# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_GS
_database_code_depnum_ccdc_archive 'CCDC 1441774'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_GS                  
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         13 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
;
# end Validation Reply Form 

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5457(4)
_cell_length_b                   13.4021(5)
_cell_length_c                   29.7173(12)
_cell_angle_alpha                90
_cell_angle_beta                 95.335(4)
_cell_angle_gamma                90
_cell_volume                     4578.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5349
_cell_measurement_theta_min      3.5440
_cell_measurement_theta_max      28.4710

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.451
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            19627
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.843
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9335
_reflns_number_gt                6758
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0287P)²+1.2965P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9335
_refine_ls_number_parameters     521
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0761
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.5493(2) 0.9625(2) 0.62887(10) 0.0197(7) Uani 1 1 d . . . . .
H1A H 0.4743 0.9561 0.6423 0.024 Uiso 1 1 calc R U . . .
H1B H 0.5605 1.0336 0.6214 0.024 Uiso 1 1 calc R U . . .
C2 C 0.5460(3) 0.9007(2) 0.58651(10) 0.0197(7) Uani 1 1 d . . . . .
H2A H 0.4776 0.9189 0.5655 0.024 Uiso 1 1 calc R U . . .
H2B H 0.6172 0.9120 0.5710 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5600(2) 0.7184(2) 0.56622(10) 0.0170(6) Uani 1 1 d . . . . .
H3A H 0.6303 0.7354 0.5511 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4929 0.7143 0.5430 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5767(2) 0.6203(2) 0.59087(10) 0.0162(6) Uani 1 1 d . . . . .
H4A H 0.5027 0.6003 0.6027 0.019 Uiso 1 1 calc R U . . .
H4B H 0.5981 0.5682 0.5696 0.019 Uiso 1 1 calc R U . . .
C5 C 0.7625(2) 0.9672(2) 0.65000(11) 0.0198(7) Uani 1 1 d . . . . .
H5A H 0.7710 0.9485 0.6183 0.024 Uiso 1 1 calc R U . . .
H5B H 0.8252 0.9331 0.6691 0.024 Uiso 1 1 calc R U . . .
C6 C 0.7816(3) 1.0794(2) 0.65471(11) 0.0248(7) Uani 1 1 d . . . . .
H6A H 0.7187 1.1151 0.6363 0.030 Uiso 1 1 calc R U . . .
H6B H 0.7785 1.0991 0.6867 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8981(3) 1.1091(2) 0.63929(12) 0.0271(8) Uani 1 1 d . . . . .
H7A H 0.8970 1.0986 0.6063 0.032 Uiso 1 1 calc R U . . .
H7B H 0.9598 1.0662 0.6544 0.032 Uiso 1 1 calc R U . . .
C8 C 0.9255(3) 1.2180(2) 0.65028(13) 0.0367(9) Uani 1 1 d . . . . .
H8A H 0.9332 1.2273 0.6831 0.055 Uiso 1 1 calc R U . . .
H8B H 0.8625 1.2603 0.6366 0.055 Uiso 1 1 calc R U . . .
H8C H 0.9986 1.2366 0.6381 0.055 Uiso 1 1 calc R U . . .
C9 C 0.6274(2) 0.9618(2) 0.70884(10) 0.0179(7) Uani 1 1 d . . . . .
H9A H 0.6176 1.0352 0.7083 0.022 Uiso 1 1 calc R U . . .
H9B H 0.6980 0.9467 0.7292 0.022 Uiso 1 1 calc R U . . .
C10 C 0.5240(2) 0.9162(2) 0.72860(10) 0.0198(7) Uani 1 1 d . . . . .
H10A H 0.5281 0.8426 0.7265 0.024 Uiso 1 1 calc R U . . .
H10B H 0.4515 0.9385 0.7111 0.024 Uiso 1 1 calc R U . . .
C11 C 0.5216(2) 0.9465(2) 0.77775(11) 0.0234(7) Uani 1 1 d . . . . .
H11A H 0.5878 0.9147 0.7959 0.028 Uiso 1 1 calc R U . . .
H11B H 0.5318 1.0197 0.7803 0.028 Uiso 1 1 calc R U . . .
C12 C 0.4094(3) 0.9174(3) 0.79714(12) 0.0315(8) Uani 1 1 d . . . . .
H12A H 0.4147 0.9342 0.8294 0.047 Uiso 1 1 calc R U . . .
H12B H 0.3966 0.8455 0.7933 0.047 Uiso 1 1 calc R U . . .
H12C H 0.3442 0.9538 0.7812 0.047 Uiso 1 1 calc R U . . .
C13 C 0.7902(2) 0.6236(2) 0.61275(10) 0.0152(6) Uani 1 1 d . . . . .
H13A H 0.8481 0.6380 0.6386 0.018 Uiso 1 1 calc R U . . .
H13B H 0.7960 0.6775 0.5903 0.018 Uiso 1 1 calc R U . . .
C14 C 0.8237(2) 0.5260(2) 0.59143(10) 0.0171(6) Uani 1 1 d . . . . .
H14A H 0.7668 0.5104 0.5654 0.020 Uiso 1 1 calc R U . . .
H14B H 0.8212 0.4715 0.6138 0.020 Uiso 1 1 calc R U . . .
C15 C 0.9452(2) 0.5320(2) 0.57557(11) 0.0212(7) Uani 1 1 d . . . . .
H15A H 0.9472 0.5868 0.5533 0.025 Uiso 1 1 calc R U . . .
H15B H 1.0015 0.5484 0.6017 0.025 Uiso 1 1 calc R U . . .
C16 C 0.9828(2) 0.4357(2) 0.55416(11) 0.0239(7) Uani 1 1 d . . . . .
H16A H 1.0617 0.4435 0.5451 0.036 Uiso 1 1 calc R U . . .
H16B H 0.9292 0.4203 0.5275 0.036 Uiso 1 1 calc R U . . .
H16C H 0.9817 0.3812 0.5761 0.036 Uiso 1 1 calc R U . . .
C17 C 0.6575(2) 0.5461(2) 0.66249(10) 0.0173(7) Uani 1 1 d . . . . .
H17A H 0.7273 0.5451 0.6845 0.021 Uiso 1 1 calc R U . . .
H17B H 0.6544 0.4817 0.6461 0.021 Uiso 1 1 calc R U . . .
C18 C 0.5504(2) 0.5548(2) 0.68816(11) 0.0237(7) Uani 1 1 d . . . . .
H18A H 0.5538 0.6180 0.7054 0.028 Uiso 1 1 calc R U . . .
H18B H 0.4801 0.5565 0.6664 0.028 Uiso 1 1 calc R U . . .
C19 C 0.5417(3) 0.4692(3) 0.71997(14) 0.0418(10) Uani 1 1 d . . . . .
H19A H 0.5500 0.4064 0.7030 0.050 Uiso 1 1 calc R U . . .
H19B H 0.6082 0.4730 0.7435 0.050 Uiso 1 1 calc R U . . .
C20 C 0.4336(3) 0.4632(3) 0.74268(12) 0.0380(9) Uani 1 1 d . . . . .
H20A H 0.4387 0.4071 0.7639 0.057 Uiso 1 1 calc R U . . .
H20B H 0.3673 0.4531 0.7200 0.057 Uiso 1 1 calc R U . . .
H20C H 0.4228 0.5254 0.7591 0.057 Uiso 1 1 calc R U . . .
C21 C 0.4903(2) 0.2311(2) 0.55682(9) 0.0151(6) Uani 1 1 d . . . . .
C22 C 0.5833(2) 0.2965(2) 0.56730(11) 0.0204(7) Uani 1 1 d . . . . .
H22 H 0.5690 0.3569 0.5826 0.024 Uiso 1 1 calc R U . . .
C23 C 0.6954(2) 0.2773(2) 0.55650(11) 0.0230(7) Uani 1 1 d . . . . .
H23 H 0.7557 0.3241 0.5644 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7198(2) 0.1904(2) 0.53430(10) 0.0205(7) Uani 1 1 d . . . . .
H24 H 0.7964 0.1769 0.5267 0.025 Uiso 1 1 calc R U . . .
C25 C 0.6309(2) 0.1236(2) 0.52340(10) 0.0185(7) Uani 1 1 d . . . . .
H25 H 0.6460 0.0633 0.5082 0.022 Uiso 1 1 calc R U . . .
C26 C 0.5192(2) 0.1441(2) 0.53453(10) 0.0172(6) Uani 1 1 d . . . . .
H26 H 0.4596 0.0967 0.5266 0.021 Uiso 1 1 calc R U . . .
C27 C 0.2597(2) 0.1994(2) 0.53721(10) 0.0156(6) Uani 1 1 d . . . . .
C28 C 0.1854(2) 0.2491(2) 0.50493(10) 0.0195(7) Uani 1 1 d . . . . .
H28 H 0.1907 0.3197 0.5030 0.023 Uiso 1 1 calc R U . . .
C29 C 0.1038(2) 0.1998(2) 0.47541(11) 0.0248(7) Uani 1 1 d . . . . .
H29 H 0.0552 0.2369 0.4539 0.030 Uiso 1 1 calc R U . . .
C30 C 0.0932(2) 0.0975(2) 0.47717(11) 0.0235(7) Uani 1 1 d . . . . .
H30 H 0.0387 0.0634 0.4567 0.028 Uiso 1 1 calc R U . . .
C31 C 0.1631(2) 0.0456(2) 0.50913(11) 0.0236(7) Uani 1 1 d . . . . .
H31 H 0.1557 -0.0248 0.5113 0.028 Uiso 1 1 calc R U . . .
C32 C 0.2441(2) 0.0955(2) 0.53811(11) 0.0200(7) Uani 1 1 d . . . . .
H32 H 0.2914 0.0576 0.5597 0.024 Uiso 1 1 calc R U . . .
C33 C 0.3526(2) 0.2100(2) 0.62373(10) 0.0172(6) Uani 1 1 d . . . . .
C34 C 0.2498(3) 0.1720(2) 0.63862(11) 0.0277(8) Uani 1 1 d . . . . .
H34 H 0.1831 0.1666 0.6175 0.033 Uiso 1 1 calc R U . . .
C35 C 0.2413(3) 0.1421(3) 0.68249(12) 0.0365(9) Uani 1 1 d . . . . .
H35 H 0.1701 0.1155 0.6908 0.044 Uiso 1 1 calc R U . . .
C36 C 0.3349(3) 0.1505(2) 0.71448(11) 0.0309(8) Uani 1 1 d . . . . .
H36 H 0.3287 0.1307 0.7449 0.037 Uiso 1 1 calc R U . . .
C37 C 0.4385(3) 0.1883(2) 0.70133(11) 0.0261(7) Uani 1 1 d . . . . .
H37 H 0.5044 0.1947 0.7228 0.031 Uiso 1 1 calc R U . . .
C38 C 0.4455(2) 0.2167(2) 0.65700(10) 0.0208(7) Uani 1 1 d . . . . .
H38 H 0.5175 0.2421 0.6488 0.025 Uiso 1 1 calc R U . . .
C39 C 0.3363(2) 0.3746(2) 0.57269(10) 0.0161(6) Uani 1 1 d . . . . .
C40 C 0.2881(2) 0.4240(2) 0.60764(11) 0.0217(7) Uani 1 1 d . . . . .
H40 H 0.2733 0.3874 0.6338 0.026 Uiso 1 1 calc R U . . .
C41 C 0.2607(2) 0.5254(2) 0.60562(12) 0.0269(8) Uani 1 1 d . . . . .
H41 H 0.2285 0.5562 0.6304 0.032 Uiso 1 1 calc R U . . .
C42 C 0.2797(2) 0.5809(2) 0.56839(13) 0.0279(8) Uani 1 1 d . . . . .
H42 H 0.2591 0.6495 0.5668 0.033 Uiso 1 1 calc R U . . .
C43 C 0.3295(3) 0.5351(2) 0.53313(12) 0.0261(8) Uani 1 1 d . . . . .
H43 H 0.3443 0.5725 0.5071 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3578(2) 0.4347(2) 0.53586(11) 0.0204(7) Uani 1 1 d . . . . .
H44 H 0.3934 0.4053 0.5116 0.025 Uiso 1 1 calc R U . . .
C45 C 0.2672(2) 0.7616(3) 0.67510(11) 0.0273(7) Uani 1 1 d . . . . .
H45A H 0.2864 0.8018 0.7027 0.033 Uiso 1 1 calc R U . . .
H45B H 0.2989 0.6935 0.6803 0.033 Uiso 1 1 calc R U . . .
C46 C 0.1371(2) 0.7580(2) 0.66323(13) 0.0320(8) Uani 1 1 d . . . . .
H46A H 0.0946 0.7575 0.6907 0.038 Uiso 1 1 calc R U . . .
H46B H 0.1141 0.6989 0.6445 0.038 Uiso 1 1 calc R U . . .
C47 C 0.1161(3) 0.8542(3) 0.63666(13) 0.0428(10) Uani 1 1 d . . . . .
H47A H 0.0465 0.8487 0.6147 0.051 Uiso 1 1 calc R U . . .
H47B H 0.1058 0.9113 0.6571 0.051 Uiso 1 1 calc R U . . .
C48 C 0.2239(3) 0.8659(3) 0.61306(14) 0.0467(10) Uani 1 1 d . . . . .
H48A H 0.2100 0.8426 0.5814 0.056 Uiso 1 1 calc R U . . .
H48B H 0.2475 0.9369 0.6129 0.056 Uiso 1 1 calc R U . . .
B1 B 0.3590(3) 0.2534(2) 0.57239(12) 0.0172(7) Uani 1 1 d . . . . .
N1 N 0.77204(19) 0.75164(17) 0.70785(8) 0.0189(6) Uani 1 1 d . . . . .
N2 N 0.64737(19) 0.92800(17) 0.66242(8) 0.0160(5) Uani 1 1 d . . . . .
N3 N 0.53861(19) 0.79493(16) 0.60029(8) 0.0145(5) Uani 1 1 d D . . . .
N4 N 0.67039(17) 0.62850(16) 0.62938(8) 0.0132(5) Uani 1 1 d . . . . .
O1 O 0.87665(17) 0.76215(19) 0.70438(7) 0.0361(6) Uani 1 1 d . . . . .
O2 O 0.73848(19) 0.7272(2) 0.74439(8) 0.0413(6) Uani 1 1 d . . . . .
O3 O 0.31385(17) 0.80671(16) 0.63721(8) 0.0309(5) Uani 1 1 d . . . . .
Pd1 Pd 0.65646(2) 0.77370(2) 0.65400(2) 0.01326(7) Uani 1 1 d . . . . .
H3 H 0.4644(17) 0.787(2) 0.6106(9) 0.016 Uiso 1 1 d D 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
C1 C2 1.504(4) . ?
C1 N2 1.510(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.480(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.478(4) . ?
C3 C4 1.508(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.504(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.507(3) . ?
C5 C6 1.524(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.514(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.523(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.490(4) . ?
C9 C10 1.508(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.519(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.517(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.513(3) . ?
C13 C14 1.519(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.523(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.520(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.495(4) . ?
C17 C18 1.516(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.496(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.476(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.397(4) . ?
C21 C22 1.398(4) . ?
C21 B1 1.653(4) . ?
C22 C23 1.386(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.395(4) . ?
C27 C32 1.406(4) . ?
C27 B1 1.645(4) . ?
C28 C29 1.393(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.376(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.393(4) . ?
C33 C34 1.401(4) . ?
C33 B1 1.640(4) . ?
C34 C35 1.376(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.375(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.388(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.381(4) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.391(4) . ?
C39 C44 1.399(4) . ?
C39 B1 1.646(4) . ?
C40 C41 1.394(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.368(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.384(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.385(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.427(4) . ?
C45 C46 1.511(4) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.520(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.493(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.443(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1 O1 1.230(3) . ?
N1 O2 1.231(3) . ?
N1 Pd1 2.008(2) . ?
N2 Pd1 2.087(2) . ?
N3 Pd1 2.019(2) . ?
N3 H3 0.942(17) . ?
N4 Pd1 2.090(2) . ?

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
C2 C1 N2 110.0(2) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.0(2) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 107.1(2) . . ?
N3 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
N3 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
N4 C4 C3 110.9(2) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 116.4(2) . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 110.9(2) . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 111.1(3) . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.7(2) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.6(2) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.9(3) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 116.7(2) . . ?
N4 C13 H13A 108.1 . . ?
C14 C13 H13A 108.1 . . ?
N4 C13 H13B 108.1 . . ?
C14 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 C15 111.2(2) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 113.1(2) . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15B 109.0 . . ?
C14 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 114.2(2) . . ?
N4 C17 H17A 108.7 . . ?
C18 C17 H17A 108.7 . . ?
N4 C17 H17B 108.7 . . ?
C18 C17 H17B 108.7 . . ?
H17A C17 H17B 107.6 . . ?
C19 C18 C17 111.4(3) . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C17 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 116.1(3) . . ?
C20 C19 H19A 108.3 . . ?
C18 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C18 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.6(2) . . ?
C26 C21 B1 123.3(2) . . ?
C22 C21 B1 122.0(3) . . ?
C23 C22 C21 123.1(3) . . ?
C23 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
C24 C23 C22 120.2(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 123.1(3) . . ?
C25 C26 H26 118.5 . . ?
C21 C26 H26 118.5 . . ?
C28 C27 C32 114.5(3) . . ?
C28 C27 B1 125.1(3) . . ?
C32 C27 B1 120.5(3) . . ?
C29 C28 C27 122.9(3) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 118.7(3) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 120.3(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.2(3) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C38 C33 C34 114.7(3) . . ?
C38 C33 B1 122.6(2) . . ?
C34 C33 B1 122.4(3) . . ?
C35 C34 C33 122.8(3) . . ?
C35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C36 C35 C34 120.7(3) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C35 C36 C37 118.5(3) . . ?
C35 C36 H36 120.8 . . ?
C37 C36 H36 120.8 . . ?
C38 C37 C36 119.9(3) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C33 123.4(3) . . ?
C37 C38 H38 118.3 . . ?
C33 C38 H38 118.3 . . ?
C40 C39 C44 115.0(3) . . ?
C40 C39 B1 123.3(3) . . ?
C44 C39 B1 121.6(3) . . ?
C39 C40 C41 122.4(3) . . ?
C39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
C42 C41 C40 120.8(3) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C41 C42 C43 118.7(3) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 119.9(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C39 123.2(3) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 105.6(2) . . ?
O3 C45 H45A 110.6 . . ?
C46 C45 H45A 110.6 . . ?
O3 C45 H45B 110.6 . . ?
C46 C45 H45B 110.6 . . ?
H45A C45 H45B 108.7 . . ?
C45 C46 C47 101.6(3) . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46B 111.5 . . ?
C47 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 103.5(3) . . ?
C48 C47 H47A 111.1 . . ?
C46 C47 H47A 111.1 . . ?
C48 C47 H47B 111.1 . . ?
C46 C47 H47B 111.1 . . ?
H47A C47 H47B 109.0 . . ?
O3 C48 C47 107.6(3) . . ?
O3 C48 H48A 110.2 . . ?
C47 C48 H48A 110.2 . . ?
O3 C48 H48B 110.2 . . ?
C47 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
C33 B1 C27 110.3(2) . . ?
C33 B1 C39 108.9(2) . . ?
C27 B1 C39 109.6(2) . . ?
C33 B1 C21 108.5(2) . . ?
C27 B1 C21 110.2(2) . . ?
C39 B1 C21 109.3(2) . . ?
O1 N1 O2 119.8(2) . . ?
O1 N1 Pd1 120.1(2) . . ?
O2 N1 Pd1 120.13(18) . . ?
C9 N2 C5 109.7(2) . . ?
C9 N2 C1 110.3(2) . . ?
C5 N2 C1 110.9(2) . . ?
C9 N2 Pd1 115.21(17) . . ?
C5 N2 Pd1 105.14(16) . . ?
C1 N2 Pd1 105.49(16) . . ?
C3 N3 C2 117.2(2) . . ?
C3 N3 Pd1 107.49(16) . . ?
C2 N3 Pd1 107.55(16) . . ?
C3 N3 H3 111.0(17) . . ?
C2 N3 H3 106.0(17) . . ?
Pd1 N3 H3 107.1(17) . . ?
C17 N4 C4 109.8(2) . . ?
C17 N4 C13 109.5(2) . . ?
C4 N4 C13 111.3(2) . . ?
C17 N4 Pd1 116.19(17) . . ?
C4 N4 Pd1 105.11(15) . . ?
C13 N4 Pd1 104.89(15) . . ?
C45 O3 C48 108.5(2) . . ?
N1 Pd1 N3 179.23(10) . . ?
N1 Pd1 N2 95.02(9) . . ?
N3 Pd1 N2 85.27(9) . . ?
N1 Pd1 N4 94.29(9) . . ?
N3 Pd1 N4 85.56(9) . . ?
N2 Pd1 N4 166.12(9) . . ?

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
N2 C1 C2 N3 54.9(3) . . . . ?
N3 C3 C4 N4 -54.2(3) . . . . ?
N2 C5 C6 C7 -177.6(3) . . . . ?
C5 C6 C7 C8 -171.7(3) . . . . ?
N2 C9 C10 C11 173.1(2) . . . . ?
C9 C10 C11 C12 170.4(3) . . . . ?
N4 C13 C14 C15 179.1(2) . . . . ?
C13 C14 C15 C16 179.7(3) . . . . ?
N4 C17 C18 C19 178.9(3) . . . . ?
C17 C18 C19 C20 -172.8(3) . . . . ?
C26 C21 C22 C23 0.2(4) . . . . ?
B1 C21 C22 C23 176.9(3) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C22 C23 C24 C25 -0.3(5) . . . . ?
C23 C24 C25 C26 0.2(4) . . . . ?
C24 C25 C26 C21 0.0(5) . . . . ?
C22 C21 C26 C25 -0.2(4) . . . . ?
B1 C21 C26 C25 -176.9(3) . . . . ?
C32 C27 C28 C29 -1.1(4) . . . . ?
B1 C27 C28 C29 179.0(3) . . . . ?
C27 C28 C29 C30 0.1(5) . . . . ?
C28 C29 C30 C31 1.2(4) . . . . ?
C29 C30 C31 C32 -1.5(4) . . . . ?
C30 C31 C32 C27 0.4(4) . . . . ?
C28 C27 C32 C31 0.8(4) . . . . ?
B1 C27 C32 C31 -179.3(3) . . . . ?
C38 C33 C34 C35 -0.9(5) . . . . ?
B1 C33 C34 C35 -175.2(3) . . . . ?
C33 C34 C35 C36 1.4(5) . . . . ?
C34 C35 C36 C37 -0.9(5) . . . . ?
C35 C36 C37 C38 0.1(5) . . . . ?
C36 C37 C38 C33 0.3(5) . . . . ?
C34 C33 C38 C37 0.1(4) . . . . ?
B1 C33 C38 C37 174.3(3) . . . . ?
C44 C39 C40 C41 1.4(4) . . . . ?
B1 C39 C40 C41 -174.6(3) . . . . ?
C39 C40 C41 C42 0.6(4) . . . . ?
C40 C41 C42 C43 -1.7(4) . . . . ?
C41 C42 C43 C44 0.8(4) . . . . ?
C42 C43 C44 C39 1.3(4) . . . . ?
C40 C39 C44 C43 -2.4(4) . . . . ?
B1 C39 C44 C43 173.7(3) . . . . ?
O3 C45 C46 C47 -35.3(3) . . . . ?
C45 C46 C47 C48 33.5(4) . . . . ?
C46 C47 C48 O3 -20.7(4) . . . . ?
C38 C33 B1 C27 159.0(3) . . . . ?
C34 C33 B1 C27 -27.1(4) . . . . ?
C38 C33 B1 C39 -80.6(3) . . . . ?
C34 C33 B1 C39 93.2(3) . . . . ?
C38 C33 B1 C21 38.2(4) . . . . ?
C34 C33 B1 C21 -148.0(3) . . . . ?
C28 C27 B1 C33 133.8(3) . . . . ?
C32 C27 B1 C33 -46.0(3) . . . . ?
C28 C27 B1 C39 14.0(4) . . . . ?
C32 C27 B1 C39 -165.9(2) . . . . ?
C28 C27 B1 C21 -106.3(3) . . . . ?
C32 C27 B1 C21 73.8(3) . . . . ?
C40 C39 B1 C33 -16.3(3) . . . . ?
C44 C39 B1 C33 168.0(2) . . . . ?
C40 C39 B1 C27 104.4(3) . . . . ?
C44 C39 B1 C27 -71.3(3) . . . . ?
C40 C39 B1 C21 -134.7(3) . . . . ?
C44 C39 B1 C21 49.5(3) . . . . ?
C26 C21 B1 C33 90.3(3) . . . . ?
C22 C21 B1 C33 -86.1(3) . . . . ?
C26 C21 B1 C27 -30.6(4) . . . . ?
C22 C21 B1 C27 153.0(3) . . . . ?
C26 C21 B1 C39 -151.1(3) . . . . ?
C22 C21 B1 C39 32.5(4) . . . . ?
C10 C9 N2 C5 -171.5(2) . . . . ?
C10 C9 N2 C1 66.1(3) . . . . ?
C10 C9 N2 Pd1 -53.1(3) . . . . ?
C6 C5 N2 C9 -53.5(3) . . . . ?
C6 C5 N2 C1 68.5(3) . . . . ?
C6 C5 N2 Pd1 -178.0(2) . . . . ?
C2 C1 N2 C9 -160.2(2) . . . . ?
C2 C1 N2 C5 78.1(3) . . . . ?
C2 C1 N2 Pd1 -35.2(3) . . . . ?
C4 C3 N3 C2 166.5(2) . . . . ?
C4 C3 N3 Pd1 45.3(2) . . . . ?
C1 C2 N3 C3 -167.0(2) . . . . ?
C1 C2 N3 Pd1 -45.9(2) . . . . ?
C18 C17 N4 C4 -68.6(3) . . . . ?
C18 C17 N4 C13 169.0(2) . . . . ?
C18 C17 N4 Pd1 50.4(3) . . . . ?
C3 C4 N4 C17 160.0(2) . . . . ?
C3 C4 N4 C13 -78.7(3) . . . . ?
C3 C4 N4 Pd1 34.4(2) . . . . ?
C14 C13 N4 C17 56.4(3) . . . . ?
C14 C13 N4 C4 -65.1(3) . . . . ?
C14 C13 N4 Pd1 -178.3(2) . . . . ?
C46 C45 O3 C48 23.5(3) . . . . ?
C47 C48 O3 C45 -1.5(4) . . . . ?

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
C5 H5B O1 0.99 2.57 3.392(4) 141.0 .
C13 H13A O1 0.99 2.56 3.369(4) 138.4 .
C46 H46A O1 0.99 2.59 3.350(4) 133.9 1_455
N3 H3 O3 0.942(17) 1.993(18) 2.914(3) 165(2) .

_refine_diff_density_max         0.750
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_UV-1h
_database_code_depnum_ccdc_archive 'CCDC 1441775'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_UV-1h               
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         14 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.4775(4)
_cell_length_b                   13.3647(5)
_cell_length_c                   29.9849(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.569(3)
_cell_angle_gamma                90
_cell_volume                     4584.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6952
_cell_measurement_theta_min      3.5640
_cell_measurement_theta_max      28.0060

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            31062
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9355
_reflns_number_gt                6577
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0318P)²+2.4508P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9355
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0790
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.5484(3) 0.9632(2) 0.62802(9) 0.0216(7) Uani 1 1 d . . . . .
H1A H 0.5601 1.0342 0.6202 0.026 Uiso 1 1 calc R U . . .
H1B H 0.4735 0.9577 0.6421 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5436(3) 0.8999(2) 0.58628(9) 0.0200(7) Uani 1 1 d . . . . .
H2A H 0.4742 0.9177 0.5661 0.024 Uiso 1 1 calc R U . . .
H2B H 0.6145 0.9108 0.5701 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5599(3) 0.7176(2) 0.56642(9) 0.0170(6) Uani 1 1 d . . . . .
H3A H 0.6308 0.7354 0.5514 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4930 0.7130 0.5435 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5774(2) 0.6195(2) 0.59088(9) 0.0150(7) Uani 1 1 d . . . . .
H4A H 0.5033 0.5988 0.6029 0.018 Uiso 1 1 calc R U . . .
H4B H 0.5998 0.5672 0.5698 0.018 Uiso 1 1 calc R U . . .
C5 C 0.7631(3) 0.9681(2) 0.64733(10) 0.0211(7) Uani 1 1 d . . . . .
H5A H 0.7723 0.9474 0.6161 0.025 Uiso 1 1 calc R U . . .
H5B H 0.8260 0.9351 0.6665 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7821(3) 1.0803(2) 0.65047(10) 0.0226(7) Uani 1 1 d . . . . .
H6A H 0.7763 1.1022 0.6818 0.027 Uiso 1 1 calc R U . . .
H6B H 0.7202 1.1148 0.6314 0.027 Uiso 1 1 calc R U . . .
C7 C 0.9008(3) 1.1096(3) 0.63564(11) 0.0277(8) Uani 1 1 d . . . . .
H7A H 0.9024 1.0966 0.6032 0.033 Uiso 1 1 calc R U . . .
H7B H 0.9619 1.0677 0.6516 0.033 Uiso 1 1 calc R U . . .
C8 C 0.9277(3) 1.2191(3) 0.64496(11) 0.0334(8) Uani 1 1 d . . . . .
H8A H 0.9334 1.2309 0.6773 0.050 Uiso 1 1 calc R U . . .
H8B H 0.8651 1.2606 0.6306 0.050 Uiso 1 1 calc R U . . .
H8C H 1.0021 1.2366 0.6330 0.050 Uiso 1 1 calc R U . . .
C9 C 0.6288(3) 0.9627(2) 0.70685(9) 0.0187(7) Uani 1 1 d . . . . .
H9A H 0.6238 1.0366 0.7068 0.022 Uiso 1 1 calc R U . . .
H9B H 0.6983 0.9437 0.7268 0.022 Uiso 1 1 calc R U . . .
C10 C 0.5212(3) 0.9212(3) 0.72638(9) 0.0211(7) Uani 1 1 d . . . . .
H10A H 0.5183 0.8477 0.7224 0.025 Uiso 1 1 calc R U . . .
H10B H 0.4501 0.9502 0.7105 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5247(3) 0.9469(3) 0.77608(10) 0.0246(8) Uani 1 1 d . . . . .
H11A H 0.5908 0.9111 0.7922 0.030 Uiso 1 1 calc R U . . .
H11B H 0.5389 1.0196 0.7799 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4123(3) 0.9194(3) 0.79681(11) 0.0329(9) Uani 1 1 d . . . . .
H12A H 0.4206 0.9342 0.8289 0.049 Uiso 1 1 calc R U . . .
H12B H 0.3965 0.8479 0.7924 0.049 Uiso 1 1 calc R U . . .
H12C H 0.3473 0.9584 0.7825 0.049 Uiso 1 1 calc R U . . .
C13 C 0.7914(2) 0.6242(2) 0.61181(9) 0.0169(7) Uani 1 1 d . . . . .
H13A H 0.8493 0.6392 0.6372 0.020 Uiso 1 1 calc R U . . .
H13B H 0.7972 0.6781 0.5894 0.020 Uiso 1 1 calc R U . . .
C14 C 0.8265(3) 0.5263(2) 0.59073(10) 0.0203(7) Uani 1 1 d . . . . .
H14A H 0.8254 0.4719 0.6131 0.024 Uiso 1 1 calc R U . . .
H14B H 0.7692 0.5095 0.5654 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9477(3) 0.5336(2) 0.57408(10) 0.0229(7) Uani 1 1 d . . . . .
H15A H 1.0043 0.5512 0.5995 0.027 Uiso 1 1 calc R U . . .
H15B H 0.9482 0.5882 0.5518 0.027 Uiso 1 1 calc R U . . .
C16 C 0.9874(3) 0.4373(3) 0.55284(10) 0.0262(8) Uani 1 1 d . . . . .
H16A H 1.0655 0.4470 0.5425 0.039 Uiso 1 1 calc R U . . .
H16B H 0.9325 0.4197 0.5274 0.039 Uiso 1 1 calc R U . . .
H16C H 0.9900 0.3833 0.5750 0.039 Uiso 1 1 calc R U . . .
C17 C 0.6591(3) 0.5489(2) 0.66271(9) 0.0193(7) Uani 1 1 d . . . . .
H17A H 0.7234 0.5563 0.6865 0.023 Uiso 1 1 calc R U . . .
H17B H 0.6687 0.4831 0.6483 0.023 Uiso 1 1 calc R U . . .
C18 C 0.5444(3) 0.5487(2) 0.68427(9) 0.0211(7) Uani 1 1 d . . . . .
H18A H 0.4811 0.5259 0.6622 0.025 Uiso 1 1 calc R U . . .
H18B H 0.5257 0.6177 0.6934 0.025 Uiso 1 1 calc R U . . .
C19 C 0.5499(3) 0.4805(3) 0.72488(10) 0.0277(8) Uani 1 1 d . . . . .
H19A H 0.5837 0.4153 0.7169 0.033 Uiso 1 1 calc R U . . .
H19B H 0.6024 0.5106 0.7490 0.033 Uiso 1 1 calc R U . . .
C20 C 0.4315(3) 0.4631(3) 0.74193(11) 0.0375(9) Uani 1 1 d . . . . .
H20A H 0.4404 0.4238 0.7696 0.056 Uiso 1 1 calc R U . . .
H20B H 0.3818 0.4266 0.7194 0.056 Uiso 1 1 calc R U . . .
H20C H 0.3953 0.5276 0.7479 0.056 Uiso 1 1 calc R U . . .
C21 C 0.4929(2) 0.2316(2) 0.55721(8) 0.0150(6) Uani 1 1 d . . . . .
C22 C 0.5873(3) 0.2969(2) 0.56675(9) 0.0205(7) Uani 1 1 d . . . . .
H22 H 0.5739 0.3575 0.5821 0.025 Uiso 1 1 calc R U . . .
C23 C 0.6991(3) 0.2770(3) 0.55477(10) 0.0225(7) Uani 1 1 d . . . . .
H23 H 0.7601 0.3238 0.5619 0.027 Uiso 1 1 calc R U . . .
C24 C 0.7224(3) 0.1899(2) 0.53255(9) 0.0206(7) Uani 1 1 d . . . . .
H24 H 0.7987 0.1762 0.5241 0.025 Uiso 1 1 calc R U . . .
C25 C 0.6325(3) 0.1231(2) 0.52292(9) 0.0185(7) Uani 1 1 d . . . . .
H25 H 0.6471 0.0621 0.5081 0.022 Uiso 1 1 calc R U . . .
C26 C 0.5209(3) 0.1446(2) 0.53475(9) 0.0162(6) Uani 1 1 d . . . . .
H26 H 0.4604 0.0976 0.5272 0.019 Uiso 1 1 calc R U . . .
C27 C 0.2620(2) 0.1998(2) 0.53951(9) 0.0173(7) Uani 1 1 d . . . . .
C28 C 0.1892(3) 0.2488(2) 0.50683(9) 0.0211(7) Uani 1 1 d . . . . .
H28 H 0.1951 0.3195 0.5042 0.025 Uiso 1 1 calc R U . . .
C29 C 0.1085(3) 0.1981(3) 0.47795(10) 0.0263(8) Uani 1 1 d . . . . .
H29 H 0.0609 0.2346 0.4563 0.032 Uiso 1 1 calc R U . . .
C30 C 0.0966(3) 0.0964(3) 0.48035(10) 0.0254(8) Uani 1 1 d . . . . .
H30 H 0.0428 0.0619 0.4601 0.030 Uiso 1 1 calc R U . . .
C31 C 0.1647(3) 0.0452(3) 0.51286(11) 0.0260(8) Uani 1 1 d . . . . .
H31 H 0.1563 -0.0252 0.5158 0.031 Uiso 1 1 calc R U . . .
C32 C 0.2450(3) 0.0963(2) 0.54120(10) 0.0228(7) Uani 1 1 d . . . . .
H32 H 0.2911 0.0590 0.5630 0.027 Uiso 1 1 calc R U . . .
C33 C 0.3552(3) 0.2133(2) 0.62489(9) 0.0182(7) Uani 1 1 d . . . . .
C34 C 0.2519(3) 0.1755(3) 0.63991(10) 0.0289(8) Uani 1 1 d . . . . .
H34 H 0.1854 0.1692 0.6191 0.035 Uiso 1 1 calc R U . . .
C35 C 0.2422(3) 0.1470(3) 0.68375(11) 0.0361(9) Uani 1 1 d . . . . .
H35 H 0.1701 0.1214 0.6924 0.043 Uiso 1 1 calc R U . . .
C36 C 0.3364(3) 0.1553(3) 0.71507(10) 0.0302(8) Uani 1 1 d . . . . .
H36 H 0.3299 0.1354 0.7452 0.036 Uiso 1 1 calc R U . . .
C37 C 0.4399(3) 0.1929(2) 0.70200(10) 0.0265(8) Uani 1 1 d . . . . .
H37 H 0.5054 0.1998 0.7232 0.032 Uiso 1 1 calc R U . . .
C38 C 0.4486(3) 0.2210(2) 0.65752(9) 0.0222(7) Uani 1 1 d . . . . .
H38 H 0.5211 0.2463 0.6491 0.027 Uiso 1 1 calc R U . . .
C39 C 0.3389(2) 0.3763(2) 0.57289(9) 0.0168(7) Uani 1 1 d . . . . .
C40 C 0.2877(3) 0.4276(2) 0.60702(10) 0.0209(7) Uani 1 1 d . . . . .
H40 H 0.2711 0.3918 0.6331 0.025 Uiso 1 1 calc R U . . .
C41 C 0.2601(3) 0.5287(3) 0.60433(11) 0.0253(8) Uani 1 1 d . . . . .
H41 H 0.2265 0.5607 0.6285 0.030 Uiso 1 1 calc R U . . .
C42 C 0.2812(3) 0.5828(3) 0.56665(11) 0.0284(8) Uani 1 1 d . . . . .
H42 H 0.2607 0.6516 0.5644 0.034 Uiso 1 1 calc R U . . .
C43 C 0.3328(3) 0.5354(3) 0.53216(10) 0.0249(8) Uani 1 1 d . . . . .
H43 H 0.3486 0.5717 0.5061 0.030 Uiso 1 1 calc R U . . .
C44 C 0.3612(3) 0.4351(2) 0.53588(9) 0.0203(7) Uani 1 1 d . . . . .
H44 H 0.3979 0.4045 0.5121 0.024 Uiso 1 1 calc R U . . .
C45 C 0.2588(3) 0.7650(3) 0.67650(12) 0.0419(7) Uani 1 1 d . . . . .
H45A H 0.2754 0.8097 0.7025 0.050 Uiso 1 1 calc R U . . .
H45B H 0.2915 0.6980 0.6841 0.050 Uiso 1 1 calc R U . . .
C46 C 0.1283(3) 0.7582(3) 0.66425(13) 0.0500(8) Uani 1 1 d . . . . .
H46A H 0.1070 0.6945 0.6489 0.060 Uiso 1 1 calc R U . . .
H46B H 0.0834 0.7650 0.6910 0.060 Uiso 1 1 calc R U . . .
C47 C 0.1085(3) 0.8469(3) 0.63307(13) 0.0500(8) Uani 1 1 d . . . . .
H47A H 0.0468 0.8318 0.6090 0.060 Uiso 1 1 calc R U . . .
H47B H 0.0847 0.9065 0.6497 0.060 Uiso 1 1 calc R U . . .
C48 C 0.2213(3) 0.8645(3) 0.61419(12) 0.0419(7) Uani 1 1 d . . . . .
H48A H 0.2154 0.8466 0.5820 0.050 Uiso 1 1 calc R U . . .
H48B H 0.2428 0.9361 0.6170 0.050 Uiso 1 1 calc R U . . .
B1 B 0.3616(3) 0.2560(3) 0.57348(11) 0.0172(8) Uani 1 1 d . . . . .
N1A N 0.7782(3) 0.7319(2) 0.73906(8) 0.0311(7) Uani 1 1 d . . . . .
N2 N 0.6474(2) 0.92848(19) 0.66038(7) 0.0162(6) Uani 1 1 d . . . . .
N3 N 0.5366(2) 0.79419(18) 0.60056(7) 0.0158(6) Uani 1 1 d D . . . .
N4 N 0.6714(2) 0.62896(18) 0.62864(7) 0.0147(5) Uani 1 1 d . . . . .
O1A O 0.79713(18) 0.76046(17) 0.69866(7) 0.0252(5) Uani 1 1 d . . . . .
O2A O 0.6769(2) 0.71789(19) 0.74537(7) 0.0360(6) Uani 1 1 d . . . . .
O3 O 0.30822(19) 0.80432(18) 0.63802(7) 0.0317(6) Uani 1 1 d . . . . .
Pd1 Pd 0.65840(2) 0.77518(2) 0.65199(2) 0.01427(7) Uani 1 1 d . . . . .
H3 H 0.4599(17) 0.786(2) 0.6108(9) 0.017 Uiso 1 1 d D 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
C1 N2 1.508(4) . ?
C1 C2 1.508(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.480(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.487(4) . ?
C3 C4 1.508(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.505(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.510(4) . ?
C5 C6 1.517(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.517(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.518(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.498(3) . ?
C9 C10 1.513(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.527(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.522(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.506(3) . ?
C13 C14 1.521(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.518(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.521(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.493(4) . ?
C17 C18 1.513(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.519(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.508(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.394(4) . ?
C21 C22 1.402(4) . ?
C21 B1 1.654(4) . ?
C22 C23 1.386(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.398(4) . ?
C27 C28 1.399(4) . ?
C27 B1 1.650(4) . ?
C28 C29 1.393(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.368(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.396(4) . ?
C33 C38 1.397(4) . ?
C33 B1 1.650(4) . ?
C34 C35 1.382(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.375(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.397(4) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.400(4) . ?
C39 C44 1.401(4) . ?
C39 B1 1.629(5) . ?
C40 C41 1.388(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.379(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.385(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.382(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.426(4) . ?
C45 C46 1.516(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.516(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.473(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.428(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1A O2A 1.207(4) . ?
N1A O1A 1.305(3) . ?
N2 Pd1 2.069(2) . ?
N3 Pd1 2.013(2) . ?
N3 H3 0.963(17) . ?
N4 Pd1 2.085(2) . ?
O1A Pd1 2.0437(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 109.7(2) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.1(2) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
N3 C3 C4 106.8(2) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 110.6(2) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 117.1(2) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 C7 111.4(3) . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 111.7(3) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.4(2) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 109.7(2) . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C12 C11 C10 112.8(3) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.1(2) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.2(2) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.4(3) . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.2(2) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.2(2) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 112.5(3) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.5(3) . . ?
C26 C21 B1 123.9(3) . . ?
C22 C21 B1 121.6(3) . . ?
C23 C22 C21 123.0(3) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 118.6(3) . . ?
C25 C24 H24 120.7 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 123.3(3) . . ?
C25 C26 H26 118.4 . . ?
C21 C26 H26 118.4 . . ?
C32 C27 C28 114.3(3) . . ?
C32 C27 B1 121.3(3) . . ?
C28 C27 B1 124.4(3) . . ?
C29 C28 C27 122.5(3) . . ?
C29 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
C30 C29 C28 121.0(3) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 118.5(3) . . ?
C29 C30 H30 120.8 . . ?
C31 C30 H30 120.8 . . ?
C30 C31 C32 120.0(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 123.7(3) . . ?
C31 C32 H32 118.2 . . ?
C27 C32 H32 118.2 . . ?
C34 C33 C38 115.1(3) . . ?
C34 C33 B1 121.9(3) . . ?
C38 C33 B1 122.7(3) . . ?
C35 C34 C33 122.8(3) . . ?
C35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C36 C35 C34 120.5(3) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C37 C36 C35 118.9(3) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 120.0(3) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 122.7(3) . . ?
C33 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
C40 C39 C44 114.7(3) . . ?
C40 C39 B1 123.5(3) . . ?
C44 C39 B1 121.6(3) . . ?
C41 C40 C39 122.8(3) . . ?
C41 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
C42 C41 C40 120.2(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 119.0(3) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C44 C43 C42 119.7(3) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C43 C44 C39 123.5(3) . . ?
C43 C44 H44 118.3 . . ?
C39 C44 H44 118.3 . . ?
O3 C45 C46 105.9(3) . . ?
O3 C45 H45A 110.5 . . ?
C46 C45 H45A 110.5 . . ?
O3 C45 H45B 110.5 . . ?
C46 C45 H45B 110.5 . . ?
H45A C45 H45B 108.7 . . ?
C47 C46 C45 101.5(3) . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46B 111.5 . . ?
C45 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 105.6(3) . . ?
C48 C47 H47A 110.6 . . ?
C46 C47 H47A 110.6 . . ?
C48 C47 H47B 110.6 . . ?
C46 C47 H47B 110.6 . . ?
H47A C47 H47B 108.8 . . ?
O3 C48 C47 108.6(3) . . ?
O3 C48 H48A 110.0 . . ?
C47 C48 H48A 110.0 . . ?
O3 C48 H48B 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.4 . . ?
C39 B1 C27 109.9(2) . . ?
C39 B1 C33 109.4(2) . . ?
C27 B1 C33 109.8(2) . . ?
C39 B1 C21 109.9(2) . . ?
C27 B1 C21 109.3(2) . . ?
C33 B1 C21 108.4(2) . . ?
O2A N1A O1A 115.1(2) . . ?
C9 N2 C1 110.4(2) . . ?
C9 N2 C5 109.1(2) . . ?
C1 N2 C5 111.0(2) . . ?
C9 N2 Pd1 115.44(18) . . ?
C1 N2 Pd1 106.05(17) . . ?
C5 N2 Pd1 104.64(17) . . ?
C2 N3 C3 116.2(2) . . ?
C2 N3 Pd1 106.97(17) . . ?
C3 N3 Pd1 106.77(17) . . ?
C2 N3 H3 106.0(18) . . ?
C3 N3 H3 111.0(18) . . ?
Pd1 N3 H3 109.8(17) . . ?
C17 N4 C4 110.7(2) . . ?
C17 N4 C13 109.7(2) . . ?
C4 N4 C13 111.3(2) . . ?
C17 N4 Pd1 115.38(17) . . ?
C4 N4 Pd1 105.40(17) . . ?
C13 N4 Pd1 104.11(17) . . ?
N1A O1A Pd1 119.04(19) . . ?
C45 O3 C48 107.8(3) . . ?
N3 Pd1 O1A 172.79(9) . . ?
N3 Pd1 N2 85.58(9) . . ?
O1A Pd1 N2 93.65(9) . . ?
N3 Pd1 N4 85.69(9) . . ?
O1A Pd1 N4 93.85(9) . . ?
N2 Pd1 N4 167.27(8) . . ?

