) -0.2759(2) 0.0329(10) Uani 1 1 d . U . . .
C1 C 0.8592(5) 1.0583(5) -0.3616(3) 0.0300(14) Uani 1 1 d D U . . .
C2 C 0.9194(5) 0.9882(5) -0.2962(3) 0.0269(13) Uani 1 1 d D U . . .
C3 C 0.9394(5) 0.8305(4) -0.2063(3) 0.0273(14) Uani 1 1 d . U . . .
C4 C 0.8659(5) 0.8033(4) -0.1455(3) 0.0284(14) Uani 1 1 d . U . . .
H4 H 0.7821 0.8314 -0.1448 0.034 Uiso 1 1 calc R U . . .
C5 C 0.9126(6) 0.7352(5) -0.0851(3) 0.0298(14) Uani 1 1 d . U . . .
H5 H 0.8604 0.7183 -0.0437 0.036 Uiso 1 1 calc R U . . .
C6 C 1.0358(6) 0.6917(5) -0.0852(3) 0.0307(14) Uani 1 1 d . U . . .
C7 C 1.1089(6) 0.7207(5) -0.1464(3) 0.0362(16) Uani 1 1 d . U . . .
H7 H 1.1928 0.6941 -0.1469 0.043 Uiso 1 1 calc R U . . .
C8 C 1.0635(6) 0.7875(5) -0.2071(3) 0.0340(16) Uani 1 1 d . . . . .
H8 H 1.1156 0.8039 -0.2486 0.041 Uiso 1 1 calc R U . . .
C9 C 1.0898(6) 0.6170(5) -0.0237(3) 0.0348(16) Uani 1 1 d . . . . .
H9 H 1.1744 0.5961 -0.0283 0.042 Uiso 1 1 calc R U . . .
C10 C 1.0348(6) 0.5753(5) 0.0372(3) 0.0337(16) Uani 1 1 d . . . . .
H10 H 0.9502 0.5989 0.0430 0.040 Uiso 1 1 calc R U . . .
C11 C 1.0908(6) 0.4960(4) 0.0973(3) 0.0314(15) Uani 1 1 d . . . . .
C12 C 1.0213(6) 0.4624(5) 0.1586(3) 0.0308(15) Uani 1 1 d . . . . .
H12 H 0.9373 0.4914 0.1617 0.037 Uiso 1 1 calc R U . . .
C13 C 1.0708(6) 0.3871(5) 0.2160(3) 0.0295(15) Uani 1 1 d . . . . .
H13 H 1.0208 0.3661 0.2576 0.035 Uiso 1 1 calc R U . . .
C14 C 1.1927(5) 0.3433(4) 0.2123(3) 0.0260(14) Uani 1 1 d . . . . .
C15 C 1.2638(6) 0.3758(5) 0.1506(3) 0.0342(16) Uani 1 1 d . . . . .
H15 H 1.3478 0.3461 0.1476 0.041 Uiso 1 1 calc R U . . .
C16 C 1.2143(6) 0.4503(5) 0.0940(3) 0.0367(16) Uani 1 1 d . . . . .
H16 H 1.2644 0.4710 0.0524 0.044 Uiso 1 1 calc R U . . .
C17 C 1.3216(5) 0.2848(5) 0.2977(3) 0.0293(15) Uani 1 1 d D . . . .
C18 C 1.3710(5) 0.1998(5) 0.3601(3) 0.0278(15) Uani 1 1 d D . . . .
O4 O 1.3377(4) 0.1154(3) 0.3774(2) 0.0285(10) Uani 1 1 d . . . . .
O5 O 1.4395(4) 0.2127(3) 0.3899(2) 0.0339(10) Uani 1 1 d . . . . .
O6 O 1.3485(4) 0.3701(3) 0.2768(2) 0.0371(11) Uani 1 1 d . . . . .
N2 N 1.2444(4) 0.2644(4) 0.2705(2) 0.0263(12) Uani 1 1 d . . . . .
N3 N 1.2148(5) 0.6815(4) -0.7481(3) 0.0422(14) Uani 1 1 d . . . . .
C19 C 1.2477(6) 0.7780(5) -0.7519(4) 0.0435(18) Uani 1 1 d . . . . .
H19A H 1.2002 0.8389 -0.7847 0.052 Uiso 1 1 calc R U . . .
H19B H 1.2234 0.7905 -0.7058 0.052 Uiso 1 1 calc R U . . .
C20 C 1.3771(7) 0.7752(6) -0.7736(4) 0.054(2) Uani 1 1 d . . . . .
H20A H 1.4048 0.7594 -0.8187 0.065 Uiso 1 1 calc R U . . .
H20B H 1.4258 0.7192 -0.7390 0.065 Uiso 1 1 calc R U . . .
C21 C 1.3924(8) 0.8815(7) -0.7798(5) 0.063(2) Uani 1 1 d . . . . .
H21A H 1.3424 0.9369 -0.8140 0.076 Uiso 1 1 calc R U . . .
H21B H 1.3637 0.8967 -0.7346 0.076 Uiso 1 1 calc R U . . .
C22 C 1.5168(9) 0.8856(9) -0.8011(5) 0.084(3) Uani 1 1 d . . . . .
H22A H 1.5210 0.9550 -0.8041 0.126 Uiso 1 1 calc R U . . .
H22B H 1.5453 0.8725 -0.8465 0.126 Uiso 1 1 calc R U . . .
H22C H 1.5668 0.8320 -0.7670 0.126 Uiso 1 1 calc R U . . .
C23 C 1.2562(7) 0.6530(6) -0.8154(4) 0.0498(19) Uani 1 1 d . . . . .
H23A H 1.3444 0.6308 -0.8224 0.060 Uiso 1 1 calc R U . . .
H23B H 1.2294 0.5920 -0.8111 0.060 Uiso 1 1 calc R U . . .
C24 C 1.2133(8) 0.7386(7) -0.8785(4) 0.065(2) Uani 1 1 d . . . . .
H24A H 1.1255 0.7561 -0.8738 0.077 Uiso 1 1 calc R U . . .
H24B H 1.2335 0.8020 -0.8806 0.077 Uiso 1 1 calc R U . . .
C25 C 1.2650(9) 0.7108(8) -0.9446(5) 0.078(3) Uani 1 1 d . . . . .
H25A H 1.2434 0.6486 -0.9434 0.093 Uiso 1 1 calc R U . . .
H25B H 1.3530 0.6926 -0.9495 0.093 Uiso 1 1 calc R U . . .
C26 C 1.2204(10) 0.8004(9) -1.0060(5) 0.086(3) Uani 1 1 d . . . . .
H26A H 1.2560 0.7801 -1.0486 0.129 Uiso 1 1 calc R U . . .
H26B H 1.2427 0.8618 -1.0075 0.129 Uiso 1 1 calc R U . . .
H26C H 1.1335 0.8176 -1.0016 0.129 Uiso 1 1 calc R U . . .
C27 C 1.0794(6) 0.7073(5) -0.7307(4) 0.0411(17) Uani 1 1 d . . . . .
H27A H 1.0573 0.7192 -0.6845 0.049 Uiso 1 1 calc R U . . .
H27B H 1.0439 0.7739 -0.7645 0.049 Uiso 1 1 calc R U . . .
C28 C 1.0240(6) 0.6259(5) -0.7306(4) 0.0431(17) Uani 1 1 d . . . . .
H28A H 1.0687 0.5556 -0.7043 0.052 Uiso 1 1 calc R U . . .
H28B H 1.0278 0.6250 -0.7786 0.052 Uiso 1 1 calc R U . . .
C29 C 0.8937(7) 0.6516(6) -0.6971(4) 0.0468(18) Uani 1 1 d . . . . .
H29A H 0.8921 0.6431 -0.6475 0.056 Uiso 1 1 calc R U . . .
H29B H 0.8538 0.7260 -0.7189 0.056 Uiso 1 1 calc R U . . .
C30 C 0.8235(7) 0.5848(6) -0.7030(4) 0.056(2) Uani 1 1 d . . . . .
H30A H 0.7418 0.6060 -0.6804 0.084 Uiso 1 1 calc R U . . .
H30B H 0.8609 0.5109 -0.6805 0.084 Uiso 1 1 calc R U . . .
H30C H 0.8223 0.5942 -0.7520 0.084 Uiso 1 1 calc R U . . .
C31 C 1.2757(7) 0.5873(5) -0.6916(4) 0.0430(18) Uani 1 1 d . . . . .
H31A H 1.2643 0.5234 -0.6955 0.052 Uiso 1 1 calc R U . . .
H31B H 1.3622 0.5796 -0.7010 0.052 Uiso 1 1 calc R U . . .
C32 C 1.2337(6) 0.5916(5) -0.6183(4) 0.0378(17) Uani 1 1 d . . . . .
H32A H 1.1520 0.5843 -0.6045 0.045 Uiso 1 1 calc R U . . .
H32B H 1.2318 0.6603 -0.6148 0.045 Uiso 1 1 calc R U . . .
C33 C 1.3166(6) 0.5040(5) -0.5698(4) 0.0446(18) Uani 1 1 d . . . . .
H33C H 1.3258 0.4363 -0.5777 0.053 Uiso 1 1 calc R U . . .
H33B H 1.3961 0.5161 -0.5807 0.053 Uiso 1 1 calc R U . . .
C34 C 1.2705(8) 0.4978(6) -0.4949(4) 0.061(2) Uani 1 1 d . . . . .
H34A H 1.3262 0.4406 -0.4656 0.091 Uiso 1 1 calc R U . . .
H34B H 1.1925 0.4844 -0.4837 0.091 Uiso 1 1 calc R U . . .
H34C H 1.2628 0.5642 -0.4867 0.091 Uiso 1 1 calc R U . . .
N4 N 1.2786(4) 0.0639(4) -0.4005(2) 0.0266(12) Uani 1 1 d . . . . .
C35 C 1.2811(5) -0.0190(5) -0.4329(3) 0.0270(14) Uani 1 1 d . . . . .
H35A H 1.2919 0.0104 -0.4839 0.032 Uiso 1 1 calc R U . . .
H35B H 1.3517 -0.0795 -0.4204 0.032 Uiso 1 1 calc R U . . .
C36 C 1.1729(6) -0.0586(5) -0.4125(3) 0.0317(15) Uani 1 1 d . . . . .