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
N2 C1 C2 N3 54.4(3) . . . . ?
N3 C3 C4 N4 -54.5(3) . . . . ?
N2 C5 C6 C7 -179.0(2) . . . . ?
C5 C6 C7 C8 -171.8(3) . . . . ?
N2 C9 C10 C11 170.1(3) . . . . ?
C9 C10 C11 C12 172.7(3) . . . . ?
N4 C13 C14 C15 178.2(2) . . . . ?
C13 C14 C15 C16 179.7(3) . . . . ?
N4 C17 C18 C19 -167.8(3) . . . . ?
C17 C18 C19 C20 -169.1(3) . . . . ?
C26 C21 C22 C23 0.2(4) . . . . ?
B1 C21 C22 C23 178.0(3) . . . . ?
C21 C22 C23 C24 -0.2(5) . . . . ?
C22 C23 C24 C25 -0.5(4) . . . . ?
C23 C24 C25 C26 1.1(4) . . . . ?
C24 C25 C26 C21 -1.1(4) . . . . ?
C22 C21 C26 C25 0.4(4) . . . . ?
B1 C21 C26 C25 -177.3(3) . . . . ?
C32 C27 C28 C29 -1.2(4) . . . . ?
B1 C27 C28 C29 178.1(3) . . . . ?
C27 C28 C29 C30 0.0(5) . . . . ?
C28 C29 C30 C31 1.6(5) . . . . ?
C29 C30 C31 C32 -1.9(5) . . . . ?
C30 C31 C32 C27 0.6(5) . . . . ?
C28 C27 C32 C31 0.9(4) . . . . ?
B1 C27 C32 C31 -178.5(3) . . . . ?
C38 C33 C34 C35 -0.4(5) . . . . ?
B1 C33 C34 C35 -174.6(3) . . . . ?
C33 C34 C35 C36 0.2(6) . . . . ?
C34 C35 C36 C37 0.3(6) . . . . ?
C35 C36 C37 C38 -0.6(5) . . . . ?
C34 C33 C38 C37 0.1(5) . . . . ?
B1 C33 C38 C37 174.2(3) . . . . ?
C36 C37 C38 C33 0.4(5) . . . . ?
C44 C39 C40 C41 0.6(4) . . . . ?
B1 C39 C40 C41 -174.5(3) . . . . ?
C39 C40 C41 C42 1.0(5) . . . . ?
C40 C41 C42 C43 -1.6(5) . . . . ?
C41 C42 C43 C44 0.5(4) . . . . ?
C42 C43 C44 C39 1.1(5) . . . . ?
C40 C39 C44 C43 -1.7(4) . . . . ?
B1 C39 C44 C43 173.5(3) . . . . ?
O3 C45 C46 C47 -32.7(4) . . . . ?
C45 C46 C47 C48 25.5(4) . . . . ?
C46 C47 C48 O3 -10.0(4) . . . . ?
C40 C39 B1 C27 103.0(3) . . . . ?
C44 C39 B1 C27 -71.8(3) . . . . ?
C40 C39 B1 C33 -17.7(4) . . . . ?
C44 C39 B1 C33 167.5(3) . . . . ?
C40 C39 B1 C21 -136.7(3) . . . . ?
C44 C39 B1 C21 48.6(3) . . . . ?
C32 C27 B1 C39 -165.4(3) . . . . ?
C28 C27 B1 C39 15.3(4) . . . . ?
C32 C27 B1 C33 -44.9(4) . . . . ?
C28 C27 B1 C33 135.8(3) . . . . ?
C32 C27 B1 C21 73.9(3) . . . . ?
C28 C27 B1 C21 -105.4(3) . . . . ?
C34 C33 B1 C39 93.3(3) . . . . ?
C38 C33 B1 C39 -80.5(3) . . . . ?
C34 C33 B1 C27 -27.5(4) . . . . ?
C38 C33 B1 C27 158.8(3) . . . . ?
C34 C33 B1 C21 -146.9(3) . . . . ?
C38 C33 B1 C21 39.4(4) . . . . ?
C26 C21 B1 C39 -149.3(3) . . . . ?
C22 C21 B1 C39 33.1(3) . . . . ?
C26 C21 B1 C27 -28.6(4) . . . . ?
C22 C21 B1 C27 153.8(3) . . . . ?
C26 C21 B1 C33 91.1(3) . . . . ?
C22 C21 B1 C33 -86.4(3) . . . . ?
C10 C9 N2 C1 62.9(3) . . . . ?
C10 C9 N2 C5 -174.8(3) . . . . ?
C10 C9 N2 Pd1 -57.3(3) . . . . ?
C2 C1 N2 C9 -159.6(3) . . . . ?
C2 C1 N2 C5 79.2(3) . . . . ?
C2 C1 N2 Pd1 -33.9(3) . . . . ?
C6 C5 N2 C9 -55.3(3) . . . . ?
C6 C5 N2 C1 66.6(3) . . . . ?
C6 C5 N2 Pd1 -179.4(2) . . . . ?
C1 C2 N3 C3 -165.7(2) . . . . ?
C1 C2 N3 Pd1 -46.6(3) . . . . ?
C4 C3 N3 C2 166.4(2) . . . . ?
C4 C3 N3 Pd1 47.2(2) . . . . ?
C18 C17 N4 C4 -59.9(3) . . . . ?
C18 C17 N4 C13 176.9(2) . . . . ?
C18 C17 N4 Pd1 59.7(3) . . . . ?
C3 C4 N4 C17 158.5(2) . . . . ?
C3 C4 N4 C13 -79.1(3) . . . . ?
C3 C4 N4 Pd1 33.1(2) . . . . ?
C14 C13 N4 C17 58.1(3) . . . . ?
C14 C13 N4 C4 -64.8(3) . . . . ?
C14 C13 N4 Pd1 -177.9(2) . . . . ?
O2A N1A O1A Pd1 -1.0(4) . . . . ?
C46 C45 O3 C48 27.9(4) . . . . ?
C47 C48 O3 C45 -11.1(4) . . . . ?

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
C5 H5B O1A 0.99 2.56 3.182(4) 121.0 .
C10 H10A O2A 0.99 2.57 3.277(4) 128.5 .
C13 H13A O1A 0.99 2.56 3.174(3) 120.0 .
C18 H18B O2A 0.99 2.61 3.215(4) 119.7 .
N3 H3 O3 0.963(17) 1.996(19) 2.936(3) 165(3) .

_refine_diff_density_max         1.110
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.085

_shelxl_version_number           2014-1

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# 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 
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# 
#######################################################################

data_PSS-200K
_database_code_depnum_ccdc_archive 'CCDC 1441776'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_PSS-200K            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         16 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation for an extended time, 
leading to even weaker diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5673(12)
_cell_length_b                   13.4937(8)
_cell_length_c                   30.088(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.738(10)
_cell_angle_gamma                90
_cell_volume                     4686.3(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    2894
_cell_measurement_theta_min      3.5420
_cell_measurement_theta_max      23.8280

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.439
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.19582
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            28100
_diffrn_reflns_av_unetI/netI     0.1463
_diffrn_reflns_av_R_equivalents  0.1164
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.095
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             9491
_reflns_number_gt                5238
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9491
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0650
_refine_ls_wR_factor_ref         0.1395
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_restrained_S_all      0.989
_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
C1 C 0.5531(5) 0.9623(3) 0.62809(18) 0.0428(15) Uani 1 1 d . . . . .
H1A H 0.4788 0.9568 0.6425 0.051 Uiso 1 1 calc R U . . .
H1B H 0.5648 1.0327 0.6203 0.051 Uiso 1 1 calc R U . . .
C2 C 0.5481(5) 0.9008(3) 0.58679(17) 0.0438(15) Uani 1 1 d . . . . .
H2A H 0.4793 0.9187 0.5672 0.053 Uiso 1 1 calc R U . . .
H2B H 0.6183 0.9117 0.5703 0.053 Uiso 1 1 calc R U . . .
C3 C 0.5608(5) 0.7204(3) 0.56624(16) 0.0348(12) Uani 1 1 d . . . . .
H3A H 0.6300 0.7375 0.5501 0.042 Uiso 1 1 calc R U . . .
H3B H 0.4930 0.7164 0.5445 0.042 Uiso 1 1 calc R U . . .
C4 C 0.5787(5) 0.6229(3) 0.59067(17) 0.0351(13) Uani 1 1 d . . . . .
H4A H 0.5048 0.6021 0.6026 0.042 Uiso 1 1 calc R U . . .
H4B H 0.6014 0.5715 0.5694 0.042 Uiso 1 1 calc R U . . .
C5 C 0.7665(5) 0.9658(3) 0.64673(18) 0.0421(14) Uani 1 1 d . . . . .
H5A H 0.7768 0.9438 0.6158 0.050 Uiso 1 1 calc R U . . .
H5B H 0.8281 0.9338 0.6661 0.050 Uiso 1 1 calc R U . . .
C6 C 0.7856(5) 1.0770(3) 0.6489(2) 0.0533(17) Uani 1 1 d . . . . .
H6A H 0.7253 1.1105 0.6294 0.064 Uiso 1 1 calc R U . . .
H6B H 0.7781 1.1002 0.6797 0.064 Uiso 1 1 calc R U . . .
C7 C 0.9028(6) 1.1046(4) 0.6344(2) 0.067(2) Uani 1 1 d . . . . .
H7A H 0.9070 1.0877 0.6025 0.080 Uiso 1 1 calc R U . . .
H7B H 0.9624 1.0652 0.6516 0.080 Uiso 1 1 calc R U . . .
C8 C 0.9295(6) 1.2133(4) 0.6408(3) 0.085(2) Uani 1 1 d . . . . .
H8A H 0.9457 1.2270 0.6726 0.128 Uiso 1 1 calc R U . . .
H8B H 0.8628 1.2527 0.6294 0.128 Uiso 1 1 calc R U . . .
H8C H 0.9973 1.2307 0.6245 0.128 Uiso 1 1 calc R U . . .
C9 C 0.6336(5) 0.9605(3) 0.70710(17) 0.0405(14) Uani 1 1 d . . . . .
H9A H 0.6300 1.0338 0.7077 0.049 Uiso 1 1 calc R U . . .
H9B H 0.7018 0.9400 0.7265 0.049 Uiso 1 1 calc R U . . .
C10 C 0.5254(5) 0.9199(3) 0.72647(18) 0.0443(15) Uani 1 1 d . . . . .
H10A H 0.5216 0.8472 0.7222 0.053 Uiso 1 1 calc R U . . .
H10B H 0.4557 0.9496 0.7110 0.053 Uiso 1 1 calc R U . . .
C11 C 0.5281(6) 0.9440(4) 0.7759(2) 0.0550(17) Uani 1 1 d . . . . .
H11A H 0.5939 0.9088 0.7915 0.066 Uiso 1 1 calc R U . . .
H11B H 0.5410 1.0161 0.7800 0.066 Uiso 1 1 calc R U . . .
C12 C 0.4169(6) 0.9149(5) 0.7964(2) 0.076(2) Uani 1 1 d . . . . .
H12A H 0.4247 0.9271 0.8286 0.114 Uiso 1 1 calc R U . . .
H12B H 0.4015 0.8443 0.7910 0.114 Uiso 1 1 calc R U . . .
H12C H 0.3525 0.9543 0.7830 0.114 Uiso 1 1 calc R U . . .
C13 C 0.7906(4) 0.6244(3) 0.61133(18) 0.0363(13) Uani 1 1 d . . . . .
H13A H 0.8474 0.6384 0.6366 0.044 Uiso 1 1 calc R U . . .
H13B H 0.7979 0.6779 0.5892 0.044 Uiso 1 1 calc R U . . .
C14 C 0.8248(5) 0.5275(3) 0.59015(19) 0.0440(15) Uani 1 1 d . . . . .
H14A H 0.8206 0.4732 0.6121 0.053 Uiso 1 1 calc R U . . .
H14B H 0.7694 0.5123 0.5646 0.053 Uiso 1 1 calc R U . . .
C15 C 0.9444(5) 0.5326(3) 0.5745(2) 0.0465(15) Uani 1 1 d . . . . .
H15A H 0.9989 0.5486 0.6003 0.056 Uiso 1 1 calc R U . . .
H15B H 0.9478 0.5876 0.5528 0.056 Uiso 1 1 calc R U . . .
C16 C 0.9851(5) 0.4380(3) 0.5528(2) 0.0525(16) Uani 1 1 d . . . . .
H16A H 1.0644 0.4470 0.5440 0.079 Uiso 1 1 calc R U . . .
H16B H 0.9339 0.4230 0.5264 0.079 Uiso 1 1 calc R U . . .
H16C H 0.9830 0.3830 0.5740 0.079 Uiso 1 1 calc R U . . .
C17 C 0.6570(5) 0.5506(3) 0.66189(16) 0.0360(13) Uani 1 1 d . . . . .
H17A H 0.7217 0.5557 0.6850 0.043 Uiso 1 1 calc R U . . .
H17B H 0.6633 0.4855 0.6471 0.043 Uiso 1 1 calc R U . . .
C18 C 0.5445(5) 0.5539(4) 0.68431(18) 0.0456(15) Uani 1 1 d . . . . .
H18A H 0.4796 0.5386 0.6623 0.055 Uiso 1 1 calc R U . . .
H18B H 0.5323 0.6214 0.6960 0.055 Uiso 1 1 calc R U . . .
C19 C 0.5453(6) 0.4800(4) 0.7221(2) 0.071(2) Uani 1 1 d . . . . .
H19A H 0.5690 0.4145 0.7110 0.085 Uiso 1 1 calc R U . . .
H19B H 0.6041 0.5008 0.7457 0.085 Uiso 1 1 calc R U . . .
C20 C 0.4326(7) 0.4690(5) 0.7422(3) 0.097(3) Uani 1 1 d . . . . .
H20A H 0.4443 0.4356 0.7711 0.145 Uiso 1 1 calc R U . . .
H20B H 0.3802 0.4295 0.7224 0.145 Uiso 1 1 calc R U . . .
H20C H 0.3987 0.5346 0.7464 0.145 Uiso 1 1 calc R U . . .
C21 C 0.4937(4) 0.2311(3) 0.55647(15) 0.0285(11) Uani 1 1 d . . . . .
C22 C 0.5860(5) 0.2949(3) 0.56541(19) 0.0417(14) Uani 1 1 d . . . . .
H22 H 0.5726 0.3546 0.5810 0.050 Uiso 1 1 calc R U . . .
C23 C 0.6967(5) 0.2762(4) 0.55278(19) 0.0456(14) Uani 1 1 d . . . . .
H23 H 0.7568 0.3229 0.5596 0.055 Uiso 1 1 calc R U . . .
C24 C 0.7203(5) 0.1900(3) 0.53032(19) 0.0429(15) Uani 1 1 d . . . . .
H24 H 0.7960 0.1765 0.5214 0.052 Uiso 1 1 calc R U . . .
C25 C 0.6310(5) 0.1245(3) 0.52129(18) 0.0413(14) Uani 1 1 d . . . . .
H25 H 0.6451 0.0643 0.5062 0.050 Uiso 1 1 calc R U . . .
C26 C 0.5202(4) 0.1451(3) 0.53397(16) 0.0314(12) Uani 1 1 d . . . . .
H26 H 0.4603 0.0984 0.5270 0.038 Uiso 1 1 calc R U . . .
C27 C 0.2638(4) 0.2007(3) 0.54065(17) 0.0328(13) Uani 1 1 d . . . . .
C28 C 0.1900(5) 0.2492(4) 0.50955(19) 0.0448(15) Uani 1 1 d . . . . .
H28 H 0.1959 0.3192 0.5076 0.054 Uiso 1 1 calc R U . . .
C29 C 0.1083(5) 0.2022(4) 0.4811(2) 0.0534(16) Uani 1 1 d . . . . .
H29 H 0.0606 0.2398 0.4605 0.064 Uiso 1 1 calc R U . . .
C30 C 0.0966(5) 0.0996(4) 0.4830(2) 0.0509(16) Uani 1 1 d . . . . .
H30 H 0.0423 0.0657 0.4634 0.061 Uiso 1 1 calc R U . . .
C31 C 0.1659(5) 0.0495(4) 0.5139(2) 0.0520(18) Uani 1 1 d . . . . .
H31 H 0.1580 -0.0203 0.5162 0.062 Uiso 1 1 calc R U . . .
C32 C 0.2465(5) 0.0971(3) 0.5416(2) 0.0453(15) Uani 1 1 d . . . . .
H32 H 0.2928 0.0588 0.5624 0.054 Uiso 1 1 calc R U . . .
C33 C 0.3580(5) 0.2129(3) 0.62469(18) 0.0363(13) Uani 1 1 d . . . . .
C34 C 0.2572(6) 0.1748(4) 0.6408(2) 0.0642(19) Uani 1 1 d . . . . .
H34 H 0.1908 0.1681 0.6207 0.077 Uiso 1 1 calc R U . . .
C35 C 0.2486(7) 0.1459(5) 0.6851(2) 0.083(2) Uani 1 1 d . . . . .
H35 H 0.1773 0.1211 0.6946 0.100 Uiso 1 1 calc R U . . .
C36 C 0.3417(7) 0.1534(4) 0.7145(2) 0.068(2) Uani 1 1 d . . . . .
H36 H 0.3368 0.1326 0.7445 0.082 Uiso 1 1 calc R U . . .
C37 C 0.4431(6) 0.1912(4) 0.7006(2) 0.0586(18) Uani 1 1 d . . . . .
H37 H 0.5087 0.1980 0.7211 0.070 Uiso 1 1 calc R U . . .
C38 C 0.4498(6) 0.2194(3) 0.65645(19) 0.0472(15) Uani 1 1 d . . . . .
H38 H 0.5214 0.2447 0.6475 0.057 Uiso 1 1 calc R U . . .
C39 C 0.3404(4) 0.3751(3) 0.57320(17) 0.0335(12) Uani 1 1 d . . . . .
C40 C 0.2884(5) 0.4248(3) 0.60709(19) 0.0420(14) Uani 1 1 d . . . . .
H40 H 0.2710 0.3892 0.6331 0.050 Uiso 1 1 calc R U . . .
C41 C 0.2610(5) 0.5244(4) 0.6043(2) 0.0513(17) Uani 1 1 d . . . . .
H41 H 0.2261 0.5557 0.6283 0.062 Uiso 1 1 calc R U . . .
C42 C 0.2834(5) 0.5786(4) 0.5673(2) 0.0552(18) Uani 1 1 d . . . . .
H42 H 0.2630 0.6467 0.5652 0.066 Uiso 1 1 calc R U . . .
C43 C 0.3360(5) 0.5327(3) 0.5333(2) 0.0481(16) Uani 1 1 d . . . . .
H43 H 0.3527 0.5692 0.5075 0.058 Uiso 1 1 calc R U . . .
C44 C 0.3650(5) 0.4324(3) 0.53656(18) 0.0392(14) Uani 1 1 d . . . . .
H44 H 0.4029 0.4022 0.5130 0.047 Uiso 1 1 calc R U . . .
C45 C 0.2605(7) 0.7654(5) 0.6752(2) 0.0787(16) Uani 1 1 d . . . . .
H45A H 0.2772 0.8090 0.7013 0.094 Uiso 1 1 calc R U . . .
H45B H 0.2919 0.6987 0.6824 0.094 Uiso 1 1 calc R U . . .
C46 C 0.1331(7) 0.7598(6) 0.6641(3) 0.0985(19) Uani 1 1 d . . . . .
H46A H 0.1104 0.6938 0.6522 0.118 Uiso 1 1 calc R U . . .
H46B H 0.0892 0.7740 0.6906 0.118 Uiso 1 1 calc R U . . .
C47 C 0.1143(7) 0.8365(6) 0.6304(3) 0.0985(19) Uani 1 1 d . . . . .
H47A H 0.0611 0.8119 0.6057 0.118 Uiso 1 1 calc R U . . .
H47B H 0.0790 0.8957 0.6435 0.118 Uiso 1 1 calc R U . . .
C48 C 0.2254(7) 0.8621(5) 0.6138(2) 0.0787(16) Uani 1 1 d . . . . .
H48A H 0.2250 0.8480 0.5815 0.094 Uiso 1 1 calc R U . . .
H48B H 0.2415 0.9335 0.6185 0.094 Uiso 1 1 calc R U . . .
B1 B 0.3631(5) 0.2546(3) 0.5734(2) 0.0317(14) Uani 1 1 d . . . . .
N1A N 0.7836(7) 0.7325(4) 0.7373(2) 0.0720(18) Uani 1 1 d . . . . .
N2 N 0.6515(4) 0.9276(3) 0.65997(14) 0.0357(11) Uani 1 1 d . . . . .
N3 N 0.5411(4) 0.7952(3) 0.60090(13) 0.0313(10) Uani 1 1 d D . . . .
N4 N 0.6703(4) 0.6301(2) 0.62825(14) 0.0332(10) Uani 1 1 d . . . . .
O1A O 0.7982(3) 0.7601(2) 0.69670(14) 0.0530(11) Uani 1 1 d . . . . .
O2A O 0.6831(6) 0.7189(3) 0.74528(16) 0.0812(15) Uani 1 1 d . . . . .
O3 O 0.3112(4) 0.8043(3) 0.63741(15) 0.0639(12) Uani 1 1 d . . . . .
Pd1 Pd 0.66044(4) 0.77557(3) 0.65161(2) 0.03321(13) Uani 1 1 d . . . . .
H3 H 0.465(2) 0.787(3) 0.6129(15) 0.040 Uiso 1 1 d D 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
C1 C2 1.493(6) . ?
C1 N2 1.515(7) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.491(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.480(5) . ?
C3 C4 1.514(6) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.501(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.504(6) . ?
C5 C6 1.517(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.498(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.508(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.513(6) . ?
C9 C10 1.518(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.520(7) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.516(8) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.515(6) . ?
C13 C14 1.518(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.492(7) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.523(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.490(5) . ?
C17 C18 1.505(6) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.513(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.479(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.384(6) . ?
C21 C26 1.389(6) . ?
C21 B1 1.655(7) . ?
C22 C23 1.383(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.382(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.374(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(7) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.389(7) . ?
C27 C32 1.412(6) . ?
C27 B1 1.634(8) . ?
C28 C29 1.386(8) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.368(8) . ?
C30 H30 0.9500 . ?
C31 C32 1.369(8) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.385(8) . ?
C33 C34 1.390(7) . ?
C33 B1 1.649(7) . ?
C34 C35 1.399(8) . ?
C34 H34 0.9500 . ?
C35 C36 1.352(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.368(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.390(7) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.390(6) . ?
C39 C44 1.391(6) . ?
C39 B1 1.647(6) . ?
C40 C41 1.382(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.371(8) . ?
C41 H41 0.9500 . ?
C42 C43 1.372(7) . ?
C42 H42 0.9500 . ?
C43 C44 1.397(6) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.414(7) . ?
C45 C46 1.491(10) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.456(9) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.450(9) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.417(8) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1A O2A 1.217(7) . ?
N1A O1A 1.297(6) . ?
N2 Pd1 2.071(3) . ?
N3 Pd1 2.007(4) . ?
N3 H3 0.983(19) . ?
N4 Pd1 2.090(3) . ?
O1A Pd1 2.035(4) . ?

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
C2 C1 N2 110.0(4) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.1(4) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.5 . . ?
N3 C3 C4 105.8(4) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 112.1(4) . . ?
N4 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N4 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
N2 C5 C6 117.2(4) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.5(5) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 112.8(5) . . ?
C6 C7 H7A 109.0 . . ?
C8 C7 H7A 109.0 . . ?
C6 C7 H7B 109.0 . . ?
C8 C7 H7B 109.0 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 114.9(4) . . ?
N2 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 109.4(5) . . ?
C9 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
C9 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C12 C11 C10 112.3(6) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.1(4) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.4(4) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 114.5(4) . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15B 108.6 . . ?
C16 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 114.5(4) . . ?
N4 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
N4 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 110.8(5) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 114.3(6) . . ?
C20 C19 H19A 108.7 . . ?
C18 C19 H19A 108.7 . . ?
C20 C19 H19B 108.7 . . ?
C18 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 115.0(4) . . ?
C22 C21 B1 122.0(4) . . ?
C26 C21 B1 123.0(4) . . ?
C23 C22 C21 123.4(4) . . ?
C23 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
C24 C23 C22 120.3(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 117.9(5) . . ?
C25 C24 H24 121.0 . . ?
C23 C24 H24 121.0 . . ?
C24 C25 C26 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 122.6(5) . . ?
C25 C26 H26 118.7 . . ?
C21 C26 H26 118.7 . . ?
C28 C27 C32 113.4(5) . . ?
C28 C27 B1 125.0(4) . . ?
C32 C27 B1 121.6(5) . . ?
C29 C28 C27 124.4(5) . . ?
C29 C28 H28 117.8 . . ?
C27 C28 H28 117.8 . . ?
C28 C29 C30 119.6(6) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C31 C30 C29 117.7(6) . . ?
C31 C30 H30 121.2 . . ?
C29 C30 H30 121.2 . . ?
C30 C31 C32 121.9(5) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 H31 119.1 . . ?
C31 C32 C27 123.0(6) . . ?
C31 C32 H32 118.5 . . ?
C27 C32 H32 118.5 . . ?
C38 C33 C34 114.0(5) . . ?
C38 C33 B1 123.5(5) . . ?
C34 C33 B1 122.4(6) . . ?
C33 C34 C35 123.3(7) . . ?
C33 C34 H34 118.3 . . ?
C35 C34 H34 118.3 . . ?
C36 C35 C34 119.9(7) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 119.5(7) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C36 C37 C38 119.7(7) . . ?
C36 C37 H37 120.2 . . ?
C38 C37 H37 120.2 . . ?
C33 C38 C37 123.7(6) . . ?
C33 C38 H38 118.2 . . ?
C37 C38 H38 118.2 . . ?
C40 C39 C44 115.7(4) . . ?
C40 C39 B1 123.5(4) . . ?
C44 C39 B1 120.7(4) . . ?
C41 C40 C39 122.2(5) . . ?
C41 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?
C42 C41 C40 121.0(5) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 118.7(5) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 120.1(5) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C39 C44 C43 122.3(5) . . ?
C39 C44 H44 118.9 . . ?
C43 C44 H44 118.9 . . ?
O3 C45 C46 107.2(6) . . ?
O3 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
O3 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.5 . . ?
C47 C46 C45 102.7(7) . . ?
C47 C46 H46A 111.2 . . ?
C45 C46 H46A 111.2 . . ?
C47 C46 H46B 111.2 . . ?
C45 C46 H46B 111.2 . . ?
H46A C46 H46B 109.1 . . ?
C48 C47 C46 108.3(7) . . ?
C48 C47 H47A 110.0 . . ?
C46 C47 H47A 110.0 . . ?
C48 C47 H47B 110.0 . . ?
C46 C47 H47B 110.0 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 107.7(6) . . ?
O3 C48 H48A 110.2 . . ?
C47 C48 H48A 110.2 . . ?
O3 C48 H48B 110.2 . . ?
C47 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
C27 B1 C39 109.4(4) . . ?
C27 B1 C33 110.2(4) . . ?
C39 B1 C33 108.9(4) . . ?
C27 B1 C21 110.5(4) . . ?
C39 B1 C21 109.7(4) . . ?
C33 B1 C21 108.1(4) . . ?
O2A N1A O1A 114.4(6) . . ?
C5 N2 C9 109.0(4) . . ?
C5 N2 C1 111.6(4) . . ?
C9 N2 C1 111.1(4) . . ?
C5 N2 Pd1 104.8(3) . . ?
C9 N2 Pd1 114.6(3) . . ?
C1 N2 Pd1 105.7(3) . . ?
C3 N3 C2 115.9(4) . . ?
C3 N3 Pd1 108.4(3) . . ?
C2 N3 Pd1 107.2(3) . . ?
C3 N3 H3 112(3) . . ?
C2 N3 H3 106(2) . . ?
Pd1 N3 H3 107(3) . . ?
C17 N4 C4 111.4(4) . . ?
C17 N4 C13 109.3(4) . . ?
C4 N4 C13 111.2(4) . . ?
C17 N4 Pd1 115.9(3) . . ?
C4 N4 Pd1 105.2(3) . . ?
C13 N4 Pd1 103.5(3) . . ?
N1A O1A Pd1 120.9(4) . . ?
C45 O3 C48 107.1(5) . . ?
N3 Pd1 O1A 171.92(17) . . ?
N3 Pd1 N2 85.67(16) . . ?
O1A Pd1 N2 93.67(16) . . ?
N3 Pd1 N4 85.30(16) . . ?
O1A Pd1 N4 94.01(15) . . ?
N2 Pd1 N4 167.29(16) . . ?

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
N2 C1 C2 N3 54.3(6) . . . . ?
N3 C3 C4 N4 -52.3(5) . . . . ?
N2 C5 C6 C7 -179.4(5) . . . . ?
C5 C6 C7 C8 -173.8(5) . . . . ?
N2 C9 C10 C11 170.6(4) . . . . ?
C9 C10 C11 C12 174.1(5) . . . . ?
N4 C13 C14 C15 179.3(5) . . . . ?
C13 C14 C15 C16 -180.0(5) . . . . ?
N4 C17 C18 C19 -172.2(5) . . . . ?
C17 C18 C19 C20 -172.4(6) . . . . ?
C26 C21 C22 C23 0.7(8) . . . . ?
B1 C21 C22 C23 178.3(5) . . . . ?
C21 C22 C23 C24 -0.5(9) . . . . ?
C22 C23 C24 C25 -0.2(8) . . . . ?
C23 C24 C25 C26 0.7(8) . . . . ?
C24 C25 C26 C21 -0.6(8) . . . . ?
C22 C21 C26 C25 -0.1(7) . . . . ?
B1 C21 C26 C25 -177.7(5) . . . . ?
C32 C27 C28 C29 -1.4(7) . . . . ?
B1 C27 C28 C29 178.1(5) . . . . ?
C27 C28 C29 C30 0.2(8) . . . . ?
C28 C29 C30 C31 1.3(8) . . . . ?
C29 C30 C31 C32 -1.6(8) . . . . ?
C30 C31 C32 C27 0.4(8) . . . . ?
C28 C27 C32 C31 1.1(7) . . . . ?
B1 C27 C32 C31 -178.4(5) . . . . ?
C38 C33 C34 C35 0.2(8) . . . . ?
B1 C33 C34 C35 -175.0(5) . . . . ?
C33 C34 C35 C36 -0.8(11) . . . . ?
C34 C35 C36 C37 1.3(11) . . . . ?
C35 C36 C37 C38 -1.3(9) . . . . ?
C34 C33 C38 C37 -0.2(7) . . . . ?
B1 C33 C38 C37 175.0(4) . . . . ?
C36 C37 C38 C33 0.8(8) . . . . ?
C44 C39 C40 C41 1.1(8) . . . . ?
B1 C39 C40 C41 -174.1(5) . . . . ?
C39 C40 C41 C42 0.6(9) . . . . ?
C40 C41 C42 C43 -1.3(9) . . . . ?
C41 C42 C43 C44 0.4(9) . . . . ?
C40 C39 C44 C43 -2.0(8) . . . . ?
B1 C39 C44 C43 173.3(5) . . . . ?
C42 C43 C44 C39 1.3(8) . . . . ?
O3 C45 C46 C47 -25.9(8) . . . . ?
C45 C46 C47 C48 16.3(9) . . . . ?
C46 C47 C48 O3 -1.3(9) . . . . ?
C28 C27 B1 C39 14.5(6) . . . . ?
C32 C27 B1 C39 -166.1(4) . . . . ?
C28 C27 B1 C33 134.2(5) . . . . ?
C32 C27 B1 C33 -46.4(6) . . . . ?
C28 C27 B1 C21 -106.4(5) . . . . ?
C32 C27 B1 C21 73.1(5) . . . . ?
C40 C39 B1 C27 101.2(6) . . . . ?
C44 C39 B1 C27 -73.8(6) . . . . ?
C40 C39 B1 C33 -19.3(7) . . . . ?
C44 C39 B1 C33 165.7(5) . . . . ?
C40 C39 B1 C21 -137.5(5) . . . . ?
C44 C39 B1 C21 47.5(7) . . . . ?
C38 C33 B1 C27 159.1(4) . . . . ?
C34 C33 B1 C27 -26.1(6) . . . . ?
C38 C33 B1 C39 -80.9(6) . . . . ?
C34 C33 B1 C39 93.9(6) . . . . ?
C38 C33 B1 C21 38.3(6) . . . . ?
C34 C33 B1 C21 -146.9(5) . . . . ?
C22 C21 B1 C27 153.6(5) . . . . ?
C26 C21 B1 C27 -28.9(6) . . . . ?
C22 C21 B1 C39 32.9(7) . . . . ?
C26 C21 B1 C39 -149.6(4) . . . . ?
C22 C21 B1 C33 -85.7(5) . . . . ?
C26 C21 B1 C33 91.7(6) . . . . ?
C6 C5 N2 C9 -57.7(6) . . . . ?
C6 C5 N2 C1 65.4(6) . . . . ?
C6 C5 N2 Pd1 179.3(4) . . . . ?
C10 C9 N2 C5 -175.0(4) . . . . ?
C10 C9 N2 C1 61.7(5) . . . . ?
C10 C9 N2 Pd1 -58.0(5) . . . . ?
C2 C1 N2 C5 78.8(5) . . . . ?
C2 C1 N2 C9 -159.3(4) . . . . ?
C2 C1 N2 Pd1 -34.5(5) . . . . ?
C4 C3 N3 C2 166.4(4) . . . . ?
C4 C3 N3 Pd1 45.9(4) . . . . ?
C1 C2 N3 C3 -167.3(5) . . . . ?
C1 C2 N3 Pd1 -46.0(5) . . . . ?
C18 C17 N4 C4 -61.8(5) . . . . ?
C18 C17 N4 C13 174.9(4) . . . . ?
C18 C17 N4 Pd1 58.5(5) . . . . ?
C3 C4 N4 C17 158.2(4) . . . . ?
C3 C4 N4 C13 -79.6(4) . . . . ?
C3 C4 N4 Pd1 31.8(4) . . . . ?
C14 C13 N4 C17 58.1(6) . . . . ?
C14 C13 N4 C4 -65.3(5) . . . . ?
C14 C13 N4 Pd1 -177.8(4) . . . . ?
O2A N1A O1A Pd1 -1.0(7) . . . . ?
C46 C45 O3 C48 26.0(7) . . . . ?
C47 C48 O3 C45 -15.4(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
C5 H5B O1A 0.99 2.55 3.167(6) 120.3 .
C10 H10A O2A 0.99 2.61 3.296(7) 126.7 .
C13 H13A O1A 0.99 2.53 3.151(6) 120.2 .
C18 H18B O2A 0.99 2.58 3.242(8) 124.6 .
N3 H3 O3 0.983(19) 1.98(2) 2.946(6) 167(3) .

_refine_diff_density_max         0.706
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.089

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_PSS-220K
_database_code_depnum_ccdc_archive 'CCDC 1441777'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_PSS-220K            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         14 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation for an extended time, 
leading to even weaker diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5830(5)
_cell_length_b                   13.5168(4)
_cell_length_c                   30.1137(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.570(4)
_cell_angle_gamma                90
_cell_volume                     4705.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    5026
_cell_measurement_theta_min      3.2960
_cell_measurement_theta_max      25.3330

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.437
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71664
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            28079
_diffrn_reflns_av_unetI/netI     0.0921
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.011
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             9521
_reflns_number_gt                6156
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0377P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9521
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1141
_refine_ls_wR_factor_gt          0.0966
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_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
C1 C 0.5542(4) 0.9627(2) 0.62858(13) 0.0494(10) Uani 1 1 d . . . . .
H1A H 0.4808 0.9572 0.6429 0.059 Uiso 1 1 calc R U . . .
H1B H 0.5658 1.0324 0.6210 0.059 Uiso 1 1 calc R U . . .
C2 C 0.5496(4) 0.9013(2) 0.58708(12) 0.0478(10) Uani 1 1 d . . . . .
H2A H 0.4825 0.9199 0.5674 0.057 Uiso 1 1 calc R U . . .
H2B H 0.6197 0.9112 0.5711 0.057 Uiso 1 1 calc R U . . .
C3 C 0.5622(3) 0.7206(2) 0.56665(11) 0.0374(8) Uani 1 1 d . . . . .
H3A H 0.6318 0.7373 0.5513 0.045 Uiso 1 1 calc R U . . .
H3B H 0.4965 0.7166 0.5446 0.045 Uiso 1 1 calc R U . . .
C4 C 0.5783(3) 0.6234(2) 0.59101(12) 0.0384(9) Uani 1 1 d . . . . .
H4A H 0.5054 0.6042 0.6034 0.046 Uiso 1 1 calc R U . . .
H4B H 0.5992 0.5719 0.5701 0.046 Uiso 1 1 calc R U . . .
C5 C 0.7666(4) 0.9658(2) 0.64662(13) 0.0491(10) Uani 1 1 d . . . . .
H5A H 0.7768 0.9437 0.6161 0.059 Uiso 1 1 calc R U . . .
H5B H 0.8273 0.9344 0.6658 0.059 Uiso 1 1 calc R U . . .
C6 C 0.7855(4) 1.0771(2) 0.64847(14) 0.0588(12) Uani 1 1 d . . . . .
H6A H 0.7259 1.1100 0.6292 0.071 Uiso 1 1 calc R U . . .
H6B H 0.7781 1.1005 0.6790 0.071 Uiso 1 1 calc R U . . .
C7 C 0.9032(4) 1.1044(3) 0.63370(17) 0.0743(14) Uani 1 1 d . . . . .
H7A H 0.9074 1.0871 0.6022 0.089 Uiso 1 1 calc R U . . .
H7B H 0.9621 1.0657 0.6508 0.089 Uiso 1 1 calc R U . . .
C8 C 0.9292(5) 1.2131(3) 0.6398(2) 0.104(2) Uani 1 1 d . . . . .
H8A H 0.9401 1.2279 0.6713 0.156 Uiso 1 1 calc R U . . .
H8B H 0.8651 1.2517 0.6268 0.156 Uiso 1 1 calc R U . . .
H8C H 0.9991 1.2295 0.6253 0.156 Uiso 1 1 calc R U . . .
C9 C 0.6332(4) 0.9609(2) 0.70650(12) 0.0457(10) Uani 1 1 d . . . . .
H9A H 0.6282 1.0333 0.7068 0.055 Uiso 1 1 calc R U . . .
H9B H 0.7014 0.9420 0.7255 0.055 Uiso 1 1 calc R U . . .
C10 C 0.5278(4) 0.9197(3) 0.72641(13) 0.0505(11) Uani 1 1 d . . . . .
H10A H 0.5252 0.8479 0.7221 0.061 Uiso 1 1 calc R U . . .
H10B H 0.4582 0.9482 0.7112 0.061 Uiso 1 1 calc R U . . .
C11 C 0.5289(4) 0.9429(3) 0.77574(14) 0.0618(13) Uani 1 1 d . . . . .
H11A H 0.5933 0.9075 0.7912 0.074 Uiso 1 1 calc R U . . .
H11B H 0.5423 1.0139 0.7801 0.074 Uiso 1 1 calc R U . . .
C12 C 0.4178(5) 0.9148(4) 0.79626(17) 0.0850(17) Uani 1 1 d . . . . .
H12A H 0.4248 0.9284 0.8279 0.128 Uiso 1 1 calc R U . . .
H12B H 0.4029 0.8448 0.7915 0.128 Uiso 1 1 calc R U . . .
H12C H 0.3543 0.9530 0.7825 0.128 Uiso 1 1 calc R U . . .
C13 C 0.7898(3) 0.6247(2) 0.61089(13) 0.0414(9) Uani 1 1 d . . . . .
H13A H 0.8459 0.6384 0.6359 0.050 Uiso 1 1 calc R U . . .
H13B H 0.7974 0.6775 0.5890 0.050 Uiso 1 1 calc R U . . .
C14 C 0.8237(3) 0.5279(2) 0.58977(14) 0.0488(11) Uani 1 1 d . . . . .
H14A H 0.8182 0.4742 0.6114 0.059 Uiso 1 1 calc R U . . .
H14B H 0.7696 0.5135 0.5643 0.059 Uiso 1 1 calc R U . . .
C15 C 0.9451(4) 0.5321(2) 0.57449(15) 0.0564(12) Uani 1 1 d . . . . .
H15A H 0.9983 0.5479 0.6001 0.068 Uiso 1 1 calc R U . . .
H15B H 0.9497 0.5860 0.5529 0.068 Uiso 1 1 calc R U . . .
C16 C 0.9848(4) 0.4373(3) 0.55345(16) 0.0634(13) Uani 1 1 d . . . . .
H16A H 1.0629 0.4457 0.5442 0.095 Uiso 1 1 calc R U . . .
H16B H 0.9335 0.4216 0.5277 0.095 Uiso 1 1 calc R U . . .
H16C H 0.9833 0.3838 0.5749 0.095 Uiso 1 1 calc R U . . .
C17 C 0.6559(3) 0.5519(2) 0.66150(12) 0.0424(10) Uani 1 1 d . . . . .
H17A H 0.7205 0.5558 0.6840 0.051 Uiso 1 1 calc R U . . .
H17B H 0.6606 0.4875 0.6467 0.051 Uiso 1 1 calc R U . . .
C18 C 0.5444(4) 0.5559(3) 0.68473(13) 0.0538(11) Uani 1 1 d . . . . .
H18A H 0.4791 0.5430 0.6632 0.065 Uiso 1 1 calc R U . . .
H18B H 0.5344 0.6222 0.6971 0.065 Uiso 1 1 calc R U . . .
C19 C 0.5449(5) 0.4797(3) 0.72193(17) 0.0798(16) Uani 1 1 d . . . . .
H19A H 0.5657 0.4151 0.7100 0.096 Uiso 1 1 calc R U . . .
H19B H 0.6047 0.4978 0.7449 0.096 Uiso 1 1 calc R U . . .
C20 C 0.4336(6) 0.4705(4) 0.7426(2) 0.116(2) Uani 1 1 d . . . . .
H20A H 0.4433 0.4288 0.7688 0.174 Uiso 1 1 calc R U . . .
H20B H 0.3769 0.4410 0.7215 0.174 Uiso 1 1 calc R U . . .
H20C H 0.4073 0.5355 0.7511 0.174 Uiso 1 1 calc R U . . .
C21 C 0.4931(3) 0.2308(2) 0.55651(11) 0.0345(8) Uani 1 1 d . . . . .
C22 C 0.5860(3) 0.2945(2) 0.56497(13) 0.0468(10) Uani 1 1 d . . . . .
H22 H 0.5731 0.3537 0.5803 0.056 Uiso 1 1 calc R U . . .
C23 C 0.6961(3) 0.2758(2) 0.55210(14) 0.0518(11) Uani 1 1 d . . . . .
H23 H 0.7553 0.3221 0.5585 0.062 Uiso 1 1 calc R U . . .
C24 C 0.7199(4) 0.1894(2) 0.52979(13) 0.0478(10) Uani 1 1 d . . . . .
H24 H 0.7947 0.1756 0.5210 0.057 Uiso 1 1 calc R U . . .
C25 C 0.6303(3) 0.1246(2) 0.52095(12) 0.0437(10) Uani 1 1 d . . . . .
H25 H 0.6440 0.0651 0.5060 0.052 Uiso 1 1 calc R U . . .
C26 C 0.5207(3) 0.1452(2) 0.53366(11) 0.0356(8) Uani 1 1 d . . . . .
H26 H 0.4616 0.0992 0.5266 0.043 Uiso 1 1 calc R U . . .
C27 C 0.2638(3) 0.2010(2) 0.54079(12) 0.0372(9) Uani 1 1 d . . . . .
C28 C 0.1902(4) 0.2497(2) 0.51004(14) 0.0461(10) Uani 1 1 d . . . . .
H28 H 0.1959 0.3189 0.5081 0.055 Uiso 1 1 calc R U . . .
C29 C 0.1091(4) 0.2025(3) 0.48213(15) 0.0597(12) Uani 1 1 d . . . . .
H29 H 0.0616 0.2394 0.4618 0.072 Uiso 1 1 calc R U . . .
C30 C 0.0974(4) 0.1014(3) 0.48391(15) 0.0595(12) Uani 1 1 d . . . . .
H30 H 0.0432 0.0685 0.4646 0.071 Uiso 1 1 calc R U . . .
C31 C 0.1655(4) 0.0496(3) 0.51418(17) 0.0597(13) Uani 1 1 d . . . . .
H31 H 0.1574 -0.0194 0.5162 0.072 Uiso 1 1 calc R U . . .
C32 C 0.2466(4) 0.0980(2) 0.54185(15) 0.0513(11) Uani 1 1 d . . . . .
H32 H 0.2925 0.0603 0.5624 0.062 Uiso 1 1 calc R U . . .
C33 C 0.3585(4) 0.2128(2) 0.62496(13) 0.0461(10) Uani 1 1 d . . . . .
C34 C 0.2564(5) 0.1753(3) 0.64075(16) 0.0755(14) Uani 1 1 d . . . . .
H34 H 0.1907 0.1696 0.6210 0.091 Uiso 1 1 calc R U . . .
C35 C 0.2487(6) 0.1462(4) 0.68471(19) 0.0936(19) Uani 1 1 d . . . . .
H35 H 0.1784 0.1213 0.6941 0.112 Uiso 1 1 calc R U . . .
C36 C 0.3424(6) 0.1535(3) 0.71428(17) 0.0798(17) Uani 1 1 d . . . . .
H36 H 0.3374 0.1330 0.7439 0.096 Uiso 1 1 calc R U . . .
C37 C 0.4431(5) 0.1905(3) 0.70040(15) 0.0675(14) Uani 1 1 d . . . . .
H37 H 0.5079 0.1968 0.7206 0.081 Uiso 1 1 calc R U . . .
C38 C 0.4504(4) 0.2192(2) 0.65623(14) 0.0523(11) Uani 1 1 d . . . . .
H38 H 0.5212 0.2440 0.6473 0.063 Uiso 1 1 calc R U . . .
C39 C 0.3403(3) 0.3746(2) 0.57332(12) 0.0365(9) Uani 1 1 d . . . . .
C40 C 0.2890(3) 0.4247(2) 0.60717(14) 0.0477(10) Uani 1 1 d . . . . .
H40 H 0.2726 0.3896 0.6330 0.057 Uiso 1 1 calc R U . . .
C41 C 0.2612(4) 0.5242(3) 0.60443(16) 0.0602(13) Uani 1 1 d . . . . .
H41 H 0.2270 0.5554 0.6282 0.072 Uiso 1 1 calc R U . . .
C42 C 0.2833(4) 0.5772(3) 0.56715(17) 0.0608(13) Uani 1 1 d . . . . .
H42 H 0.2622 0.6442 0.5649 0.073 Uiso 1 1 calc R U . . .
C43 C 0.3365(4) 0.5318(2) 0.53317(15) 0.0541(11) Uani 1 1 d . . . . .
H43 H 0.3533 0.5677 0.5076 0.065 Uiso 1 1 calc R U . . .
C44 C 0.3653(3) 0.4322(2) 0.53688(12) 0.0430(10) Uani 1 1 d . . . . .
H44 H 0.4034 0.4024 0.5137 0.052 Uiso 1 1 calc R U . . .
C45 C 0.2608(5) 0.7662(4) 0.67515(18) 0.0867(12) Uani 1 1 d . . . . .
H45A H 0.2772 0.8098 0.7007 0.104 Uiso 1 1 calc R U . . .
H45B H 0.2917 0.7003 0.6825 0.104 Uiso 1 1 calc R U . . .
C46 C 0.1327(5) 0.7607(5) 0.6638(2) 0.1111(15) Uani 1 1 d . . . . .
H46A H 0.1104 0.6955 0.6519 0.133 Uiso 1 1 calc R U . . .
H46B H 0.0889 0.7745 0.6900 0.133 Uiso 1 1 calc R U . . .
C47 C 0.1143(5) 0.8366(4) 0.6306(2) 0.1111(15) Uani 1 1 d . . . . .
H47A H 0.0806 0.8955 0.6437 0.133 Uiso 1 1 calc R U . . .
H47B H 0.0610 0.8129 0.6063 0.133 Uiso 1 1 calc R U . . .
C48 C 0.2252(5) 0.8604(4) 0.61379(18) 0.0867(12) Uani 1 1 d . . . . .
H48A H 0.2243 0.8454 0.5819 0.104 Uiso 1 1 calc R U . . .
H48B H 0.2414 0.9311 0.6178 0.104 Uiso 1 1 calc R U . . .
B1 B 0.3642(4) 0.2546(3) 0.57366(14) 0.0359(10) Uani 1 1 d . . . . .
N1A N 0.7845(5) 0.7315(3) 0.73675(16) 0.0808(14) Uani 1 1 d . . . . .
N2 N 0.6514(3) 0.92841(18) 0.66009(10) 0.0411(8) Uani 1 1 d . . . . .
N3 N 0.5402(3) 0.79644(18) 0.60105(9) 0.0382(7) Uani 1 1 d D . . . .
N4 N 0.6708(3) 0.63124(17) 0.62774(10) 0.0374(7) Uani 1 1 d . . . . .
O1A O 0.7995(3) 0.75932(19) 0.69627(11) 0.0634(8) Uani 1 1 d . . . . .
O2A O 0.6851(4) 0.7200(3) 0.74519(12) 0.0919(12) Uani 1 1 d . . . . .
O3 O 0.3116(3) 0.8040(2) 0.63719(11) 0.0686(9) Uani 1 1 d . . . . .
Pd1 Pd 0.66066(3) 0.77583(2) 0.65147(2) 0.03636(10) Uani 1 1 d . . . . .
H3 H 0.4658(17) 0.789(2) 0.6151(11) 0.044 Uiso 1 1 d D 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
C1 C2 1.499(5) . ?
C1 N2 1.500(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.484(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.491(4) . ?
C3 C4 1.510(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.495(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.505(4) . ?
C5 C6 1.521(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.505(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.509(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N2 1.492(4) . ?
C9 C10 1.501(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.518(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.511(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.501(4) . ?
C13 C14 1.517(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.508(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.514(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 N4 1.495(4) . ?
C17 C18 1.508(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.522(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.471(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C22 1.390(5) . ?
C21 C26 1.393(4) . ?
C21 B1 1.641(5) . ?
C22 C23 1.379(5) . ?
C22 H22 0.9400 . ?
C23 C24 1.384(5) . ?
C23 H23 0.9400 . ?
C24 C25 1.371(5) . ?
C24 H24 0.9400 . ?
C25 C26 1.377(5) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.386(5) . ?
C27 C32 1.407(4) . ?
C27 B1 1.647(6) . ?
C28 C29 1.378(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.374(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.362(6) . ?
C30 H30 0.9400 . ?
C31 C32 1.380(6) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.379(6) . ?
C33 C34 1.397(5) . ?
C33 B1 1.650(5) . ?
C34 C35 1.389(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.364(8) . ?
C35 H35 0.9400 . ?
C36 C37 1.359(7) . ?
C36 H36 0.9400 . ?
C37 C38 1.393(5) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C40 1.387(4) . ?
C39 C44 1.391(4) . ?
C39 B1 1.646(4) . ?
C40 C41 1.384(5) . ?
C40 H40 0.9400 . ?
C41 C42 1.369(6) . ?
C41 H41 0.9400 . ?
C42 C43 1.371(5) . ?
C42 H42 0.9400 . ?
C43 C44 1.390(4) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.414(5) . ?
C45 C46 1.503(8) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.441(7) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.446(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.412(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N1A O2A 1.205(5) . ?
N1A O1A 1.297(5) . ?
N2 Pd1 2.082(2) . ?
N3 Pd1 2.016(3) . ?
N3 H3 0.989(10) . ?
N4 Pd1 2.087(2) . ?
O1A Pd1 2.046(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
C2 C1 N2 110.0(3) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.0(3) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.4(3) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 111.1(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.8(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.2(3) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 112.3(4) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.5(3) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 110.9(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 113.1(4) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.4(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.5(3) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 114.1(3) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.3(3) . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 110.6(3) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 113.9(4) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 113.9(3) . . ?
C22 C21 B1 122.0(3) . . ?
C26 C21 B1 124.0(3) . . ?
C23 C22 C21 123.6(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C22 C23 C24 120.5(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C25 C24 C23 117.5(3) . . ?
C25 C24 H24 121.2 . . ?
C23 C24 H24 121.2 . . ?
C24 C25 C26 121.1(3) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C25 C26 C21 123.4(3) . . ?
C25 C26 H26 118.3 . . ?
C21 C26 H26 118.3 . . ?
C28 C27 C32 113.8(4) . . ?
C28 C27 B1 125.1(3) . . ?
C32 C27 B1 121.1(3) . . ?
C29 C28 C27 123.7(3) . . ?
C29 C28 H28 118.1 . . ?
C27 C28 H28 118.1 . . ?
C30 C29 C28 120.1(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 118.8(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 120.3(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.2(4) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C38 C33 C34 115.1(4) . . ?
C38 C33 B1 122.9(4) . . ?
C34 C33 B1 121.8(4) . . ?
C35 C34 C33 122.2(5) . . ?
C35 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?
C36 C35 C34 120.4(5) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C37 C36 C35 119.3(5) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C36 C37 C38 120.1(5) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 123.0(4) . . ?
C33 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C40 C39 C44 115.2(3) . . ?
C40 C39 B1 123.8(3) . . ?
C44 C39 B1 120.9(3) . . ?
C41 C40 C39 122.6(4) . . ?
C41 C40 H40 118.7 . . ?
C39 C40 H40 118.7 . . ?
C42 C41 C40 120.1(4) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C43 119.6(3) . . ?
C41 C42 H42 120.2 . . ?
C43 C42 H42 120.2 . . ?
C42 C43 C44 119.3(4) . . ?
C42 C43 H43 120.3 . . ?
C44 C43 H43 120.3 . . ?
C43 C44 C39 123.0(3) . . ?
C43 C44 H44 118.5 . . ?
C39 C44 H44 118.5 . . ?
O3 C45 C46 106.8(5) . . ?
O3 C45 H45A 110.4 . . ?
C46 C45 H45A 110.4 . . ?
O3 C45 H45B 110.4 . . ?
C46 C45 H45B 110.4 . . ?
H45A C45 H45B 108.6 . . ?
C47 C46 C45 102.9(5) . . ?
C47 C46 H46A 111.2 . . ?
C45 C46 H46A 111.2 . . ?
C47 C46 H46B 111.2 . . ?
C45 C46 H46B 111.2 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 107.8(5) . . ?
C46 C47 H47A 110.1 . . ?
C48 C47 H47A 110.1 . . ?
C46 C47 H47B 110.1 . . ?
C48 C47 H47B 110.1 . . ?
H47A C47 H47B 108.5 . . ?
O3 C48 C47 108.9(4) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C21 B1 C39 110.3(3) . . ?
C21 B1 C27 110.3(3) . . ?
C39 B1 C27 108.5(3) . . ?
C21 B1 C33 108.5(3) . . ?
C39 B1 C33 109.1(3) . . ?
C27 B1 C33 110.1(3) . . ?
O2A N1A O1A 114.9(4) . . ?
C9 N2 C1 110.9(3) . . ?
C9 N2 C5 109.4(3) . . ?
C1 N2 C5 111.6(3) . . ?
C9 N2 Pd1 114.8(2) . . ?
C1 N2 Pd1 105.7(2) . . ?
C5 N2 Pd1 104.24(19) . . ?
C2 N3 C3 116.2(3) . . ?
C2 N3 Pd1 106.6(2) . . ?
C3 N3 Pd1 106.7(2) . . ?
C2 N3 H3 107.2(17) . . ?
C3 N3 H3 114.9(19) . . ?
Pd1 N3 H3 104(2) . . ?
C4 N4 C17 110.2(3) . . ?
C4 N4 C13 112.1(3) . . ?
C17 N4 C13 109.6(3) . . ?
C4 N4 Pd1 105.44(19) . . ?
C17 N4 Pd1 115.3(2) . . ?
C13 N4 Pd1 104.09(18) . . ?
N1A O1A Pd1 120.4(3) . . ?
C48 O3 C45 106.3(4) . . ?
N3 Pd1 O1A 171.98(12) . . ?
N3 Pd1 N2 85.33(12) . . ?
O1A Pd1 N2 94.03(12) . . ?
N3 Pd1 N4 85.57(11) . . ?
O1A Pd1 N4 93.71(11) . . ?
N2 Pd1 N4 167.10(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 55.4(4) . . . . ?
N3 C3 C4 N4 -54.6(4) . . . . ?
N2 C5 C6 C7 -179.3(4) . . . . ?
C5 C6 C7 C8 -173.9(4) . . . . ?
N2 C9 C10 C11 170.2(3) . . . . ?
C9 C10 C11 C12 172.6(3) . . . . ?
N4 C13 C14 C15 -180.0(3) . . . . ?
C13 C14 C15 C16 179.4(4) . . . . ?
N4 C17 C18 C19 -173.3(4) . . . . ?
C17 C18 C19 C20 -172.8(4) . . . . ?
C26 C21 C22 C23 0.0(6) . . . . ?
B1 C21 C22 C23 178.3(4) . . . . ?
C21 C22 C23 C24 -0.6(6) . . . . ?
C22 C23 C24 C25 0.4(6) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
C24 C25 C26 C21 -0.9(6) . . . . ?
C22 C21 C26 C25 0.7(5) . . . . ?
B1 C21 C26 C25 -177.5(3) . . . . ?
C32 C27 C28 C29 -1.5(5) . . . . ?
B1 C27 C28 C29 178.1(3) . . . . ?
C27 C28 C29 C30 0.3(6) . . . . ?
C28 C29 C30 C31 1.2(6) . . . . ?
C29 C30 C31 C32 -1.4(7) . . . . ?
C30 C31 C32 C27 0.1(6) . . . . ?
C28 C27 C32 C31 1.3(5) . . . . ?
B1 C27 C32 C31 -178.3(4) . . . . ?
C38 C33 C34 C35 -0.3(6) . . . . ?
B1 C33 C34 C35 -175.5(4) . . . . ?
C33 C34 C35 C36 0.0(8) . . . . ?
C34 C35 C36 C37 0.7(8) . . . . ?
C35 C36 C37 C38 -1.0(7) . . . . ?
C34 C33 C38 C37 0.1(5) . . . . ?
B1 C33 C38 C37 175.2(3) . . . . ?
C36 C37 C38 C33 0.6(6) . . . . ?
C44 C39 C40 C41 2.0(6) . . . . ?
B1 C39 C40 C41 -174.5(4) . . . . ?
C39 C40 C41 C42 0.5(7) . . . . ?
C40 C41 C42 C43 -2.0(7) . . . . ?
C41 C42 C43 C44 1.0(6) . . . . ?
C42 C43 C44 C39 1.6(6) . . . . ?
C40 C39 C44 C43 -3.0(6) . . . . ?
B1 C39 C44 C43 173.6(4) . . . . ?
O3 C45 C46 C47 -26.7(6) . . . . ?
C45 C46 C47 C48 17.3(7) . . . . ?
C46 C47 C48 O3 -2.4(7) . . . . ?
C22 C21 B1 C39 33.1(5) . . . . ?
C26 C21 B1 C39 -148.8(3) . . . . ?
C22 C21 B1 C27 153.0(3) . . . . ?
C26 C21 B1 C27 -28.9(4) . . . . ?
C22 C21 B1 C33 -86.3(4) . . . . ?
C26 C21 B1 C33 91.8(4) . . . . ?
C40 C39 B1 C21 -137.3(4) . . . . ?
C44 C39 B1 C21 46.4(5) . . . . ?
C40 C39 B1 C27 101.8(4) . . . . ?
C44 C39 B1 C27 -74.5(4) . . . . ?
C40 C39 B1 C33 -18.2(5) . . . . ?
C44 C39 B1 C33 165.5(4) . . . . ?
C28 C27 B1 C21 -106.5(4) . . . . ?
C32 C27 B1 C21 73.1(4) . . . . ?
C28 C27 B1 C39 14.5(5) . . . . ?
C32 C27 B1 C39 -165.9(3) . . . . ?
C28 C27 B1 C33 133.8(3) . . . . ?
C32 C27 B1 C33 -46.6(4) . . . . ?
C38 C33 B1 C21 38.4(4) . . . . ?
C34 C33 B1 C21 -146.8(3) . . . . ?
C38 C33 B1 C39 -81.8(4) . . . . ?
C34 C33 B1 C39 93.0(4) . . . . ?
C38 C33 B1 C27 159.2(3) . . . . ?
C34 C33 B1 C27 -26.0(5) . . . . ?
C10 C9 N2 C1 62.9(4) . . . . ?
C10 C9 N2 C5 -173.5(3) . . . . ?
C10 C9 N2 Pd1 -56.8(4) . . . . ?
C2 C1 N2 C9 -159.5(3) . . . . ?
C2 C1 N2 C5 78.2(3) . . . . ?
C2 C1 N2 Pd1 -34.5(3) . . . . ?
C6 C5 N2 C9 -57.9(4) . . . . ?
C6 C5 N2 C1 65.2(4) . . . . ?
C6 C5 N2 Pd1 178.8(3) . . . . ?
C1 C2 N3 C3 -166.0(3) . . . . ?
C1 C2 N3 Pd1 -47.2(3) . . . . ?
C4 C3 N3 C2 165.8(3) . . . . ?
C4 C3 N3 Pd1 47.1(3) . . . . ?
C3 C4 N4 C17 158.4(3) . . . . ?
C3 C4 N4 C13 -79.3(3) . . . . ?
C3 C4 N4 Pd1 33.3(3) . . . . ?
C18 C17 N4 C4 -62.1(4) . . . . ?
C18 C17 N4 C13 174.1(3) . . . . ?
C18 C17 N4 Pd1 57.1(4) . . . . ?
C14 C13 N4 C4 -64.7(4) . . . . ?
C14 C13 N4 C17 58.0(4) . . . . ?
C14 C13 N4 Pd1 -178.1(3) . . . . ?
O2A N1A O1A Pd1 -2.1(5) . . . . ?
C47 C48 O3 C45 -14.9(6) . . . . ?
C46 C45 O3 C48 25.8(6) . . . . ?

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
C5 H5B O1A 0.98 2.57 3.178(5) 120.6 .
C10 H10A O2A 0.98 2.60 3.286(5) 127.5 .
C13 H13A O1A 0.98 2.53 3.146(5) 120.9 .
C18 H18B O2A 0.98 2.56 3.244(6) 126.4 .
N3 H3 O3 0.989(10) 1.954(12) 2.926(4) 167(3) .

_refine_diff_density_max         0.665
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.068

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_PSS-240K
_database_code_depnum_ccdc_archive 'CCDC 1441778'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_PSS-240K            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ... 14 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation for an extended time, 
leading to even weaker diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5844(6)
_cell_length_b                   13.5468(5)
_cell_length_c                   30.1451(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.333(4)
_cell_angle_gamma                90
_cell_volume                     4722.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    5162
_cell_measurement_theta_min      3.5130
_cell_measurement_theta_max      24.4100