H36A H 1.1019 0.0003 -0.4267 0.038 Uiso 1 1 calc R U . . .
H36B H 1.1601 -0.0876 -0.3615 0.038 Uiso 1 1 calc R U . . .
C37 C 1.1885(6) -0.1431(5) -0.4465(3) 0.0379(16) Uani 1 1 d . . . . .
H37A H 1.2630 -0.1992 -0.4350 0.045 Uiso 1 1 calc R U . . .
H37B H 1.1961 -0.1124 -0.4974 0.045 Uiso 1 1 calc R U . . .
C38 C 1.0845(8) -0.1907(7) -0.4233(5) 0.065(2) Uani 1 1 d . . . . .
H38A H 1.0984 -0.2446 -0.4464 0.097 Uiso 1 1 calc R U . . .
H38B H 1.0107 -0.1358 -0.4354 0.097 Uiso 1 1 calc R U . . .
H38C H 1.0776 -0.2225 -0.3730 0.097 Uiso 1 1 calc R U . . .
C39 C 1.3960(5) 0.0914(5) -0.4294(3) 0.0286(14) Uani 1 1 d . . . . .
H39A H 1.4619 0.0265 -0.4169 0.034 Uiso 1 1 calc R U . . .
H39B H 1.4016 0.1153 -0.4805 0.034 Uiso 1 1 calc R U . . .
C40 C 1.4155(6) 0.1737(5) -0.4059(3) 0.0359(16) Uani 1 1 d . . . . .
H40A H 1.4166 0.1494 -0.3552 0.043 Uiso 1 1 calc R U . . .
H40B H 1.3498 0.2392 -0.4169 0.043 Uiso 1 1 calc R U . . .
C41 C 1.5325(6) 0.1939(5) -0.4423(3) 0.0348(16) Uani 1 1 d . . . . .
H41A H 1.5961 0.1266 -0.4331 0.042 Uiso 1 1 calc R U . . .
H41B H 1.5289 0.2195 -0.4928 0.042 Uiso 1 1 calc R U . . .
C42 C 1.5663(7) 0.2717(6) -0.4214(4) 0.052(2) Uani 1 1 d . . . . .
H42A H 1.6432 0.2801 -0.4473 0.078 Uiso 1 1 calc R U . . .
H42B H 1.5724 0.2463 -0.3717 0.078 Uiso 1 1 calc R U . . .
H42C H 1.5052 0.3395 -0.4315 0.078 Uiso 1 1 calc R U . . .
C43 C 1.2623(5) 0.0253(5) -0.3222(3) 0.0285(14) Uani 1 1 d . . . . .
H43A H 1.1859 0.0073 -0.3065 0.034 Uiso 1 1 calc R U . . .
H43B H 1.2562 0.0834 -0.3039 0.034 Uiso 1 1 calc R U . . .
C44 C 1.3612(6) -0.0699(5) -0.2904(3) 0.0336(15) Uani 1 1 d . . . . .
H44A H 1.4384 -0.0532 -0.3046 0.040 Uiso 1 1 calc R U . . .
H44B H 1.3677 -0.1297 -0.3071 0.040 Uiso 1 1 calc R U . . .
C45 C 1.3323(6) -0.0996(5) -0.2111(3) 0.0393(17) Uani 1 1 d . . . . .
H45A H 1.3210 -0.0382 -0.1948 0.047 Uiso 1 1 calc R U . . .
H45B H 1.2572 -0.1198 -0.1970 0.047 Uiso 1 1 calc R U . . .
C46 C 1.4325(7) -0.1901(7) -0.1779(4) 0.060(2) Uani 1 1 d . . . . .
H46A H 1.4128 -0.2081 -0.1274 0.089 Uiso 1 1 calc R U . . .
H46B H 1.5065 -0.1696 -0.1913 0.089 Uiso 1 1 calc R U . . .
H46C H 1.4429 -0.2511 -0.1935 0.089 Uiso 1 1 calc R U . . .
C47 C 1.1722(5) 0.1607(4) -0.4178(3) 0.0279(14) Uani 1 1 d . . . . .
H47A H 1.0983 0.1389 -0.3994 0.034 Uiso 1 1 calc R U . . .
H47B H 1.1718 0.2102 -0.3935 0.034 Uiso 1 1 calc R U . . .
C48 C 1.1693(5) 0.2185(5) -0.4946(3) 0.0321(15) Uani 1 1 d . . . . .
H48A H 1.2451 0.2365 -0.5149 0.038 Uiso 1 1 calc R U . . .
H48B H 1.1601 0.1729 -0.5191 0.038 Uiso 1 1 calc R U . . .
C49 C 1.0658(6) 0.3180(5) -0.5034(3) 0.0345(15) Uani 1 1 d . . . . .
H49A H 1.0727 0.3612 -0.4764 0.041 Uiso 1 1 calc R U . . .
H49B H 0.9900 0.2994 -0.4853 0.041 Uiso 1 1 calc R U . . .
C50 C 1.0647(6) 0.3811(5) -0.5794(4) 0.0414(17) Uani 1 1 d . . . . .
H50A H 0.9974 0.4447 -0.5839 0.062 Uiso 1 1 calc R U . . .
H50B H 1.0568 0.3386 -0.6061 0.062 Uiso 1 1 calc R U . . .
H50C H 1.1393 0.4004 -0.5971 0.062 Uiso 1 1 calc R U . . .
O1E O 1.7113(9) 0.8237(7) -0.9539(5) 0.122(3) Uani 1 1 d . . . . .
C1E C 1.6364(16) 0.8970(12) -1.0114(8) 0.158(7) Uani 1 1 d D . . . .
H1E1 H 1.5824 0.9591 -0.9972 0.190 Uiso 1 1 calc R U . . .
H1E2 H 1.6887 0.9213 -1.0541 0.190 Uiso 1 1 calc R U . . .
C2E C 1.5650(12) 0.8375(13) -1.0245(8) 0.141(6) Uani 1 1 d D . . . .
H2E1 H 1.5154 0.8835 -1.0610 0.211 Uiso 1 1 calc R U . . .
H2E2 H 1.5139 0.8135 -0.9820 0.211 Uiso 1 1 calc R U . . .
H2E3 H 1.6191 0.7769 -1.0393 0.211 Uiso 1 1 calc R U . . .
C3E C 1.7977(16) 0.8625(14) -0.9280(9) 0.202(11) Uani 1 1 d D . . . .
H3E1 H 1.8696 0.8589 -0.9629 0.243 Uiso 1 1 calc R U . . .
H3E2 H 1.7584 0.9380 -0.9330 0.243 Uiso 1 1 calc R U . . .
C4E C 1.8415(14) 0.8211(17) -0.8619(11) 0.270(17) Uani 1 1 d D . . . .
H4E1 H 1.8969 0.8581 -0.8614 0.405 Uiso 1 1 calc R U . . .
H4E2 H 1.8829 0.7462 -0.8541 0.405 Uiso 1 1 calc R U . . .
H4E3 H 1.7745 0.8307 -0.8252 0.405 Uiso 1 1 calc R U . . .
O3M O 1.0145(5) 1.0488(4) -0.1611(3) 0.0635(16) Uani 1 1 d . . . . .
H3M H 1.0131 1.0281 -0.1944 0.095 Uiso 1 1 calc R U . . .
C3M C 0.9764(14) 0.9836(8) -0.1001(5) 0.111(5) Uani 1 1 d . . . . .
H3M1 H 1.0343 0.9140 -0.0919 0.167 Uiso 1 1 calc R U . . .
H3M2 H 0.8989 0.9779 -0.1030 0.167 Uiso 1 1 calc R U . . .
H3M3 H 0.9690 1.0124 -0.0619 0.167 Uiso 1 1 calc R U . . .
O1M O 1.5453(7) 0.4165(6) 0.2710(5) 0.118(3) Uani 1 1 d . . . . .
H1M H 1.5357 0.3729 0.2551 0.177 Uiso 1 1 calc R U . . .
C1M C 1.6253(8) 0.3657(8) 0.3182(6) 0.081(3) Uani 1 1 d . . . . .
H1M1 H 1.6904 0.3984 0.3050 0.121 Uiso 1 1 calc R U . . .
H1M2 H 1.6576 0.2918 0.3190 0.121 Uiso 1 1 calc R U . . .
H1M3 H 1.5851 0.3707 0.3643 0.121 Uiso 1 1 calc R U . . .
O2M O 1.5655(8) 0.5452(8) 0.1456(6) 0.148(4) Uani 1 1 d . . . . .
H2M H 1.5699 0.4948 0.1819 0.223 Uiso 1 1 calc R U . . .
C2M C 1.6614(12) 0.5788(11) 0.1321(9) 0.138(6) Uani 1 1 d . . . . .
H2M1 H 1.6502 0.6447 0.0947 0.207 Uiso 1 1 calc R U . . .
H2M2 H 1.7313 0.5261 0.1179 0.207 Uiso 1 1 calc R U . . .
H2M3 H 1.6736 0.5905 0.1737 0.207 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 O1 2.011(4) . ?
Pd1 O4 2.014(4) 2_765 ?
Pd1 N1 2.022(5) . ?
Pd1 N2 2.027(5) 2_765 ?
Pd1 Pd1 14.7058(10) 2_765 ?
N1 C2 1.331(8) . ?
N1 C3 1.431(8) . ?
O1 C1 1.272(8) . ?
O2 C1 1.239(7) . ?
O3 C2 1.241(7) . ?
C1 C2 1.550(8) . ?
C3 C4 1.381(9) . ?
C3 C8 1.407(9) . ?
C4 C5 1.397(8) . ?
C5 C6 1.401(9) . ?
C6 C7 1.388(9) . ?
C6 C9 1.473(9) . ?
C7 C8 1.390(9) . ?
C9 C10 1.326(9) . ?
C10 C11 1.480(9) . ?
C11 C12 1.381(9) . ?
C11 C16 1.403(9) . ?
C12 C13 1.394(9) . ?
C13 C14 1.381(9) . ?
C14 C15 1.393(9) . ?
C14 N2 1.432(7) . ?
C15 C16 1.379(9) . ?
C17 O6 1.262(7) . ?
C17 N2 1.340(8) . ?
C17 C18 1.512(8) . ?
C18 O5 1.227(7) . ?
C18 O4 1.296(7) . ?
O4 Pd1 2.014(4) 2_765 ?
N2 Pd1 2.027(5) 2_765 ?
N3 C23 1.509(9) . ?
N3 C19 1.517(9) . ?
N3 C27 1.528(9) . ?
N3 C31 1.537(9) . ?
C19 C20 1.509(10) . ?
C20 C21 1.535(11) . ?
C21 C22 1.475(12) . ?
C23 C24 1.503(11) . ?
C24 C25 1.491(12) . ?
C25 C26 1.509(13) . ?
C27 C28 1.511(10) . ?
C28 C29 1.535(10) . ?
C29 C30 1.511(10) . ?
C31 C32 1.500(10) . ?
C32 C33 1.523(10) . ?
C33 C34 1.506(11) . ?
N4 C43 1.515(7) . ?
N4 C35 1.524(7) . ?
N4 C39 1.526(8) . ?
N4 C47 1.528(7) . ?
C35 C36 1.505(8) . ?
C36 C37 1.522(9) . ?
C37 C38 1.524(10) . ?
C39 C40 1.506(9) . ?
C40 C41 1.507(9) . ?
C41 C42 1.507(9) . ?
C43 C44 1.530(9) . ?
C44 C45 1.539(9) . ?
C45 C46 1.520(10) . ?
C47 C48 1.525(8) . ?
C48 C49 1.520(9) . ?
C49 C50 1.525(9) . ?
O1E C1E 1.527(17) . ?
O1E C3E 1.585(16) . ?
C1E C2E 1.507(15) . ?
C3E C4E 1.442(16) . ?
O3M C3M 1.374(12) . ?
O1M C1M 1.375(11) . ?
O2M C2M 1.331(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 O4 90.20(16) . 2_765 ?
O1 Pd1 N1 81.23(17) . . ?
O4 Pd1 N1 171.39(17) 2_765 . ?
O1 Pd1 N2 171.72(17) . 2_765 ?
O4 Pd1 N2 81.74(17) 2_765 2_765 ?
N1 Pd1 N2 106.85(18) . 2_765 ?
O1 Pd1 Pd1 137.09(12) . 2_765 ?
O4 Pd1 Pd1 132.45(11) 2_765 2_765 ?
N1 Pd1 Pd1 56.03(13) . 2_765 ?
N2 Pd1 Pd1 51.13(13) 2_765 2_765 ?
C2 N1 C3 116.6(5) . . ?
C2 N1 Pd1 114.4(4) . . ?
C3 N1 Pd1 129.0(4) . . ?
C1 O1 Pd1 115.4(4) . . ?
O2 C1 O1 124.8(5) . . ?
O2 C1 C2 119.4(5) . . ?
O1 C1 C2 115.7(5) . . ?
O3 C2 N1 128.0(5) . . ?
O3 C2 C1 119.0(5) . . ?
N1 C2 C1 113.0(5) . . ?
C4 C3 C8 118.9(5) . . ?
C4 C3 N1 120.4(5) . . ?
C8 C3 N1 120.6(5) . . ?
C3 C4 C5 121.2(6) . . ?
C4 C5 C6 120.4(6) . . ?
C7 C6 C5 117.9(5) . . ?
C7 C6 C9 119.4(6) . . ?
C5 C6 C9 122.7(6) . . ?
C6 C7 C8 122.2(6) . . ?
C7 C8 C3 119.3(6) . . ?
C10 C9 C6 127.8(6) . . ?
C9 C10 C11 127.0(6) . . ?
C12 C11 C16 117.6(5) . . ?
C12 C11 C10 120.3(6) . . ?
C16 C11 C10 122.0(6) . . ?
C11 C12 C13 122.0(6) . . ?
C14 C13 C12 119.9(6) . . ?
C13 C14 C15 118.8(5) . . ?
C13 C14 N2 120.4(5) . . ?
C15 C14 N2 120.8(5) . . ?
C16 C15 C14 121.0(6) . . ?
C15 C16 C11 120.7(6) . . ?
O6 C17 N2 124.2(5) . . ?
O6 C17 C18 120.4(5) . . ?
N2 C17 C18 115.3(5) . . ?
O5 C18 O4 124.4(5) . . ?
O5 C18 C17 120.0(6) . . ?
O4 C18 C17 115.5(5) . . ?
C18 O4 Pd1 114.7(3) . 2_765 ?
C17 N2 C14 117.7(5) . . ?
C17 N2 Pd1 112.7(4) . 2_765 ?
C14 N2 Pd1 129.6(4) . 2_765 ?
C23 N3 C19 111.5(5) . . ?
C23 N3 C27 111.2(5) . . ?
C19 N3 C27 106.5(5) . . ?
C23 N3 C31 107.2(5) . . ?
C19 N3 C31 109.9(5) . . ?
C27 N3 C31 110.6(5) . . ?
C20 C19 N3 116.8(6) . . ?
C19 C20 C21 109.7(6) . . ?
C22 C21 C20 113.2(8) . . ?
C24 C23 N3 115.4(6) . . ?
C25 C24 C23 113.8(7) . . ?
C24 C25 C26 111.2(8) . . ?
C28 C27 N3 116.3(5) . . ?
C27 C28 C29 109.7(5) . . ?
C30 C29 C28 114.6(6) . . ?
C32 C31 N3 116.5(5) . . ?
C31 C32 C33 110.3(6) . . ?
C34 C33 C32 112.1(6) . . ?
C43 N4 C35 111.9(4) . . ?
C43 N4 C39 112.1(4) . . ?
C35 N4 C39 105.9(4) . . ?
C43 N4 C47 104.4(4) . . ?
C35 N4 C47 111.5(4) . . ?
C39 N4 C47 111.2(4) . . ?
C36 C35 N4 116.0(5) . . ?
C35 C36 C37 110.6(5) . . ?
C36 C37 C38 112.4(6) . . ?
C40 C39 N4 116.6(5) . . ?
C39 C40 C41 108.9(5) . . ?
C42 C41 C40 114.8(6) . . ?
N4 C43 C44 115.4(5) . . ?
C43 C44 C45 109.3(5) . . ?
C46 C45 C44 110.5(6) . . ?
C48 C47 N4 115.4(5) . . ?
C49 C48 C47 109.5(5) . . ?
C48 C49 C50 110.8(5) . . ?
C1E O1E C3E 120.8(12) . . ?
C2E C1E O1E 108.1(13) . . ?
C4E C3E O1E 127.6(15) . . ?

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
O3M H3M O3 0.84 1.84 2.658(7) 164.4 .
O1M H1M O6 0.84 2.20 2.630(8) 111.4 .
O2M H2M O1M 0.84 1.82 2.632(13) 162.4 .

_refine_diff_density_max         2.193
_refine_diff_density_min         -1.672
_refine_diff_density_rms         0.144

_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_DATA4a
_database_code_depnum_ccdc_archive 'CCDC 1833101'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H192 N8 O20 Pd2'
_chemical_formula_weight         2135.48

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                   10.4534(7)
_cell_length_b                   14.7803(10)
_cell_length_c                   20.3003(13)
_cell_angle_alpha                102.903(2)
_cell_angle_beta                 102.983(2)
_cell_angle_gamma                105.397(2)
_cell_volume                     2809.8(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    8721
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      22.3

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             1148
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.388
_shelx_estimated_absorpt_T_min   0.906
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.904
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37656
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.151
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             9868
_reflns_number_gt                9054
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0562P)²+1.7150P] 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         9868
_refine_ls_number_parameters     630
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_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 0.55484(2) 0.38726(2) 0.30842(2) 0.01348(6) Uani 1 1 d . . . . .
O1 O 0.59462(15) 0.52872(10) 0.36055(7) 0.0196(3) Uani 1 1 d . . . . .
O2 O 0.50210(15) 0.64867(10) 0.36658(8) 0.0206(3) Uani 1 1 d . . . . .
O3 O 0.29165(15) 0.53144(10) 0.24430(8) 0.0199(3) Uani 1 1 d . . . . .
N1 N 0.39132(17) 0.40921(12) 0.24734(9) 0.0158(4) Uani 1 1 d . . . . .
C1 C 0.5015(2) 0.56605(15) 0.33859(10) 0.0161(4) Uani 1 1 d D . . . .
C2 C 0.3819(2) 0.49880(15) 0.27108(10) 0.0158(4) Uani 1 1 d D . . . .
C3 C 0.2849(2) 0.34230(14) 0.18565(10) 0.0155(4) Uani 1 1 d . . . . .
C4 C 0.3183(2) 0.30223(15) 0.12544(11) 0.0169(4) Uani 1 1 d . . . . .
H4 H 0.4125 0.3218 0.1253 0.020 Uiso 1 1 calc R U . . .
C5 C 0.2163(2) 0.23436(15) 0.06586(11) 0.0185(4) Uani 1 1 d . . . . .
H5 H 0.2410 0.2077 0.0254 0.022 Uiso 1 1 calc R U . . .
C6 C 0.0768(2) 0.20471(14) 0.06493(11) 0.0169(4) Uani 1 1 d . . . . .
C7 C 0.0430(2) 0.24670(15) 0.12491(11) 0.0198(4) Uani 1 1 d . . . . .
H7 H -0.0514 0.2288 0.1247 0.024 Uiso 1 1 calc R U . . .
C8 C 0.1455(2) 0.31392(15) 0.18439(11) 0.0186(4) Uani 1 1 d . . . . .
H8 H 0.1210 0.3411 0.2248 0.022 Uiso 1 1 calc R U . . .
C9 C -0.0290(2) 0.13018(15) 0.00506(11) 0.0190(4) Uani 1 1 d . . . . .
C10 C -0.1167(2) 0.06476(15) -0.04324(11) 0.0193(4) Uani 1 1 d . . . . .
C11 C -0.2232(2) -0.01469(15) -0.09981(11) 0.0182(4) Uani 1 1 d . . . . .
C12 C -0.1943(2) -0.05957(15) -0.16070(11) 0.0186(4) Uani 1 1 d . . . . .
H12 H -0.1031 -0.0377 -0.1647 0.022 Uiso 1 1 calc R U . . .
C13 C -0.2982(2) -0.13585(15) -0.21520(11) 0.0170(4) Uani 1 1 d . . . . .