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.435
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.77151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            28456
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.007
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             9597
_reflns_number_gt                6114
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0531P)²+0.1339P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9597
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
C1 C 0.5553(4) 0.9628(3) 0.62880(13) 0.0545(11) Uani 1 1 d . . . . .
H1A H 0.5669 1.0323 0.6213 0.065 Uiso 1 1 calc R U . . .
H1B H 0.4818 0.9571 0.6432 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5510(4) 0.9012(2) 0.58715(12) 0.0497(10) Uani 1 1 d . . . . .
H2A H 0.4840 0.9196 0.5675 0.060 Uiso 1 1 calc R U . . .
H2B H 0.6213 0.9111 0.5711 0.060 Uiso 1 1 calc R U . . .
C3 C 0.5627(3) 0.7212(2) 0.56654(11) 0.0428(9) Uani 1 1 d . . . . .
H3A H 0.6322 0.7376 0.5510 0.051 Uiso 1 1 calc R U . . .
H3B H 0.4967 0.7179 0.5447 0.051 Uiso 1 1 calc R U . . .
C4 C 0.5781(3) 0.6243(2) 0.59086(12) 0.0442(9) Uani 1 1 d . . . . .
H4A H 0.5048 0.6052 0.6031 0.053 Uiso 1 1 calc R U . . .
H4B H 0.5993 0.5730 0.5699 0.053 Uiso 1 1 calc R U . . .
C5 C 0.7674(4) 0.9655(3) 0.64639(13) 0.0572(11) Uani 1 1 d . . . . .
H5A H 0.7776 0.9433 0.6159 0.069 Uiso 1 1 calc R U . . .
H5B H 0.8281 0.9340 0.6655 0.069 Uiso 1 1 calc R U . . .
C6 C 0.7870(4) 1.0763(3) 0.64813(15) 0.0678(13) Uani 1 1 d . . . . .
H6A H 0.7270 1.1092 0.6292 0.081 Uiso 1 1 calc R U . . .
H6B H 0.7802 1.0996 0.6787 0.081 Uiso 1 1 calc R U . . .
C7 C 0.9033(5) 1.1037(3) 0.63293(18) 0.0858(16) Uani 1 1 d . . . . .
H7A H 0.9067 1.0870 0.6014 0.103 Uiso 1 1 calc R U . . .
H7B H 0.9626 1.0649 0.6496 0.103 Uiso 1 1 calc R U . . .
C8 C 0.9295(6) 1.2120(4) 0.6392(2) 0.120(2) Uani 1 1 d . . . . .
H8A H 0.9559 1.2240 0.6699 0.180 Uiso 1 1 calc R U . . .
H8B H 0.8601 1.2502 0.6321 0.180 Uiso 1 1 calc R U . . .
H8C H 0.9894 1.2314 0.6198 0.180 Uiso 1 1 calc R U . . .
C9 C 0.6342(4) 0.9605(3) 0.70653(12) 0.0521(10) Uani 1 1 d . . . . .
H9A H 0.6290 1.0327 0.7070 0.063 Uiso 1 1 calc R U . . .
H9B H 0.7022 0.9416 0.7254 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5285(4) 0.9189(3) 0.72642(12) 0.0563(11) Uani 1 1 d . . . . .
H10A H 0.5262 0.8473 0.7220 0.068 Uiso 1 1 calc R U . . .
H10B H 0.4590 0.9472 0.7113 0.068 Uiso 1 1 calc R U . . .
C11 C 0.5293(4) 0.9419(3) 0.77574(14) 0.0720(14) Uani 1 1 d . . . . .
H11A H 0.5937 0.9066 0.7911 0.086 Uiso 1 1 calc R U . . .
H11B H 0.5425 1.0128 0.7801 0.086 Uiso 1 1 calc R U . . .
C12 C 0.4189(5) 0.9137(4) 0.79620(17) 0.1007(19) Uani 1 1 d . . . . .
H12A H 0.4243 0.9301 0.8276 0.151 Uiso 1 1 calc R U . . .
H12B H 0.4062 0.8433 0.7927 0.151 Uiso 1 1 calc R U . . .
H12C H 0.3549 0.9494 0.7816 0.151 Uiso 1 1 calc R U . . .
C13 C 0.7895(3) 0.6249(2) 0.61077(13) 0.0478(10) Uani 1 1 d . . . . .
H13A H 0.8455 0.6387 0.6356 0.057 Uiso 1 1 calc R U . . .
H13B H 0.7973 0.6775 0.5888 0.057 Uiso 1 1 calc R U . . .
C14 C 0.8235(4) 0.5281(3) 0.58969(14) 0.0559(11) Uani 1 1 d . . . . .
H14A H 0.8179 0.4746 0.6113 0.067 Uiso 1 1 calc R U . . .
H14B H 0.7697 0.5136 0.5642 0.067 Uiso 1 1 calc R U . . .
C15 C 0.9447(4) 0.5328(3) 0.57447(15) 0.0638(12) Uani 1 1 d . . . . .
H15A H 0.9977 0.5488 0.6000 0.077 Uiso 1 1 calc R U . . .
H15B H 0.9494 0.5862 0.5528 0.077 Uiso 1 1 calc R U . . .
C16 C 0.9841(4) 0.4378(3) 0.55373(16) 0.0704(14) Uani 1 1 d . . . . .
H16A H 1.0618 0.4462 0.5439 0.106 Uiso 1 1 calc R U . . .
H16B H 0.9321 0.4211 0.5285 0.106 Uiso 1 1 calc R U . . .
H16C H 0.9838 0.3851 0.5755 0.106 Uiso 1 1 calc R U . . .
C17 C 0.6547(4) 0.5520(3) 0.66105(12) 0.0499(10) Uani 1 1 d . . . . .
H17A H 0.7199 0.5544 0.6832 0.060 Uiso 1 1 calc R U . . .
H17B H 0.6575 0.4880 0.6459 0.060 Uiso 1 1 calc R U . . .
C18 C 0.5444(4) 0.5577(3) 0.68467(13) 0.0637(12) Uani 1 1 d . . . . .
H18A H 0.4784 0.5472 0.6634 0.076 Uiso 1 1 calc R U . . .
H18B H 0.5369 0.6236 0.6977 0.076 Uiso 1 1 calc R U . . .
C19 C 0.5434(5) 0.4798(4) 0.72137(17) 0.0923(18) Uani 1 1 d . . . . .
H19A H 0.5620 0.4155 0.7087 0.111 Uiso 1 1 calc R U . . .
H19B H 0.6042 0.4956 0.7442 0.111 Uiso 1 1 calc R U . . .
C20 C 0.4342(6) 0.4721(5) 0.7422(2) 0.130(3) Uani 1 1 d . . . . .
H20A H 0.4437 0.4304 0.7683 0.196 Uiso 1 1 calc R U . . .
H20B H 0.3767 0.4434 0.7214 0.196 Uiso 1 1 calc R U . . .
H20C H 0.4092 0.5373 0.7508 0.196 Uiso 1 1 calc R U . . .
C21 C 0.4932(3) 0.2306(2) 0.55619(11) 0.0389(8) Uani 1 1 d . . . . .
C22 C 0.5864(4) 0.2943(3) 0.56444(14) 0.0535(11) Uani 1 1 d . . . . .
H22 H 0.5735 0.3536 0.5796 0.064 Uiso 1 1 calc R U . . .
C23 C 0.6965(4) 0.2752(3) 0.55160(15) 0.0591(11) Uani 1 1 d . . . . .
H23 H 0.7562 0.3209 0.5581 0.071 Uiso 1 1 calc R U . . .
C24 C 0.7191(4) 0.1895(3) 0.52935(13) 0.0543(11) Uani 1 1 d . . . . .
H24 H 0.7938 0.1758 0.5203 0.065 Uiso 1 1 calc R U . . .
C25 C 0.6294(4) 0.1243(3) 0.52061(12) 0.0471(10) Uani 1 1 d . . . . .
H25 H 0.6429 0.0650 0.5055 0.057 Uiso 1 1 calc R U . . .
C26 C 0.5204(3) 0.1452(2) 0.53373(11) 0.0402(9) Uani 1 1 d . . . . .
H26 H 0.4612 0.0991 0.5271 0.048 Uiso 1 1 calc R U . . .
C27 C 0.2642(3) 0.2009(2) 0.54121(12) 0.0427(9) Uani 1 1 d . . . . .
C28 C 0.1904(4) 0.2504(3) 0.51089(14) 0.0511(10) Uani 1 1 d . . . . .
H28 H 0.1960 0.3195 0.5092 0.061 Uiso 1 1 calc R U . . .
C29 C 0.1084(4) 0.2030(3) 0.48288(15) 0.0654(12) Uani 1 1 d . . . . .
H29 H 0.0609 0.2398 0.4627 0.079 Uiso 1 1 calc R U . . .
C30 C 0.0970(4) 0.1018(3) 0.48481(16) 0.0674(13) Uani 1 1 d . . . . .
H30 H 0.0427 0.0688 0.4658 0.081 Uiso 1 1 calc R U . . .
C31 C 0.1662(4) 0.0506(3) 0.51499(17) 0.0661(13) Uani 1 1 d . . . . .
H31 H 0.1585 -0.0183 0.5171 0.079 Uiso 1 1 calc R U . . .
C32 C 0.2465(4) 0.0989(3) 0.54213(15) 0.0582(11) Uani 1 1 d . . . . .
H32 H 0.2925 0.0613 0.5625 0.070 Uiso 1 1 calc R U . . .
C33 C 0.3588(4) 0.2129(3) 0.62505(12) 0.0487(10) Uani 1 1 d . . . . .
C34 C 0.2580(5) 0.1748(4) 0.64112(15) 0.0860(16) Uani 1 1 d . . . . .
H34 H 0.1927 0.1682 0.6213 0.103 Uiso 1 1 calc R U . . .
C35 C 0.2491(6) 0.1461(4) 0.68469(19) 0.107(2) Uani 1 1 d . . . . .
H35 H 0.1787 0.1215 0.6941 0.128 Uiso 1 1 calc R U . . .
C36 C 0.3424(7) 0.1533(4) 0.71417(17) 0.092(2) Uani 1 1 d . . . . .
H36 H 0.3373 0.1332 0.7438 0.111 Uiso 1 1 calc R U . . .
C37 C 0.4434(5) 0.1902(3) 0.70005(14) 0.0761(16) Uani 1 1 d . . . . .
H37 H 0.5082 0.1963 0.7201 0.091 Uiso 1 1 calc R U . . .
C38 C 0.4504(4) 0.2191(3) 0.65569(13) 0.0595(11) Uani 1 1 d . . . . .
H38 H 0.5211 0.2437 0.6466 0.071 Uiso 1 1 calc R U . . .
C39 C 0.3408(3) 0.3746(2) 0.57338(12) 0.0413(9) Uani 1 1 d . . . . .
C40 C 0.2892(4) 0.4243(3) 0.60710(14) 0.0533(11) Uani 1 1 d . . . . .
H40 H 0.2726 0.3894 0.6329 0.064 Uiso 1 1 calc R U . . .
C41 C 0.2613(4) 0.5230(3) 0.60415(17) 0.0689(13) Uani 1 1 d . . . . .
H41 H 0.2262 0.5538 0.6278 0.083 Uiso 1 1 calc R U . . .
C42 C 0.2837(4) 0.5767(3) 0.56745(18) 0.0675(13) Uani 1 1 d . . . . .
H42 H 0.2630 0.6437 0.5654 0.081 Uiso 1 1 calc R U . . .
C43 C 0.3376(4) 0.5309(3) 0.53320(15) 0.0590(11) Uani 1 1 d . . . . .
H43 H 0.3547 0.5668 0.5077 0.071 Uiso 1 1 calc R U . . .
C44 C 0.3660(4) 0.4321(2) 0.53667(12) 0.0474(10) Uani 1 1 d . . . . .
H44 H 0.4039 0.4023 0.5134 0.057 Uiso 1 1 calc R U . . .
C45 C 0.2615(6) 0.7671(4) 0.67501(18) 0.0980(13) Uani 1 1 d . . . . .
H45A H 0.2788 0.8108 0.7005 0.118 Uiso 1 1 calc R U . . .
H45B H 0.2920 0.7013 0.6824 0.118 Uiso 1 1 calc R U . . .
C46 C 0.1337(6) 0.7622(5) 0.6645(2) 0.1238(16) Uani 1 1 d . . . . .
H46A H 0.1104 0.6964 0.6539 0.149 Uiso 1 1 calc R U . . .
H46B H 0.0910 0.7786 0.6907 0.149 Uiso 1 1 calc R U . . .
C47 C 0.1146(6) 0.8350(5) 0.6302(2) 0.1238(16) Uani 1 1 d . . . . .
H47A H 0.0791 0.8941 0.6423 0.149 Uiso 1 1 calc R U . . .
H47B H 0.0626 0.8087 0.6062 0.149 Uiso 1 1 calc R U . . .
C48 C 0.2260(6) 0.8593(4) 0.61336(18) 0.0980(13) Uani 1 1 d . . . . .
H48A H 0.2258 0.8438 0.5816 0.118 Uiso 1 1 calc R U . . .
H48B H 0.2415 0.9300 0.6172 0.118 Uiso 1 1 calc R U . . .
B1 B 0.3640(4) 0.2545(3) 0.57368(14) 0.0422(10) Uani 1 1 d . . . . .
N1A N 0.7869(6) 0.7323(4) 0.73556(18) 0.0979(17) Uani 1 1 d . . . . .
N2 N 0.6524(3) 0.9282(2) 0.66001(9) 0.0460(8) Uani 1 1 d . . . . .
N3 N 0.5418(3) 0.79681(19) 0.60138(9) 0.0416(7) Uani 1 1 d D . . . .
N4 N 0.6700(3) 0.63160(19) 0.62774(10) 0.0410(7) Uani 1 1 d . . . . .
O1A O 0.7992(3) 0.7597(2) 0.69572(11) 0.0718(9) Uani 1 1 d . . . . .
O2A O 0.6893(5) 0.7201(3) 0.74468(13) 0.1091(15) Uani 1 1 d . . . . .
O3 O 0.3121(3) 0.8042(2) 0.63689(11) 0.0762(9) Uani 1 1 d . . . . .
Pd1 Pd 0.66091(3) 0.77608(2) 0.65140(2) 0.04107(10) Uani 1 1 d . . . . .
H3 H 0.4627(14) 0.792(2) 0.6120(11) 0.049 Uiso 1 1 d D 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
C1 N2 1.499(5) . ?
C1 C2 1.506(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.484(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.496(4) . ?
C3 C4 1.509(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.497(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.505(5) . ?
C5 C6 1.519(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.495(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.508(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N2 1.496(4) . ?
C9 C10 1.504(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.501(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.507(4) . ?
C13 C14 1.519(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.504(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.513(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 N4 1.491(4) . ?
C17 C18 1.500(5) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.530(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.448(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C26 1.387(4) . ?
C21 C22 1.393(5) . ?
C21 B1 1.648(5) . ?
C22 C23 1.379(5) . ?
C22 H22 0.9400 . ?
C23 C24 1.373(5) . ?
C23 H23 0.9400 . ?
C24 C25 1.378(5) . ?
C24 H24 0.9400 . ?
C25 C26 1.375(5) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.388(6) . ?
C27 C32 1.397(5) . ?
C27 B1 1.640(6) . ?
C28 C29 1.391(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.378(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.366(6) . ?
C30 H30 0.9400 . ?
C31 C32 1.370(6) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.368(6) . ?
C33 C34 1.390(6) . ?
C33 B1 1.652(5) . ?
C34 C35 1.379(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.362(8) . ?
C35 H35 0.9400 . ?
C36 C37 1.362(7) . ?
C36 H36 0.9400 . ?
C37 C38 1.400(6) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C40 1.384(5) . ?
C39 C44 1.398(5) . ?
C39 B1 1.649(5) . ?
C40 C41 1.377(5) . ?
C40 H40 0.9400 . ?
C41 C42 1.362(6) . ?
C41 H41 0.9400 . ?
C42 C43 1.384(6) . ?
C42 H42 0.9400 . ?
C43 C44 1.381(5) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.413(5) . ?
C45 C46 1.497(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.436(8) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.452(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.404(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N1A O2A 1.190(6) . ?
N1A O1A 1.273(6) . ?
N2 Pd1 2.080(3) . ?
N3 Pd1 2.004(3) . ?
N3 H3 0.990(10) . ?
N4 Pd1 2.088(3) . ?
O1A Pd1 2.038(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
N2 C1 C2 109.7(3) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.6(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 105.9(3) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.3(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 117.0(3) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.7(4) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 112.4(5) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.3(3) . . ?
N2 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 110.8(4) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.1(4) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.3(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.1(3) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.6(4) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 114.8(3) . . ?
N4 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
N4 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 110.5(4) . . ?
C17 C18 H18A 109.6 . . ?
C19 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
C19 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 114.0(5) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.1(3) . . ?
C26 C21 B1 123.8(3) . . ?
C22 C21 B1 122.0(3) . . ?
C23 C22 C21 123.6(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.1(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 118.2(4) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C26 C25 C24 120.6(3) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C21 123.4(3) . . ?
C25 C26 H26 118.3 . . ?
C21 C26 H26 118.3 . . ?
C28 C27 C32 113.9(4) . . ?
C28 C27 B1 124.4(3) . . ?
C32 C27 B1 121.7(4) . . ?
C27 C28 C29 123.3(4) . . ?
C27 C28 H28 118.3 . . ?
C29 C28 H28 118.3 . . ?
C30 C29 C28 119.8(4) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 118.6(4) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
C30 C31 C32 120.5(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.8(4) . . ?
C31 C32 H32 118.1 . . ?
C27 C32 H32 118.1 . . ?
C38 C33 C34 114.9(4) . . ?
C38 C33 B1 122.9(4) . . ?
C34 C33 B1 122.0(4) . . ?
C35 C34 C33 123.2(6) . . ?
C35 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?
C36 C35 C34 120.0(6) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 119.0(5) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 120.0(5) . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C33 C38 C37 122.8(5) . . ?
C33 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C40 C39 C44 115.4(3) . . ?
C40 C39 B1 123.6(3) . . ?
C44 C39 B1 120.8(3) . . ?
C41 C40 C39 122.3(4) . . ?
C41 C40 H40 118.8 . . ?
C39 C40 H40 118.8 . . ?
C42 C41 C40 121.1(4) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 118.8(4) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C44 C43 C42 119.6(4) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C39 122.7(3) . . ?
C43 C44 H44 118.7 . . ?
C39 C44 H44 118.7 . . ?
O3 C45 C46 107.2(5) . . ?
O3 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
O3 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.5 . . ?
C47 C46 C45 103.4(6) . . ?
C47 C46 H46A 111.1 . . ?
C45 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
C45 C46 H46B 111.1 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 107.7(6) . . ?
C46 C47 H47A 110.2 . . ?
C48 C47 H47A 110.2 . . ?
C46 C47 H47B 110.2 . . ?
C48 C47 H47B 110.2 . . ?
H47A C47 H47B 108.5 . . ?
O3 C48 C47 108.8(5) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C27 B1 C21 110.1(3) . . ?
C27 B1 C39 109.0(3) . . ?
C21 B1 C39 110.0(3) . . ?
C27 B1 C33 110.2(3) . . ?
C21 B1 C33 108.4(3) . . ?
C39 B1 C33 109.1(3) . . ?
O2A N1A O1A 114.7(5) . . ?
C9 N2 C1 110.8(3) . . ?
C9 N2 C5 109.5(3) . . ?
C1 N2 C5 111.6(3) . . ?
C9 N2 Pd1 114.7(2) . . ?
C1 N2 Pd1 105.7(2) . . ?
C5 N2 Pd1 104.4(2) . . ?
C2 N3 C3 115.6(3) . . ?
C2 N3 Pd1 107.0(2) . . ?
C3 N3 Pd1 107.4(2) . . ?
C2 N3 H3 103.8(19) . . ?
C3 N3 H3 112(2) . . ?
Pd1 N3 H3 111(2) . . ?
C17 N4 C4 110.2(3) . . ?
C17 N4 C13 109.4(3) . . ?
C4 N4 C13 111.8(3) . . ?
C17 N4 Pd1 116.0(2) . . ?
C4 N4 Pd1 105.5(2) . . ?
C13 N4 Pd1 103.75(19) . . ?
N1A O1A Pd1 121.6(4) . . ?
C48 O3 C45 106.5(4) . . ?
N3 Pd1 O1A 171.71(13) . . ?
N3 Pd1 N2 85.38(12) . . ?
O1A Pd1 N2 93.86(12) . . ?
N3 Pd1 N4 85.45(11) . . ?
O1A Pd1 N4 93.93(12) . . ?
N2 Pd1 N4 167.18(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 55.4(4) . . . . ?
N3 C3 C4 N4 -53.9(4) . . . . ?
N2 C5 C6 C7 -178.8(4) . . . . ?
C5 C6 C7 C8 -173.6(4) . . . . ?
N2 C9 C10 C11 170.3(3) . . . . ?
C9 C10 C11 C12 172.6(4) . . . . ?
N4 C13 C14 C15 -179.9(3) . . . . ?
C13 C14 C15 C16 179.2(4) . . . . ?
N4 C17 C18 C19 -173.9(4) . . . . ?
C17 C18 C19 C20 -172.7(5) . . . . ?
C26 C21 C22 C23 0.0(6) . . . . ?
B1 C21 C22 C23 177.8(4) . . . . ?
C21 C22 C23 C24 0.1(7) . . . . ?
C22 C23 C24 C25 -0.2(6) . . . . ?
C23 C24 C25 C26 0.3(6) . . . . ?
C24 C25 C26 C21 -0.2(6) . . . . ?
C22 C21 C26 C25 0.0(5) . . . . ?
B1 C21 C26 C25 -177.7(3) . . . . ?
C32 C27 C28 C29 -1.9(5) . . . . ?
B1 C27 C28 C29 178.3(4) . . . . ?
C27 C28 C29 C30 0.7(6) . . . . ?
C28 C29 C30 C31 1.0(6) . . . . ?
C29 C30 C31 C32 -1.2(7) . . . . ?
C30 C31 C32 C27 -0.2(7) . . . . ?
C28 C27 C32 C31 1.7(6) . . . . ?
B1 C27 C32 C31 -178.5(4) . . . . ?
C38 C33 C34 C35 0.8(7) . . . . ?
B1 C33 C34 C35 -175.2(5) . . . . ?
C33 C34 C35 C36 -0.9(9) . . . . ?
C34 C35 C36 C37 0.8(9) . . . . ?
C35 C36 C37 C38 -0.7(8) . . . . ?
C34 C33 C38 C37 -0.6(6) . . . . ?
B1 C33 C38 C37 175.3(3) . . . . ?
C36 C37 C38 C33 0.6(6) . . . . ?
C44 C39 C40 C41 1.9(6) . . . . ?
B1 C39 C40 C41 -173.9(4) . . . . ?
C39 C40 C41 C42 -0.1(7) . . . . ?
C40 C41 C42 C43 -1.3(7) . . . . ?
C41 C42 C43 C44 0.8(7) . . . . ?
C42 C43 C44 C39 1.2(6) . . . . ?
C40 C39 C44 C43 -2.5(6) . . . . ?
B1 C39 C44 C43 173.5(4) . . . . ?
O3 C45 C46 C47 -24.7(7) . . . . ?
C45 C46 C47 C48 15.1(8) . . . . ?
C46 C47 C48 O3 -0.7(8) . . . . ?
C28 C27 B1 C21 -107.0(4) . . . . ?
C32 C27 B1 C21 73.2(4) . . . . ?
C28 C27 B1 C39 13.7(5) . . . . ?
C32 C27 B1 C39 -166.1(3) . . . . ?
C28 C27 B1 C33 133.4(4) . . . . ?
C32 C27 B1 C33 -46.4(4) . . . . ?
C26 C21 B1 C27 -29.3(5) . . . . ?
C22 C21 B1 C27 153.2(3) . . . . ?
C26 C21 B1 C39 -149.4(3) . . . . ?
C22 C21 B1 C39 33.0(5) . . . . ?
C26 C21 B1 C33 91.4(4) . . . . ?
C22 C21 B1 C33 -86.2(4) . . . . ?
C40 C39 B1 C27 101.3(4) . . . . ?
C44 C39 B1 C27 -74.3(4) . . . . ?
C40 C39 B1 C21 -137.9(4) . . . . ?
C44 C39 B1 C21 46.5(5) . . . . ?
C40 C39 B1 C33 -19.1(5) . . . . ?
C44 C39 B1 C33 165.3(4) . . . . ?
C38 C33 B1 C27 158.7(3) . . . . ?
C34 C33 B1 C27 -25.6(5) . . . . ?
C38 C33 B1 C21 38.1(4) . . . . ?
C34 C33 B1 C21 -146.2(4) . . . . ?
C38 C33 B1 C39 -81.7(4) . . . . ?
C34 C33 B1 C39 94.0(5) . . . . ?
C10 C9 N2 C1 63.1(4) . . . . ?
C10 C9 N2 C5 -173.4(3) . . . . ?
C10 C9 N2 Pd1 -56.5(4) . . . . ?
C2 C1 N2 C9 -159.5(3) . . . . ?
C2 C1 N2 C5 78.2(4) . . . . ?
C2 C1 N2 Pd1 -34.7(3) . . . . ?
C6 C5 N2 C9 -58.1(5) . . . . ?
C6 C5 N2 C1 65.0(4) . . . . ?
C6 C5 N2 Pd1 178.7(3) . . . . ?
C1 C2 N3 C3 -166.9(3) . . . . ?
C1 C2 N3 Pd1 -47.3(3) . . . . ?
C4 C3 N3 C2 166.3(3) . . . . ?
C4 C3 N3 Pd1 46.9(3) . . . . ?
C18 C17 N4 C4 -63.7(4) . . . . ?
C18 C17 N4 C13 172.9(3) . . . . ?
C18 C17 N4 Pd1 56.0(4) . . . . ?
C3 C4 N4 C17 158.8(3) . . . . ?
C3 C4 N4 C13 -79.2(3) . . . . ?
C3 C4 N4 Pd1 32.9(3) . . . . ?
C14 C13 N4 C17 57.3(4) . . . . ?
C14 C13 N4 C4 -65.0(4) . . . . ?
C14 C13 N4 Pd1 -178.3(3) . . . . ?
O2A N1A O1A Pd1 -2.0(7) . . . . ?
C47 C48 O3 C45 -15.2(7) . . . . ?
C46 C45 O3 C48 24.8(6) . . . . ?

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
C5 H5B O1A 0.98 2.56 3.171(5) 120.4 .
C10 H10A O2A 0.98 2.62 3.303(6) 127.1 .
C13 H13A O1A 0.98 2.52 3.142(5) 120.9 .
C18 H18B O2A 0.98 2.56 3.252(7) 127.7 .
N3 H3 O3 0.990(10) 1.946(12) 2.927(4) 171(3) .

_refine_diff_density_max         0.681
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.064

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_PSS-250K
_database_code_depnum_ccdc_archive 'CCDC 1441779'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_PSS-250K            
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially decayed nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_PSS-250K            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation for an extended time, 
leading to even weaker diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6183(7)
_cell_length_b                   13.5540(5)
_cell_length_c                   30.111(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.455(5)
_cell_angle_gamma                90
_cell_volume                     4733.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    3161
_cell_measurement_theta_min      3.5120
_cell_measurement_theta_max      21.9380

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.434
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70823
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            25662
_diffrn_reflns_av_unetI/netI     0.1155
_diffrn_reflns_av_R_equivalents  0.0933
_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       -35
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.008
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8634
_reflns_number_gt                4857
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0473P)²+0.1899P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8634
_refine_ls_number_parameters     504
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1357
_refine_ls_wR_factor_gt          0.1085
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.5561(5) 0.9636(3) 0.62903(19) 0.0542(16) Uani 1 1 d . . . . .
H1A H 0.4824 0.9578 0.6430 0.065 Uiso 1 1 calc R U . . .
H1B H 0.5680 1.0331 0.6216 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5532(5) 0.9024(3) 0.58741(19) 0.0530(15) Uani 1 1 d . . . . .
H2A H 0.4871 0.9212 0.5674 0.064 Uiso 1 1 calc R U . . .
H2B H 0.6239 0.9122 0.5718 0.064 Uiso 1 1 calc R U . . .
C3 C 0.5640(4) 0.7221(3) 0.56662(16) 0.0439(12) Uani 1 1 d . . . . .
H3A H 0.6337 0.7384 0.5514 0.053 Uiso 1 1 calc R U . . .
H3B H 0.4986 0.7190 0.5446 0.053 Uiso 1 1 calc R U . . .
C4 C 0.5786(4) 0.6250(3) 0.59100(17) 0.0444(13) Uani 1 1 d . . . . .
H4A H 0.5052 0.6061 0.6030 0.053 Uiso 1 1 calc R U . . .
H4B H 0.5998 0.5737 0.5701 0.053 Uiso 1 1 calc R U . . .
C5 C 0.7682(5) 0.9656(3) 0.6474(2) 0.0595(16) Uani 1 1 d . . . . .
H5A H 0.7784 0.9437 0.6169 0.071 Uiso 1 1 calc R U . . .
H5B H 0.8288 0.9341 0.6666 0.071 Uiso 1 1 calc R U . . .
C6 C 0.7867(5) 1.0761(4) 0.6494(2) 0.0726(19) Uani 1 1 d . . . . .
H6A H 0.7799 1.0992 0.6800 0.087 Uiso 1 1 calc R U . . .
H6B H 0.7271 1.1090 0.6303 0.087 Uiso 1 1 calc R U . . .
C7 C 0.9049(6) 1.1028(4) 0.6341(3) 0.098(3) Uani 1 1 d . . . . .
H7A H 0.9640 1.0643 0.6510 0.117 Uiso 1 1 calc R U . . .
H7B H 0.9087 1.0861 0.6026 0.117 Uiso 1 1 calc R U . . .
C8 C 0.9291(7) 1.2113(5) 0.6406(3) 0.139(4) Uani 1 1 d . . . . .
H8A H 0.9502 1.2241 0.6718 0.209 Uiso 1 1 calc R U . . .
H8B H 0.8607 1.2490 0.6315 0.209 Uiso 1 1 calc R U . . .
H8C H 0.9921 1.2307 0.6228 0.209 Uiso 1 1 calc R U . . .
C9 C 0.6341(5) 0.9608(3) 0.70724(19) 0.0529(15) Uani 1 1 d . . . . .
H9A H 0.6276 1.0328 0.7075 0.063 Uiso 1 1 calc R U . . .
H9B H 0.7023 0.9430 0.7263 0.063 Uiso 1 1 calc R U . . .
C10 C 0.5292(5) 0.9180(4) 0.7272(2) 0.0585(16) Uani 1 1 d . . . . .
H10A H 0.5289 0.8462 0.7234 0.070 Uiso 1 1 calc R U . . .
H10B H 0.4595 0.9444 0.7116 0.070 Uiso 1 1 calc R U . . .
C11 C 0.5285(6) 0.9428(4) 0.7763(2) 0.0746(19) Uani 1 1 d . . . . .
H11A H 0.5935 0.9093 0.7922 0.090 Uiso 1 1 calc R U . . .
H11B H 0.5398 1.0140 0.7801 0.090 Uiso 1 1 calc R U . . .
C12 C 0.4192(6) 0.9134(5) 0.7968(3) 0.106(3) Uani 1 1 d . . . . .
H12A H 0.4244 0.9303 0.8281 0.159 Uiso 1 1 calc R U . . .
H12B H 0.4078 0.8428 0.7935 0.159 Uiso 1 1 calc R U . . .
H12C H 0.3547 0.9480 0.7820 0.159 Uiso 1 1 calc R U . . .
C13 C 0.7887(4) 0.6241(3) 0.61125(19) 0.0477(14) Uani 1 1 d . . . . .
H13A H 0.8446 0.6371 0.6363 0.057 Uiso 1 1 calc R U . . .
H13B H 0.7971 0.6770 0.5895 0.057 Uiso 1 1 calc R U . . .
C14 C 0.8218(4) 0.5280(3) 0.5899(2) 0.0552(15) Uani 1 1 d . . . . .
H14A H 0.7681 0.5143 0.5643 0.066 Uiso 1 1 calc R U . . .
H14B H 0.8157 0.4742 0.6114 0.066 Uiso 1 1 calc R U . . .
C15 C 0.9436(4) 0.5317(4) 0.5747(2) 0.0619(17) Uani 1 1 d . . . . .
H15A H 0.9488 0.5855 0.5532 0.074 Uiso 1 1 calc R U . . .
H15B H 0.9965 0.5470 0.6004 0.074 Uiso 1 1 calc R U . . .
C16 C 0.9824(5) 0.4371(4) 0.5536(2) 0.0747(19) Uani 1 1 d . . . . .
H16A H 1.0611 0.4446 0.5450 0.112 Uiso 1 1 calc R U . . .
H16B H 0.9323 0.4225 0.5275 0.112 Uiso 1 1 calc R U . . .
H16C H 0.9789 0.3835 0.5748 0.112 Uiso 1 1 calc R U . . .
C17 C 0.6526(4) 0.5513(3) 0.66164(19) 0.0500(15) Uani 1 1 d . . . . .
H17A H 0.6523 0.4876 0.6463 0.060 Uiso 1 1 calc R U . . .
H17B H 0.7186 0.5515 0.6835 0.060 Uiso 1 1 calc R U . . .
C18 C 0.5447(5) 0.5598(4) 0.6858(2) 0.0618(16) Uani 1 1 d . . . . .
H18A H 0.4778 0.5545 0.6645 0.074 Uiso 1 1 calc R U . . .
H18B H 0.5421 0.6245 0.7001 0.074 Uiso 1 1 calc R U . . .
C19 C 0.5388(6) 0.4789(5) 0.7208(3) 0.100(3) Uani 1 1 d . . . . .
H19A H 0.5520 0.4152 0.7067 0.120 Uiso 1 1 calc R U . . .
H19B H 0.6018 0.4893 0.7435 0.120 Uiso 1 1 calc R U . . .
C20 C 0.4336(8) 0.4739(6) 0.7423(3) 0.143(4) Uani 1 1 d . . . . .
H20A H 0.4400 0.4247 0.7657 0.214 Uiso 1 1 calc R U . . .
H20B H 0.3717 0.4560 0.7208 0.214 Uiso 1 1 calc R U . . .
H20C H 0.4172 0.5377 0.7551 0.214 Uiso 1 1 calc R U . . .
C21 C 0.4930(4) 0.2315(3) 0.55628(16) 0.0387(12) Uani 1 1 d . . . . .
C22 C 0.5869(4) 0.2937(3) 0.5647(2) 0.0532(15) Uani 1 1 d . . . . .
H22 H 0.5749 0.3527 0.5801 0.064 Uiso 1 1 calc R U . . .
C23 C 0.6975(5) 0.2743(4) 0.5517(2) 0.0640(17) Uani 1 1 d . . . . .
H23 H 0.7572 0.3197 0.5584 0.077 Uiso 1 1 calc R U . . .
C24 C 0.7196(5) 0.1896(4) 0.5294(2) 0.0594(16) Uani 1 1 d . . . . .
H24 H 0.7939 0.1758 0.5203 0.071 Uiso 1 1 calc R U . . .
C25 C 0.6300(4) 0.1251(3) 0.52072(18) 0.0502(14) Uani 1 1 d . . . . .
H25 H 0.6434 0.0658 0.5057 0.060 Uiso 1 1 calc R U . . .
C26 C 0.5211(4) 0.1456(3) 0.53356(17) 0.0433(13) Uani 1 1 d . . . . .
H26 H 0.4623 0.0995 0.5267 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2654(4) 0.2018(3) 0.54122(18) 0.0424(13) Uani 1 1 d . . . . .
C28 C 0.1911(4) 0.2508(3) 0.51080(19) 0.0516(15) Uani 1 1 d . . . . .
H28 H 0.1964 0.3198 0.5089 0.062 Uiso 1 1 calc R U . . .
C29 C 0.1097(5) 0.2031(4) 0.4831(2) 0.0659(17) Uani 1 1 d . . . . .
H29 H 0.0623 0.2399 0.4629 0.079 Uiso 1 1 calc R U . . .
C30 C 0.0975(5) 0.1022(4) 0.4851(2) 0.0690(18) Uani 1 1 d . . . . .
H30 H 0.0430 0.0693 0.4661 0.083 Uiso 1 1 calc R U . . .
C31 C 0.1672(5) 0.0507(4) 0.5155(2) 0.069(2) Uani 1 1 d . . . . .
H31 H 0.1592 -0.0181 0.5179 0.083 Uiso 1 1 calc R U . . .
C32 C 0.2479(5) 0.0992(3) 0.5422(2) 0.0596(17) Uani 1 1 d . . . . .
H32 H 0.2945 0.0618 0.5625 0.071 Uiso 1 1 calc R U . . .
C33 C 0.3601(5) 0.2138(3) 0.62484(19) 0.0504(14) Uani 1 1 d . . . . .
C34 C 0.2601(6) 0.1754(5) 0.6413(3) 0.090(2) Uani 1 1 d . . . . .
H34 H 0.1942 0.1684 0.6218 0.108 Uiso 1 1 calc R U . . .
C35 C 0.2540(9) 0.1471(6) 0.6854(3) 0.117(3) Uani 1 1 d . . . . .
H35 H 0.1844 0.1223 0.6952 0.141 Uiso 1 1 calc R U . . .
C36 C 0.3456(9) 0.1546(5) 0.7141(3) 0.096(3) Uani 1 1 d . . . . .
H36 H 0.3405 0.1346 0.7438 0.115 Uiso 1 1 calc R U . . .
C37 C 0.4466(7) 0.1914(4) 0.7002(3) 0.081(2) Uani 1 1 d . . . . .
H37 H 0.5112 0.1981 0.7203 0.097 Uiso 1 1 calc R U . . .
C38 C 0.4527(6) 0.2189(4) 0.6560(2) 0.0658(17) Uani 1 1 d . . . . .
H38 H 0.5235 0.2422 0.6467 0.079 Uiso 1 1 calc R U . . .
C39 C 0.3420(4) 0.3751(3) 0.57332(19) 0.0428(13) Uani 1 1 d . . . . .
C40 C 0.2900(4) 0.4244(3) 0.6073(2) 0.0559(16) Uani 1 1 d . . . . .
H40 H 0.2736 0.3898 0.6332 0.067 Uiso 1 1 calc R U . . .
C41 C 0.2619(5) 0.5235(4) 0.6038(2) 0.0686(19) Uani 1 1 d . . . . .
H41 H 0.2269 0.5546 0.6275 0.082 Uiso 1 1 calc R U . . .
C42 C 0.2839(5) 0.5770(4) 0.5667(3) 0.069(2) Uani 1 1 d . . . . .
H42 H 0.2626 0.6438 0.5644 0.083 Uiso 1 1 calc R U . . .
C43 C 0.3372(5) 0.5314(4) 0.5333(2) 0.0637(18) Uani 1 1 d . . . . .
H43 H 0.3542 0.5672 0.5077 0.076 Uiso 1 1 calc R U . . .
C44 C 0.3667(4) 0.4326(3) 0.5367(2) 0.0504(15) Uani 1 1 d . . . . .
H44 H 0.4049 0.4031 0.5135 0.061 Uiso 1 1 calc R U . . .
C45 C 0.2642(7) 0.7663(5) 0.6743(3) 0.0972(17) Uani 1 1 d . . . . .
H45A H 0.2817 0.8084 0.7003 0.117 Uiso 1 1 calc R U . . .
H45B H 0.2946 0.7001 0.6809 0.117 Uiso 1 1 calc R U . . .
C46 C 0.1371(7) 0.7620(7) 0.6639(3) 0.136(3) Uani 1 1 d . . . . .
H46A H 0.1134 0.6964 0.6531 0.163 Uiso 1 1 calc R U . . .
H46B H 0.0947 0.7782 0.6901 0.163 Uiso 1 1 calc R U . . .
C47 C 0.1187(7) 0.8342(7) 0.6302(3) 0.136(3) Uani 1 1 d . . . . .
H47A H 0.0826 0.8928 0.6424 0.163 Uiso 1 1 calc R U . . .
H47B H 0.0669 0.8080 0.6061 0.163 Uiso 1 1 calc R U . . .
C48 C 0.2296(7) 0.8608(5) 0.6128(3) 0.0972(17) Uani 1 1 d . . . . .
H48A H 0.2298 0.8453 0.5810 0.117 Uiso 1 1 calc R U . . .
H48B H 0.2444 0.9315 0.6168 0.117 Uiso 1 1 calc R U . . .
B1 B 0.3659(5) 0.2546(3) 0.5738(2) 0.0429(15) Uani 1 1 d . . . . .
N2 N 0.6529(4) 0.9284(3) 0.66103(15) 0.0463(12) Uani 1 1 d . . . . .
N3 N 0.5429(3) 0.7969(2) 0.60135(14) 0.0397(10) Uani 1 1 d D . . . .
N4 N 0.6696(3) 0.6317(3) 0.62821(15) 0.0421(10) Uani 1 1 d . . . . .
O3 O 0.3139(4) 0.8054(3) 0.63693(17) 0.0803(13) Uani 1 1 d . . . . .
Pd1 Pd 0.66039(3) 0.77565(3) 0.65236(2) 0.04119(14) Uani 1 1 d . . . . .
N1_a N 0.7744(12) 0.7484(12) 0.7070(6) 0.089(4) Uiso 0.530(9) 1 d D . P A 1
O1_a O 0.8697(10) 0.7597(6) 0.7002(4) 0.098(2) Uiso 0.530(9) 1 d D . P A 1
O2_a O 0.7373(12) 0.7231(10) 0.7416(5) 0.098(2) Uiso 0.530(9) 1 d D . P A 1
N1A_b N 0.7879(11) 0.7334(11) 0.7360(5) 0.089(4) Uiso 0.470(9) 1 d D . P A 2
O1A_b O 0.7935(11) 0.7599(8) 0.6957(4) 0.062(3) Uiso 0.470(9) 1 d D . P A 2
O2A_b O 0.6859(10) 0.7202(9) 0.7459(5) 0.098(2) Uiso 0.470(9) 1 d D . P A 2
H3 H 0.468(3) 0.788(4) 0.615(2) 0.117 Uiso 1 1 d D 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
C1 C2 1.501(7) . ?
C1 N2 1.513(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.497(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.488(6) . ?
C3 C4 1.511(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.496(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.511(6) . ?
C5 C6 1.514(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.518(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.508(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N2 1.488(6) . ?
C9 C10 1.507(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.518(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.498(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.508(6) . ?
C13 C14 1.512(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.513(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.512(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 C18 1.491(7) . ?
C17 N4 1.504(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.526(8) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.418(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C22 1.391(6) . ?
C21 C26 1.399(6) . ?
C21 B1 1.628(7) . ?
C22 C23 1.390(7) . ?
C22 H22 0.9400 . ?
C23 C24 1.362(7) . ?
C23 H23 0.9400 . ?
C24 C25 1.373(7) . ?
C24 H24 0.9400 . ?
C25 C26 1.374(6) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.389(7) . ?
C27 C32 1.406(6) . ?
C27 B1 1.643(8) . ?
C28 C29 1.382(7) . ?
C28 H28 0.9400 . ?
C29 C30 1.377(7) . ?
C29 H29 0.9400 . ?
C30 C31 1.376(8) . ?
C30 H30 0.9400 . ?
C31 C32 1.368(7) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.386(7) . ?
C33 C34 1.392(8) . ?
C33 B1 1.638(8) . ?
C34 C35 1.389(9) . ?
C34 H34 0.9400 . ?
C35 C36 1.333(10) . ?
C35 H35 0.9400 . ?
C36 C37 1.364(10) . ?
C36 H36 0.9400 . ?
C37 C38 1.388(9) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C40 1.391(7) . ?
C39 C44 1.393(7) . ?
C39 B1 1.656(6) . ?
C40 C41 1.384(7) . ?
C40 H40 0.9400 . ?
C41 C42 1.370(8) . ?
C41 H41 0.9400 . ?
C42 C43 1.362(8) . ?
C42 H42 0.9400 . ?
C43 C44 1.385(6) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.400(8) . ?
C45 C46 1.492(10) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.417(10) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.465(10) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.401(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N2 Pd1 2.089(4) . ?
N3 Pd1 2.013(4) . ?
N3 H3 0.99(2) . ?
N4 Pd1 2.088(4) . ?
Pd1 O1A_b 1.974(13) . ?
Pd1 N1_a 2.082(18) . ?
N1_a O1_a 1.148(15) . ?
N1_a O2_a 1.202(15) . ?
N1A_b O2A_b 1.252(13) . ?
N1A_b O1A_b 1.273(16) . ?