H13 H -0.2774 -0.1661 -0.2561 0.020 Uiso 1 1 calc R U . . .
C14 C -0.4329(2) -0.16843(14) -0.21042(10) 0.0156(4) Uani 1 1 d . . . . .
C15 C -0.4614(2) -0.12488(15) -0.14962(11) 0.0183(4) Uani 1 1 d . . . . .
H15 H -0.5526 -0.1473 -0.1457 0.022 Uiso 1 1 calc R U . . .
C16 C -0.3584(2) -0.04938(15) -0.09495(11) 0.0202(4) Uani 1 1 d . . . . .
H16 H -0.3792 -0.0206 -0.0537 0.024 Uiso 1 1 calc R U . . .
C17 C -0.6483(2) -0.22250(15) -0.29834(11) 0.0172(4) Uani 1 1 d D . . . .
C18 C -0.7601(2) -0.30848(15) -0.35902(10) 0.0171(4) Uani 1 1 d D . . . .
N2 N -0.53919(17) -0.24538(12) -0.26727(9) 0.0152(3) Uani 1 1 d . . . . .
O6 O -0.66303(15) -0.14021(10) -0.28355(8) 0.0233(3) Uani 1 1 d . . . . .
O5 O -0.86972(15) -0.29863(11) -0.38834(8) 0.0216(3) Uani 1 1 d . . . . .
O4 O -0.72809(14) -0.38748(10) -0.37615(7) 0.0180(3) Uani 1 1 d . . . . .
N3 N 0.47326(18) 0.82458(12) 0.23292(9) 0.0182(4) Uani 1 1 d . . . . .
C19 C 0.5136(2) 0.73179(15) 0.22879(11) 0.0197(4) Uani 1 1 d . . . . .
H19A H 0.5094 0.7134 0.2725 0.024 Uiso 1 1 calc R U . . .
H19B H 0.4431 0.6776 0.1883 0.024 Uiso 1 1 calc R U . . .
C20 C 0.6569(2) 0.73939(17) 0.22022(13) 0.0261(5) Uani 1 1 d . . . . .
H20A H 0.7298 0.7864 0.2635 0.031 Uiso 1 1 calc R U . . .
H20B H 0.6668 0.7643 0.1796 0.031 Uiso 1 1 calc R U . . .
C21 C 0.6760(3) 0.63813(18) 0.20762(13) 0.0288(5) Uani 1 1 d . . . . .
H21A H 0.7737 0.6465 0.2087 0.035 Uiso 1 1 calc R U . . .
H21B H 0.6600 0.6124 0.2472 0.035 Uiso 1 1 calc R U . . .
C22 C 0.5809(3) 0.5624(2) 0.13851(16) 0.0426(7) Uani 1 1 d . . . . .
H22A H 0.5996 0.5002 0.1348 0.064 Uiso 1 1 calc R U . . .
H22B H 0.5979 0.5860 0.0988 0.064 Uiso 1 1 calc R U . . .
H22C H 0.4837 0.5521 0.1372 0.064 Uiso 1 1 calc R U . . .
C23 C 0.4577(2) 0.84915(16) 0.16352(11) 0.0220(5) Uani 1 1 d . . . . .
H23A H 0.5467 0.8572 0.1523 0.026 Uiso 1 1 calc R U . . .
H23B H 0.4420 0.9133 0.1704 0.026 Uiso 1 1 calc R U . . .
C24 C 0.3410(3) 0.7742(2) 0.09987(12) 0.0316(6) Uani 1 1 d . . . . .
H24A H 0.3362 0.7069 0.1013 0.038 Uiso 1 1 calc R U . . .
H24B H 0.2510 0.7825 0.1021 0.038 Uiso 1 1 calc R U . . .
C25 C 0.3653(3) 0.78699(19) 0.03079(12) 0.0323(6) Uani 1 1 d . . . . .
H25A H 0.2770 0.7526 -0.0082 0.039 Uiso 1 1 calc R U . . .
H25B H 0.3924 0.8578 0.0345 0.039 Uiso 1 1 calc R U . . .
C26 C 0.4774(3) 0.7475(2) 0.01232(13) 0.0409(7) Uani 1 1 d . . . . .
H26A H 0.4889 0.7585 -0.0322 0.061 Uiso 1 1 calc R U . . .
H26B H 0.4498 0.6768 0.0069 0.061 Uiso 1 1 calc R U . . .
H26C H 0.5655 0.7818 0.0504 0.061 Uiso 1 1 calc R U . . .
C27 C 0.3368(2) 0.80235(16) 0.25065(11) 0.0202(4) Uani 1 1 d . . . . .
H27A H 0.3526 0.7878 0.2965 0.024 Uiso 1 1 calc R U . . .
H27B H 0.2690 0.7421 0.2140 0.024 Uiso 1 1 calc R U . . .
C28 C 0.2717(2) 0.88359(16) 0.25562(11) 0.0226(5) Uani 1 1 d . . . . .
H28A H 0.2240 0.8830 0.2074 0.027 Uiso 1 1 calc R U . . .
H28B H 0.3451 0.9485 0.2798 0.027 Uiso 1 1 calc R U . . .
C29 C 0.1666(3) 0.86674(18) 0.29746(13) 0.0284(5) Uani 1 1 d . . . . .
H29A H 0.1039 0.7975 0.2777 0.034 Uiso 1 1 calc R U . . .
H29B H 0.2178 0.8769 0.3473 0.034 Uiso 1 1 calc R U . . .
C30 C 0.0793(3) 0.9338(2) 0.29604(14) 0.0344(6) Uani 1 1 d . . . . .
H30A H 0.0152 0.9195 0.3238 0.052 Uiso 1 1 calc R U . . .
H30B H 0.0260 0.9228 0.2469 0.052 Uiso 1 1 calc R U . . .
H30C H 0.1404 1.0026 0.3164 0.052 Uiso 1 1 calc R U . . .
C31 C 0.5849(2) 0.91318(15) 0.28901(11) 0.0197(4) Uani 1 1 d . . . . .
H31A H 0.5620 0.9730 0.2851 0.024 Uiso 1 1 calc R U . . .
H31B H 0.6747 0.9193 0.2789 0.024 Uiso 1 1 calc R U . . .
C32 C 0.6034(2) 0.90993(16) 0.36487(11) 0.0218(5) Uani 1 1 d . . . . .
H32A H 0.6062 0.8444 0.3676 0.026 Uiso 1 1 calc R U . . .
H32B H 0.5237 0.9209 0.3800 0.026 Uiso 1 1 calc R U . . .
C33 C 0.7385(2) 0.98924(17) 0.41392(12) 0.0265(5) Uani 1 1 d . . . . .
H33A H 0.7408 1.0534 0.4062 0.032 Uiso 1 1 calc R U . . .
H33B H 0.8186 0.9733 0.4024 0.032 Uiso 1 1 calc R U . . .
C34 C 0.7512(3) 0.99698(18) 0.49176(12) 0.0310(5) Uani 1 1 d . . . . .
H34A H 0.8379 1.0490 0.5221 0.047 Uiso 1 1 calc R U . . .
H34B H 0.7519 0.9341 0.4998 0.047 Uiso 1 1 calc R U . . .
H34C H 0.6719 1.0128 0.5032 0.047 Uiso 1 1 calc R U . . .
N4 N 0.10576(17) 0.61112(12) 0.40034(9) 0.0157(4) Uani 1 1 d . . . . .
C35 C -0.0022(2) 0.64541(15) 0.42868(11) 0.0177(4) Uani 1 1 d . . . . .
H35A H -0.0869 0.5876 0.4163 0.021 Uiso 1 1 calc R U . . .
H35B H 0.0348 0.6704 0.4811 0.021 Uiso 1 1 calc R U . . .
C36 C -0.0441(2) 0.72455(17) 0.40200(12) 0.0232(5) Uani 1 1 d . . . . .
H36A H -0.0900 0.6988 0.3501 0.028 Uiso 1 1 calc R U . . .
H36B H 0.0397 0.7819 0.4116 0.028 Uiso 1 1 calc R U . . .
C37 C -0.1445(2) 0.75649(17) 0.43940(12) 0.0252(5) Uani 1 1 d . . . . .
H37A H -0.1885 0.7952 0.4136 0.030 Uiso 1 1 calc R U . . .
H37B H -0.2193 0.6969 0.4364 0.030 Uiso 1 1 calc R U . . .
C38 C -0.0776(3) 0.81700(18) 0.51638(13) 0.0306(5) Uani 1 1 d . . . . .
H38A H -0.1483 0.8342 0.5362 0.046 Uiso 1 1 calc R U . . .
H38B H -0.0052 0.8773 0.5200 0.046 Uiso 1 1 calc R U . . .
H38C H -0.0358 0.7788 0.5429 0.046 Uiso 1 1 calc R U . . .
C39 C 0.2421(2) 0.69502(15) 0.41993(11) 0.0176(4) Uani 1 1 d . . . . .
H39A H 0.3053 0.6700 0.3970 0.021 Uiso 1 1 calc R U . . .
H39B H 0.2230 0.7469 0.3998 0.021 Uiso 1 1 calc R U . . .
C40 C 0.3180(2) 0.74191(15) 0.49862(11) 0.0201(4) Uani 1 1 d . . . . .
H40A H 0.3340 0.6907 0.5205 0.024 Uiso 1 1 calc R U . . .
H40B H 0.2604 0.7732 0.5220 0.024 Uiso 1 1 calc R U . . .
C41 C 0.4570(2) 0.81899(16) 0.50938(11) 0.0223(5) Uani 1 1 d . . . . .
H41A H 0.4403 0.8703 0.4879 0.027 Uiso 1 1 calc R U . . .
H41B H 0.5134 0.7876 0.4851 0.027 Uiso 1 1 calc R U . . .
C42 C 0.5376(2) 0.86686(17) 0.58818(12) 0.0275(5) Uani 1 1 d . . . . .
H42A H 0.6261 0.9162 0.5935 0.041 Uiso 1 1 calc R U . . .
H42B H 0.5560 0.8164 0.6093 0.041 Uiso 1 1 calc R U . . .
H42C H 0.4824 0.8987 0.6122 0.041 Uiso 1 1 calc R U . . .
C43 C 0.0578(2) 0.57276(15) 0.31969(10) 0.0176(4) Uani 1 1 d . . . . .
H43A H 0.0409 0.6262 0.3009 0.021 Uiso 1 1 calc R U . . .
H43B H 0.1342 0.5566 0.3039 0.021 Uiso 1 1 calc R U . . .
C44 C -0.0726(2) 0.48276(16) 0.28735(11) 0.0210(5) Uani 1 1 d . . . . .
H44A H -0.1508 0.4977 0.3020 0.025 Uiso 1 1 calc R U . . .
H44B H -0.0569 0.4278 0.3046 0.025 Uiso 1 1 calc R U . . .
C45 C -0.1093(2) 0.45270(17) 0.20646(11) 0.0229(5) Uani 1 1 d . . . . .
H45A H -0.1333 0.5054 0.1891 0.027 Uiso 1 1 calc R U . . .
H45B H -0.0276 0.4442 0.1922 0.027 Uiso 1 1 calc R U . . .
C46 C -0.2320(3) 0.35671(19) 0.17289(12) 0.0334(6) Uani 1 1 d . . . . .
H46A H -0.2541 0.3388 0.1212 0.050 Uiso 1 1 calc R U . . .
H46B H -0.3132 0.3654 0.1865 0.050 Uiso 1 1 calc R U . . .
H46C H -0.2076 0.3043 0.1894 0.050 Uiso 1 1 calc R U . . .
C47 C 0.1272(2) 0.53147(15) 0.43343(10) 0.0165(4) Uani 1 1 d . . . . .
H47A H 0.1551 0.5595 0.4856 0.020 Uiso 1 1 calc R U . . .
H47B H 0.0369 0.4778 0.4188 0.020 Uiso 1 1 calc R U . . .
C48 C 0.2346(2) 0.48732(15) 0.41467(11) 0.0186(4) Uani 1 1 d . . . . .
H48A H 0.3243 0.5403 0.4257 0.022 Uiso 1 1 calc R U . . .
H48B H 0.2033 0.4520 0.3633 0.022 Uiso 1 1 calc R U . . .
C49 C 0.2535(2) 0.41620(16) 0.45711(11) 0.0200(4) Uani 1 1 d . . . . .
H49A H 0.2850 0.4524 0.5083 0.024 Uiso 1 1 calc R U . . .
H49B H 0.1626 0.3647 0.4466 0.024 Uiso 1 1 calc R U . . .
C50 C 0.3583(2) 0.36731(17) 0.44045(13) 0.0271(5) Uani 1 1 d . . . . .
H50A H 0.3670 0.3227 0.4691 0.041 Uiso 1 1 calc R U . . .
H50B H 0.4490 0.4179 0.4515 0.041 Uiso 1 1 calc R U . . .
H50C H 0.3265 0.3299 0.3900 0.041 Uiso 1 1 calc R U . . .
C1M C -1.0056(3) -0.16488(19) -0.29322(15) 0.0378(6) Uani 1 1 d . . . . .
H1M1 H -0.9933 -0.2278 -0.3126 0.057 Uiso 1 1 calc R U . . .
H1M2 H -1.0899 -0.1614 -0.3240 0.057 Uiso 1 1 calc R U . . .
H1M3 H -1.0146 -0.1595 -0.2456 0.057 Uiso 1 1 calc R U . . .
O1M O -0.88887(17) -0.08670(12) -0.28956(9) 0.0307(4) Uani 1 1 d . . . . .
H1M H -0.8232 -0.1080 -0.2935 0.046 Uiso 1 1 calc R U . . .
C2M C -0.7708(3) 0.0058(2) -0.11045(16) 0.0469(7) Uani 1 1 d . . . . .
H2M1 H -0.7004 -0.0245 -0.1181 0.070 Uiso 1 1 calc R U . . .
H2M2 H -0.8574 -0.0455 -0.1159 0.070 Uiso 1 1 calc R U . . .
H2M3 H -0.7374 0.0521 -0.0625 0.070 Uiso 1 1 calc R U . . .
O2M O -0.7955(2) 0.05629(13) -0.16052(9) 0.0357(4) Uani 1 1 d . . . . .
H2M H -0.8190 0.0173 -0.2016 0.054 Uiso 1 1 calc R U . . .
C3M C 0.1389(3) 0.4753(2) 0.06190(15) 0.0478(7) Uani 1 1 d . . . . .
H3M1 H 0.1274 0.4979 0.0197 0.072 Uiso 1 1 calc R U . . .
H3M2 H 0.0546 0.4216 0.0560 0.072 Uiso 1 1 calc R U . . .
H3M3 H 0.2188 0.4518 0.0681 0.072 Uiso 1 1 calc R U . . .
O3M O 0.16168(19) 0.55414(13) 0.12218(9) 0.0349(4) Uani 1 1 d . . . . .
H3M H 0.1928 0.5400 0.1590 0.052 Uiso 1 1 calc R U . . .
C4M C -0.0687(3) 0.7054(2) 0.10557(16) 0.0441(7) Uani 1 1 d . . . . .
H4M1 H -0.0898 0.7627 0.1292 0.066 Uiso 1 1 calc R U . . .
H4M2 H -0.1550 0.6552 0.0729 0.066 Uiso 1 1 calc R U . . .
H4M3 H -0.0043 0.7254 0.0790 0.066 Uiso 1 1 calc R U . . .
O4M O -0.0068(2) 0.66648(16) 0.15695(11) 0.0492(5) Uani 1 1 d . . . . .
H4M H 0.0290 0.6269 0.1383 0.074 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 O1 2.0042(14) . ?
Pd1 O4 2.0116(14) 2 ?
Pd1 N1 2.0215(17) . ?
Pd1 N2 2.0239(17) 2 ?
Pd1 Pd1 14.9200(8) 2 ?
O1 C1 1.285(3) . ?
O2 C1 1.224(2) . ?
O3 C2 1.243(3) . ?
N1 C2 1.342(3) . ?
N1 C3 1.422(3) . ?
C1 C2 1.547(3) . ?
C3 C4 1.395(3) . ?
C3 C8 1.397(3) . ?
C4 C5 1.385(3) . ?
C5 C6 1.401(3) . ?
C6 C7 1.402(3) . ?
C6 C9 1.437(3) . ?
C7 C8 1.383(3) . ?
C9 C10 1.200(3) . ?
C10 C11 1.437(3) . ?
C11 C12 1.403(3) . ?
C11 C16 1.404(3) . ?
C12 C13 1.388(3) . ?
C13 C14 1.395(3) . ?
C14 C15 1.393(3) . ?
C14 N2 1.424(3) . ?
C15 C16 1.382(3) . ?
C17 O6 1.245(3) . ?
C17 N2 1.338(3) . ?
C17 C18 1.538(3) . ?
C18 O5 1.228(3) . ?
C18 O4 1.294(3) . ?
N2 Pd1 2.0239(16) 2 ?
O4 Pd1 2.0116(14) 2 ?
N3 C31 1.516(3) . ?
N3 C23 1.516(3) . ?
N3 C27 1.519(3) . ?
N3 C19 1.529(3) . ?
C19 C20 1.524(3) . ?
C20 C21 1.535(3) . ?
C21 C22 1.513(4) . ?
C23 C24 1.523(3) . ?
C24 C25 1.523(3) . ?
C25 C26 1.522(3) . ?
C27 C28 1.525(3) . ?
C28 C29 1.535(3) . ?
C29 C30 1.516(3) . ?
C31 C32 1.522(3) . ?
C32 C33 1.525(3) . ?
C33 C34 1.531(3) . ?
N4 C47 1.521(3) . ?
N4 C39 1.521(2) . ?
N4 C43 1.523(2) . ?
N4 C35 1.525(3) . ?
C35 C36 1.517(3) . ?
C36 C37 1.536(3) . ?
C37 C38 1.511(3) . ?
C39 C40 1.518(3) . ?
C40 C41 1.525(3) . ?
C41 C42 1.530(3) . ?
C43 C44 1.518(3) . ?
C44 C45 1.530(3) . ?
C45 C46 1.527(3) . ?
C47 C48 1.517(3) . ?
C48 C49 1.525(3) . ?
C49 C50 1.522(3) . ?
C1M O1M 1.415(3) . ?
C2M O2M 1.407(3) . ?
C3M O3M 1.413(3) . ?
C4M O4M 1.415(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
O1 Pd1 O4 89.89(6) . 2 ?
O1 Pd1 N1 81.59(6) . . ?
O4 Pd1 N1 171.36(6) 2 . ?
O1 Pd1 N2 171.50(6) . 2 ?
O4 Pd1 N2 81.65(6) 2 2 ?
N1 Pd1 N2 106.90(7) . 2 ?
O1 Pd1 Pd1 136.88(4) . 2 ?
O4 Pd1 Pd1 133.21(4) 2 2 ?
N1 Pd1 Pd1 55.36(5) . 2 ?
N2 Pd1 Pd1 51.56(5) 2 2 ?
C1 O1 Pd1 115.47(12) . . ?
C2 N1 C3 117.07(17) . . ?
C2 N1 Pd1 113.91(13) . . ?
C3 N1 Pd1 128.97(13) . . ?
O2 C1 O1 125.15(19) . . ?
O2 C1 C2 119.49(18) . . ?
O1 C1 C2 115.36(17) . . ?
O3 C2 N1 127.38(18) . . ?
O3 C2 C1 119.26(17) . . ?
N1 C2 C1 113.34(17) . . ?
C4 C3 C8 118.69(18) . . ?
C4 C3 N1 120.32(18) . . ?
C8 C3 N1 120.97(18) . . ?
C5 C4 C3 120.96(19) . . ?
C4 C5 C6 120.40(19) . . ?
C5 C6 C7 118.57(18) . . ?
C5 C6 C9 121.02(19) . . ?
C7 C6 C9 120.37(19) . . ?
C8 C7 C6 120.68(19) . . ?
C7 C8 C3 120.68(19) . . ?
C10 C9 C6 176.9(2) . . ?
C9 C10 C11 178.5(2) . . ?
C12 C11 C16 118.60(18) . . ?
C12 C11 C10 120.90(19) . . ?
C16 C11 C10 120.50(19) . . ?
C13 C12 C11 120.37(19) . . ?