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
C2 C1 N2 109.7(4) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.9(4) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 105.7(4) . . ?
N3 C3 H3A 110.6 . . ?
C4 C3 H3A 110.6 . . ?
N3 C3 H3B 110.6 . . ?
C4 C3 H3B 110.6 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.4(4) . . ?
N4 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N4 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.4(4) . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 C7 110.7(5) . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 111.0(6) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.3(4) . . ?
N2 C9 H9A 108.5 . . ?
C10 C9 H9A 108.5 . . ?
N2 C9 H9B 108.5 . . ?
C10 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 110.8(5) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.4(6) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.7(4) . . ?
N4 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
N4 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 C15 111.5(4) . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 114.1(4) . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15B 108.7 . . ?
C14 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N4 114.7(4) . . ?
C18 C17 H17A 108.6 . . ?
N4 C17 H17A 108.6 . . ?
C18 C17 H17B 108.6 . . ?
N4 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C17 C18 C19 110.8(5) . . ?
C17 C18 H18A 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
C20 C19 C18 115.2(7) . . ?
C20 C19 H19A 108.5 . . ?
C18 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 113.0(4) . . ?
C22 C21 B1 122.8(4) . . ?
C26 C21 B1 124.2(4) . . ?
C23 C22 C21 124.2(5) . . ?
C23 C22 H22 117.9 . . ?
C21 C22 H22 117.9 . . ?
C24 C23 C22 120.2(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 117.9(5) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C24 C25 C26 121.2(5) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
C25 C26 C21 123.5(4) . . ?
C25 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C28 C27 C32 113.7(5) . . ?
C28 C27 B1 125.2(4) . . ?
C32 C27 B1 121.1(5) . . ?
C29 C28 C27 123.3(4) . . ?
C29 C28 H28 118.3 . . ?
C27 C28 H28 118.3 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 118.4(5) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C32 C31 C30 120.2(5) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C31 C32 C27 124.0(5) . . ?
C31 C32 H32 118.0 . . ?
C27 C32 H32 118.0 . . ?
C38 C33 C34 114.1(6) . . ?
C38 C33 B1 123.0(5) . . ?
C34 C33 B1 122.8(6) . . ?
C35 C34 C33 122.4(7) . . ?
C35 C34 H34 118.8 . . ?
C33 C34 H34 118.8 . . ?
C36 C35 C34 121.0(8) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 119.8(8) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C36 C37 C38 119.1(7) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C33 C38 C37 123.6(7) . . ?
C33 C38 H38 118.2 . . ?
C37 C38 H38 118.2 . . ?
C40 C39 C44 115.6(4) . . ?
C40 C39 B1 123.2(5) . . ?
C44 C39 B1 121.1(5) . . ?
C41 C40 C39 121.5(6) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C42 C41 C40 121.4(6) . . ?
C42 C41 H41 119.3 . . ?
C40 C41 H41 119.3 . . ?
C43 C42 C41 118.6(5) . . ?
C43 C42 H42 120.7 . . ?
C41 C42 H42 120.7 . . ?
C42 C43 C44 120.3(6) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C39 122.5(6) . . ?
C43 C44 H44 118.7 . . ?
C39 C44 H44 118.7 . . ?
O3 C45 C46 107.2(6) . . ?
O3 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
O3 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.5 . . ?
C47 C46 C45 103.2(8) . . ?
C47 C46 H46A 111.1 . . ?
C45 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
C45 C46 H46B 111.1 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 109.1(7) . . ?
C46 C47 H47A 109.9 . . ?
C48 C47 H47A 109.9 . . ?
C46 C47 H47B 109.9 . . ?
C48 C47 H47B 109.9 . . ?
H47A C47 H47B 108.3 . . ?
O3 C48 C47 106.6(6) . . ?
O3 C48 H48A 110.4 . . ?
C47 C48 H48A 110.4 . . ?
O3 C48 H48B 110.4 . . ?
C47 C48 H48B 110.4 . . ?
H48A C48 H48B 108.6 . . ?
C21 B1 C33 109.1(4) . . ?
C21 B1 C27 110.3(4) . . ?
C33 B1 C27 110.2(4) . . ?
C21 B1 C39 109.9(4) . . ?
C33 B1 C39 109.0(4) . . ?
C27 B1 C39 108.2(4) . . ?
C9 N2 C5 109.8(4) . . ?
C9 N2 C1 110.9(4) . . ?
C5 N2 C1 111.1(4) . . ?
C9 N2 Pd1 114.7(3) . . ?
C5 N2 Pd1 104.6(3) . . ?
C1 N2 Pd1 105.5(3) . . ?
C3 N3 C2 115.8(4) . . ?
C3 N3 Pd1 107.8(3) . . ?
C2 N3 Pd1 106.8(3) . . ?
C3 N3 H3 113(4) . . ?
C2 N3 H3 109(3) . . ?
Pd1 N3 H3 104(4) . . ?
C4 N4 C17 110.0(3) . . ?
C4 N4 C13 111.3(4) . . ?
C17 N4 C13 109.7(4) . . ?
C4 N4 Pd1 105.6(3) . . ?
C17 N4 Pd1 115.6(3) . . ?
C13 N4 Pd1 104.4(3) . . ?
C45 O3 C48 108.1(5) . . ?
O1A_b Pd1 N3 171.1(3) . . ?
N3 Pd1 N1_a 176.5(4) . . ?
O1A_b Pd1 N4 94.3(4) . . ?
N3 Pd1 N4 85.11(15) . . ?
N1_a Pd1 N4 93.8(5) . . ?
O1A_b Pd1 N2 93.5(4) . . ?
N3 Pd1 N2 85.51(16) . . ?
N1_a Pd1 N2 96.1(5) . . ?
N4 Pd1 N2 166.72(17) . . ?
O1_a N1_a O2_a 126(2) . . ?
O1_a N1_a Pd1 114.2(14) . . ?
O2_a N1_a Pd1 119.5(12) . . ?
O2A_b N1A_b O1A_b 111.7(14) . . ?
N1A_b O1A_b Pd1 125.4(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 55.6(5) . . . . ?
N3 C3 C4 N4 -53.9(5) . . . . ?
N2 C5 C6 C7 -179.0(5) . . . . ?
C5 C6 C7 C8 -173.9(6) . . . . ?
N2 C9 C10 C11 171.2(4) . . . . ?
C9 C10 C11 C12 172.7(5) . . . . ?
N4 C13 C14 C15 -179.9(5) . . . . ?
C13 C14 C15 C16 179.2(5) . . . . ?
N4 C17 C18 C19 -176.5(5) . . . . ?
C17 C18 C19 C20 -173.4(7) . . . . ?
C26 C21 C22 C23 0.6(8) . . . . ?
B1 C21 C22 C23 177.4(5) . . . . ?
C21 C22 C23 C24 -0.3(9) . . . . ?
C22 C23 C24 C25 -0.4(9) . . . . ?
C23 C24 C25 C26 0.8(9) . . . . ?
C24 C25 C26 C21 -0.4(8) . . . . ?
C22 C21 C26 C25 -0.3(7) . . . . ?
B1 C21 C26 C25 -177.0(5) . . . . ?
C32 C27 C28 C29 -1.8(8) . . . . ?
B1 C27 C28 C29 178.3(5) . . . . ?
C27 C28 C29 C30 0.9(9) . . . . ?
C28 C29 C30 C31 0.9(9) . . . . ?
C29 C30 C31 C32 -1.5(10) . . . . ?
C30 C31 C32 C27 0.5(10) . . . . ?
C28 C27 C32 C31 1.1(8) . . . . ?
B1 C27 C32 C31 -178.9(6) . . . . ?
C38 C33 C34 C35 1.4(10) . . . . ?
B1 C33 C34 C35 -175.6(6) . . . . ?
C33 C34 C35 C36 -0.8(13) . . . . ?
C34 C35 C36 C37 0.6(13) . . . . ?
C35 C36 C37 C38 -1.1(11) . . . . ?
C34 C33 C38 C37 -2.0(8) . . . . ?
B1 C33 C38 C37 175.0(5) . . . . ?
C36 C37 C38 C33 1.9(9) . . . . ?
C44 C39 C40 C41 2.0(7) . . . . ?
B1 C39 C40 C41 -173.9(5) . . . . ?
C39 C40 C41 C42 0.1(9) . . . . ?
C40 C41 C42 C43 -1.7(9) . . . . ?
C41 C42 C43 C44 1.0(8) . . . . ?
C42 C43 C44 C39 1.3(8) . . . . ?
C40 C39 C44 C43 -2.7(7) . . . . ?
B1 C39 C44 C43 173.3(5) . . . . ?
O3 C45 C46 C47 -23.4(10) . . . . ?
C45 C46 C47 C48 14.6(11) . . . . ?
C46 C47 C48 O3 -1.0(11) . . . . ?
C22 C21 B1 C33 -85.1(5) . . . . ?
C26 C21 B1 C33 91.3(6) . . . . ?
C22 C21 B1 C27 153.6(5) . . . . ?
C26 C21 B1 C27 -30.0(7) . . . . ?
C22 C21 B1 C39 34.4(7) . . . . ?
C26 C21 B1 C39 -149.2(5) . . . . ?
C38 C33 B1 C21 37.2(6) . . . . ?
C34 C33 B1 C21 -146.1(5) . . . . ?
C38 C33 B1 C27 158.5(4) . . . . ?
C34 C33 B1 C27 -24.8(7) . . . . ?
C38 C33 B1 C39 -82.9(6) . . . . ?
C34 C33 B1 C39 93.8(6) . . . . ?
C28 C27 B1 C21 -106.5(5) . . . . ?
C32 C27 B1 C21 73.5(6) . . . . ?
C28 C27 B1 C33 132.9(5) . . . . ?
C32 C27 B1 C33 -47.1(6) . . . . ?
C28 C27 B1 C39 13.8(7) . . . . ?
C32 C27 B1 C39 -166.2(5) . . . . ?
C40 C39 B1 C21 -138.3(5) . . . . ?
C44 C39 B1 C21 46.0(6) . . . . ?
C40 C39 B1 C33 -18.7(7) . . . . ?
C44 C39 B1 C33 165.6(5) . . . . ?
C40 C39 B1 C27 101.2(6) . . . . ?
C44 C39 B1 C27 -74.5(6) . . . . ?
C10 C9 N2 C5 -172.6(4) . . . . ?
C10 C9 N2 C1 64.3(5) . . . . ?
C10 C9 N2 Pd1 -55.1(5) . . . . ?
C6 C5 N2 C9 -57.7(6) . . . . ?
C6 C5 N2 C1 65.4(6) . . . . ?
C6 C5 N2 Pd1 178.7(4) . . . . ?
C2 C1 N2 C9 -159.9(4) . . . . ?
C2 C1 N2 C5 77.7(5) . . . . ?
C2 C1 N2 Pd1 -35.1(5) . . . . ?
C4 C3 N3 C2 166.1(4) . . . . ?
C4 C3 N3 Pd1 46.6(4) . . . . ?
C1 C2 N3 C3 -167.2(4) . . . . ?
C1 C2 N3 Pd1 -47.2(4) . . . . ?
C3 C4 N4 C17 158.7(4) . . . . ?
C3 C4 N4 C13 -79.4(5) . . . . ?
C3 C4 N4 Pd1 33.3(4) . . . . ?
C18 C17 N4 C4 -65.8(6) . . . . ?
C18 C17 N4 C13 171.4(5) . . . . ?
C18 C17 N4 Pd1 53.7(5) . . . . ?
C14 C13 N4 C4 -64.7(6) . . . . ?
C14 C13 N4 C17 57.4(6) . . . . ?
C14 C13 N4 Pd1 -178.1(4) . . . . ?
C46 C45 O3 C48 23.7(8) . . . . ?
C47 C48 O3 C45 -14.3(8) . . . . ?
O2A_b N1A_b O1A_b Pd1 -1.6(16) . . . . ?

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
C5 H5B O1_a 0.98 2.60 3.388(11) 137.0 .
C5 H5B O1A_b 0.98 2.56 3.149(12) 118.6 .
C10 H10A O2A_b 0.98 2.56 3.270(14) 129.3 .
C13 H13A O1_a 0.98 2.55 3.337(11) 137.6 .
C18 H18B O2A_b 0.98 2.47 3.217(14) 132.8 .
C46 H46B O1_a 0.98 2.66 3.356(14) 128.0 1_455
N3 H3 O3 0.99(2) 1.96(2) 2.930(6) 165(5) .

_refine_diff_density_max         0.726
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.080

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_PSS-260K
_database_code_depnum_ccdc_archive 'CCDC 1441780'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_PSS-260K            
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         18 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6500(5)
_cell_length_b                   13.5543(6)
_cell_length_c                   30.0680(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.859(4)
_cell_angle_gamma                90
_cell_volume                     4737.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    5008
_cell_measurement_theta_min      3.4690
_cell_measurement_theta_max      27.3120

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.434
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96037
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20129
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.156
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9670
_reflns_number_gt                6254
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0392P)²+0.8439P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9670
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.1040
_refine_ls_wR_factor_gt          0.0888
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
C1 C 0.5577(3) 0.9629(3) 0.63015(12) 0.0543(10) Uani 1 1 d . . . . .
H1A H 0.5698 1.0319 0.6232 0.065 Uiso 1 1 calc R U . . .
H1B H 0.4847 0.9572 0.6436 0.065 Uiso 1 1 calc R U . . .
C2 C 0.5544(3) 0.9029(3) 0.58798(11) 0.0508(9) Uani 1 1 d . . . . .
H2A H 0.4889 0.9217 0.5682 0.061 Uiso 1 1 calc R U . . .
H2B H 0.6240 0.9131 0.5726 0.061 Uiso 1 1 calc R U . . .
C3 C 0.5653(3) 0.7227(3) 0.56715(10) 0.0444(8) Uani 1 1 d . . . . .
H3A H 0.6344 0.7384 0.5523 0.053 Uiso 1 1 calc R U . . .
H3B H 0.5009 0.7202 0.5450 0.053 Uiso 1 1 calc R U . . .
C4 C 0.5789(3) 0.6254(2) 0.59105(10) 0.0433(8) Uani 1 1 d . . . . .
H4A H 0.5061 0.6067 0.6025 0.052 Uiso 1 1 calc R U . . .
H4B H 0.5998 0.5749 0.5702 0.052 Uiso 1 1 calc R U . . .
C5 C 0.7673(3) 0.9658(3) 0.64932(12) 0.0549(10) Uani 1 1 d . . . . .
H5A H 0.7773 0.9452 0.6189 0.066 Uiso 1 1 calc R U . . .
H5B H 0.8273 0.9343 0.6682 0.066 Uiso 1 1 calc R U . . .
C6 C 0.7857(4) 1.0761(3) 0.65205(15) 0.0756(13) Uani 1 1 d . . . . .
H6A H 0.7805 1.0977 0.6826 0.091 Uiso 1 1 calc R U . . .
H6B H 0.7259 1.1092 0.6337 0.091 Uiso 1 1 calc R U . . .
C7 C 0.9026(4) 1.1040(4) 0.63635(19) 0.0992(17) Uani 1 1 d . . . . .
H7A H 0.9616 1.0645 0.6522 0.119 Uiso 1 1 calc R U . . .
H7B H 0.9042 1.0895 0.6048 0.119 Uiso 1 1 calc R U . . .
C8 C 0.9282(6) 1.2112(4) 0.6441(3) 0.152(3) Uani 1 1 d . . . . .
H8A H 0.9551 1.2212 0.6746 0.229 Uiso 1 1 calc R U . . .
H8B H 0.8595 1.2491 0.6376 0.229 Uiso 1 1 calc R U . . .
H8C H 0.9863 1.2320 0.6250 0.229 Uiso 1 1 calc R U . . .
C9 C 0.6332(3) 0.9608(3) 0.70882(11) 0.0514(9) Uani 1 1 d . . . . .
H9A H 0.6239 1.0319 0.7087 0.062 Uiso 1 1 calc R U . . .
H9B H 0.7012 0.9455 0.7280 0.062 Uiso 1 1 calc R U . . .
C10 C 0.5302(3) 0.9152(3) 0.72860(11) 0.0595(10) Uani 1 1 d . . . . .
H10A H 0.5336 0.8440 0.7258 0.071 Uiso 1 1 calc R U . . .
H10B H 0.4603 0.9380 0.7125 0.071 Uiso 1 1 calc R U . . .
C11 C 0.5277(4) 0.9430(4) 0.77753(13) 0.0775(13) Uani 1 1 d . . . . .
H11A H 0.5915 0.9112 0.7942 0.093 Uiso 1 1 calc R U . . .
H11B H 0.5379 1.0138 0.7806 0.093 Uiso 1 1 calc R U . . .
C12 C 0.4176(4) 0.9137(5) 0.79689(16) 0.1101(19) Uani 1 1 d . . . . .
H12A H 0.4215 0.9299 0.8280 0.165 Uiso 1 1 calc R U . . .
H12B H 0.4061 0.8440 0.7933 0.165 Uiso 1 1 calc R U . . .
H12C H 0.3546 0.9485 0.7818 0.165 Uiso 1 1 calc R U . . .
C13 C 0.7886(3) 0.6239(2) 0.61177(11) 0.0454(8) Uani 1 1 d . . . . .
H13A H 0.8444 0.6365 0.6365 0.055 Uiso 1 1 calc R U . . .
H13B H 0.7963 0.6764 0.5903 0.055 Uiso 1 1 calc R U . . .
C14 C 0.8210(3) 0.5279(3) 0.59016(12) 0.0532(9) Uani 1 1 d . . . . .
H14A H 0.8141 0.4742 0.6111 0.064 Uiso 1 1 calc R U . . .
H14B H 0.7682 0.5152 0.5645 0.064 Uiso 1 1 calc R U . . .
C15 C 0.9419(3) 0.5312(3) 0.57571(14) 0.0630(11) Uani 1 1 d . . . . .
H15A H 0.9938 0.5457 0.6015 0.076 Uiso 1 1 calc R U . . .
H15B H 0.9478 0.5848 0.5546 0.076 Uiso 1 1 calc R U . . .
C16 C 0.9801(3) 0.4367(3) 0.55455(15) 0.0740(12) Uani 1 1 d . . . . .
H16A H 1.0566 0.4448 0.5451 0.111 Uiso 1 1 calc R U . . .
H16B H 0.9286 0.4213 0.5292 0.111 Uiso 1 1 calc R U . . .
H16C H 0.9792 0.3840 0.5758 0.111 Uiso 1 1 calc R U . . .
C17 C 0.6522(3) 0.5505(3) 0.66138(11) 0.0478(9) Uani 1 1 d . . . . .
H17A H 0.7192 0.5475 0.6823 0.057 Uiso 1 1 calc R U . . .
H17B H 0.6476 0.4883 0.6454 0.057 Uiso 1 1 calc R U . . .
C18 C 0.5471(3) 0.5610(3) 0.68710(12) 0.0602(10) Uani 1 1 d . . . . .
H18A H 0.4794 0.5633 0.6665 0.072 Uiso 1 1 calc R U . . .
H18B H 0.5512 0.6226 0.7036 0.072 Uiso 1 1 calc R U . . .
C19 C 0.5360(4) 0.4764(4) 0.71913(16) 0.0947(16) Uani 1 1 d . . . . .
H19A H 0.5399 0.4151 0.7027 0.114 Uiso 1 1 calc R U . . .
H19B H 0.6014 0.4780 0.7409 0.114 Uiso 1 1 calc R U . . .
C20 C 0.4312(5) 0.4762(4) 0.74279(19) 0.121(2) Uani 1 1 d . . . . .
H20A H 0.4348 0.4240 0.7644 0.181 Uiso 1 1 calc R U . . .
H20B H 0.3662 0.4660 0.7220 0.181 Uiso 1 1 calc R U . . .
H20C H 0.4234 0.5383 0.7576 0.181 Uiso 1 1 calc R U . . .
C21 C 0.4944(3) 0.2307(2) 0.55601(10) 0.0392(7) Uani 1 1 d . . . . .
C22 C 0.5871(3) 0.2932(3) 0.56470(13) 0.0567(10) Uani 1 1 d . . . . .
H22 H 0.5750 0.3518 0.5798 0.068 Uiso 1 1 calc R U . . .
C23 C 0.6963(3) 0.2735(3) 0.55228(14) 0.0640(11) Uani 1 1 d . . . . .
H23 H 0.7554 0.3182 0.5591 0.077 Uiso 1 1 calc R U . . .
C24 C 0.7182(3) 0.1884(3) 0.52998(13) 0.0573(10) Uani 1 1 d . . . . .
H24 H 0.7917 0.1748 0.5213 0.069 Uiso 1 1 calc R U . . .
C25 C 0.6297(3) 0.1235(3) 0.52077(11) 0.0506(9) Uani 1 1 d . . . . .
H25 H 0.6431 0.0648 0.5060 0.061 Uiso 1 1 calc R U . . .
C26 C 0.5200(3) 0.1450(2) 0.53337(10) 0.0432(8) Uani 1 1 d . . . . .
H26 H 0.4612 0.1001 0.5263 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2653(3) 0.2016(2) 0.54104(11) 0.0393(8) Uani 1 1 d . . . . .
C28 C 0.1917(3) 0.2512(3) 0.51048(12) 0.0517(9) Uani 1 1 d . . . . .
H28 H 0.1979 0.3195 0.5086 0.062 Uiso 1 1 calc R U . . .
C29 C 0.1095(3) 0.2040(3) 0.48272(14) 0.0674(12) Uani 1 1 d . . . . .
H29 H 0.0623 0.2406 0.4627 0.081 Uiso 1 1 calc R U . . .
C30 C 0.0972(3) 0.1035(3) 0.48457(15) 0.0695(12) Uani 1 1 d . . . . .
H30 H 0.0424 0.0715 0.4658 0.083 Uiso 1 1 calc R U . . .
C31 C 0.1669(3) 0.0513(3) 0.51437(17) 0.0699(12) Uani 1 1 d . . . . .
H31 H 0.1595 -0.0168 0.5161 0.084 Uiso 1 1 calc R U . . .
C32 C 0.2481(3) 0.0997(3) 0.54187(14) 0.0582(10) Uani 1 1 d . . . . .
H32 H 0.2939 0.0624 0.5621 0.070 Uiso 1 1 calc R U . . .
C33 C 0.3620(3) 0.2132(3) 0.62506(11) 0.0503(9) Uani 1 1 d . . . . .
C34 C 0.2626(4) 0.1760(4) 0.64132(14) 0.0886(15) Uani 1 1 d . . . . .
H34 H 0.1973 0.1697 0.6219 0.106 Uiso 1 1 calc R U . . .
C35 C 0.2564(6) 0.1477(5) 0.68543(18) 0.119(2) Uani 1 1 d . . . . .
H35 H 0.1876 0.1236 0.6951 0.143 Uiso 1 1 calc R U . . .
C36 C 0.3509(7) 0.1552(4) 0.71468(17) 0.105(2) Uani 1 1 d . . . . .
H36 H 0.3475 0.1347 0.7441 0.126 Uiso 1 1 calc R U . . .
C37 C 0.4495(5) 0.1928(3) 0.70037(15) 0.0857(15) Uani 1 1 d . . . . .
H37 H 0.5137 0.2005 0.7202 0.103 Uiso 1 1 calc R U . . .
C38 C 0.4546(4) 0.2200(3) 0.65582(12) 0.0632(11) Uani 1 1 d . . . . .
H38 H 0.5239 0.2438 0.6465 0.076 Uiso 1 1 calc R U . . .
C39 C 0.3433(3) 0.3744(2) 0.57301(11) 0.0420(8) Uani 1 1 d . . . . .
C40 C 0.2915(3) 0.4240(3) 0.60654(12) 0.0535(9) Uani 1 1 d . . . . .
H40 H 0.2755 0.3896 0.6322 0.064 Uiso 1 1 calc R U . . .
C41 C 0.2626(3) 0.5228(3) 0.60331(16) 0.0694(12) Uani 1 1 d . . . . .
H41 H 0.2274 0.5530 0.6266 0.083 Uiso 1 1 calc R U . . .
C42 C 0.2849(3) 0.5766(3) 0.56655(18) 0.0689(12) Uani 1 1 d . . . . .
H42 H 0.2638 0.6427 0.5643 0.083 Uiso 1 1 calc R U . . .
C43 C 0.3389(3) 0.5310(3) 0.53309(14) 0.0605(11) Uani 1 1 d . . . . .
H43 H 0.3560 0.5664 0.5079 0.073 Uiso 1 1 calc R U . . .
C44 C 0.3681(3) 0.4322(2) 0.53685(11) 0.0489(9) Uani 1 1 d . . . . .
H44 H 0.4062 0.4032 0.5140 0.059 Uiso 1 1 calc R U . . .
C45 C 0.2670(4) 0.7669(4) 0.67392(17) 0.1000(12) Uani 1 1 d . . . . .
H45A H 0.2860 0.8080 0.6998 0.120 Uiso 1 1 calc R U . . .
H45B H 0.2959 0.7009 0.6802 0.120 Uiso 1 1 calc R U . . .
C46 C 0.1419(5) 0.7641(5) 0.6644(2) 0.1325(17) Uani 1 1 d . . . . .
H46A H 0.1168 0.6991 0.6544 0.159 Uiso 1 1 calc R U . . .
H46B H 0.1020 0.7819 0.6905 0.159 Uiso 1 1 calc R U . . .
C47 C 0.1222(5) 0.8353(5) 0.6297(2) 0.1325(17) Uani 1 1 d . . . . .
H47A H 0.0870 0.8940 0.6414 0.159 Uiso 1 1 calc R U . . .
H47B H 0.0707 0.8085 0.6061 0.159 Uiso 1 1 calc R U . . .
C48 C 0.2316(4) 0.8600(4) 0.61268(17) 0.1000(12) Uani 1 1 d . . . . .
H48A H 0.2307 0.8440 0.5812 0.120 Uiso 1 1 calc R U . . .
H48B H 0.2465 0.9301 0.6162 0.120 Uiso 1 1 calc R U . . .
B1 B 0.3659(3) 0.2551(3) 0.57366(12) 0.0407(9) Uani 1 1 d . . . . .
N2 N 0.6529(2) 0.9276(2) 0.66237(8) 0.0454(7) Uani 1 1 d . . . . .
N3 N 0.5448(2) 0.79798(19) 0.60158(8) 0.0388(6) Uani 1 1 d D . . . .
N4 N 0.6697(2) 0.63098(19) 0.62892(8) 0.0398(6) Uani 1 1 d . . . . .
O3 O 0.3175(2) 0.8055(2) 0.63657(10) 0.0788(9) Uani 1 1 d . . . . .
Pd1 Pd 0.65981(2) 0.77498(2) 0.65373(2) 0.03761(9) Uani 1 1 d . . . . .
N1 N 0.7727(3) 0.7504(2) 0.70606(10) 0.0530(8) Uani 1 1 d . . . . .
O1 O 0.8747(3) 0.7599(3) 0.70254(10) 0.1053(12) Uani 1 1 d . . . . .
O2 O 0.7393(3) 0.7249(3) 0.74126(10) 0.1100(13) Uani 1 1 d . . . . .
H3 H 0.469(2) 0.789(4) 0.6131(16) 0.132 Uiso 1 1 d D 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
C1 N2 1.501(4) . ?
C1 C2 1.505(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.486(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.484(4) . ?
C3 C4 1.505(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.503(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.506(4) . ?
C5 C6 1.511(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.518(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.499(7) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N2 1.500(4) . ?
C9 C10 1.507(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.521(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.498(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N4 1.513(4) . ?
C13 C14 1.514(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.502(5) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.511(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N4 1.487(4) . ?
C17 C18 1.499(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.508(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.454(6) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.385(5) . ?
C21 C26 1.389(4) . ?
C21 B1 1.654(5) . ?
C22 C23 1.376(5) . ?
C22 H22 0.9300 . ?
C23 C24 1.367(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.369(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C28 1.388(5) . ?
C27 C32 1.397(4) . ?
C27 B1 1.645(5) . ?
C28 C29 1.385(5) . ?
C28 H28 0.9300 . ?
C29 C30 1.370(5) . ?
C29 H29 0.9300 . ?
C30 C31 1.365(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.380(5) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C38 1.377(5) . ?
C33 C34 1.382(5) . ?
C33 B1 1.650(5) . ?
C34 C35 1.387(6) . ?
C34 H34 0.9300 . ?
C35 C36 1.366(8) . ?
C35 H35 0.9300 . ?
C36 C37 1.354(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.394(6) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.384(4) . ?
C39 C44 1.386(4) . ?
C39 B1 1.639(5) . ?
C40 C41 1.383(5) . ?
C40 H40 0.9300 . ?
C41 C42 1.364(6) . ?
C41 H41 0.9300 . ?
C42 C43 1.370(5) . ?
C42 H42 0.9300 . ?
C43 C44 1.384(5) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 O3 1.404(5) . ?
C45 C46 1.466(7) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.427(7) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.445(6) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 O3 1.402(5) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
N2 Pd1 2.087(3) . ?
N3 Pd1 2.017(3) . ?
N3 H3 0.973(19) . ?
N4 Pd1 2.095(3) . ?
Pd1 N1 2.010(3) . ?
N1 O2 1.203(4) . ?
N1 O1 1.206(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 110.3(3) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.5(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.6(2) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 111.3(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.8(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 C7 110.9(4) . . ?
C5 C6 H6A 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 111.5(5) . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 114.8(3) . . ?
N2 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N2 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 110.3(3) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.5(4) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.5(3) . . ?
N4 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
N4 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.3(3) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.9(3) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.0(3) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.4(3) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 115.1(4) . . ?
C20 C19 H19A 108.5 . . ?
C18 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 114.4(3) . . ?
C22 C21 B1 121.9(3) . . ?
C26 C21 B1 123.6(3) . . ?
C23 C22 C21 123.6(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 118.5(3) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 122.8(3) . . ?
C25 C26 H26 118.6 . . ?
C21 C26 H26 118.6 . . ?
C28 C27 C32 114.1(3) . . ?
C28 C27 B1 124.4(3) . . ?
C32 C27 B1 121.5(3) . . ?
C29 C28 C27 123.1(4) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 118.8(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 120.1(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 123.5(4) . . ?
C31 C32 H32 118.2 . . ?
C27 C32 H32 118.2 . . ?
C38 C33 C34 115.1(4) . . ?
C38 C33 B1 122.4(3) . . ?
C34 C33 B1 122.3(3) . . ?
C33 C34 C35 122.5(5) . . ?
C33 C34 H34 118.7 . . ?
C35 C34 H34 118.7 . . ?
C36 C35 C34 120.2(5) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 119.2(5) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C36 C37 C38 119.8(5) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C33 C38 C37 123.1(4) . . ?
C33 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C40 C39 C44 114.9(3) . . ?
C40 C39 B1 123.2(3) . . ?
C44 C39 B1 121.7(3) . . ?
C41 C40 C39 122.4(4) . . ?
C41 C40 H40 118.8 . . ?
C39 C40 H40 118.8 . . ?
C42 C41 C40 121.1(4) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 118.4(4) . . ?
C41 C42 H42 120.8 . . ?
C43 C42 H42 120.8 . . ?
C42 C43 C44 119.9(4) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 123.2(3) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 108.5(4) . . ?
O3 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
O3 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
C47 C46 C45 103.6(5) . . ?
C47 C46 H46A 111.0 . . ?
C45 C46 H46A 111.0 . . ?
C47 C46 H46B 111.0 . . ?
C45 C46 H46B 111.0 . . ?
H46A C46 H46B 109.0 . . ?
C46 C47 C48 108.2(5) . . ?
C46 C47 H47A 110.1 . . ?
C48 C47 H47A 110.1 . . ?
C46 C47 H47B 110.1 . . ?
C48 C47 H47B 110.1 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 108.2(4) . . ?
O3 C48 H48A 110.1 . . ?
C47 C48 H48A 110.1 . . ?
O3 C48 H48B 110.1 . . ?
C47 C48 H48B 110.1 . . ?
H48A C48 H48B 108.4 . . ?
C39 B1 C27 108.7(3) . . ?
C39 B1 C33 109.7(3) . . ?
C27 B1 C33 110.1(3) . . ?
C39 B1 C21 110.0(3) . . ?
C27 B1 C21 110.1(3) . . ?
C33 B1 C21 108.3(3) . . ?
C9 N2 C1 110.6(3) . . ?
C9 N2 C5 109.4(3) . . ?
C1 N2 C5 110.5(3) . . ?
C9 N2 Pd1 115.0(2) . . ?
C1 N2 Pd1 105.6(2) . . ?
C5 N2 Pd1 105.5(2) . . ?
C3 N3 C2 116.6(2) . . ?
C3 N3 Pd1 107.81(19) . . ?
C2 N3 Pd1 107.64(19) . . ?
C3 N3 H3 111(3) . . ?
C2 N3 H3 107(3) . . ?
Pd1 N3 H3 106(3) . . ?
C17 N4 C4 109.9(2) . . ?
C17 N4 C13 110.3(2) . . ?
C4 N4 C13 110.6(2) . . ?
C17 N4 Pd1 115.9(2) . . ?
C4 N4 Pd1 105.30(18) . . ?
C13 N4 Pd1 104.72(18) . . ?
C48 O3 C45 106.5(3) . . ?
N1 Pd1 N3 179.08(12) . . ?
N1 Pd1 N2 95.48(11) . . ?
N3 Pd1 N2 85.09(10) . . ?
N1 Pd1 N4 94.33(11) . . ?
N3 Pd1 N4 85.23(10) . . ?
N2 Pd1 N4 166.18(10) . . ?
O2 N1 O1 119.2(3) . . ?
O2 N1 Pd1 120.2(3) . . ?
O1 N1 Pd1 120.7(3) . . ?

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
N2 C1 C2 N3 55.0(4) . . . . ?
N3 C3 C4 N4 -53.7(3) . . . . ?
N2 C5 C6 C7 -177.9(3) . . . . ?
C5 C6 C7 C8 -173.0(4) . . . . ?
N2 C9 C10 C11 172.3(3) . . . . ?
C9 C10 C11 C12 170.6(4) . . . . ?
N4 C13 C14 C15 -178.8(3) . . . . ?
C13 C14 C15 C16 179.0(3) . . . . ?
N4 C17 C18 C19 180.0(3) . . . . ?
C17 C18 C19 C20 -175.0(4) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
B1 C21 C22 C23 177.1(4) . . . . ?
C21 C22 C23 C24 0.2(6) . . . . ?
C22 C23 C24 C25 -0.6(6) . . . . ?
C23 C24 C25 C26 0.9(6) . . . . ?
C24 C25 C26 C21 -0.9(5) . . . . ?
C22 C21 C26 C25 0.4(5) . . . . ?
B1 C21 C26 C25 -176.7(3) . . . . ?
C32 C27 C28 C29 -0.9(5) . . . . ?
B1 C27 C28 C29 178.5(3) . . . . ?
C27 C28 C29 C30 0.2(6) . . . . ?
C28 C29 C30 C31 0.4(6) . . . . ?
C29 C30 C31 C32 -0.2(6) . . . . ?
C30 C31 C32 C27 -0.6(6) . . . . ?
C28 C27 C32 C31 1.2(5) . . . . ?
B1 C27 C32 C31 -178.3(3) . . . . ?
C38 C33 C34 C35 0.1(7) . . . . ?
B1 C33 C34 C35 -174.9(5) . . . . ?
C33 C34 C35 C36 -0.6(9) . . . . ?
C34 C35 C36 C37 1.7(9) . . . . ?
C35 C36 C37 C38 -2.3(8) . . . . ?
C34 C33 C38 C37 -0.8(6) . . . . ?
B1 C33 C38 C37 174.2(3) . . . . ?
C36 C37 C38 C33 1.9(7) . . . . ?
C44 C39 C40 C41 2.4(5) . . . . ?
B1 C39 C40 C41 -173.3(3) . . . . ?
C39 C40 C41 C42 -0.4(6) . . . . ?
C40 C41 C42 C43 -1.3(6) . . . . ?
C41 C42 C43 C44 0.9(6) . . . . ?
C42 C43 C44 C39 1.3(5) . . . . ?
C40 C39 C44 C43 -2.9(5) . . . . ?
B1 C39 C44 C43 172.9(3) . . . . ?
O3 C45 C46 C47 -22.0(7) . . . . ?
C45 C46 C47 C48 13.4(8) . . . . ?
C46 C47 C48 O3 -0.5(8) . . . . ?
C40 C39 B1 C27 100.5(4) . . . . ?
C44 C39 B1 C27 -74.9(4) . . . . ?
C40 C39 B1 C33 -19.9(4) . . . . ?
C44 C39 B1 C33 164.7(3) . . . . ?
C40 C39 B1 C21 -138.9(3) . . . . ?
C44 C39 B1 C21 45.7(4) . . . . ?
C28 C27 B1 C39 13.9(4) . . . . ?
C32 C27 B1 C39 -166.7(3) . . . . ?
C28 C27 B1 C33 134.0(3) . . . . ?
C32 C27 B1 C33 -46.6(4) . . . . ?
C28 C27 B1 C21 -106.7(4) . . . . ?
C32 C27 B1 C21 72.7(4) . . . . ?
C38 C33 B1 C39 -81.3(4) . . . . ?
C34 C33 B1 C39 93.4(4) . . . . ?
C38 C33 B1 C27 159.2(3) . . . . ?
C34 C33 B1 C27 -26.1(5) . . . . ?
C38 C33 B1 C21 38.7(4) . . . . ?
C34 C33 B1 C21 -146.6(4) . . . . ?
C22 C21 B1 C39 34.2(4) . . . . ?
C26 C21 B1 C39 -148.9(3) . . . . ?
C22 C21 B1 C27 153.9(3) . . . . ?
C26 C21 B1 C27 -29.2(4) . . . . ?
C22 C21 B1 C33 -85.6(4) . . . . ?
C26 C21 B1 C33 91.3(4) . . . . ?
C10 C9 N2 C1 66.7(4) . . . . ?
C10 C9 N2 C5 -171.3(3) . . . . ?
C10 C9 N2 Pd1 -52.8(4) . . . . ?
C2 C1 N2 C9 -160.6(3) . . . . ?
C2 C1 N2 C5 78.1(3) . . . . ?
C2 C1 N2 Pd1 -35.5(3) . . . . ?
C6 C5 N2 C9 -56.2(4) . . . . ?
C6 C5 N2 C1 65.8(4) . . . . ?
C6 C5 N2 Pd1 179.5(3) . . . . ?
C4 C3 N3 C2 166.8(3) . . . . ?
C4 C3 N3 Pd1 45.7(3) . . . . ?
C1 C2 N3 C3 -167.1(3) . . . . ?
C1 C2 N3 Pd1 -45.9(3) . . . . ?
C18 C17 N4 C4 -69.0(4) . . . . ?
C18 C17 N4 C13 168.8(3) . . . . ?
C18 C17 N4 Pd1 50.1(4) . . . . ?
C3 C4 N4 C17 159.0(3) . . . . ?
C3 C4 N4 C13 -79.0(3) . . . . ?
C3 C4 N4 Pd1 33.6(3) . . . . ?
C14 C13 N4 C17 56.5(4) . . . . ?
C14 C13 N4 C4 -65.2(4) . . . . ?
C14 C13 N4 Pd1 -178.2(3) . . . . ?
C47 C48 O3 C45 -13.4(6) . . . . ?
C46 C45 O3 C48 22.2(6) . . . . ?

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
C5 H5B O1 0.97 2.62 3.413(5) 138.8 .
C13 H13A O1 0.97 2.60 3.389(5) 138.5 .
N3 H3 O3 0.973(19) 1.96(2) 2.916(4) 167(4) .