C12 C13 C14 120.54(19) . . ?
C15 C14 C13 119.22(18) . . ?
C15 C14 N2 120.78(18) . . ?
C13 C14 N2 120.00(18) . . ?
C16 C15 C14 120.59(19) . . ?
C15 C16 C11 120.66(19) . . ?
O6 C17 N2 126.18(19) . . ?
O6 C17 C18 119.90(18) . . ?
N2 C17 C18 113.90(17) . . ?
O5 C18 O4 124.63(19) . . ?
O5 C18 C17 119.99(18) . . ?
O4 C18 C17 115.37(17) . . ?
C17 N2 C14 116.17(16) . . ?
C17 N2 Pd1 113.64(13) . 2 ?
C14 N2 Pd1 130.18(13) . 2 ?
C18 O4 Pd1 114.57(12) . 2 ?
C31 N3 C23 106.25(16) . . ?
C31 N3 C27 111.35(16) . . ?
C23 N3 C27 111.44(16) . . ?
C31 N3 C19 111.08(16) . . ?
C23 N3 C19 111.31(16) . . ?
C27 N3 C19 105.51(15) . . ?
C20 C19 N3 115.93(17) . . ?
C19 C20 C21 110.17(18) . . ?
C22 C21 C20 114.8(2) . . ?
N3 C23 C24 115.91(18) . . ?
C25 C24 C23 110.9(2) . . ?
C26 C25 C24 113.3(2) . . ?
N3 C27 C28 115.76(17) . . ?
C27 C28 C29 109.24(18) . . ?
C30 C29 C28 113.7(2) . . ?
N3 C31 C32 114.94(17) . . ?
C31 C32 C33 109.75(18) . . ?
C32 C33 C34 111.11(19) . . ?
C47 N4 C39 110.69(15) . . ?
C47 N4 C43 111.67(15) . . ?
C39 N4 C43 105.43(15) . . ?
C47 N4 C35 105.75(15) . . ?
C39 N4 C35 111.74(15) . . ?
C43 N4 C35 111.69(15) . . ?
C36 C35 N4 116.04(17) . . ?
C35 C36 C37 109.76(18) . . ?
C38 C37 C36 114.66(19) . . ?
C40 C39 N4 116.08(17) . . ?
C39 C40 C41 109.77(17) . . ?
C40 C41 C42 111.29(18) . . ?
C44 C43 N4 115.23(16) . . ?
C43 C44 C45 109.71(17) . . ?
C46 C45 C44 110.71(18) . . ?
C48 C47 N4 115.74(16) . . ?
C47 C48 C49 109.27(17) . . ?
C50 C49 C48 112.58(18) . . ?

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
O1M H1M O6 0.84 1.84 2.668(2) 168.6 .
O2M H2M O1M 0.84 1.92 2.750(2) 170.9 .
O3M H3M O3 0.84 1.86 2.684(2) 168.5 .
O4M H4M O3M 0.84 2.01 2.819(3) 162.2 .

_refine_diff_density_max         0.618
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.057


_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_DATA3a
_database_code_depnum_ccdc_archive 'CCDC 1833100'
_audit_update_record             
;
2018-05-28 deposited with the CCDC.
2018-07-04 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_DATA3a              
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       5.38 Report
RESPONSE: Ripples being near the heavy Pd(1) atoms.
;
_vrf_PLAT097_DATA3a              
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       5.19 eA-3
RESPONSE: ripples being near the heavy Pd(1) atoms.
;
_vrf_PLAT990_DATA3a              
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note
RESPONSE: ABIN command in the last refinement gave an higher R factor thus has not been used 
;
# Added during the CSD deposition process: Monday 28 May 2018 02:36 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H192 N12 O20 Pd2'
_chemical_formula_weight         2143.48

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                   11.9627(13)
_cell_length_b                   14.2598(16)
_cell_length_c                   20.435(2)
_cell_angle_alpha                69.618(5)
_cell_angle_beta                 89.594(5)
_cell_angle_gamma                69.736(5)
_cell_volume                     3039.8(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5690
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      23.9

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_F_000             1152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.359
_shelx_estimated_absorpt_T_min   0.919
_shelx_estimated_absorpt_T_max   0.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            50895
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.958
_diffrn_reflns_theta_max         24.433
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.890
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.890
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.890
_reflns_number_total             9807
_reflns_number_gt                8638
_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 APEX'
_computing_cell_refinement       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1656P)²+17.9469P] 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         9807
_refine_ls_number_parameters     587
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0934
_refine_ls_wR_factor_ref         0.2659
_refine_ls_wR_factor_gt          0.2602
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.022
_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 1.22478(4) 0.43483(4) 0.18634(2) 0.0326(2) Uani 1 1 d . . . . .
O1 O 1.2160(4) 0.3490(4) 0.1280(2) 0.0405(11) Uani 1 1 d . . . . .
C1 C 1.1442(6) 0.2977(6) 0.1448(3) 0.0363(15) Uani 1 1 d . . . . .
O2 O 1.1226(4) 0.2455(4) 0.1131(3) 0.0437(12) Uani 1 1 d . . . . .
O3 O 1.0190(4) 0.2499(4) 0.2341(3) 0.0408(11) Uani 1 1 d . . . . .
C2 C 1.0840(6) 0.3029(6) 0.2119(3) 0.0363(15) Uani 1 1 d . . . . .
N1 N 1.1127(5) 0.3650(5) 0.2400(3) 0.0351(12) Uani 1 1 d . . . . .
C3 C 1.0640(6) 0.3725(6) 0.3027(3) 0.0345(14) Uani 1 1 d . . . . .
C4 C 1.1391(7) 0.3412(6) 0.3635(4) 0.0385(15) Uani 1 1 d . . . . .
H4A H 1.2237 0.3129 0.3639 0.046 Uiso 1 1 calc R U . . .
C5 C 1.0917(7) 0.3508(6) 0.4248(4) 0.0404(16) Uani 1 1 d . . . . .
H5A H 1.1437 0.3298 0.4664 0.048 Uiso 1 1 calc R U . . .
C6 C 0.9667(7) 0.3917(6) 0.4240(4) 0.0395(16) Uani 1 1 d . . . . .
C7 C 0.8923(7) 0.4217(7) 0.3634(4) 0.0454(18) Uani 1 1 d . . . . .
H7A H 0.8077 0.4487 0.3632 0.055 Uiso 1 1 calc R U . . .
C8 C 0.9390(7) 0.4132(6) 0.3027(4) 0.0422(17) Uani 1 1 d . . . . .
H8A H 0.8865 0.4348 0.2611 0.051 Uiso 1 1 calc R U . . .
N3 N 0.9071(6) 0.4095(5) 0.4824(3) 0.0442(15) Uani 1 1 d . . . . .
N4 N 0.9775(6) 0.3836(5) 0.5364(3) 0.0436(14) Uani 1 1 d . . . . .
C11 C 0.9139(7) 0.4058(6) 0.5935(4) 0.0408(16) Uani 1 1 d . . . . .
C12 C 0.9855(7) 0.3791(6) 0.6547(4) 0.0415(17) Uani 1 1 d . . . . .
H12A H 1.0704 0.3472 0.6578 0.050 Uiso 1 1 calc R U . . .
C13 C 0.9330(7) 0.3990(6) 0.7126(4) 0.0386(15) Uani 1 1 d . . . . .
H13A H 0.9823 0.3812 0.7546 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8093(7) 0.4446(6) 0.7082(3) 0.0373(15) Uani 1 1 d . . . . .
C15 C 0.7368(7) 0.4722(6) 0.6458(4) 0.0412(16) Uani 1 1 d . . . . .
H15A H 0.6520 0.5052 0.6422 0.049 Uiso 1 1 calc R U . . .
C16 C 0.7903(7) 0.4509(7) 0.5889(4) 0.0465(18) Uani 1 1 d . . . . .
H16A H 0.7415 0.4675 0.5469 0.056 Uiso 1 1 calc R U . . .
N2 N 0.7553(5) 0.4670(5) 0.7666(3) 0.0343(12) Uani 1 1 d . . . . .
C17 C 0.6795(6) 0.4175(6) 0.7939(3) 0.0366(15) Uani 1 1 d . . . . .
O6 O 0.6505(5) 0.3555(4) 0.7742(3) 0.0460(12) Uani 1 1 d . . . . .
O5 O 0.5583(4) 0.4015(4) 0.8892(2) 0.0412(11) Uani 1 1 d . . . . .
C18 C 0.6275(6) 0.4438(6) 0.8585(3) 0.0356(15) Uani 1 1 d . . . . .
O4 O 0.6623(4) 0.5092(4) 0.8751(2) 0.0378(11) Uani 1 1 d . . . . .
N5 N 0.7255(5) 0.3323(5) 0.0986(3) 0.0339(12) Uani 1 1 d . . . . .
C19 C 0.6066(6) 0.3346(6) 0.0704(3) 0.0366(15) Uani 1 1 d . . . . .
H19A H 0.5408 0.3856 0.0846 0.044 Uiso 1 1 calc R U . . .
H19B H 0.5989 0.3640 0.0183 0.044 Uiso 1 1 calc R U . . .
C20 C 0.5870(6) 0.2295(6) 0.0929(4) 0.0428(16) Uani 1 1 d . . . . .
H20A H 0.5871 0.2013 0.1446 0.051 Uiso 1 1 calc R U . . .
H20B H 0.6531 0.1761 0.0807 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4675(7) 0.2466(6) 0.0562(4) 0.0449(17) Uani 1 1 d . . . . .
H21A H 0.4032 0.3029 0.0672 0.054 Uiso 1 1 calc R U . . .
H21B H 0.4695 0.2742 0.0048 0.054 Uiso 1 1 calc R U . . .
C22 C 0.4342(8) 0.1483(8) 0.0755(6) 0.065(2) Uani 1 1 d . . . . .
H22A H 0.3562 0.1674 0.0493 0.097 Uiso 1 1 calc R U . . .
H22B H 0.4293 0.1212 0.1261 0.097 Uiso 1 1 calc R U . . .
H22C H 0.4956 0.0926 0.0635 0.097 Uiso 1 1 calc R U . . .
C23 C 0.8323(6) 0.2543(6) 0.0801(4) 0.0377(15) Uani 1 1 d . . . . .