_refine_diff_density_max         0.497
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.061

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_1minUV
_database_code_depnum_ccdc_archive 'CCDC 1441781'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_1minUV              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially excited nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_1minUV              
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         17 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5238(7)
_cell_length_b                   13.4068(5)
_cell_length_c                   29.8526(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.231(5)
_cell_angle_gamma                90
_cell_volume                     4592.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3211
_cell_measurement_theta_min      3.2180
_cell_measurement_theta_max      29.0070

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85188
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            19311
_diffrn_reflns_av_unetI/netI     0.1116
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.134
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9343
_reflns_number_gt                6075
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0415P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9343
_refine_ls_number_parameters     504
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1061
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1117
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
C1 C 0.5489(4) 0.9629(3) 0.62875(12) 0.0191(9) Uani 1 1 d . . . . .
H1A H 0.5603 1.0340 0.6213 0.023 Uiso 1 1 calc R U . . .
H1B H 0.4740 0.9566 0.6423 0.023 Uiso 1 1 calc R U . . .
C2 C 0.5455(4) 0.9003(3) 0.58621(12) 0.0206(9) Uani 1 1 d . . . . .
H2A H 0.4769 0.9183 0.5654 0.025 Uiso 1 1 calc R U . . .
H2B H 0.6168 0.9115 0.5707 0.025 Uiso 1 1 calc R U . . .
C3 C 0.5598(3) 0.7180(3) 0.56611(11) 0.0162(8) Uani 1 1 d . . . . .
H3A H 0.6301 0.7352 0.5510 0.019 Uiso 1 1 calc R U . . .
H3B H 0.4924 0.7137 0.5431 0.019 Uiso 1 1 calc R U . . .
C4 C 0.5771(3) 0.6198(2) 0.59124(12) 0.0149(9) Uani 1 1 d . . . . .
H4A H 0.5032 0.6000 0.6032 0.018 Uiso 1 1 calc R U . . .
H4B H 0.5983 0.5672 0.5702 0.018 Uiso 1 1 calc R U . . .
C5 C 0.7626(4) 0.9673(3) 0.64944(13) 0.0208(9) Uani 1 1 d . . . . .
H5A H 0.7713 0.9478 0.6179 0.025 Uiso 1 1 calc R U . . .
H5B H 0.8254 0.9337 0.6686 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7816(4) 1.0797(3) 0.65357(14) 0.0257(10) Uani 1 1 d . . . . .
H6A H 0.7187 1.1148 0.6350 0.031 Uiso 1 1 calc R U . . .
H6B H 0.7780 1.1001 0.6853 0.031 Uiso 1 1 calc R U . . .
C7 C 0.8980(4) 1.1091(3) 0.63832(14) 0.0295(11) Uani 1 1 d . . . . .
H7A H 0.8972 1.0979 0.6055 0.035 Uiso 1 1 calc R U . . .
H7B H 0.9597 1.0664 0.6535 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9261(4) 1.2182(3) 0.64878(16) 0.0390(12) Uani 1 1 d . . . . .
H8A H 0.9362 1.2278 0.6814 0.058 Uiso 1 1 calc R U . . .
H8B H 0.8621 1.2603 0.6358 0.058 Uiso 1 1 calc R U . . .
H8C H 0.9982 1.2367 0.6358 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6275(4) 0.9624(3) 0.70829(12) 0.0175(9) Uani 1 1 d . . . . .
H9A H 0.6184 1.0358 0.7077 0.021 Uiso 1 1 calc R U . . .
H9B H 0.6981 0.9469 0.7286 0.021 Uiso 1 1 calc R U . . .
C10 C 0.5234(4) 0.9177(3) 0.72811(12) 0.0202(9) Uani 1 1 d . . . . .
H10A H 0.5257 0.8441 0.7253 0.024 Uiso 1 1 calc R U . . .
H10B H 0.4510 0.9418 0.7112 0.024 Uiso 1 1 calc R U . . .
C11 C 0.5225(4) 0.9461(3) 0.77755(13) 0.0244(10) Uani 1 1 d . . . . .
H11A H 0.5885 0.9127 0.7951 0.029 Uiso 1 1 calc R U . . .
H11B H 0.5342 1.0190 0.7807 0.029 Uiso 1 1 calc R U . . .
C12 C 0.4103(4) 0.9177(3) 0.79700(14) 0.0335(11) Uani 1 1 d . . . . .
H12A H 0.4161 0.9345 0.8291 0.050 Uiso 1 1 calc R U . . .
H12B H 0.3971 0.8459 0.7933 0.050 Uiso 1 1 calc R U . . .
H12C H 0.3452 0.9544 0.7813 0.050 Uiso 1 1 calc R U . . .
C13 C 0.7902(3) 0.6235(3) 0.61263(12) 0.0169(9) Uani 1 1 d . . . . .
H13A H 0.8481 0.6373 0.6385 0.020 Uiso 1 1 calc R U . . .
H13B H 0.7965 0.6779 0.5906 0.020 Uiso 1 1 calc R U . . .
C14 C 0.8243(4) 0.5263(3) 0.59091(13) 0.0197(9) Uani 1 1 d . . . . .
H14A H 0.8217 0.4714 0.6129 0.024 Uiso 1 1 calc R U . . .
H14B H 0.7671 0.5112 0.5650 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9450(4) 0.5318(3) 0.57495(13) 0.0223(9) Uani 1 1 d . . . . .
H15A H 1.0014 0.5486 0.6009 0.027 Uiso 1 1 calc R U . . .
H15B H 0.9467 0.5866 0.5528 0.027 Uiso 1 1 calc R U . . .
C16 C 0.9838(4) 0.4363(3) 0.55372(13) 0.0257(10) Uani 1 1 d . . . . .
H16A H 1.0624 0.4453 0.5443 0.039 Uiso 1 1 calc R U . . .
H16B H 0.9298 0.4200 0.5275 0.039 Uiso 1 1 calc R U . . .
H16C H 0.9844 0.3820 0.5757 0.039 Uiso 1 1 calc R U . . .
C17 C 0.6579(4) 0.5469(3) 0.66244(11) 0.0161(9) Uani 1 1 d . . . . .
H17A H 0.7267 0.5480 0.6848 0.019 Uiso 1 1 calc R U . . .
H17B H 0.6579 0.4821 0.6466 0.019 Uiso 1 1 calc R U . . .
C18 C 0.5493(4) 0.5529(3) 0.68719(13) 0.0232(10) Uani 1 1 d . . . . .
H18A H 0.5471 0.6185 0.7024 0.028 Uiso 1 1 calc R U . . .
H18B H 0.4798 0.5482 0.6652 0.028 Uiso 1 1 calc R U . . .
C19 C 0.5446(4) 0.4722(3) 0.72123(16) 0.0406(13) Uani 1 1 d . . . . .
H19A H 0.5603 0.4078 0.7067 0.049 Uiso 1 1 calc R U . . .
H19B H 0.6081 0.4835 0.7453 0.049 Uiso 1 1 calc R U . . .
C20 C 0.4334(4) 0.4632(3) 0.74228(15) 0.0372(12) Uani 1 1 d . . . . .
H20A H 0.4425 0.4144 0.7668 0.056 Uiso 1 1 calc R U . . .
H20B H 0.3718 0.4410 0.7197 0.056 Uiso 1 1 calc R U . . .
H20C H 0.4125 0.5282 0.7543 0.056 Uiso 1 1 calc R U . . .
C21 C 0.4904(3) 0.2315(3) 0.55704(11) 0.0148(8) Uani 1 1 d . . . . .
C22 C 0.5842(4) 0.2964(3) 0.56703(13) 0.0209(9) Uani 1 1 d . . . . .
H22 H 0.5705 0.3568 0.5824 0.025 Uiso 1 1 calc R U . . .
C23 C 0.6962(4) 0.2775(3) 0.55580(13) 0.0231(9) Uani 1 1 d . . . . .
H23 H 0.7562 0.3249 0.5632 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7212(4) 0.1902(3) 0.53395(13) 0.0222(9) Uani 1 1 d . . . . .
H24 H 0.7979 0.1765 0.5264 0.027 Uiso 1 1 calc R U . . .
C25 C 0.6312(4) 0.1234(3) 0.52343(12) 0.0181(9) Uani 1 1 d . . . . .
H25 H 0.6461 0.0627 0.5085 0.022 Uiso 1 1 calc R U . . .
C26 C 0.5203(4) 0.1443(3) 0.53446(12) 0.0176(9) Uani 1 1 d . . . . .
H26 H 0.4605 0.0971 0.5264 0.021 Uiso 1 1 calc R U . . .
C27 C 0.2598(4) 0.1994(3) 0.53771(12) 0.0170(9) Uani 1 1 d . . . . .
C28 C 0.1860(4) 0.2488(3) 0.50547(12) 0.0197(9) Uani 1 1 d . . . . .
H28 H 0.1909 0.3194 0.5036 0.024 Uiso 1 1 calc R U . . .
C29 C 0.1053(4) 0.1993(3) 0.47589(13) 0.0252(10) Uani 1 1 d . . . . .
H29 H 0.0575 0.2361 0.4542 0.030 Uiso 1 1 calc R U . . .
C30 C 0.0944(4) 0.0974(3) 0.47786(14) 0.0254(10) Uani 1 1 d . . . . .
H30 H 0.0400 0.0634 0.4575 0.030 Uiso 1 1 calc R U . . .
C31 C 0.1635(4) 0.0454(3) 0.50993(14) 0.0262(10) Uani 1 1 d . . . . .
H31 H 0.1560 -0.0250 0.5122 0.031 Uiso 1 1 calc R U . . .
C32 C 0.2442(4) 0.0960(3) 0.53885(13) 0.0211(9) Uani 1 1 d . . . . .
H32 H 0.2913 0.0585 0.5605 0.025 Uiso 1 1 calc R U . . .
C33 C 0.3528(4) 0.2111(2) 0.62417(12) 0.0200(9) Uani 1 1 d . . . . .
C34 C 0.2512(4) 0.1727(3) 0.63881(14) 0.0301(11) Uani 1 1 d . . . . .
H34 H 0.1848 0.1662 0.6177 0.036 Uiso 1 1 calc R U . . .
C35 C 0.2420(5) 0.1433(3) 0.68298(14) 0.0358(12) Uani 1 1 d . . . . .
H35 H 0.1705 0.1171 0.6914 0.043 Uiso 1 1 calc R U . . .
C36 C 0.3357(4) 0.1519(3) 0.71439(14) 0.0308(11) Uani 1 1 d . . . . .
H36 H 0.3295 0.1321 0.7446 0.037 Uiso 1 1 calc R U . . .
C37 C 0.4397(4) 0.1898(3) 0.70171(13) 0.0266(10) Uani 1 1 d . . . . .
H37 H 0.5054 0.1966 0.7231 0.032 Uiso 1 1 calc R U . . .
C38 C 0.4465(4) 0.2178(3) 0.65698(12) 0.0221(9) Uani 1 1 d . . . . .
H38 H 0.5186 0.2425 0.6485 0.027 Uiso 1 1 calc R U . . .
C39 C 0.3365(3) 0.3755(3) 0.57282(12) 0.0172(9) Uani 1 1 d . . . . .
C40 C 0.2880(4) 0.4248(3) 0.60763(13) 0.0217(9) Uani 1 1 d . . . . .
H40 H 0.2729 0.3883 0.6337 0.026 Uiso 1 1 calc R U . . .
C41 C 0.2608(4) 0.5261(3) 0.60542(14) 0.0285(11) Uani 1 1 d . . . . .
H41 H 0.2287 0.5574 0.6300 0.034 Uiso 1 1 calc R U . . .
C42 C 0.2802(4) 0.5810(3) 0.56789(15) 0.0296(11) Uani 1 1 d . . . . .
H42 H 0.2593 0.6495 0.5659 0.036 Uiso 1 1 calc R U . . .
C43 C 0.3304(4) 0.5350(3) 0.53321(14) 0.0244(10) Uani 1 1 d . . . . .
H43 H 0.3460 0.5723 0.5074 0.029 Uiso 1 1 calc R U . . .
C44 C 0.3584(4) 0.4340(3) 0.53591(13) 0.0220(10) Uani 1 1 d . . . . .
H44 H 0.3937 0.4039 0.5117 0.026 Uiso 1 1 calc R U . . .
C45 C 0.2657(4) 0.7627(3) 0.67531(15) 0.0383(8) Uani 1 1 d . . . . .
H45A H 0.2843 0.8042 0.7024 0.046 Uiso 1 1 calc R U . . .
H45B H 0.2978 0.6949 0.6812 0.046 Uiso 1 1 calc R U . . .
C46 C 0.1348(4) 0.7583(3) 0.66309(15) 0.0385(8) Uani 1 1 d . . . . .
H46A H 0.1124 0.6985 0.6448 0.046 Uiso 1 1 calc R U . . .
H46B H 0.0915 0.7588 0.6903 0.046 Uiso 1 1 calc R U . . .
C47 C 0.1144(4) 0.8533(3) 0.63599(15) 0.0385(8) Uani 1 1 d . . . . .
H47A H 0.0461 0.8465 0.6136 0.046 Uiso 1 1 calc R U . . .
H47B H 0.1020 0.9108 0.6558 0.046 Uiso 1 1 calc R U . . .
C48 C 0.2229(4) 0.8652(3) 0.61374(16) 0.0383(8) Uani 1 1 d . . . . .
H48A H 0.2101 0.8433 0.5820 0.046 Uiso 1 1 calc R U . . .
H48B H 0.2464 0.9362 0.6142 0.046 Uiso 1 1 calc R U . . .
B1 B 0.3603(4) 0.2543(3) 0.57255(14) 0.0172(10) Uani 1 1 d . . . . .
N2 N 0.6474(3) 0.9282(2) 0.66197(10) 0.0173(7) Uani 1 1 d . . . . .
N3 N 0.5382(3) 0.7942(2) 0.60049(10) 0.0148(7) Uani 1 1 d D . . . .
N4 N 0.6705(3) 0.6283(2) 0.62907(9) 0.0131(7) Uani 1 1 d . . . . .
O3 O 0.3126(3) 0.8063(2) 0.63712(9) 0.0327(7) Uani 1 1 d . . . . .
Pd1 Pd 0.65678(3) 0.77399(2) 0.65349(2) 0.01424(9) Uani 1 1 d . . . . .
N1_a N 0.7720(5) 0.7524(4) 0.7077(2) 0.0209(16) Uiso 0.745(5) 1 d D . P A 1
O1_a O 0.8745(4) 0.7622(3) 0.70394(13) 0.0369(8) Uiso 0.745(5) 1 d D . P A 1
O2_a O 0.7365(4) 0.7276(4) 0.74415(16) 0.0369(8) Uiso 0.745(5) 1 d D . P A 1
N1A_b N 0.7824(12) 0.7296(11) 0.7413(4) 0.0209(16) Uiso 0.255(5) 1 d D . P A 2
O1A_b O 0.7948(16) 0.7583(11) 0.6995(4) 0.027(4) Uiso 0.255(5) 1 d D . P A 2
O2A_b O 0.6754(11) 0.7152(9) 0.7461(4) 0.0369(8) Uiso 0.255(5) 1 d D . P A 2
H3 H 0.460(2) 0.785(3) 0.6088(14) 0.044 Uiso 1 1 d D 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
C1 N2 1.511(5) . ?
C1 C2 1.519(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.491(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.484(4) . ?
C3 C4 1.520(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.492(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.507(5) . ?
C5 C6 1.525(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.508(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.524(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.494(4) . ?
C9 C10 1.510(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.525(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.513(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.507(5) . ?
C13 C14 1.523(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.513(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.514(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.494(4) . ?
C17 C18 1.512(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.489(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.482(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.399(5) . ?
C21 C26 1.408(5) . ?
C21 B1 1.637(6) . ?
C22 C23 1.385(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.392(5) . ?
C27 C32 1.400(5) . ?
C27 B1 1.656(6) . ?
C28 C29 1.391(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.373(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.378(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.387(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.386(6) . ?
C33 C38 1.393(5) . ?
C33 B1 1.655(5) . ?
C34 C35 1.390(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.369(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.385(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.396(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.391(5) . ?
C39 C44 1.394(5) . ?
C39 B1 1.648(5) . ?
C40 C41 1.393(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.376(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.377(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.393(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.430(5) . ?
C45 C46 1.521(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.516(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.477(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.431(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N2 Pd1 2.086(3) . ?
N3 Pd1 2.013(3) . ?
N3 H3 0.966(19) . ?
N4 Pd1 2.096(3) . ?
Pd1 O1A_b 2.015(17) . ?
Pd1 N1_a 2.018(6) . ?
N1_a O1_a 1.203(8) . ?
N1_a O2_a 1.243(7) . ?
N1A_b O2A_b 1.269(14) . ?
N1A_b O1A_b 1.325(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 109.8(3) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.6(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.1(3) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.1(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.6(3) . . ?
N2 C5 H5A 108.2 . . ?
C6 C5 H5A 108.2 . . ?
N2 C5 H5B 108.2 . . ?
C6 C5 H5B 108.2 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.0(3) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 111.5(4) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.8(3) . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.9(4) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.0(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.9(3) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 113.9(3) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.0(3) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C19 C18 C17 112.2(3) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 115.8(4) . . ?
C20 C19 H19A 108.3 . . ?
C18 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C18 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 113.6(4) . . ?
C22 C21 B1 122.3(3) . . ?
C26 C21 B1 124.1(3) . . ?
C23 C22 C21 123.6(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.5(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.1(4) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 123.8(4) . . ?
C25 C26 H26 118.1 . . ?
C21 C26 H26 118.1 . . ?
C28 C27 C32 114.6(3) . . ?
C28 C27 B1 124.9(3) . . ?
C32 C27 B1 120.6(3) . . ?
C29 C28 C27 122.9(3) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 118.9(4) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 119.8(4) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C27 123.3(4) . . ?
C31 C32 H32 118.3 . . ?
C27 C32 H32 118.3 . . ?
C34 C33 C38 115.1(3) . . ?
C34 C33 B1 122.7(4) . . ?
C38 C33 B1 122.0(4) . . ?
C33 C34 C35 123.0(4) . . ?
C33 C34 H34 118.5 . . ?
C35 C34 H34 118.5 . . ?
C36 C35 C34 120.1(5) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 119.5(4) . . ?
C35 C36 H36 120.3 . . ?
C37 C36 H36 120.3 . . ?
C36 C37 C38 119.0(4) . . ?
C36 C37 H37 120.5 . . ?
C38 C37 H37 120.5 . . ?
C33 C38 C37 123.2(4) . . ?
C33 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
C40 C39 C44 115.9(3) . . ?
C40 C39 B1 123.4(3) . . ?
C44 C39 B1 120.6(3) . . ?
C39 C40 C41 122.1(4) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C42 C41 C40 120.5(4) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 118.9(4) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 120.2(4) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C39 122.3(4) . . ?
C43 C44 H44 118.8 . . ?
C39 C44 H44 118.8 . . ?
O3 C45 C46 105.3(4) . . ?
O3 C45 H45A 110.7 . . ?
C46 C45 H45A 110.7 . . ?
O3 C45 H45B 110.7 . . ?
C46 C45 H45B 110.7 . . ?
H45A C45 H45B 108.8 . . ?
C47 C46 C45 101.4(4) . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46B 111.5 . . ?
C45 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 103.6(4) . . ?
C48 C47 H47A 111.0 . . ?
C46 C47 H47A 111.0 . . ?
C48 C47 H47B 111.0 . . ?
C46 C47 H47B 111.0 . . ?
H47A C47 H47B 109.0 . . ?
O3 C48 C47 108.9(4) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C21 B1 C39 110.0(3) . . ?
C21 B1 C33 108.9(3) . . ?
C39 B1 C33 108.5(3) . . ?
C21 B1 C27 110.2(3) . . ?
C39 B1 C27 109.5(3) . . ?
C33 B1 C27 109.7(3) . . ?
C9 N2 C5 109.6(3) . . ?
C9 N2 C1 110.1(3) . . ?
C5 N2 C1 110.8(3) . . ?
C9 N2 Pd1 115.5(2) . . ?
C5 N2 Pd1 105.0(2) . . ?
C1 N2 Pd1 105.7(2) . . ?
C3 N3 C2 116.2(3) . . ?
C3 N3 Pd1 107.9(2) . . ?
C2 N3 Pd1 107.5(2) . . ?
C3 N3 H3 108(3) . . ?
C2 N3 H3 106(2) . . ?
Pd1 N3 H3 111(3) . . ?
C4 N4 C17 109.9(3) . . ?
C4 N4 C13 111.7(3) . . ?
C17 N4 C13 109.5(3) . . ?
C4 N4 Pd1 105.2(2) . . ?
C17 N4 Pd1 115.7(2) . . ?
C13 N4 Pd1 104.7(2) . . ?
C45 O3 C48 107.8(3) . . ?
N3 Pd1 O1A_b 170.7(4) . . ?
N3 Pd1 N1_a 178.4(2) . . ?
N3 Pd1 N2 85.59(12) . . ?
O1A_b Pd1 N2 93.9(4) . . ?
N1_a Pd1 N2 94.74(18) . . ?
N3 Pd1 N4 85.37(11) . . ?
O1A_b Pd1 N4 93.4(4) . . ?
N1_a Pd1 N4 94.59(18) . . ?
N2 Pd1 N4 166.36(11) . . ?
O1_a N1_a O2_a 121.0(6) . . ?
O1_a N1_a Pd1 119.3(4) . . ?
O2_a N1_a Pd1 119.7(5) . . ?
O2A_b N1A_b O1A_b 109.9(14) . . ?
N1A_b O1A_b Pd1 121.7(14) . . ?

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
N2 C1 C2 N3 54.8(4) . . . . ?
N3 C3 C4 N4 -54.4(4) . . . . ?
N2 C5 C6 C7 -177.8(3) . . . . ?
C5 C6 C7 C8 -171.5(3) . . . . ?
N2 C9 C10 C11 171.6(3) . . . . ?
C9 C10 C11 C12 170.6(3) . . . . ?
N4 C13 C14 C15 178.7(3) . . . . ?
C13 C14 C15 C16 179.1(3) . . . . ?
N4 C17 C18 C19 -177.6(4) . . . . ?
C17 C18 C19 C20 -171.3(4) . . . . ?
C26 C21 C22 C23 0.2(5) . . . . ?
B1 C21 C22 C23 177.6(3) . . . . ?
C21 C22 C23 C24 -0.7(6) . . . . ?
C22 C23 C24 C25 0.5(6) . . . . ?
C23 C24 C25 C26 0.2(6) . . . . ?
C24 C25 C26 C21 -0.8(6) . . . . ?
C22 C21 C26 C25 0.6(5) . . . . ?
B1 C21 C26 C25 -176.7(3) . . . . ?
C32 C27 C28 C29 -1.7(5) . . . . ?
B1 C27 C28 C29 177.8(4) . . . . ?
C27 C28 C29 C30 0.9(6) . . . . ?
C28 C29 C30 C31 0.7(6) . . . . ?
C29 C30 C31 C32 -1.4(6) . . . . ?
C30 C31 C32 C27 0.4(6) . . . . ?
C28 C27 C32 C31 1.1(5) . . . . ?
B1 C27 C32 C31 -178.5(4) . . . . ?
C38 C33 C34 C35 0.4(6) . . . . ?
B1 C33 C34 C35 -175.1(4) . . . . ?
C33 C34 C35 C36 0.2(6) . . . . ?
C34 C35 C36 C37 -0.3(6) . . . . ?
C35 C36 C37 C38 -0.4(6) . . . . ?
C34 C33 C38 C37 -1.1(5) . . . . ?
B1 C33 C38 C37 174.4(3) . . . . ?
C36 C37 C38 C33 1.1(6) . . . . ?
C44 C39 C40 C41 1.2(6) . . . . ?
B1 C39 C40 C41 -175.1(4) . . . . ?
C39 C40 C41 C42 0.8(6) . . . . ?
C40 C41 C42 C43 -2.1(6) . . . . ?
C41 C42 C43 C44 1.4(6) . . . . ?
C42 C43 C44 C39 0.6(6) . . . . ?
C40 C39 C44 C43 -1.9(6) . . . . ?
B1 C39 C44 C43 174.5(4) . . . . ?
O3 C45 C46 C47 -35.5(4) . . . . ?
C45 C46 C47 C48 32.4(5) . . . . ?
C46 C47 C48 O3 -18.9(5) . . . . ?
C22 C21 B1 C39 32.3(5) . . . . ?
C26 C21 B1 C39 -150.5(3) . . . . ?
C22 C21 B1 C33 -86.4(4) . . . . ?
C26 C21 B1 C33 90.7(4) . . . . ?
C22 C21 B1 C27 153.2(3) . . . . ?
C26 C21 B1 C27 -29.7(5) . . . . ?
C40 C39 B1 C21 -134.7(4) . . . . ?
C44 C39 B1 C21 49.2(5) . . . . ?
C40 C39 B1 C33 -15.7(5) . . . . ?
C44 C39 B1 C33 168.2(4) . . . . ?
C40 C39 B1 C27 104.0(4) . . . . ?
C44 C39 B1 C27 -72.1(5) . . . . ?
C34 C33 B1 C21 -146.8(4) . . . . ?
C38 C33 B1 C21 38.0(4) . . . . ?
C34 C33 B1 C39 93.5(4) . . . . ?
C38 C33 B1 C39 -81.7(4) . . . . ?
C34 C33 B1 C27 -26.1(5) . . . . ?
C38 C33 B1 C27 158.7(3) . . . . ?
C28 C27 B1 C21 -106.1(4) . . . . ?
C32 C27 B1 C21 73.4(4) . . . . ?
C28 C27 B1 C39 15.1(5) . . . . ?
C32 C27 B1 C39 -165.5(3) . . . . ?
C28 C27 B1 C33 134.0(4) . . . . ?
C32 C27 B1 C33 -46.5(4) . . . . ?
C10 C9 N2 C5 -172.0(3) . . . . ?
C10 C9 N2 C1 65.8(4) . . . . ?
C10 C9 N2 Pd1 -53.7(4) . . . . ?
C6 C5 N2 C9 -54.0(4) . . . . ?
C6 C5 N2 C1 67.7(4) . . . . ?
C6 C5 N2 Pd1 -178.6(3) . . . . ?
C2 C1 N2 C9 -160.4(3) . . . . ?
C2 C1 N2 C5 78.2(4) . . . . ?
C2 C1 N2 Pd1 -35.0(3) . . . . ?
C4 C3 N3 C2 166.4(3) . . . . ?
C4 C3 N3 Pd1 45.7(3) . . . . ?
C1 C2 N3 C3 -167.1(3) . . . . ?
C1 C2 N3 Pd1 -46.2(3) . . . . ?
C3 C4 N4 C17 159.8(3) . . . . ?
C3 C4 N4 C13 -78.4(3) . . . . ?
C3 C4 N4 Pd1 34.6(3) . . . . ?
C18 C17 N4 C4 -66.3(4) . . . . ?
C18 C17 N4 C13 170.7(3) . . . . ?
C18 C17 N4 Pd1 52.6(4) . . . . ?
C14 C13 N4 C4 -64.3(4) . . . . ?
C14 C13 N4 C17 57.7(4) . . . . ?
C14 C13 N4 Pd1 -177.6(3) . . . . ?
C46 C45 O3 C48 24.9(4) . . . . ?
C47 C48 O3 C45 -3.8(5) . . . . ?
O2A_b N1A_b O1A_b Pd1 0.0(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
C5 H5B O1_a 0.99 2.57 3.389(6) 140.1 .
C5 H5B O1A_b 0.99 2.56 3.182(15) 120.6 .
C10 H10A O2A_b 0.99 2.48 3.248(13) 134.1 .
C13 H13A O1_a 0.99 2.57 3.369(5) 137.6 .
C18 H18A O2A_b 0.99 2.28 3.078(13) 136.3 .
C46 H46B O1_a 0.99 2.57 3.340(7) 134.5 1_455
N3 H3 O3 0.966(19) 1.98(2) 2.915(4) 161(4) .

_refine_diff_density_max         0.881
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.104

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_2minUV
_database_code_depnum_ccdc_archive 'CCDC 1441782'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_2minUV              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially excited nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_2minUV              
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         17 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5241(6)
_cell_length_b                   13.4062(4)
_cell_length_c                   29.8989(11)
_cell_angle_alpha                90
_cell_angle_beta                 95.061(4)
_cell_angle_gamma                90
_cell_volume                     4601.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3850
_cell_measurement_theta_min      3.2100
_cell_measurement_theta_max      28.9450

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.447
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            19330
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.130
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9353
_reflns_number_gt                6371
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0377P)²+1.5210P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9353
_refine_ls_number_parameters     504
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.0898
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.010
_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
C1 C 0.5486(4) 0.9627(2) 0.62856(11) 0.0215(9) Uani 1 1 d . . . . .
H1A H 0.5597 1.0338 0.6210 0.026 Uiso 1 1 calc R U . . .
H1B H 0.4738 0.9562 0.6422 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5452(3) 0.9001(2) 0.58617(11) 0.0198(8) Uani 1 1 d . . . . .
H2A H 0.4767 0.9180 0.5654 0.024 Uiso 1 1 calc R U . . .
H2B H 0.6165 0.9110 0.5706 0.024 Uiso 1 1 calc R U . . .
C3 C 0.5600(3) 0.7179(2) 0.56605(10) 0.0163(8) Uani 1 1 d . . . . .
H3A H 0.6306 0.7352 0.5511 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4931 0.7135 0.5430 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5770(3) 0.6199(2) 0.59103(11) 0.0164(8) Uani 1 1 d . . . . .
H4A H 0.5030 0.6002 0.6031 0.020 Uiso 1 1 calc R U . . .
H4B H 0.5981 0.5672 0.5700 0.020 Uiso 1 1 calc R U . . .
C5 C 0.7624(3) 0.9674(2) 0.64894(12) 0.0222(9) Uani 1 1 d . . . . .
H5A H 0.7713 0.9474 0.6176 0.027 Uiso 1 1 calc R U . . .
H5B H 0.8248 0.9337 0.6682 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7825(4) 1.0795(2) 0.65270(13) 0.0253(9) Uani 1 1 d . . . . .
H6A H 0.7202 1.1148 0.6340 0.030 Uiso 1 1 calc R U . . .
H6B H 0.7783 1.1005 0.6843 0.030 Uiso 1 1 calc R U . . .
C7 C 0.8993(4) 1.1086(3) 0.63766(13) 0.0288(9) Uani 1 1 d . . . . .
H7A H 0.8994 1.0968 0.6050 0.035 Uiso 1 1 calc R U . . .
H7B H 0.9607 1.0663 0.6532 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9265(4) 1.2183(3) 0.64782(15) 0.0398(11) Uani 1 1 d . . . . .
H8A H 0.9354 1.2285 0.6804 0.060 Uiso 1 1 calc R U . . .
H8B H 0.8625 1.2599 0.6345 0.060 Uiso 1 1 calc R U . . .
H8C H 0.9989 1.2368 0.6351 0.060 Uiso 1 1 calc R U . . .
C9 C 0.6279(3) 0.9620(2) 0.70815(11) 0.0172(8) Uani 1 1 d . . . . .
H9A H 0.6206 1.0356 0.7081 0.021 Uiso 1 1 calc R U . . .
H9B H 0.6979 0.9446 0.7283 0.021 Uiso 1 1 calc R U . . .
C10 C 0.5225(3) 0.9185(2) 0.72761(11) 0.0196(8) Uani 1 1 d . . . . .
H10A H 0.5233 0.8450 0.7246 0.024 Uiso 1 1 calc R U . . .
H10B H 0.4508 0.9441 0.7108 0.024 Uiso 1 1 calc R U . . .
C11 C 0.5224(4) 0.9464(3) 0.77689(11) 0.0247(9) Uani 1 1 d . . . . .
H11A H 0.5889 0.9130 0.7940 0.030 Uiso 1 1 calc R U . . .
H11B H 0.5341 1.0193 0.7801 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4113(4) 0.9180(3) 0.79708(13) 0.0350(11) Uani 1 1 d . . . . .
H12A H 0.4187 0.9338 0.8292 0.052 Uiso 1 1 calc R U . . .
H12B H 0.3972 0.8464 0.7930 0.052 Uiso 1 1 calc R U . . .
H12C H 0.3459 0.9555 0.7821 0.052 Uiso 1 1 calc R U . . .
C13 C 0.7906(3) 0.6238(2) 0.61240(11) 0.0179(8) Uani 1 1 d . . . . .
H13A H 0.8485 0.6379 0.6381 0.022 Uiso 1 1 calc R U . . .
H13B H 0.7967 0.6780 0.5902 0.022 Uiso 1 1 calc R U . . .
C14 C 0.8248(3) 0.5263(2) 0.59089(12) 0.0197(8) Uani 1 1 d . . . . .
H14A H 0.8225 0.4716 0.6130 0.024 Uiso 1 1 calc R U . . .
H14B H 0.7677 0.5108 0.5651 0.024 Uiso 1 1 calc R U . . .
C15 C 0.9460(3) 0.5325(2) 0.57478(12) 0.0216(8) Uani 1 1 d . . . . .
H15A H 0.9475 0.5873 0.5526 0.026 Uiso 1 1 calc R U . . .
H15B H 1.0023 0.5493 0.6006 0.026 Uiso 1 1 calc R U . . .
C16 C 0.9848(4) 0.4368(3) 0.55346(12) 0.0254(9) Uani 1 1 d . . . . .
H16A H 1.0637 0.4455 0.5442 0.038 Uiso 1 1 calc R U . . .
H16B H 0.9312 0.4209 0.5271 0.038 Uiso 1 1 calc R U . . .
H16C H 0.9846 0.3822 0.5753 0.038 Uiso 1 1 calc R U . . .
C17 C 0.6576(3) 0.5473(2) 0.66253(11) 0.0177(8) Uani 1 1 d . . . . .
H17A H 0.7253 0.5497 0.6853 0.021 Uiso 1 1 calc R U . . .
H17B H 0.6600 0.4823 0.6469 0.021 Uiso 1 1 calc R U . . .
C18 C 0.5482(4) 0.5514(3) 0.68642(12) 0.0257(9) Uani 1 1 d . . . . .
H18A H 0.5410 0.6185 0.6997 0.031 Uiso 1 1 calc R U . . .
H18B H 0.4801 0.5409 0.6643 0.031 Uiso 1 1 calc R U . . .
C19 C 0.5467(4) 0.4749(3) 0.72258(14) 0.0371(11) Uani 1 1 d . . . . .
H19A H 0.5687 0.4097 0.7102 0.045 Uiso 1 1 calc R U . . .
H19B H 0.6069 0.4926 0.7470 0.045 Uiso 1 1 calc R U . . .
C20 C 0.4334(4) 0.4630(3) 0.74231(14) 0.0388(11) Uani 1 1 d . . . . .
H20A H 0.4437 0.4188 0.7685 0.058 Uiso 1 1 calc R U . . .
H20B H 0.3761 0.4341 0.7199 0.058 Uiso 1 1 calc R U . . .
H20C H 0.4060 0.5284 0.7516 0.058 Uiso 1 1 calc R U . . .
C21 C 0.4913(3) 0.2311(2) 0.55700(10) 0.0152(7) Uani 1 1 d . . . . .
C22 C 0.5853(3) 0.2965(2) 0.56689(11) 0.0212(8) Uani 1 1 d . . . . .
H22 H 0.5714 0.3568 0.5822 0.025 Uiso 1 1 calc R U . . .
C23 C 0.6971(3) 0.2776(3) 0.55546(12) 0.0234(8) Uani 1 1 d . . . . .
H23 H 0.7572 0.3248 0.5627 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7216(3) 0.1903(3) 0.53349(12) 0.0224(8) Uani 1 1 d . . . . .
H24 H 0.7981 0.1766 0.5256 0.027 Uiso 1 1 calc R U . . .
C25 C 0.6313(3) 0.1232(2) 0.52322(11) 0.0193(8) Uani 1 1 d . . . . .
H25 H 0.6461 0.0627 0.5083 0.023 Uiso 1 1 calc R U . . .
C26 C 0.5201(3) 0.1437(2) 0.53452(11) 0.0161(8) Uani 1 1 d . . . . .
H26 H 0.4602 0.0965 0.5267 0.019 Uiso 1 1 calc R U . . .
C27 C 0.2610(3) 0.1999(2) 0.53815(11) 0.0168(8) Uani 1 1 d . . . . .
C28 C 0.1871(3) 0.2490(2) 0.50594(11) 0.0207(8) Uani 1 1 d . . . . .
H28 H 0.1922 0.3196 0.5039 0.025 Uiso 1 1 calc R U . . .
C29 C 0.1062(4) 0.1995(3) 0.47658(12) 0.0265(9) Uani 1 1 d . . . . .
H29 H 0.0584 0.2363 0.4549 0.032 Uiso 1 1 calc R U . . .
C30 C 0.0951(4) 0.0971(3) 0.47874(13) 0.0264(9) Uani 1 1 d . . . . .
H30 H 0.0407 0.0629 0.4585 0.032 Uiso 1 1 calc R U . . .
C31 C 0.1640(3) 0.0458(3) 0.51057(13) 0.0247(9) Uani 1 1 d . . . . .
H31 H 0.1566 -0.0246 0.5128 0.030 Uiso 1 1 calc R U . . .
C32 C 0.2446(3) 0.0959(2) 0.53963(12) 0.0214(8) Uani 1 1 d . . . . .
H32 H 0.2907 0.0584 0.5615 0.026 Uiso 1 1 calc R U . . .
C33 C 0.3535(3) 0.2118(2) 0.62451(11) 0.0192(8) Uani 1 1 d . . . . .
C34 C 0.2512(4) 0.1734(3) 0.63910(12) 0.0292(10) Uani 1 1 d . . . . .
H34 H 0.1851 0.1668 0.6180 0.035 Uiso 1 1 calc R U . . .
C35 C 0.2414(4) 0.1442(3) 0.68320(13) 0.0383(11) Uani 1 1 d . . . . .
H35 H 0.1698 0.1186 0.6917 0.046 Uiso 1 1 calc R U . . .
C36 C 0.3361(4) 0.1526(3) 0.71459(13) 0.0324(11) Uani 1 1 d . . . . .
H36 H 0.3303 0.1325 0.7448 0.039 Uiso 1 1 calc R U . . .
C37 C 0.4394(4) 0.1904(3) 0.70165(12) 0.0273(9) Uani 1 1 d . . . . .
H37 H 0.5050 0.1972 0.7230 0.033 Uiso 1 1 calc R U . . .
C38 C 0.4470(3) 0.2187(2) 0.65707(11) 0.0210(8) Uani 1 1 d . . . . .
H38 H 0.5191 0.2437 0.6486 0.025 Uiso 1 1 calc R U . . .
C39 C 0.3371(3) 0.3758(2) 0.57290(11) 0.0167(8) Uani 1 1 d . . . . .
C40 C 0.2876(3) 0.4259(3) 0.60754(12) 0.0212(8) Uani 1 1 d . . . . .
H40 H 0.2718 0.3898 0.6337 0.025 Uiso 1 1 calc R U . . .
C41 C 0.2607(3) 0.5267(3) 0.60501(13) 0.0280(10) Uani 1 1 d . . . . .
H41 H 0.2283 0.5582 0.6295 0.034 Uiso 1 1 calc R U . . .
C42 C 0.2805(3) 0.5819(3) 0.56735(14) 0.0294(10) Uani 1 1 d . . . . .
H42 H 0.2601 0.6505 0.5653 0.035 Uiso 1 1 calc R U . . .
C43 C 0.3308(3) 0.5347(3) 0.53285(13) 0.0257(9) Uani 1 1 d . . . . .
H43 H 0.3458 0.5713 0.5068 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3595(3) 0.4346(2) 0.53591(12) 0.0215(9) Uani 1 1 d . . . . .
H44 H 0.3959 0.4045 0.5120 0.026 Uiso 1 1 calc R U . . .
C45 C 0.2635(4) 0.7626(3) 0.67573(14) 0.0402(8) Uani 1 1 d . . . . .
H45A H 0.2814 0.8047 0.7027 0.048 Uiso 1 1 calc R U . . .
H45B H 0.2955 0.6950 0.6819 0.048 Uiso 1 1 calc R U . . .
C46 C 0.1331(4) 0.7582(3) 0.66313(14) 0.0406(8) Uani 1 1 d . . . . .
H46A H 0.0890 0.7594 0.6901 0.049 Uiso 1 1 calc R U . . .
H46B H 0.1112 0.6980 0.6452 0.049 Uiso 1 1 calc R U . . .
C47 C 0.1133(4) 0.8528(3) 0.63546(14) 0.0406(8) Uani 1 1 d . . . . .
H47A H 0.0459 0.8453 0.6128 0.049 Uiso 1 1 calc R U . . .
H47B H 0.0996 0.9107 0.6549 0.049 Uiso 1 1 calc R U . . .
C48 C 0.2230(4) 0.8649(3) 0.61367(15) 0.0402(8) Uani 1 1 d . . . . .
H48A H 0.2114 0.8433 0.5819 0.048 Uiso 1 1 calc R U . . .
H48B H 0.2467 0.9359 0.6143 0.048 Uiso 1 1 calc R U . . .
B1 B 0.3605(4) 0.2544(3) 0.57282(13) 0.0170(9) Uani 1 1 d . . . . .
N2 N 0.6471(3) 0.92844(19) 0.66144(9) 0.0172(7) Uani 1 1 d . . . . .
N3 N 0.5377(3) 0.79424(19) 0.60059(9) 0.0152(6) Uani 1 1 d D . . . .
N4 N 0.6712(3) 0.62850(18) 0.62894(9) 0.0133(6) Uani 1 1 d . . . . .
O3 O 0.3114(2) 0.80564(19) 0.63733(9) 0.0328(7) Uani 1 1 d . . . . .
Pd1 Pd 0.65726(3) 0.77430(2) 0.65312(2) 0.01445(8) Uani 1 1 d . . . . .
N1_a N 0.7715(7) 0.7529(5) 0.7079(2) 0.0223(15) Uiso 0.549(5) 1 d D . P A 1
O1_a O 0.8736(5) 0.7632(4) 0.70364(16) 0.0358(9) Uiso 0.549(5) 1 d D . P A 1
O2_a O 0.7341(6) 0.7284(5) 0.7442(2) 0.0358(9) Uiso 0.549(5) 1 d D . P A 1
N1A_b N 0.7797(7) 0.7299(6) 0.7402(2) 0.0223(15) Uiso 0.451(5) 1 d D . P A 2
O1A_b O 0.7958(8) 0.7588(6) 0.6992(2) 0.0274(19) Uiso 0.451(5) 1 d D . P A 2
O2A_b O 0.6758(6) 0.7151(5) 0.7458(2) 0.0358(9) Uiso 0.451(5) 1 d D . P A 2
H3 H 0.462(2) 0.783(3) 0.6109(13) 0.043 Uiso 1 1 d D 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
C1 N2 1.507(4) . ?
C1 C2 1.518(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.488(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.492(4) . ?
C3 C4 1.516(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.503(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.504(5) . ?
C5 C6 1.523(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.508(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.528(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.502(4) . ?
C9 C10 1.509(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.520(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.512(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.505(4) . ?
C13 C14 1.523(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.520(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.517(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.498(4) . ?
C17 C18 1.504(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.492(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.487(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.404(5) . ?
C21 C26 1.404(4) . ?
C21 B1 1.649(5) . ?
C22 C23 1.385(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.384(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.389(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.393(5) . ?
C27 C32 1.408(4) . ?
C27 B1 1.648(5) . ?
C28 C29 1.391(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.381(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.370(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.388(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.390(5) . ?
C33 C34 1.391(5) . ?
C33 B1 1.657(5) . ?
C34 C35 1.389(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.379(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.380(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.396(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.398(5) . ?
C39 C44 1.400(5) . ?
C39 B1 1.649(5) . ?
C40 C41 1.387(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.384(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.380(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.384(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.437(5) . ?
C45 C46 1.518(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.521(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.482(6) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.429(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N2 Pd1 2.086(3) . ?
N3 Pd1 2.014(3) . ?
N3 H3 0.964(19) . ?
N4 Pd1 2.095(3) . ?
Pd1 O1A_b 2.026(9) . ?
Pd1 N1_a 2.029(8) . ?
N1_a O1_a 1.203(9) . ?
N1_a O2_a 1.248(9) . ?
N1A_b O2A_b 1.239(9) . ?
N1A_b O1A_b 1.316(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 109.8(3) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.5(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.0(3) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.0(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 117.2(3) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.5(3) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 111.2(3) . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.6(3) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.4(3) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.5(3) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 116.9(3) . . ?
N4 C13 H13A 108.1 . . ?
C14 C13 H13A 108.1 . . ?
N4 C13 H13B 108.1 . . ?
C14 C13 H13B 108.1 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.5(3) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 113.6(3) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.7(3) . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C17 112.6(3) . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18B 109.1 . . ?
C17 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 115.3(4) . . ?
C20 C19 H19A 108.4 . . ?
C18 C19 H19A 108.4 . . ?
C20 C19 H19B 108.4 . . ?
C18 C19 H19B 108.4 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 114.3(3) . . ?
C22 C21 B1 121.9(3) . . ?
C26 C21 B1 123.7(3) . . ?
C23 C22 C21 123.4(3) . . ?
C23 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.1(4) . . ?
C23 C24 H24 120.9 . . ?
C25 C24 H24 120.9 . . ?
C26 C25 C24 120.7(3) . . ?
C26 C25 H25 119.6 . . ?
C24 C25 H25 119.6 . . ?
C25 C26 C21 123.1(3) . . ?
C25 C26 H26 118.5 . . ?
C21 C26 H26 118.5 . . ?
C28 C27 C32 114.5(3) . . ?
C28 C27 B1 125.1(3) . . ?
C32 C27 B1 120.5(3) . . ?
C29 C28 C27 123.0(3) . . ?
C29 C28 H28 118.5 . . ?
C27 C28 H28 118.5 . . ?
C30 C29 C28 120.3(4) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C31 C30 C29 118.8(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.0(3) . . ?
C31 C32 H32 118.5 . . ?
C27 C32 H32 118.5 . . ?
C38 C33 C34 115.5(3) . . ?
C38 C33 B1 122.1(3) . . ?
C34 C33 B1 122.2(3) . . ?
C35 C34 C33 122.9(4) . . ?
C35 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C36 C35 C34 119.8(4) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C37 119.3(4) . . ?
C35 C36 H36 120.4 . . ?
C37 C36 H36 120.4 . . ?
C36 C37 C38 119.8(4) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C33 C38 C37 122.7(4) . . ?
C33 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
C40 C39 C44 115.5(3) . . ?
C40 C39 B1 123.6(3) . . ?
C44 C39 B1 120.8(3) . . ?
C41 C40 C39 122.1(3) . . ?
C41 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?
C42 C41 C40 120.9(3) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C43 C42 C41 118.2(3) . . ?
C43 C42 H42 120.9 . . ?
C41 C42 H42 120.9 . . ?
C42 C43 C44 120.6(3) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
C43 C44 C39 122.6(3) . . ?
C43 C44 H44 118.7 . . ?
C39 C44 H44 118.7 . . ?
O3 C45 C46 105.0(3) . . ?
O3 C45 H45A 110.8 . . ?
C46 C45 H45A 110.8 . . ?
O3 C45 H45B 110.8 . . ?
C46 C45 H45B 110.8 . . ?
H45A C45 H45B 108.8 . . ?
C45 C46 C47 101.6(4) . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46B 111.5 . . ?
C47 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 103.7(4) . . ?
C48 C47 H47A 111.0 . . ?
C46 C47 H47A 111.0 . . ?
C48 C47 H47B 111.0 . . ?
C46 C47 H47B 111.0 . . ?
H47A C47 H47B 109.0 . . ?
O3 C48 C47 108.7(3) . . ?
O3 C48 H48A 110.0 . . ?
C47 C48 H48A 110.0 . . ?
O3 C48 H48B 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.3 . . ?
C27 B1 C39 109.5(3) . . ?
C27 B1 C21 109.8(3) . . ?
C39 B1 C21 110.0(3) . . ?
C27 B1 C33 110.2(3) . . ?
C39 B1 C33 108.5(3) . . ?
C21 B1 C33 108.9(3) . . ?
C9 N2 C5 109.4(3) . . ?
C9 N2 C1 110.5(3) . . ?
C5 N2 C1 111.3(3) . . ?
C9 N2 Pd1 114.94(19) . . ?
C5 N2 Pd1 104.7(2) . . ?
C1 N2 Pd1 105.74(19) . . ?
C2 N3 C3 115.8(3) . . ?
C2 N3 Pd1 107.4(2) . . ?
C3 N3 Pd1 107.5(2) . . ?
C2 N3 H3 109(2) . . ?
C3 N3 H3 109(2) . . ?
Pd1 N3 H3 108(2) . . ?
C17 N4 C4 109.8(3) . . ?
C17 N4 C13 110.0(3) . . ?
C4 N4 C13 111.7(3) . . ?
C17 N4 Pd1 115.52(19) . . ?
C4 N4 Pd1 105.06(18) . . ?
C13 N4 Pd1 104.63(19) . . ?
C48 O3 C45 108.2(3) . . ?
N3 Pd1 O1A_b 171.2(2) . . ?
N3 Pd1 N1_a 177.3(2) . . ?
N3 Pd1 N2 85.41(11) . . ?
O1A_b Pd1 N2 94.0(2) . . ?
N1_a Pd1 N2 94.8(2) . . ?
N3 Pd1 N4 85.56(10) . . ?
O1A_b Pd1 N4 93.4(2) . . ?
N1_a Pd1 N4 94.7(2) . . ?
N2 Pd1 N4 166.47(10) . . ?
O1_a N1_a O2_a 122.6(8) . . ?
O1_a N1_a Pd1 118.0(5) . . ?
O2_a N1_a Pd1 119.4(6) . . ?
O2A_b N1A_b O1A_b 113.0(8) . . ?
N1A_b O1A_b Pd1 119.8(7) . . ?