H23A H 0.9066 0.2582 0.0981 0.045 Uiso 1 1 calc R U . . .
H23B H 0.8342 0.1806 0.1056 0.045 Uiso 1 1 calc R U . . .
C24 C 0.8354(6) 0.2715(6) 0.0028(4) 0.0388(15) Uani 1 1 d . . . . .
H24A H 0.8414 0.3422 -0.0230 0.047 Uiso 1 1 calc R U . . .
H24B H 0.7600 0.2716 -0.0169 0.047 Uiso 1 1 calc R U . . .
C25 C 0.9415(7) 0.1836(6) -0.0071(4) 0.0439(17) Uani 1 1 d . . . . .
H25A H 0.9366 0.1128 0.0201 0.053 Uiso 1 1 calc R U . . .
H25B H 1.0169 0.1848 0.0116 0.053 Uiso 1 1 calc R U . . .
C26 C 0.9448(8) 0.1973(7) -0.0849(4) 0.055(2) Uani 1 1 d . . . . .
H26A H 1.0143 0.1390 -0.0892 0.083 Uiso 1 1 calc R U . . .
H26B H 0.9515 0.2666 -0.1117 0.083 Uiso 1 1 calc R U . . .
H26C H 0.8709 0.1950 -0.1034 0.083 Uiso 1 1 calc R U . . .
C27 C 0.7229(6) 0.4464(6) 0.0667(3) 0.0345(14) Uani 1 1 d . . . . .
H27A H 0.7119 0.4691 0.0148 0.041 Uiso 1 1 calc R U . . .
H27B H 0.6517 0.4940 0.0798 0.041 Uiso 1 1 calc R U . . .
C28 C 0.8320(7) 0.4643(6) 0.0878(4) 0.0409(16) Uani 1 1 d . . . . .
H28A H 0.9040 0.4191 0.0738 0.049 Uiso 1 1 calc R U . . .
H28B H 0.8442 0.4427 0.1396 0.049 Uiso 1 1 calc R U . . .
C29 C 0.8164(7) 0.5821(7) 0.0527(4) 0.0470(18) Uani 1 1 d . . . . .
H29A H 0.8062 0.6027 0.0010 0.056 Uiso 1 1 calc R U . . .
H29B H 0.7425 0.6270 0.0655 0.056 Uiso 1 1 calc R U . . .
C30 C 0.9222(9) 0.6046(8) 0.0741(6) 0.073(3) Uani 1 1 d . . . . .
H30A H 0.9084 0.6811 0.0503 0.110 Uiso 1 1 calc R U . . .
H30B H 0.9953 0.5614 0.0607 0.110 Uiso 1 1 calc R U . . .
H30C H 0.9317 0.5857 0.1252 0.110 Uiso 1 1 calc R U . . .
C31 C 0.7409(6) 0.2911(6) 0.1791(3) 0.0379(15) Uani 1 1 d . . . . .
H31A H 0.7447 0.2159 0.1971 0.045 Uiso 1 1 calc R U . . .
H31B H 0.8191 0.2902 0.1955 0.045 Uiso 1 1 calc R U . . .
C32 C 0.6440(7) 0.3546(6) 0.2117(4) 0.0427(16) Uani 1 1 d . . . . .
H32A H 0.5654 0.3539 0.1976 0.051 Uiso 1 1 calc R U . . .
H32B H 0.6387 0.4302 0.1945 0.051 Uiso 1 1 calc R U . . .
C33 C 0.6720(8) 0.3063(8) 0.2914(4) 0.054(2) Uani 1 1 d . . . . .
H33A H 0.7488 0.3103 0.3054 0.065 Uiso 1 1 calc R U . . .
H33B H 0.6819 0.2295 0.3082 0.065 Uiso 1 1 calc R U . . .
C34 C 0.5722(10) 0.3651(10) 0.3265(5) 0.080(3) Uani 1 1 d . . . . .
H34A H 0.5933 0.3319 0.3777 0.121 Uiso 1 1 calc R U . . .
H34B H 0.4964 0.3600 0.3135 0.121 Uiso 1 1 calc R U . . .
H34C H 0.5632 0.4409 0.3106 0.121 Uiso 1 1 calc R U . . .
N6 N 0.7809(7) 0.0660(6) 0.7465(5) 0.065(2) Uani 1 1 d . . . . .
C35 C 0.7388(10) 0.1628(9) 0.6760(5) 0.071(3) Uani 1 1 d . . . . .
H35A H 0.6499 0.1942 0.6692 0.085 Uiso 1 1 calc R U . . .
H35B H 0.7684 0.2182 0.6787 0.085 Uiso 1 1 calc R U . . .
C36 C 0.7813(13) 0.1352(9) 0.6115(7) 0.091(4) Uani 1 1 d . . . . .
H36A H 0.8699 0.0992 0.6192 0.109 Uiso 1 1 calc R U . . .
H36B H 0.7463 0.0845 0.6059 0.109 Uiso 1 1 calc R U . . .
C37 C 0.7452(13) 0.2340(11) 0.5454(7) 0.093(4) Uani 1 1 d . . . . .
H37A H 0.6565 0.2684 0.5362 0.111 Uiso 1 1 calc R U . . .
H37B H 0.7775 0.2862 0.5514 0.111 Uiso 1 1 calc R U . . .
C38 C 0.7899(19) 0.2064(18) 0.4875(9) 0.160(8) Uani 1 1 d . . . . .
H38A H 0.7647 0.2712 0.4446 0.241 Uiso 1 1 calc R U . . .
H38B H 0.7581 0.1545 0.4818 0.241 Uiso 1 1 calc R U . . .
H38C H 0.8779 0.1744 0.4961 0.241 Uiso 1 1 calc R U . . .
C39 C 0.7498(9) -0.0234(8) 0.7422(6) 0.065(2) Uani 1 1 d . . . . .
H39A H 0.7783 -0.0837 0.7882 0.078 Uiso 1 1 calc R U . . .
H39B H 0.7951 -0.0483 0.7069 0.078 Uiso 1 1 calc R U . . .
C40 C 0.6198(9) -0.0001(8) 0.7235(6) 0.072(3) Uani 1 1 d . . . . .
H40A H 0.5898 0.0600 0.6774 0.086 Uiso 1 1 calc R U . . .
H40B H 0.5734 0.0225 0.7592 0.086 Uiso 1 1 calc R U . . .
C41 C 0.5990(10) -0.1004(9) 0.7194(7) 0.081(3) Uani 1 1 d . . . . .
H41A H 0.6487 -0.1249 0.6853 0.097 Uiso 1 1 calc R U . . .
H41B H 0.6263 -0.1595 0.7661 0.097 Uiso 1 1 calc R U . . .
C42 C 0.4781(12) -0.0799(11) 0.6991(7) 0.096(4) Uani 1 1 d . . . . .
H42A H 0.4706 -0.1455 0.6977 0.145 Uiso 1 1 calc R U . . .
H42B H 0.4511 -0.0229 0.6523 0.145 Uiso 1 1 calc R U . . .
H42C H 0.4285 -0.0569 0.7331 0.145 Uiso 1 1 calc R U . . .
C43 C 0.7303(9) 0.1065(7) 0.8029(5) 0.064(2) Uani 1 1 d . . . . .
H43A H 0.7549 0.1675 0.7992 0.076 Uiso 1 1 calc R U . . .
H43B H 0.6416 0.1358 0.7923 0.076 Uiso 1 1 calc R U . . .
C44 C 0.7627(9) 0.0301(7) 0.8779(5) 0.063(2) Uani 1 1 d . . . . .
H44A H 0.8478 0.0142 0.8931 0.076 Uiso 1 1 calc R U . . .
H44B H 0.7554 -0.0383 0.8806 0.076 Uiso 1 1 calc R U . . .
C45 C 0.6864(9) 0.0711(9) 0.9278(6) 0.072(3) Uani 1 1 d . . . . .
H45A H 0.6839 0.1442 0.9206 0.087 Uiso 1 1 calc R U . . .
H45B H 0.6033 0.0762 0.9176 0.087 Uiso 1 1 calc R U . . .
C46 C 0.7331(11) 0.0002(11) 1.0019(7) 0.088(3) Uani 1 1 d . . . . .
H46A H 0.6812 0.0293 1.0329 0.132 Uiso 1 1 calc R U . . .
H46B H 0.8148 -0.0038 1.0124 0.132 Uiso 1 1 calc R U . . .
H46C H 0.7344 -0.0720 1.0095 0.132 Uiso 1 1 calc R U . . .
C47 C 0.9210(8) 0.0245(7) 0.7603(6) 0.064(2) Uani 1 1 d . . . . .
H47A H 0.9475 -0.0362 0.8062 0.077 Uiso 1 1 calc R U . . .
H47B H 0.9537 -0.0046 0.7238 0.077 Uiso 1 1 calc R U . . .
C48 C 0.9783(9) 0.1041(7) 0.7610(6) 0.067(2) Uani 1 1 d . . . . .
H48A H 0.9325 0.1483 0.7874 0.080 Uiso 1 1 calc R U . . .
H48B H 0.9751 0.1529 0.7122 0.080 Uiso 1 1 calc R U . . .
C49 C 1.1098(9) 0.0450(7) 0.7956(5) 0.065(2) Uani 1 1 d . . . . .
H49A H 1.1106 0.0046 0.8461 0.078 Uiso 1 1 calc R U . . .
H49B H 1.1506 -0.0081 0.7740 0.078 Uiso 1 1 calc R U . . .
C50 C 1.1810(10) 0.1152(9) 0.7897(6) 0.078(3) Uani 1 1 d . . . . .
H50A H 1.2634 0.0704 0.8125 0.117 Uiso 1 1 calc R U . . .
H50B H 1.1439 0.1661 0.8128 0.117 Uiso 1 1 calc R U . . .
H50C H 1.1821 0.1550 0.7399 0.117 Uiso 1 1 calc R U . . .
C1M C 0.3661(14) 0.3193(13) 0.8197(8) 0.112(5) Uiso 1 1 d . . . . .
H1M1 H 0.4101 0.2826 0.8673 0.169 Uiso 1 1 calc R U . . .
H1M2 H 0.3129 0.2831 0.8136 0.169 Uiso 1 1 calc R U . . .
H1M3 H 0.3181 0.3943 0.8125 0.169 Uiso 1 1 calc R U . . .
O1M O 0.4457(15) 0.3166(13) 0.7716(9) 0.183(6) Uiso 1 1 d . . . . .
H1M H 0.4888 0.3506 0.7753 0.274 Uiso 1 1 calc R U . . .
C2M C 0.331(2) 0.3006(19) 0.6153(13) 0.174(9) Uiso 1 1 d . . . . .
H2M1 H 0.2948 0.2625 0.6535 0.261 Uiso 1 1 calc R U . . .
H2M2 H 0.3350 0.2734 0.5771 0.261 Uiso 1 1 calc R U . . .
H2M3 H 0.2830 0.3778 0.5975 0.261 Uiso 1 1 calc R U . . .
O2M O 0.443(3) 0.284(2) 0.6397(15) 0.299(12) Uiso 1 1 d . . . . .
H2M H 0.4416 0.2949 0.6777 0.358 Uiso 1 1 calc R U . . .
C3M C 1.0561(19) 0.1105(17) 0.4114(11) 0.155(7) Uiso 1 1 d . . . . .
H3M1 H 1.0840 0.0378 0.4474 0.232 Uiso 1 1 calc R U . . .
H3M2 H 1.0035 0.1614 0.4307 0.232 Uiso 1 1 calc R U . . .
H3M3 H 1.1254 0.1305 0.3967 0.232 Uiso 1 1 calc R U . . .
O3M O 0.9953(8) 0.1129(7) 0.3557(4) 0.086(2) Uiso 1 1 d . . . . .
H3M H 1.0126 0.1510 0.3185 0.129 Uiso 1 1 calc R U . . .
C4M C 0.8455(19) -0.0764(17) 0.4063(11) 0.157(7) Uiso 1 1 d . . . . .
H4M1 H 0.8240 -0.0598 0.4485 0.235 Uiso 1 1 calc R U . . .
H4M2 H 0.9289 -0.1268 0.4152 0.235 Uiso 1 1 calc R U . . .
H4M3 H 0.7921 -0.1088 0.3949 0.235 Uiso 1 1 calc R U . . .
O4M O 0.8327(19) 0.0234(17) 0.3470(11) 0.233(8) Uiso 1 1 d . . . . .
H4M H 0.8858 0.0461 0.3540 0.280 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 O1 2.009(5) . ?
Pd1 O4 2.015(5) 2_766 ?
Pd1 N2 2.028(6) 2_766 ?
Pd1 N1 2.033(5) . ?
Pd1 Pd1 14.3323(16) 2_766 ?
O1 C1 1.283(9) . ?
C1 O2 1.228(8) . ?
C1 C2 1.558(8) . ?
O3 C2 1.243(9) . ?
C2 N1 1.340(9) . ?
N1 C3 1.427(8) . ?
C3 C4 1.379(10) . ?
C3 C8 1.405(10) . ?
C4 C5 1.401(9) . ?
C5 C6 1.403(10) . ?
C6 C7 1.375(11) . ?
C6 N3 1.440(9) . ?
C7 C8 1.384(9) . ?
N3 N4 1.255(9) . ?
N4 C11 1.455(8) . ?
C11 C12 1.379(11) . ?
C11 C16 1.382(11) . ?
C12 C13 1.404(9) . ?
C13 C14 1.384(10) . ?
C14 C15 1.400(10) . ?
C14 N2 1.434(8) . ?
C15 C16 1.399(10) . ?
N2 C17 1.340(9) . ?
N2 Pd1 2.028(6) 2_766 ?
C17 O6 1.236(9) . ?
C17 C18 1.562(9) . ?
O5 C18 1.232(9) . ?
C18 O4 1.285(9) . ?
O4 Pd1 2.015(5) 2_766 ?
N5 C27 1.517(9) . ?
N5 C23 1.522(9) . ?
N5 C19 1.524(8) . ?
N5 C31 1.529(8) . ?
C19 C20 1.508(10) . ?
C20 C21 1.521(10) . ?
C21 C22 1.509(11) . ?
C23 C24 1.514(9) . ?
C24 C25 1.515(11) . ?
C25 C26 1.535(11) . ?
C27 C28 1.506(9) . ?
C28 C29 1.522(11) . ?
C29 C30 1.511(11) . ?
C31 C32 1.514(10) . ?
C32 C33 1.518(10) . ?
C33 C34 1.535(13) . ?
N6 C39 1.476(12) . ?
N6 C43 1.497(12) . ?
N6 C35 1.542(14) . ?
N6 C47 1.563(12) . ?
C35 C36 1.537(15) . ?
C36 C37 1.502(17) . ?
C37 C38 1.42(2) . ?
C39 C40 1.496(14) . ?
C40 C41 1.563(15) . ?
C41 C42 1.407(16) . ?
C43 C44 1.496(14) . ?
C44 C45 1.501(13) . ?
C45 C46 1.476(16) . ?
C47 C48 1.519(13) . ?
C48 C49 1.538(14) . ?
C49 C50 1.499(14) . ?
C1M O1M 1.36(2) . ?
C2M O2M 1.34(3) . ?
C3M O3M 1.34(2) . ?
C4M O4M 1.47(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
O1 Pd1 O4 90.45(18) . 2_766 ?
O1 Pd1 N2 171.5(2) . 2_766 ?
O4 Pd1 N2 81.35(19) 2_766 2_766 ?
O1 Pd1 N1 81.3(2) . . ?
O4 Pd1 N1 171.75(19) 2_766 . ?
N2 Pd1 N1 106.9(2) 2_766 . ?
O1 Pd1 Pd1 136.75(13) . 2_766 ?
O4 Pd1 Pd1 132.64(13) 2_766 2_766 ?
N2 Pd1 Pd1 51.61(15) 2_766 2_766 ?
N1 Pd1 Pd1 55.51(15) . 2_766 ?
C1 O1 Pd1 116.1(4) . . ?
O2 C1 O1 125.4(6) . . ?
O2 C1 C2 119.7(6) . . ?
O1 C1 C2 114.9(6) . . ?
O3 C2 N1 127.7(6) . . ?
O3 C2 C1 118.9(6) . . ?
N1 C2 C1 113.4(6) . . ?
C2 N1 C3 117.4(5) . . ?
C2 N1 Pd1 114.0(4) . . ?
C3 N1 Pd1 128.6(4) . . ?
C4 C3 C8 119.5(6) . . ?
C4 C3 N1 120.4(6) . . ?
C8 C3 N1 120.1(6) . . ?
C3 C4 C5 120.6(7) . . ?
C4 C5 C6 119.3(7) . . ?
C7 C6 C5 119.8(6) . . ?
C7 C6 N3 115.5(6) . . ?
C5 C6 N3 124.6(7) . . ?
C6 C7 C8 120.9(7) . . ?
C7 C8 C3 119.8(7) . . ?
N4 N3 C6 114.0(6) . . ?
N3 N4 C11 112.3(6) . . ?
C12 C11 C16 120.4(6) . . ?
C12 C11 N4 115.6(6) . . ?
C16 C11 N4 124.0(7) . . ?
C11 C12 C13 120.0(7) . . ?
C14 C13 C12 119.8(7) . . ?
C13 C14 C15 120.1(6) . . ?
C13 C14 N2 120.0(6) . . ?
C15 C14 N2 119.9(6) . . ?
C16 C15 C14 119.5(7) . . ?
C11 C16 C15 120.2(7) . . ?
C17 N2 C14 116.0(6) . . ?
C17 N2 Pd1 114.7(4) . 2_766 ?
C14 N2 Pd1 129.3(4) . 2_766 ?
O6 C17 N2 127.3(6) . . ?
O6 C17 C18 120.0(6) . . ?
N2 C17 C18 112.7(6) . . ?
O5 C18 O4 125.4(6) . . ?
O5 C18 C17 119.0(6) . . ?
O4 C18 C17 115.6(6) . . ?
C18 O4 Pd1 115.6(4) . 2_766 ?
C27 N5 C23 111.3(5) . . ?
C27 N5 C19 106.5(5) . . ?
C23 N5 C19 111.7(5) . . ?
C27 N5 C31 111.7(5) . . ?
C23 N5 C31 105.1(5) . . ?
C19 N5 C31 110.6(5) . . ?
C20 C19 N5 117.4(6) . . ?
C19 C20 C21 109.7(6) . . ?
C22 C21 C20 115.6(7) . . ?
C24 C23 N5 116.6(6) . . ?
C23 C24 C25 110.7(6) . . ?
C24 C25 C26 111.8(7) . . ?
C28 C27 N5 116.1(6) . . ?
C27 C28 C29 110.4(6) . . ?
C30 C29 C28 112.3(7) . . ?
C32 C31 N5 116.0(6) . . ?
C31 C32 C33 110.3(6) . . ?
C32 C33 C34 111.7(7) . . ?
C39 N6 C43 115.5(8) . . ?
C39 N6 C35 110.5(7) . . ?
C43 N6 C35 107.2(7) . . ?
C39 N6 C47 106.8(7) . . ?
C43 N6 C47 108.5(7) . . ?
C35 N6 C47 108.1(8) . . ?
C36 C35 N6 114.3(9) . . ?
C37 C36 C35 111.6(10) . . ?
C38 C37 C36 110.2(13) . . ?
N6 C39 C40 116.8(8) . . ?
C39 C40 C41 111.8(8) . . ?
C42 C41 C40 113.2(10) . . ?
C44 C43 N6 118.7(8) . . ?
C43 C44 C45 114.0(8) . . ?
C46 C45 C44 111.7(9) . . ?
C48 C47 N6 117.8(7) . . ?
C47 C48 C49 110.8(8) . . ?
C50 C49 C48 115.5(8) . . ?

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
O1M H1M O6 0.84 1.96 2.698(17) 146.1 .
O2M H2M O1M 0.84 2.05 2.89(3) 177.8 .
O3M H3M O3 0.84 1.83 2.659(10) 168.8 .
O4M H4M O3M 0.84 1.87 2.71(2) 171.1 .

_refine_diff_density_max         5.194
_refine_diff_density_min         -0.966
_refine_diff_density_rms         0.144

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.119 0.500 242 48 ' '
_platon_squeeze_details          
;
;

_shelxl_version_number           2013-4