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
N2 C1 C2 N3 55.1(4) . . . . ?
N3 C3 C4 N4 -54.9(4) . . . . ?
N2 C5 C6 C7 -178.0(3) . . . . ?
C5 C6 C7 C8 -171.8(3) . . . . ?
N2 C9 C10 C11 172.0(3) . . . . ?
C9 C10 C11 C12 171.9(3) . . . . ?
N4 C13 C14 C15 178.7(3) . . . . ?
C13 C14 C15 C16 179.4(3) . . . . ?
N4 C17 C18 C19 -174.0(3) . . . . ?
C17 C18 C19 C20 -170.0(4) . . . . ?
C26 C21 C22 C23 0.3(5) . . . . ?
B1 C21 C22 C23 177.7(3) . . . . ?
C21 C22 C23 C24 -0.6(5) . . . . ?
C22 C23 C24 C25 0.3(5) . . . . ?
C23 C24 C25 C26 0.3(5) . . . . ?
C24 C25 C26 C21 -0.6(5) . . . . ?
C22 C21 C26 C25 0.3(5) . . . . ?
B1 C21 C26 C25 -177.1(3) . . . . ?
C32 C27 C28 C29 -2.0(5) . . . . ?
B1 C27 C28 C29 178.3(3) . . . . ?
C27 C28 C29 C30 0.8(6) . . . . ?
C28 C29 C30 C31 0.8(5) . . . . ?
C29 C30 C31 C32 -0.9(6) . . . . ?
C30 C31 C32 C27 -0.5(6) . . . . ?
C28 C27 C32 C31 1.9(5) . . . . ?
B1 C27 C32 C31 -178.4(3) . . . . ?
C38 C33 C34 C35 0.4(5) . . . . ?
B1 C33 C34 C35 -175.1(3) . . . . ?
C33 C34 C35 C36 -0.2(6) . . . . ?
C34 C35 C36 C37 0.3(6) . . . . ?
C35 C36 C37 C38 -0.6(5) . . . . ?
C34 C33 C38 C37 -0.8(5) . . . . ?
B1 C33 C38 C37 174.7(3) . . . . ?
C36 C37 C38 C33 0.9(5) . . . . ?
C44 C39 C40 C41 1.1(5) . . . . ?
B1 C39 C40 C41 -174.9(3) . . . . ?
C39 C40 C41 C42 1.0(6) . . . . ?
C40 C41 C42 C43 -1.8(6) . . . . ?
C41 C42 C43 C44 0.5(6) . . . . ?
C42 C43 C44 C39 1.6(6) . . . . ?
C40 C39 C44 C43 -2.4(5) . . . . ?
B1 C39 C44 C43 173.7(3) . . . . ?
O3 C45 C46 C47 -35.4(4) . . . . ?
C45 C46 C47 C48 31.9(4) . . . . ?
C46 C47 C48 O3 -17.9(5) . . . . ?
C28 C27 B1 C39 14.6(5) . . . . ?
C32 C27 B1 C39 -165.1(3) . . . . ?
C28 C27 B1 C21 -106.2(4) . . . . ?
C32 C27 B1 C21 74.1(4) . . . . ?
C28 C27 B1 C33 133.9(3) . . . . ?
C32 C27 B1 C33 -45.8(4) . . . . ?
C40 C39 B1 C27 103.9(4) . . . . ?
C44 C39 B1 C27 -71.9(4) . . . . ?
C40 C39 B1 C21 -135.4(3) . . . . ?
C44 C39 B1 C21 48.8(4) . . . . ?
C40 C39 B1 C33 -16.5(5) . . . . ?
C44 C39 B1 C33 167.8(3) . . . . ?
C22 C21 B1 C27 153.0(3) . . . . ?
C26 C21 B1 C27 -29.8(4) . . . . ?
C22 C21 B1 C39 32.5(4) . . . . ?
C26 C21 B1 C39 -150.4(3) . . . . ?
C22 C21 B1 C33 -86.3(4) . . . . ?
C26 C21 B1 C33 90.9(4) . . . . ?
C38 C33 B1 C27 158.6(3) . . . . ?
C34 C33 B1 C27 -26.2(4) . . . . ?
C38 C33 B1 C39 -81.5(4) . . . . ?
C34 C33 B1 C39 93.7(4) . . . . ?
C38 C33 B1 C21 38.2(4) . . . . ?
C34 C33 B1 C21 -146.6(3) . . . . ?
C10 C9 N2 C5 -173.0(3) . . . . ?
C10 C9 N2 C1 64.1(4) . . . . ?
C10 C9 N2 Pd1 -55.4(4) . . . . ?
C6 C5 N2 C9 -55.0(4) . . . . ?
C6 C5 N2 C1 67.5(4) . . . . ?
C6 C5 N2 Pd1 -178.7(3) . . . . ?
C2 C1 N2 C9 -160.0(3) . . . . ?
C2 C1 N2 C5 78.2(3) . . . . ?
C2 C1 N2 Pd1 -35.0(3) . . . . ?
C1 C2 N3 C3 -166.8(3) . . . . ?
C1 C2 N3 Pd1 -46.6(3) . . . . ?
C4 C3 N3 C2 166.5(3) . . . . ?
C4 C3 N3 Pd1 46.4(3) . . . . ?
C18 C17 N4 C4 -64.4(4) . . . . ?
C18 C17 N4 C13 172.2(3) . . . . ?
C18 C17 N4 Pd1 54.1(4) . . . . ?
C3 C4 N4 C17 159.4(3) . . . . ?
C3 C4 N4 C13 -78.3(3) . . . . ?
C3 C4 N4 Pd1 34.6(3) . . . . ?
C14 C13 N4 C17 57.6(4) . . . . ?
C14 C13 N4 C4 -64.6(4) . . . . ?
C14 C13 N4 Pd1 -177.7(2) . . . . ?
C47 C48 O3 C45 -4.7(5) . . . . ?
C46 C45 O3 C48 25.5(4) . . . . ?
O2A_b N1A_b O1A_b Pd1 -0.1(9) . . . . ?

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
C5 H5B O1_a 0.99 2.56 3.382(6) 140.3 .
C5 H5B O1A_b 0.99 2.55 3.182(8) 121.2 .
C10 H10A O2A_b 0.99 2.52 3.269(8) 132.6 .
C13 H13A O1_a 0.99 2.58 3.375(6) 137.5 .
C18 H18A O2A_b 0.99 2.37 3.109(8) 131.0 .
C46 H46A O1_a 0.99 2.55 3.325(7) 135.0 1_455
N3 H3 O3 0.964(19) 1.99(2) 2.922(4) 161(3) .

_refine_diff_density_max         0.800
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.098

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_5minUV
_database_code_depnum_ccdc_archive 'CCDC 1441783'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_5minUV              
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially excited nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_5minUV              
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         17 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31


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'
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                   11.4898(7)
_cell_length_b                   13.3882(5)
_cell_length_c                   29.9800(13)
_cell_angle_alpha                90
_cell_angle_beta                 94.753(5)
_cell_angle_gamma                90
_cell_volume                     4595.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3481
_cell_measurement_theta_min      3.5590
_cell_measurement_theta_max      28.9030

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.447
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80762
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            19272
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.123
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             9344
_reflns_number_gt                6064
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0418P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9344
_refine_ls_number_parameters     504
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0534
_refine_ls_wR_factor_ref         0.1134
_refine_ls_wR_factor_gt          0.0953
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.5483(4) 0.9632(3) 0.62824(12) 0.0221(10) Uani 1 1 d . . . . .
H1A H 0.5597 1.0342 0.6205 0.026 Uiso 1 1 calc R U . . .
H1B H 0.4735 0.9573 0.6422 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5440(4) 0.8999(3) 0.58620(12) 0.0221(10) Uani 1 1 d . . . . .
H2A H 0.4749 0.9177 0.5658 0.027 Uiso 1 1 calc R U . . .
H2B H 0.6151 0.9108 0.5703 0.027 Uiso 1 1 calc R U . . .
C3 C 0.5596(3) 0.7179(2) 0.56609(11) 0.0169(8) Uani 1 1 d . . . . .
H3A H 0.6302 0.7358 0.5510 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4924 0.7133 0.5433 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5774(4) 0.6197(2) 0.59089(12) 0.0177(9) Uani 1 1 d . . . . .
H4A H 0.5033 0.5993 0.6029 0.021 Uiso 1 1 calc R U . . .
H4B H 0.5993 0.5673 0.5698 0.021 Uiso 1 1 calc R U . . .
C5 C 0.7624(4) 0.9675(3) 0.64780(13) 0.0211(9) Uani 1 1 d . . . . .
H5A H 0.7715 0.9468 0.6166 0.025 Uiso 1 1 calc R U . . .
H5B H 0.8251 0.9342 0.6670 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7824(4) 1.0799(3) 0.65099(13) 0.0237(10) Uani 1 1 d . . . . .
H6A H 0.7206 1.1146 0.6319 0.028 Uiso 1 1 calc R U . . .
H6B H 0.7767 1.1018 0.6823 0.028 Uiso 1 1 calc R U . . .
C7 C 0.9005(4) 1.1089(3) 0.63638(14) 0.0297(11) Uani 1 1 d . . . . .
H7A H 0.9021 1.0962 0.6039 0.036 Uiso 1 1 calc R U . . .
H7B H 0.9615 1.0670 0.6524 0.036 Uiso 1 1 calc R U . . .
C8 C 0.9271(4) 1.2181(3) 0.64589(15) 0.0365(11) Uani 1 1 d . . . . .
H8A H 0.9328 1.2295 0.6783 0.055 Uiso 1 1 calc R U . . .
H8B H 0.8644 1.2595 0.6315 0.055 Uiso 1 1 calc R U . . .
H8C H 1.0013 1.2358 0.6340 0.055 Uiso 1 1 calc R U . . .
C9 C 0.6285(4) 0.9626(3) 0.70709(12) 0.0178(9) Uani 1 1 d . . . . .
H9A H 0.6226 1.0364 0.7069 0.021 Uiso 1 1 calc R U . . .
H9B H 0.6984 0.9445 0.7270 0.021 Uiso 1 1 calc R U . . .
C10 C 0.5220(4) 0.9208(3) 0.72695(12) 0.0212(9) Uani 1 1 d . . . . .
H10A H 0.5205 0.8472 0.7234 0.025 Uiso 1 1 calc R U . . .
H10B H 0.4506 0.9483 0.7107 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5235(4) 0.9471(3) 0.77628(13) 0.0257(10) Uani 1 1 d . . . . .
H11A H 0.5902 0.9126 0.7927 0.031 Uiso 1 1 calc R U . . .
H11B H 0.5362 1.0199 0.7798 0.031 Uiso 1 1 calc R U . . .
C12 C 0.4124(4) 0.9189(3) 0.79709(15) 0.0358(12) Uani 1 1 d . . . . .
H12A H 0.4218 0.9321 0.8293 0.054 Uiso 1 1 calc R U . . .
H12B H 0.3962 0.8478 0.7920 0.054 Uiso 1 1 calc R U . . .
H12C H 0.3472 0.9586 0.7834 0.054 Uiso 1 1 calc R U . . .
C13 C 0.7910(4) 0.6239(2) 0.61218(12) 0.0178(9) Uani 1 1 d . . . . .
H13A H 0.8486 0.6382 0.6378 0.021 Uiso 1 1 calc R U . . .
H13B H 0.7971 0.6782 0.5901 0.021 Uiso 1 1 calc R U . . .
C14 C 0.8261(4) 0.5265(3) 0.59068(13) 0.0208(9) Uani 1 1 d . . . . .
H14A H 0.8242 0.4717 0.6128 0.025 Uiso 1 1 calc R U . . .
H14B H 0.7690 0.5105 0.5651 0.025 Uiso 1 1 calc R U . . .
C15 C 0.9473(4) 0.5333(3) 0.57439(13) 0.0238(9) Uani 1 1 d . . . . .
H15A H 1.0038 0.5502 0.6000 0.029 Uiso 1 1 calc R U . . .
H15B H 0.9485 0.5881 0.5523 0.029 Uiso 1 1 calc R U . . .
C16 C 0.9863(4) 0.4370(3) 0.55300(13) 0.0269(10) Uani 1 1 d . . . . .
H16A H 1.0654 0.4456 0.5436 0.040 Uiso 1 1 calc R U . . .
H16B H 0.9326 0.4210 0.5268 0.040 Uiso 1 1 calc R U . . .
H16C H 0.9860 0.3824 0.5748 0.040 Uiso 1 1 calc R U . . .
C17 C 0.6584(4) 0.5481(2) 0.66273(12) 0.0170(9) Uani 1 1 d . . . . .
H17A H 0.7237 0.5542 0.6863 0.020 Uiso 1 1 calc R U . . .
H17B H 0.6660 0.4825 0.6480 0.020 Uiso 1 1 calc R U . . .
C18 C 0.5453(4) 0.5494(3) 0.68475(13) 0.0219(9) Uani 1 1 d . . . . .
H18A H 0.4805 0.5302 0.6626 0.026 Uiso 1 1 calc R U . . .
H18B H 0.5300 0.6180 0.6951 0.026 Uiso 1 1 calc R U . . .
C19 C 0.5488(4) 0.4785(3) 0.72409(14) 0.0310(11) Uani 1 1 d . . . . .
H19A H 0.5790 0.4131 0.7148 0.037 Uiso 1 1 calc R U . . .
H19B H 0.6040 0.5048 0.7484 0.037 Uiso 1 1 calc R U . . .
C20 C 0.4320(4) 0.4631(3) 0.74199(15) 0.0409(13) Uani 1 1 d . . . . .
H20A H 0.4413 0.4221 0.7691 0.061 Uiso 1 1 calc R U . . .
H20B H 0.3795 0.4292 0.7194 0.061 Uiso 1 1 calc R U . . .
H20C H 0.3987 0.5280 0.7491 0.061 Uiso 1 1 calc R U . . .
C21 C 0.4923(3) 0.2315(3) 0.55721(11) 0.0158(8) Uani 1 1 d . . . . .
C22 C 0.5869(4) 0.2963(3) 0.56665(12) 0.0213(9) Uani 1 1 d . . . . .
H22 H 0.5736 0.3568 0.5820 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6986(4) 0.2770(3) 0.55493(12) 0.0235(9) Uani 1 1 d . . . . .
H23 H 0.7591 0.3240 0.5621 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7225(4) 0.1901(3) 0.53296(13) 0.0228(9) Uani 1 1 d . . . . .
H24 H 0.7990 0.1764 0.5248 0.027 Uiso 1 1 calc R U . . .
C25 C 0.6319(4) 0.1230(3) 0.52303(12) 0.0183(9) Uani 1 1 d . . . . .
H25 H 0.6464 0.0620 0.5083 0.022 Uiso 1 1 calc R U . . .
C26 C 0.5210(4) 0.1448(2) 0.53456(12) 0.0164(8) Uani 1 1 d . . . . .
H26 H 0.4605 0.0982 0.5267 0.020 Uiso 1 1 calc R U . . .
C27 C 0.2616(3) 0.2004(3) 0.53904(12) 0.0184(9) Uani 1 1 d . . . . .
C28 C 0.1882(4) 0.2485(3) 0.50650(12) 0.0211(9) Uani 1 1 d . . . . .
H28 H 0.1935 0.3190 0.5040 0.025 Uiso 1 1 calc R U . . .
C29 C 0.1078(4) 0.1986(3) 0.47760(13) 0.0290(10) Uani 1 1 d . . . . .
H29 H 0.0603 0.2351 0.4559 0.035 Uiso 1 1 calc R U . . .
C30 C 0.0964(4) 0.0968(3) 0.48010(14) 0.0279(10) Uani 1 1 d . . . . .
H30 H 0.0420 0.0624 0.4600 0.034 Uiso 1 1 calc R U . . .
C31 C 0.1648(4) 0.0455(3) 0.51211(15) 0.0275(10) Uani 1 1 d . . . . .
H31 H 0.1572 -0.0249 0.5145 0.033 Uiso 1 1 calc R U . . .
C32 C 0.2447(4) 0.0960(3) 0.54084(13) 0.0232(10) Uani 1 1 d . . . . .
H32 H 0.2904 0.0587 0.5628 0.028 Uiso 1 1 calc R U . . .
C33 C 0.3552(4) 0.2130(3) 0.62482(12) 0.0196(9) Uani 1 1 d . . . . .
C34 C 0.2518(4) 0.1745(3) 0.63968(13) 0.0313(11) Uani 1 1 d . . . . .
H34 H 0.1856 0.1678 0.6187 0.038 Uiso 1 1 calc R U . . .
C35 C 0.2418(5) 0.1460(3) 0.68369(14) 0.0382(12) Uani 1 1 d . . . . .
H35 H 0.1696 0.1208 0.6923 0.046 Uiso 1 1 calc R U . . .
C36 C 0.3363(4) 0.1541(3) 0.71491(14) 0.0317(11) Uani 1 1 d . . . . .
H36 H 0.3302 0.1339 0.7450 0.038 Uiso 1 1 calc R U . . .
C37 C 0.4397(4) 0.1919(3) 0.70188(13) 0.0274(10) Uani 1 1 d . . . . .
H37 H 0.5054 0.1989 0.7231 0.033 Uiso 1 1 calc R U . . .
C38 C 0.4479(4) 0.2200(3) 0.65738(12) 0.0230(9) Uani 1 1 d . . . . .
H38 H 0.5203 0.2452 0.6490 0.028 Uiso 1 1 calc R U . . .
C39 C 0.3378(4) 0.3763(3) 0.57281(12) 0.0187(9) Uani 1 1 d . . . . .
C40 C 0.2875(4) 0.4266(3) 0.60728(13) 0.0217(9) Uani 1 1 d . . . . .
H40 H 0.2712 0.3905 0.6333 0.026 Uiso 1 1 calc R U . . .
C41 C 0.2606(4) 0.5280(3) 0.60472(14) 0.0279(10) Uani 1 1 d . . . . .
H41 H 0.2279 0.5600 0.6291 0.033 Uiso 1 1 calc R U . . .
C42 C 0.2812(4) 0.5825(3) 0.56683(15) 0.0293(11) Uani 1 1 d . . . . .
H42 H 0.2605 0.6511 0.5646 0.035 Uiso 1 1 calc R U . . .
C43 C 0.3323(4) 0.5352(3) 0.53247(14) 0.0255(10) Uani 1 1 d . . . . .
H43 H 0.3478 0.5716 0.5064 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3609(4) 0.4350(3) 0.53596(13) 0.0214(9) Uani 1 1 d . . . . .
H44 H 0.3979 0.4046 0.5122 0.026 Uiso 1 1 calc R U . . .
C45 C 0.2612(4) 0.7639(3) 0.67627(16) 0.0419(9) Uani 1 1 d . . . . .
H45A H 0.2783 0.8077 0.7026 0.050 Uiso 1 1 calc R U . . .
H45B H 0.2936 0.6967 0.6833 0.050 Uiso 1 1 calc R U . . .
C46 C 0.1296(4) 0.7581(4) 0.66373(16) 0.0474(9) Uani 1 1 d . . . . .
H46A H 0.1081 0.6960 0.6471 0.057 Uiso 1 1 calc R U . . .
H46B H 0.0849 0.7623 0.6905 0.057 Uiso 1 1 calc R U . . .
C47 C 0.1100(5) 0.8496(4) 0.63419(16) 0.0474(9) Uani 1 1 d . . . . .
H47A H 0.0456 0.8380 0.6107 0.057 Uiso 1 1 calc R U . . .
H47B H 0.0906 0.9085 0.6521 0.057 Uiso 1 1 calc R U . . .
C48 C 0.2211(4) 0.8649(3) 0.61408(16) 0.0419(9) Uani 1 1 d . . . . .
H48A H 0.2125 0.8457 0.5821 0.050 Uiso 1 1 calc R U . . .
H48B H 0.2436 0.9363 0.6161 0.050 Uiso 1 1 calc R U . . .
B1 B 0.3623(4) 0.2551(3) 0.57313(14) 0.0171(10) Uani 1 1 d . . . . .
N2 N 0.6472(3) 0.9286(2) 0.66060(9) 0.0168(7) Uani 1 1 d . . . . .
N3 N 0.5368(3) 0.7937(2) 0.60060(9) 0.0156(7) Uani 1 1 d D . . . .
N4 N 0.6712(3) 0.6284(2) 0.62866(10) 0.0145(7) Uani 1 1 d . . . . .
O3 O 0.3099(3) 0.8047(2) 0.63766(9) 0.0338(7) Uani 1 1 d . . . . .
Pd1 Pd 0.65798(3) 0.77489(2) 0.65236(2) 0.01550(9) Uani 1 1 d . . . . .
N1_a N 0.7706(15) 0.7539(15) 0.7096(7) 0.0266(14) Uiso 0.203(6) 1 d D . P A 1
O1_a O 0.8685(13) 0.7639(10) 0.7019(5) 0.0312(10) Uiso 0.203(6) 1 d D . P A 1
O2_a O 0.731(2) 0.7284(14) 0.7445(5) 0.0312(10) Uiso 0.203(6) 1 d D . P A 1
N1A_b N 0.7792(4) 0.7310(4) 0.73965(16) 0.0266(14) Uiso 0.797(6) 1 d D . P A 2
O1A_b O 0.7957(4) 0.7599(3) 0.69861(12) 0.0228(10) Uiso 0.797(6) 1 d D . P A 2
O2A_b O 0.6764(4) 0.7170(3) 0.74568(12) 0.0312(10) Uiso 0.797(6) 1 d D . P A 2
H3 H 0.459(2) 0.788(3) 0.6113(13) 0.037 Uiso 1 1 d D 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
C1 N2 1.505(5) . ?
C1 C2 1.516(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.491(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.488(4) . ?
C3 C4 1.516(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.501(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.502(5) . ?
C5 C6 1.524(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.510(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.516(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.498(4) . ?
C9 C10 1.512(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.514(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.502(5) . ?
C13 C14 1.524(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.517(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.524(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.498(4) . ?
C17 C18 1.506(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.512(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.501(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.398(5) . ?
C21 C22 1.400(5) . ?
C21 B1 1.636(6) . ?
C22 C23 1.382(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.375(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.379(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.394(5) . ?
C27 C32 1.413(5) . ?
C27 B1 1.651(6) . ?
C28 C29 1.384(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.371(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.374(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.387(5) . ?
C33 C34 1.401(6) . ?
C33 B1 1.658(5) . ?
C34 C35 1.388(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.378(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.397(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.398(5) . ?
C39 C44 1.399(5) . ?
C39 B1 1.646(5) . ?
C40 C41 1.392(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.387(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.380(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.384(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.435(5) . ?
C45 C46 1.530(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.518(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.471(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.439(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N2 Pd1 2.078(3) . ?
N3 Pd1 2.013(3) . ?
N3 H3 0.974(19) . ?
N4 Pd1 2.095(3) . ?
Pd1 O1A_b 2.025(4) . ?
Pd1 N1_a 2.08(2) . ?
N1_a O1_a 1.174(17) . ?
N1_a O2_a 1.222(17) . ?
N1A_b O2A_b 1.224(6) . ?
N1A_b O1A_b 1.318(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 109.6(3) . . ?
N2 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
N2 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.9(3) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 105.9(3) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 111.2(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 117.2(3) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.2 . . ?
C7 C6 C5 111.7(3) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 111.4(3) . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7B 109.3 . . ?
C8 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.9(3) . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.7(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.7(4) . . ?
C12 C11 H11A 108.8 . . ?
C10 C11 H11A 108.8 . . ?
C12 C11 H11B 108.8 . . ?
C10 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.1(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.5(3) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.2(3) . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.3(3) . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.5(3) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.4(4) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.7(4) . . ?
C26 C21 B1 124.0(3) . . ?
C22 C21 B1 122.2(3) . . ?
C23 C22 C21 123.6(3) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.3(4) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C26 C25 C24 120.0(3) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C25 C26 C21 123.9(3) . . ?
C25 C26 H26 118.1 . . ?
C21 C26 H26 118.1 . . ?
C28 C27 C32 114.0(3) . . ?
C28 C27 B1 125.5(3) . . ?
C32 C27 B1 120.5(3) . . ?
C29 C28 C27 123.3(4) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C30 C29 C28 120.5(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C29 C30 C31 118.9(4) . . ?
C29 C30 H30 120.6 . . ?
C31 C30 H30 120.6 . . ?
C30 C31 C32 120.2(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 123.1(4) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C38 C33 C34 115.0(3) . . ?
C38 C33 B1 122.7(4) . . ?
C34 C33 B1 122.1(4) . . ?
C35 C34 C33 122.9(4) . . ?
C35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C36 C35 C34 120.1(5) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C37 C36 C35 119.1(4) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 119.8(4) . . ?
C36 C37 H37 120.1 . . ?
C38 C37 H37 120.1 . . ?
C33 C38 C37 123.1(4) . . ?
C33 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C40 C39 C44 115.5(3) . . ?
C40 C39 B1 123.5(3) . . ?
C44 C39 B1 121.0(3) . . ?
C41 C40 C39 122.2(4) . . ?
C41 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C43 C42 C41 118.8(3) . . ?
C43 C42 H42 120.6 . . ?
C41 C42 H42 120.6 . . ?
C42 C43 C44 120.1(4) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 123.0(4) . . ?
C43 C44 H44 118.5 . . ?
C39 C44 H44 118.5 . . ?
O3 C45 C46 105.4(4) . . ?
O3 C45 H45A 110.7 . . ?
C46 C45 H45A 110.7 . . ?
O3 C45 H45B 110.7 . . ?
C46 C45 H45B 110.7 . . ?
H45A C45 H45B 108.8 . . ?
C47 C46 C45 101.4(4) . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46B 111.5 . . ?
C45 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 105.1(4) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
O3 C48 C47 109.0(4) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C21 B1 C39 110.4(3) . . ?
C21 B1 C27 110.1(3) . . ?
C39 B1 C27 108.9(3) . . ?
C21 B1 C33 108.9(3) . . ?
C39 B1 C33 108.6(3) . . ?
C27 B1 C33 109.9(3) . . ?
C9 N2 C5 109.2(3) . . ?
C9 N2 C1 110.4(3) . . ?
C5 N2 C1 111.3(3) . . ?
C9 N2 Pd1 115.2(2) . . ?
C5 N2 Pd1 104.5(2) . . ?
C1 N2 Pd1 106.1(2) . . ?
C3 N3 C2 115.6(3) . . ?
C3 N3 Pd1 107.5(2) . . ?
C2 N3 Pd1 106.9(2) . . ?
C3 N3 H3 113(2) . . ?
C2 N3 H3 104(2) . . ?
Pd1 N3 H3 109(2) . . ?
C17 N4 C4 110.7(3) . . ?
C17 N4 C13 109.9(3) . . ?
C4 N4 C13 111.6(3) . . ?
C17 N4 Pd1 115.2(2) . . ?
C4 N4 Pd1 105.1(2) . . ?
C13 N4 Pd1 104.1(2) . . ?
C45 O3 C48 107.5(3) . . ?
N3 Pd1 O1A_b 172.43(13) . . ?
N3 Pd1 N2 85.61(12) . . ?
O1A_b Pd1 N2 93.88(14) . . ?
N3 Pd1 N1_a 174.7(5) . . ?
N2 Pd1 N1_a 94.3(6) . . ?
N3 Pd1 N4 85.43(11) . . ?
O1A_b Pd1 N4 93.74(14) . . ?
N2 Pd1 N4 166.89(11) . . ?
N1_a Pd1 N4 95.5(5) . . ?
O1_a N1_a O2_a 129(2) . . ?
O1_a N1_a Pd1 111.3(14) . . ?
O2_a N1_a Pd1 119.7(17) . . ?
O2A_b N1A_b O1A_b 113.4(5) . . ?
N1A_b O1A_b Pd1 120.2(3) . . ?

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
N2 C1 C2 N3 54.7(4) . . . . ?
N3 C3 C4 N4 -54.5(4) . . . . ?
N2 C5 C6 C7 -178.9(3) . . . . ?
C5 C6 C7 C8 -171.8(3) . . . . ?
N2 C9 C10 C11 170.8(3) . . . . ?
C9 C10 C11 C12 172.7(3) . . . . ?
N4 C13 C14 C15 178.4(3) . . . . ?
C13 C14 C15 C16 179.5(3) . . . . ?
N4 C17 C18 C19 -169.8(3) . . . . ?
C17 C18 C19 C20 -169.6(4) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
B1 C21 C22 C23 177.9(3) . . . . ?
C21 C22 C23 C24 -0.4(6) . . . . ?
C22 C23 C24 C25 0.0(6) . . . . ?
C23 C24 C25 C26 1.0(6) . . . . ?
C24 C25 C26 C21 -1.5(6) . . . . ?
C22 C21 C26 C25 1.1(5) . . . . ?
B1 C21 C26 C25 -176.9(3) . . . . ?
C32 C27 C28 C29 -1.7(5) . . . . ?
B1 C27 C28 C29 177.6(4) . . . . ?
C27 C28 C29 C30 0.4(6) . . . . ?
C28 C29 C30 C31 0.9(6) . . . . ?
C29 C30 C31 C32 -0.8(6) . . . . ?
C30 C31 C32 C27 -0.6(6) . . . . ?
C28 C27 C32 C31 1.7(5) . . . . ?
B1 C27 C32 C31 -177.6(4) . . . . ?
C38 C33 C34 C35 0.3(6) . . . . ?
B1 C33 C34 C35 -175.0(4) . . . . ?
C33 C34 C35 C36 -0.5(7) . . . . ?
C34 C35 C36 C37 0.8(6) . . . . ?
C35 C36 C37 C38 -0.9(6) . . . . ?
C34 C33 C38 C37 -0.5(5) . . . . ?
B1 C33 C38 C37 174.8(3) . . . . ?
C36 C37 C38 C33 0.8(6) . . . . ?
C44 C39 C40 C41 1.0(6) . . . . ?
B1 C39 C40 C41 -175.6(4) . . . . ?
C39 C40 C41 C42 1.3(6) . . . . ?
C40 C41 C42 C43 -2.1(6) . . . . ?
C41 C42 C43 C44 0.7(6) . . . . ?
C42 C43 C44 C39 1.7(6) . . . . ?
C40 C39 C44 C43 -2.5(6) . . . . ?
B1 C39 C44 C43 174.2(4) . . . . ?
O3 C45 C46 C47 -34.2(5) . . . . ?
C45 C46 C47 C48 28.5(5) . . . . ?
C46 C47 C48 O3 -13.5(5) . . . . ?
C26 C21 B1 C39 -149.2(3) . . . . ?
C22 C21 B1 C39 33.0(5) . . . . ?
C26 C21 B1 C27 -29.0(5) . . . . ?
C22 C21 B1 C27 153.2(3) . . . . ?
C26 C21 B1 C33 91.6(4) . . . . ?
C22 C21 B1 C33 -86.2(4) . . . . ?
C40 C39 B1 C21 -135.7(4) . . . . ?
C44 C39 B1 C21 47.9(5) . . . . ?
C40 C39 B1 C27 103.3(4) . . . . ?
C44 C39 B1 C27 -73.1(5) . . . . ?
C40 C39 B1 C33 -16.3(5) . . . . ?
C44 C39 B1 C33 167.3(4) . . . . ?
C28 C27 B1 C21 -105.2(4) . . . . ?
C32 C27 B1 C21 74.1(4) . . . . ?
C28 C27 B1 C39 16.0(5) . . . . ?
C32 C27 B1 C39 -164.8(3) . . . . ?
C28 C27 B1 C33 134.8(4) . . . . ?
C32 C27 B1 C33 -45.9(4) . . . . ?
C38 C33 B1 C21 38.5(4) . . . . ?
C34 C33 B1 C21 -146.5(3) . . . . ?
C38 C33 B1 C39 -81.8(4) . . . . ?
C34 C33 B1 C39 93.2(4) . . . . ?
C38 C33 B1 C27 159.2(3) . . . . ?
C34 C33 B1 C27 -25.8(5) . . . . ?
C10 C9 N2 C5 -173.8(3) . . . . ?
C10 C9 N2 C1 63.5(4) . . . . ?
C10 C9 N2 Pd1 -56.6(4) . . . . ?
C6 C5 N2 C9 -55.4(4) . . . . ?
C6 C5 N2 C1 66.7(4) . . . . ?
C6 C5 N2 Pd1 -179.2(3) . . . . ?
C2 C1 N2 C9 -159.9(3) . . . . ?
C2 C1 N2 C5 78.7(4) . . . . ?
C2 C1 N2 Pd1 -34.4(3) . . . . ?
C4 C3 N3 C2 166.3(3) . . . . ?
C4 C3 N3 Pd1 47.0(3) . . . . ?
C1 C2 N3 C3 -166.3(3) . . . . ?
C1 C2 N3 Pd1 -46.7(4) . . . . ?
C18 C17 N4 C4 -60.9(4) . . . . ?
C18 C17 N4 C13 175.3(3) . . . . ?
C18 C17 N4 Pd1 58.2(4) . . . . ?
C3 C4 N4 C17 158.6(3) . . . . ?
C3 C4 N4 C13 -78.7(3) . . . . ?
C3 C4 N4 Pd1 33.5(3) . . . . ?
C14 C13 N4 C17 58.6(4) . . . . ?
C14 C13 N4 C4 -64.6(4) . . . . ?
C14 C13 N4 Pd1 -177.5(3) . . . . ?
C46 C45 O3 C48 27.1(5) . . . . ?
C47 C48 O3 C45 -8.7(5) . . . . ?
O2A_b N1A_b O1A_b Pd1 -1.0(5) . . . . ?

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
C5 H5B O1_a 0.99 2.54 3.349(14) 138.7 .
C5 H5B O1A_b 0.99 2.55 3.177(5) 121.0 .
C10 H10A O2A_b 0.99 2.55 3.277(6) 130.3 .
C13 H13A O1_a 0.99 2.55 3.337(14) 136.4 .
C18 H18B O2A_b 0.99 2.54 3.192(6) 123.0 .
C46 H46B O1_a 0.99 2.54 3.299(16) 133.6 1_455
N3 H3 O3 0.974(19) 1.96(2) 2.921(4) 168(3) .

_refine_diff_density_max         1.042
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.104

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_10minUV
_database_code_depnum_ccdc_archive 'CCDC 1441784'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_10minUV             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially excited nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_10minUV             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         16 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.4937(3)
_cell_length_b                   13.3810(4)
_cell_length_c                   29.9575(10)
_cell_angle_alpha                90
_cell_angle_beta                 94.717(3)
_cell_angle_gamma                90
_cell_volume                     4591.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6036
_cell_measurement_theta_min      3.3290
_cell_measurement_theta_max      28.9120

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.68161
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            18404
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.120
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             9284
_reflns_number_gt                6918
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0417P)²+2.6489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9284
_refine_ls_number_parameters     504
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0466
_refine_ls_wR_factor_ref         0.1046
_refine_ls_wR_factor_gt          0.0929
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.025
_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
C1 C 0.5485(3) 0.9635(2) 0.62792(11) 0.0207(7) Uani 1 1 d . . . . .
H1A H 0.4736 0.9579 0.6419 0.025 Uiso 1 1 calc R U . . .
H1B H 0.5601 1.0344 0.6201 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5441(3) 0.9001(2) 0.58617(11) 0.0220(7) Uani 1 1 d . . . . .
H2A H 0.4750 0.9178 0.5658 0.026 Uiso 1 1 calc R U . . .
H2B H 0.6151 0.9109 0.5702 0.026 Uiso 1 1 calc R U . . .
C3 C 0.5594(3) 0.7179(2) 0.56622(10) 0.0166(6) Uani 1 1 d . . . . .
H3A H 0.6297 0.7357 0.5510 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4920 0.7133 0.5435 0.020 Uiso 1 1 calc R U . . .
C4 C 0.5774(3) 0.6197(2) 0.59096(10) 0.0175(7) Uani 1 1 d . . . . .
H4A H 0.5035 0.5992 0.6031 0.021 Uiso 1 1 calc R U . . .
H4B H 0.5993 0.5673 0.5698 0.021 Uiso 1 1 calc R U . . .
C5 C 0.7625(3) 0.9677(2) 0.64744(11) 0.0224(7) Uani 1 1 d . . . . .
H5A H 0.7713 0.9469 0.6162 0.027 Uiso 1 1 calc R U . . .
H5B H 0.8254 0.9346 0.6666 0.027 Uiso 1 1 calc R U . . .
C6 C 0.7819(3) 1.0804(2) 0.65060(12) 0.0233(7) Uani 1 1 d . . . . .
H6A H 0.7202 1.1150 0.6314 0.028 Uiso 1 1 calc R U . . .
H6B H 0.7761 1.1025 0.6819 0.028 Uiso 1 1 calc R U . . .
C7 C 0.9011(3) 1.1088(2) 0.63583(13) 0.0284(8) Uani 1 1 d . . . . .
H7A H 0.9618 1.0669 0.6520 0.034 Uiso 1 1 calc R U . . .
H7B H 0.9028 1.0956 0.6034 0.034 Uiso 1 1 calc R U . . .
C8 C 0.9277(3) 1.2181(3) 0.64513(14) 0.0352(9) Uani 1 1 d . . . . .
H8A H 0.9328 1.2299 0.6775 0.053 Uiso 1 1 calc R U . . .
H8B H 0.8654 1.2594 0.6305 0.053 Uiso 1 1 calc R U . . .
H8C H 1.0022 1.2355 0.6334 0.053 Uiso 1 1 calc R U . . .
C9 C 0.6292(3) 0.9624(2) 0.70698(11) 0.0191(7) Uani 1 1 d . . . . .
H9A H 0.6240 1.0363 0.7071 0.023 Uiso 1 1 calc R U . . .
H9B H 0.6987 0.9435 0.7269 0.023 Uiso 1 1 calc R U . . .
C10 C 0.5214(3) 0.9206(2) 0.72667(11) 0.0211(7) Uani 1 1 d . . . . .
H10A H 0.4503 0.9490 0.7106 0.025 Uiso 1 1 calc R U . . .
H10B H 0.5191 0.8471 0.7229 0.025 Uiso 1 1 calc R U . . .
C11 C 0.5242(3) 0.9466(3) 0.77608(11) 0.0248(8) Uani 1 1 d . . . . .
H11A H 0.5381 1.0193 0.7798 0.030 Uiso 1 1 calc R U . . .
H11B H 0.5904 0.9112 0.7924 0.030 Uiso 1 1 calc R U . . .
C12 C 0.4122(3) 0.9192(3) 0.79691(13) 0.0331(9) Uani 1 1 d . . . . .
H12A H 0.4209 0.9339 0.8291 0.050 Uiso 1 1 calc R U . . .
H12B H 0.3964 0.8478 0.7924 0.050 Uiso 1 1 calc R U . . .
H12C H 0.3472 0.9582 0.7826 0.050 Uiso 1 1 calc R U . . .
C13 C 0.7917(3) 0.6241(2) 0.61195(11) 0.0174(7) Uani 1 1 d . . . . .
H13A H 0.8496 0.6386 0.6374 0.021 Uiso 1 1 calc R U . . .
H13B H 0.7976 0.6781 0.5897 0.021 Uiso 1 1 calc R U . . .
C14 C 0.8261(3) 0.5264(2) 0.59065(12) 0.0210(7) Uani 1 1 d . . . . .
H14A H 0.7687 0.5101 0.5652 0.025 Uiso 1 1 calc R U . . .
H14B H 0.8247 0.4718 0.6129 0.025 Uiso 1 1 calc R U . . .
C15 C 0.9476(3) 0.5334(2) 0.57399(12) 0.0230(7) Uani 1 1 d . . . . .
H15A H 0.9482 0.5880 0.5517 0.028 Uiso 1 1 calc R U . . .
H15B H 1.0042 0.5509 0.5995 0.028 Uiso 1 1 calc R U . . .
C16 C 0.9869(3) 0.4375(2) 0.55279(12) 0.0266(8) Uani 1 1 d . . . . .
H16A H 1.0647 0.4472 0.5423 0.040 Uiso 1 1 calc R U . . .
H16B H 0.9316 0.4198 0.5274 0.040 Uiso 1 1 calc R U . . .
H16C H 0.9899 0.3836 0.5750 0.040 Uiso 1 1 calc R U . . .
C17 C 0.6591(3) 0.5482(2) 0.66261(10) 0.0174(7) Uani 1 1 d . . . . .
H17A H 0.7239 0.5543 0.6863 0.021 Uiso 1 1 calc R U . . .
H17B H 0.6672 0.4827 0.6478 0.021 Uiso 1 1 calc R U . . .
C18 C 0.5448(3) 0.5493(2) 0.68438(11) 0.0209(7) Uani 1 1 d . . . . .
H18A H 0.4808 0.5281 0.6623 0.025 Uiso 1 1 calc R U . . .
H18B H 0.5279 0.6181 0.6941 0.025 Uiso 1 1 calc R U . . .
C19 C 0.5499(3) 0.4798(3) 0.72457(13) 0.0309(8) Uani 1 1 d . . . . .
H19A H 0.5823 0.4146 0.7161 0.037 Uiso 1 1 calc R U . . .
H19B H 0.6034 0.5085 0.7489 0.037 Uiso 1 1 calc R U . . .
C20 C 0.4314(3) 0.4632(3) 0.74190(13) 0.0379(10) Uani 1 1 d . . . . .
H20A H 0.4404 0.4233 0.7694 0.057 Uiso 1 1 calc R U . . .
H20B H 0.3808 0.4277 0.7192 0.057 Uiso 1 1 calc R U . . .
H20C H 0.3964 0.5279 0.7483 0.057 Uiso 1 1 calc R U . . .
C21 C 0.4927(3) 0.2316(2) 0.55719(10) 0.0162(6) Uani 1 1 d . . . . .
C22 C 0.5869(3) 0.2965(2) 0.56681(11) 0.0214(7) Uani 1 1 d . . . . .
H22 H 0.5736 0.3567 0.5824 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6989(3) 0.2773(2) 0.55465(11) 0.0221(7) Uani 1 1 d . . . . .
H23 H 0.7595 0.3245 0.5615 0.026 Uiso 1 1 calc R U . . .
C24 C 0.7226(3) 0.1901(2) 0.53263(11) 0.0213(7) Uani 1 1 d . . . . .
H24 H 0.7990 0.1762 0.5245 0.026 Uiso 1 1 calc R U . . .
C25 C 0.6323(3) 0.1231(2) 0.52273(11) 0.0201(7) Uani 1 1 d . . . . .
H25 H 0.6466 0.0624 0.5077 0.024 Uiso 1 1 calc R U . . .
C26 C 0.5209(3) 0.1446(2) 0.53469(10) 0.0172(7) Uani 1 1 d . . . . .
H26 H 0.4606 0.0976 0.5271 0.021 Uiso 1 1 calc R U . . .
C27 C 0.2621(3) 0.2001(2) 0.53928(11) 0.0179(7) Uani 1 1 d . . . . .
C28 C 0.1891(3) 0.2486(2) 0.50681(11) 0.0208(7) Uani 1 1 d . . . . .
H28 H 0.1947 0.3192 0.5044 0.025 Uiso 1 1 calc R U . . .
C29 C 0.1084(3) 0.1987(3) 0.47771(12) 0.0268(8) Uani 1 1 d . . . . .
H29 H 0.0611 0.2353 0.4559 0.032 Uiso 1 1 calc R U . . .
C30 C 0.0967(3) 0.0967(3) 0.48033(12) 0.0277(8) Uani 1 1 d . . . . .
H30 H 0.0423 0.0623 0.4602 0.033 Uiso 1 1 calc R U . . .
C31 C 0.1647(3) 0.0452(3) 0.51244(13) 0.0273(8) Uani 1 1 d . . . . .
H31 H 0.1568 -0.0252 0.5150 0.033 Uiso 1 1 calc R U . . .
C32 C 0.2449(3) 0.0961(2) 0.54113(12) 0.0243(8) Uani 1 1 d . . . . .
H32 H 0.2905 0.0589 0.5632 0.029 Uiso 1 1 calc R U . . .
C33 C 0.3551(3) 0.2132(2) 0.62464(11) 0.0196(7) Uani 1 1 d . . . . .
C34 C 0.2519(3) 0.1755(3) 0.63998(12) 0.0307(8) Uani 1 1 d . . . . .
H34 H 0.1852 0.1695 0.6192 0.037 Uiso 1 1 calc R U . . .
C35 C 0.2424(3) 0.1467(3) 0.68385(13) 0.0367(9) Uani 1 1 d . . . . .
H35 H 0.1706 0.1208 0.6925 0.044 Uiso 1 1 calc R U . . .
C36 C 0.3367(3) 0.1552(3) 0.71504(12) 0.0321(9) Uani 1 1 d . . . . .
H36 H 0.3306 0.1357 0.7453 0.039 Uiso 1 1 calc R U . . .
C37 C 0.4400(3) 0.1925(3) 0.70166(12) 0.0280(8) Uani 1 1 d . . . . .
H37 H 0.5058 0.1990 0.7228 0.034 Uiso 1 1 calc R U . . .
C38 C 0.4484(3) 0.2207(2) 0.65765(11) 0.0224(7) Uani 1 1 d . . . . .
H38 H 0.5206 0.2463 0.6494 0.027 Uiso 1 1 calc R U . . .
C39 C 0.3379(2) 0.3763(2) 0.57286(11) 0.0167(7) Uani 1 1 d . . . . .
C40 C 0.2879(3) 0.4271(2) 0.60709(11) 0.0205(7) Uani 1 1 d . . . . .
H40 H 0.2718 0.3915 0.6333 0.025 Uiso 1 1 calc R U . . .
C41 C 0.2608(3) 0.5282(2) 0.60402(13) 0.0281(8) Uani 1 1 d . . . . .
H41 H 0.2276 0.5603 0.6283 0.034 Uiso 1 1 calc R U . . .
C42 C 0.2811(3) 0.5827(2) 0.56646(13) 0.0282(8) Uani 1 1 d . . . . .
H42 H 0.2601 0.6513 0.5642 0.034 Uiso 1 1 calc R U . . .
C43 C 0.3329(3) 0.5354(2) 0.53219(12) 0.0255(8) Uani 1 1 d . . . . .
H43 H 0.3487 0.5717 0.5061 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3617(3) 0.4348(2) 0.53594(11) 0.0216(7) Uani 1 1 d . . . . .
H44 H 0.3992 0.4043 0.5124 0.026 Uiso 1 1 calc R U . . .
C45 C 0.2601(3) 0.7645(3) 0.67632(14) 0.0419(7) Uani 1 1 d . . . . .
H45A H 0.2769 0.8090 0.7025 0.050 Uiso 1 1 calc R U . . .
H45B H 0.2927 0.6975 0.6837 0.050 Uiso 1 1 calc R U . . .
C46 C 0.1290(3) 0.7581(3) 0.66385(16) 0.0482(8) Uani 1 1 d . . . . .
H46A H 0.1077 0.6953 0.6477 0.058 Uiso 1 1 calc R U . . .
H46B H 0.0842 0.7633 0.6906 0.058 Uiso 1 1 calc R U . . .
C47 C 0.1092(3) 0.8485(3) 0.63357(15) 0.0482(8) Uani 1 1 d . . . . .
H47A H 0.0461 0.8354 0.6098 0.058 Uiso 1 1 calc R U . . .
H47B H 0.0879 0.9077 0.6510 0.058 Uiso 1 1 calc R U . . .
C48 C 0.2216(3) 0.8648(3) 0.61403(15) 0.0419(7) Uani 1 1 d . . . . .
H48A H 0.2142 0.8463 0.5819 0.050 Uiso 1 1 calc R U . . .
H48B H 0.2439 0.9361 0.6165 0.050 Uiso 1 1 calc R U . . .
B1 B 0.3617(3) 0.2555(3) 0.57338(12) 0.0186(8) Uani 1 1 d . . . . .
N2 N 0.6474(2) 0.92901(18) 0.66054(9) 0.0186(6) Uani 1 1 d . . . . .
N3 N 0.5370(2) 0.79407(18) 0.60066(9) 0.0171(6) Uani 1 1 d D . . . .
N4 N 0.6717(2) 0.62896(17) 0.62878(9) 0.0154(5) Uani 1 1 d . . . . .
O3 O 0.3088(2) 0.80439(18) 0.63769(8) 0.0331(6) Uani 1 1 d . . . . .
Pd1 Pd 0.65833(2) 0.77504(2) 0.65211(2) 0.01507(8) Uani 1 1 d . . . . .
N1_a N 0.769(2) 0.757(3) 0.7087(10) 0.0307(9) Uiso 0.094(5) 1 d D . P A 1
O1_a O 0.865(2) 0.765(2) 0.7027(9) 0.0333(8) Uiso 0.094(5) 1 d D . P A 1
O2_a O 0.740(3) 0.730(2) 0.7437(9) 0.0333(8) Uiso 0.094(5) 1 d D . P A 1
N1A_b N 0.7793(3) 0.7320(3) 0.73885(12) 0.0307(9) Uiso 0.906(5) 1 d D . P A 2
O1A_b O 0.7972(2) 0.7600(2) 0.69858(9) 0.0234(7) Uiso 0.906(5) 1 d D . P A 2
O2A_b O 0.6769(3) 0.7175(2) 0.74540(9) 0.0333(8) Uiso 0.906(5) 1 d D . P A 2
H3 H 0.461(2) 0.785(3) 0.6110(12) 0.040 Uiso 1 1 d D 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
C1 C2 1.509(4) . ?
C1 N2 1.509(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.488(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.487(4) . ?
C3 C4 1.515(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.508(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.502(4) . ?
C5 C6 1.526(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.522(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.515(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.492(4) . ?
C9 C10 1.521(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.518(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.521(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.508(4) . ?
C13 C14 1.522(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.524(4) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.517(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.497(4) . ?
C17 C18 1.514(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.518(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.513(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.397(4) . ?
C21 C22 1.400(4) . ?
C21 B1 1.650(4) . ?
C22 C23 1.391(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.379(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.384(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.387(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.392(5) . ?
C27 C32 1.407(4) . ?
C27 B1 1.647(5) . ?
C28 C29 1.390(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.374(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.374(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.400(4) . ?
C33 C38 1.401(5) . ?
C33 B1 1.644(5) . ?
C34 C35 1.383(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.375(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.378(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.382(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.393(4) . ?
C39 C44 1.400(4) . ?
C39 B1 1.639(4) . ?
C40 C41 1.391(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.381(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(4) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.430(4) . ?
C45 C46 1.525(5) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.518(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.477(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.430(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N2 Pd1 2.081(2) . ?
N3 Pd1 2.008(3) . ?
N3 H3 0.961(18) . ?
N4 Pd1 2.086(2) . ?
Pd1 O1A_b 2.040(3) . ?
Pd1 N1_a 2.04(3) . ?
N1_a O1_a 1.142(19) . ?
N1_a O2_a 1.187(19) . ?
N1A_b O2A_b 1.225(4) . ?
N1A_b O1A_b 1.296(4) . ?

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
C2 C1 N2 109.7(2) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.0(3) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.2(2) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.7 . . ?
N4 C4 C3 110.9(2) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.8(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.0(3) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 111.1(3) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.6(3) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C11 C10 C9 109.9(3) . . ?
C11 C10 H10A 109.7 . . ?
C9 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
C9 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C10 C11 C12 113.2(3) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.0(2) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C13 C14 C15 111.2(2) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C14 113.4(3) . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15B 108.9 . . ?
C14 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 114.9(2) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.0(3) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 112.6(3) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.2(3) . . ?
C26 C21 B1 123.9(3) . . ?
C22 C21 B1 121.9(3) . . ?
C23 C22 C21 123.3(3) . . ?
C23 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
C24 C23 C22 120.3(3) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.5(3) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C24 C25 C26 120.1(3) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 123.6(3) . . ?
C25 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C28 C27 C32 114.2(3) . . ?
C28 C27 B1 124.9(3) . . ?
C32 C27 B1 120.9(3) . . ?
C29 C28 C27 123.2(3) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C30 C29 C28 120.3(3) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C31 119.0(3) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C30 C31 C32 119.9(3) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 123.3(3) . . ?
C31 C32 H32 118.3 . . ?
C27 C32 H32 118.3 . . ?
C34 C33 C38 114.4(3) . . ?
C34 C33 B1 122.4(3) . . ?
C38 C33 B1 122.9(3) . . ?
C35 C34 C33 123.2(3) . . ?
C35 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?
C36 C35 C34 120.2(3) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C35 C36 C37 118.8(3) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C36 C37 C38 120.4(3) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C37 C38 C33 123.0(3) . . ?
C37 C38 H38 118.5 . . ?
C33 C38 H38 118.5 . . ?
C40 C39 C44 115.3(3) . . ?
C40 C39 B1 123.5(3) . . ?
C44 C39 B1 121.0(3) . . ?
C41 C40 C39 122.0(3) . . ?
C41 C40 H40 119.0 . . ?
C39 C40 H40 119.0 . . ?
C42 C41 C40 121.1(3) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C43 118.5(3) . . ?
C41 C42 H42 120.7 . . ?
C43 C42 H42 120.7 . . ?
C42 C43 C44 119.9(3) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C39 123.0(3) . . ?
C43 C44 H44 118.5 . . ?
C39 C44 H44 118.5 . . ?
O3 C45 C46 105.5(3) . . ?
O3 C45 H45A 110.6 . . ?
C46 C45 H45A 110.6 . . ?
O3 C45 H45B 110.6 . . ?
C46 C45 H45B 110.6 . . ?
H45A C45 H45B 108.8 . . ?
C47 C46 C45 101.4(3) . . ?
C47 C46 H46A 111.5 . . ?
C45 C46 H46A 111.5 . . ?
C47 C46 H46B 111.5 . . ?
C45 C46 H46B 111.5 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 105.2(3) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
O3 C48 C47 108.7(3) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C39 B1 C33 109.1(3) . . ?
C39 B1 C27 109.3(3) . . ?
C33 B1 C27 109.9(3) . . ?
C39 B1 C21 110.1(2) . . ?
C33 B1 C21 108.7(3) . . ?
C27 B1 C21 109.6(3) . . ?
C9 N2 C5 109.5(2) . . ?
C9 N2 C1 110.8(2) . . ?
C5 N2 C1 111.0(2) . . ?
C9 N2 Pd1 115.11(19) . . ?
C5 N2 Pd1 104.27(18) . . ?
C1 N2 Pd1 105.89(18) . . ?
C3 N3 C2 115.7(2) . . ?
C3 N3 Pd1 107.28(18) . . ?
C2 N3 Pd1 107.07(18) . . ?
C3 N3 H3 110(2) . . ?
C2 N3 H3 107(2) . . ?
Pd1 N3 H3 109(2) . . ?
C17 N4 C4 110.2(2) . . ?
C17 N4 C13 109.7(2) . . ?
C4 N4 C13 111.5(2) . . ?
C17 N4 Pd1 115.83(19) . . ?
C4 N4 Pd1 105.11(17) . . ?
C13 N4 Pd1 104.32(16) . . ?
C48 O3 C45 107.9(3) . . ?
N3 Pd1 O1A_b 172.50(10) . . ?
N3 Pd1 N1_a 174.2(8) . . ?
N3 Pd1 N2 85.56(10) . . ?
O1A_b Pd1 N2 93.80(11) . . ?
N1_a Pd1 N2 93.0(11) . . ?
N3 Pd1 N4 85.83(10) . . ?
O1A_b Pd1 N4 93.51(11) . . ?
N1_a Pd1 N4 96.4(11) . . ?
N2 Pd1 N4 167.26(10) . . ?
O1_a N1_a O2_a 121(2) . . ?
O1_a N1_a Pd1 114(2) . . ?
O2_a N1_a Pd1 125(2) . . ?
O2A_b N1A_b O1A_b 115.0(3) . . ?
N1A_b O1A_b Pd1 119.3(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
N2 C1 C2 N3 54.5(3) . . . . ?
N3 C3 C4 N4 -54.3(3) . . . . ?
N2 C5 C6 C7 -179.3(3) . . . . ?
C5 C6 C7 C8 -171.9(3) . . . . ?
N2 C9 C10 C11 170.7(3) . . . . ?
C9 C10 C11 C12 172.6(3) . . . . ?
N4 C13 C14 C15 178.3(3) . . . . ?
C13 C14 C15 C16 179.5(3) . . . . ?
N4 C17 C18 C19 -168.1(3) . . . . ?
C17 C18 C19 C20 -169.0(3) . . . . ?
C26 C21 C22 C23 0.7(5) . . . . ?
B1 C21 C22 C23 178.3(3) . . . . ?
C21 C22 C23 C24 -1.1(5) . . . . ?
C22 C23 C24 C25 0.5(5) . . . . ?
C23 C24 C25 C26 0.3(5) . . . . ?
C24 C25 C26 C21 -0.7(5) . . . . ?
C22 C21 C26 C25 0.1(5) . . . . ?
B1 C21 C26 C25 -177.4(3) . . . . ?
C32 C27 C28 C29 -1.8(4) . . . . ?
B1 C27 C28 C29 178.0(3) . . . . ?
C27 C28 C29 C30 0.6(5) . . . . ?
C28 C29 C30 C31 0.8(5) . . . . ?
C29 C30 C31 C32 -1.0(5) . . . . ?
C30 C31 C32 C27 -0.4(5) . . . . ?
C28 C27 C32 C31 1.7(4) . . . . ?
B1 C27 C32 C31 -178.1(3) . . . . ?
C38 C33 C34 C35 -0.8(5) . . . . ?
B1 C33 C34 C35 -175.0(3) . . . . ?
C33 C34 C35 C36 0.7(6) . . . . ?
C34 C35 C36 C37 -0.2(6) . . . . ?
C35 C36 C37 C38 -0.1(5) . . . . ?
C36 C37 C38 C33 -0.1(5) . . . . ?
C34 C33 C38 C37 0.5(5) . . . . ?
B1 C33 C38 C37 174.6(3) . . . . ?
C44 C39 C40 C41 1.6(4) . . . . ?
B1 C39 C40 C41 -175.0(3) . . . . ?
C39 C40 C41 C42 0.8(5) . . . . ?
C40 C41 C42 C43 -2.1(5) . . . . ?
C41 C42 C43 C44 0.8(5) . . . . ?
C42 C43 C44 C39 1.8(5) . . . . ?
C40 C39 C44 C43 -2.9(4) . . . . ?
B1 C39 C44 C43 173.8(3) . . . . ?
O3 C45 C46 C47 -33.8(4) . . . . ?
C45 C46 C47 C48 27.2(5) . . . . ?
C46 C47 C48 O3 -11.8(5) . . . . ?
C40 C39 B1 C33 -16.7(4) . . . . ?
C44 C39 B1 C33 166.9(3) . . . . ?
C40 C39 B1 C27 103.6(3) . . . . ?
C44 C39 B1 C27 -72.9(3) . . . . ?
C40 C39 B1 C21 -136.0(3) . . . . ?
C44 C39 B1 C21 47.6(4) . . . . ?
C34 C33 B1 C39 92.7(4) . . . . ?
C38 C33 B1 C39 -81.0(3) . . . . ?
C34 C33 B1 C27 -27.3(4) . . . . ?
C38 C33 B1 C27 159.1(3) . . . . ?
C34 C33 B1 C21 -147.2(3) . . . . ?
C38 C33 B1 C21 39.2(4) . . . . ?
C28 C27 B1 C39 15.4(4) . . . . ?
C32 C27 B1 C39 -164.8(3) . . . . ?
C28 C27 B1 C33 135.2(3) . . . . ?
C32 C27 B1 C33 -45.0(4) . . . . ?
C28 C27 B1 C21 -105.4(3) . . . . ?
C32 C27 B1 C21 74.4(3) . . . . ?
C26 C21 B1 C39 -149.3(3) . . . . ?
C22 C21 B1 C39 33.3(4) . . . . ?
C26 C21 B1 C33 91.1(4) . . . . ?
C22 C21 B1 C33 -86.2(3) . . . . ?
C26 C21 B1 C27 -29.1(4) . . . . ?
C22 C21 B1 C27 153.6(3) . . . . ?
C10 C9 N2 C5 -174.3(3) . . . . ?
C10 C9 N2 C1 62.9(3) . . . . ?
C10 C9 N2 Pd1 -57.2(3) . . . . ?
C6 C5 N2 C9 -55.7(4) . . . . ?
C6 C5 N2 C1 67.0(3) . . . . ?
C6 C5 N2 Pd1 -179.4(2) . . . . ?
C2 C1 N2 C9 -159.4(2) . . . . ?
C2 C1 N2 C5 78.6(3) . . . . ?
C2 C1 N2 Pd1 -34.0(3) . . . . ?
C4 C3 N3 C2 166.3(2) . . . . ?
C4 C3 N3 Pd1 46.8(3) . . . . ?
C1 C2 N3 C3 -166.4(2) . . . . ?
C1 C2 N3 Pd1 -46.9(3) . . . . ?
C18 C17 N4 C4 -60.7(3) . . . . ?
C18 C17 N4 C13 176.2(3) . . . . ?
C18 C17 N4 Pd1 58.5(3) . . . . ?
C3 C4 N4 C17 158.8(2) . . . . ?
C3 C4 N4 C13 -79.1(3) . . . . ?
C3 C4 N4 Pd1 33.4(3) . . . . ?
C14 C13 N4 C17 57.8(3) . . . . ?
C14 C13 N4 C4 -64.6(3) . . . . ?
C14 C13 N4 Pd1 -177.5(2) . . . . ?
C47 C48 O3 C45 -10.1(4) . . . . ?
C46 C45 O3 C48 27.9(4) . . . . ?
O2A_b N1A_b O1A_b Pd1 -0.6(4) . . . . ?

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
C5 H5B O1_a 0.99 2.54 3.34(3) 138.1 .
C5 H5B O1A_b 0.99 2.56 3.182(4) 121.2 .
C10 H10B O2A_b 0.99 2.56 3.276(4) 129.1 .
C13 H13A O1_a 0.99 2.58 3.36(3) 135.5 .
C18 H18B O2A_b 0.99 2.57 3.202(4) 121.3 .
C46 H46B O1_a 0.99 2.57 3.34(2) 133.9 1_455
N3 H3 O3 0.961(18) 2.00(2) 2.934(3) 164(3) .

_refine_diff_density_max         1.058
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.087

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_15minUV
_database_code_depnum_ccdc_archive 'CCDC 1441785'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_15minUV             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         14 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.4854(3)
_cell_length_b                   13.3693(3)
_cell_length_c                   30.0108(8)
_cell_angle_alpha                90
_cell_angle_beta                 94.639(2)
_cell_angle_gamma                90
_cell_volume                     4593.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    11334
_cell_measurement_theta_min      3.4680
_cell_measurement_theta_max      29.4960

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.448
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.76742
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            33768
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.012
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9369
_reflns_number_gt                7368
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0286P)²+2.4176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9369
_refine_ls_number_parameters     521
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0667
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.007
_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
C1 C 0.5483(2) 0.96340(16) 0.62804(7) 0.0223(5) Uani 1 1 d . . . . .
H1A H 0.5596 1.0345 0.6203 0.027 Uiso 1 1 calc R U . . .
H1B H 0.4737 0.9575 0.6422 0.027 Uiso 1 1 calc R U . . .
C2 C 0.5436(2) 0.90022(16) 0.58617(7) 0.0223(5) Uani 1 1 d . . . . .
H2A H 0.4741 0.9179 0.5660 0.027 Uiso 1 1 calc R U . . .
H2B H 0.6143 0.9112 0.5700 0.027 Uiso 1 1 calc R U . . .
C3 C 0.55950(19) 0.71794(15) 0.56633(7) 0.0178(5) Uani 1 1 d . . . . .
H3A H 0.6301 0.7357 0.5512 0.021 Uiso 1 1 calc R U . . .
H3B H 0.4923 0.7134 0.5436 0.021 Uiso 1 1 calc R U . . .
C4 C 0.57724(18) 0.61951(15) 0.59089(7) 0.0177(5) Uani 1 1 d . . . . .
H4A H 0.5032 0.5990 0.6030 0.021 Uiso 1 1 calc R U . . .
H4B H 0.5993 0.5672 0.5698 0.021 Uiso 1 1 calc R U . . .
C5 C 0.76276(19) 0.96804(16) 0.64737(8) 0.0211(5) Uani 1 1 d . . . . .
H5A H 0.7721 0.9472 0.6162 0.025 Uiso 1 1 calc R U . . .
H5B H 0.8255 0.9351 0.6666 0.025 Uiso 1 1 calc R U . . .
C6 C 0.7818(2) 1.08053(16) 0.65047(8) 0.0241(5) Uani 1 1 d . . . . .
H6A H 0.7202 1.1150 0.6313 0.029 Uiso 1 1 calc R U . . .
H6B H 0.7757 1.1027 0.6817 0.029 Uiso 1 1 calc R U . . .
C7 C 0.9009(2) 1.10925(18) 0.63585(9) 0.0290(6) Uani 1 1 d . . . . .
H7A H 0.9616 1.0674 0.6520 0.035 Uiso 1 1 calc R U . . .
H7B H 0.9029 1.0959 0.6035 0.035 Uiso 1 1 calc R U . . .
C8 C 0.9281(2) 1.21889(18) 0.64499(9) 0.0347(6) Uani 1 1 d . . . . .
H8A H 0.9342 1.2308 0.6773 0.052 Uiso 1 1 calc R U . . .
H8B H 0.8655 1.2604 0.6307 0.052 Uiso 1 1 calc R U . . .
H8C H 1.0023 1.2362 0.6329 0.052 Uiso 1 1 calc R U . . .
C9 C 0.62882(19) 0.96258(16) 0.70692(7) 0.0197(5) Uani 1 1 d . . . . .
H9A H 0.6240 1.0365 0.7070 0.024 Uiso 1 1 calc R U . . .
H9B H 0.6983 0.9434 0.7268 0.024 Uiso 1 1 calc R U . . .
C10 C 0.5215(2) 0.92142(17) 0.72651(7) 0.0217(5) Uani 1 1 d . . . . .
H10A H 0.5187 0.8479 0.7226 0.026 Uiso 1 1 calc R U . . .
H10B H 0.4505 0.9502 0.7106 0.026 Uiso 1 1 calc R U . . .
C11 C 0.5243(2) 0.94704(18) 0.77602(8) 0.0256(5) Uani 1 1 d . . . . .
H11A H 0.5904 0.9113 0.7922 0.031 Uiso 1 1 calc R U . . .
H11B H 0.5385 1.0197 0.7799 0.031 Uiso 1 1 calc R U . . .
C12 C 0.4122(2) 0.9198(2) 0.79681(9) 0.0343(6) Uani 1 1 d . . . . .
H12A H 0.4204 0.9356 0.8288 0.051 Uiso 1 1 calc R U . . .
H12B H 0.3970 0.8481 0.7928 0.051 Uiso 1 1 calc R U . . .
H12C H 0.3471 0.9580 0.7822 0.051 Uiso 1 1 calc R U . . .
C13 C 0.79155(18) 0.62428(16) 0.61190(7) 0.0182(5) Uani 1 1 d . . . . .
H13A H 0.8494 0.6390 0.6373 0.022 Uiso 1 1 calc R U . . .
H13B H 0.7975 0.6783 0.5896 0.022 Uiso 1 1 calc R U . . .
C14 C 0.82653(19) 0.52640(16) 0.59066(8) 0.0208(5) Uani 1 1 d . . . . .
H14A H 0.8254 0.4719 0.6129 0.025 Uiso 1 1 calc R U . . .
H14B H 0.7692 0.5098 0.5653 0.025 Uiso 1 1 calc R U . . .
C15 C 0.94786(19) 0.53375(17) 0.57396(8) 0.0236(5) Uani 1 1 d . . . . .
H15A H 1.0045 0.5517 0.5993 0.028 Uiso 1 1 calc R U . . .
H15B H 0.9482 0.5882 0.5516 0.028 Uiso 1 1 calc R U . . .
C16 C 0.9876(2) 0.43723(17) 0.55289(8) 0.0268(5) Uani 1 1 d . . . . .
H16A H 1.0653 0.4470 0.5423 0.040 Uiso 1 1 calc R U . . .
H16B H 0.9322 0.4191 0.5276 0.040 Uiso 1 1 calc R U . . .
H16C H 0.9909 0.3835 0.5752 0.040 Uiso 1 1 calc R U . . .
C17 C 0.65908(19) 0.54862(16) 0.66273(7) 0.0188(5) Uani 1 1 d . . . . .
H17A H 0.7235 0.5556 0.6865 0.023 Uiso 1 1 calc R U . . .
H17B H 0.6682 0.4829 0.6482 0.023 Uiso 1 1 calc R U . . .
C18 C 0.54466(19) 0.54881(17) 0.68429(7) 0.0222(5) Uani 1 1 d . . . . .
H18A H 0.4812 0.5264 0.6622 0.027 Uiso 1 1 calc R U . . .
H18B H 0.5265 0.6178 0.6936 0.027 Uiso 1 1 calc R U . . .
C19 C 0.5499(2) 0.48037(18) 0.72479(8) 0.0288(6) Uani 1 1 d . . . . .
H19A H 0.5830 0.4151 0.7167 0.035 Uiso 1 1 calc R U . . .
H19B H 0.6029 0.5100 0.7489 0.035 Uiso 1 1 calc R U . . .
C20 C 0.4317(2) 0.4634(2) 0.74209(9) 0.0391(7) Uani 1 1 d . . . . .
H20A H 0.4410 0.4249 0.7699 0.059 Uiso 1 1 calc R U . . .
H20B H 0.3818 0.4263 0.7198 0.059 Uiso 1 1 calc R U . . .
H20C H 0.3955 0.5281 0.7478 0.059 Uiso 1 1 calc R U . . .
C21 C 0.49311(18) 0.23164(15) 0.55734(7) 0.0168(4) Uani 1 1 d . . . . .
C22 C 0.58716(19) 0.29695(16) 0.56684(8) 0.0223(5) Uani 1 1 d . . . . .
H22 H 0.5738 0.3574 0.5823 0.027 Uiso 1 1 calc R U . . .
C23 C 0.6992(2) 0.27741(17) 0.55471(8) 0.0235(5) Uani 1 1 d . . . . .
H23 H 0.7601 0.3244 0.5617 0.028 Uiso 1 1 calc R U . . .
C24 C 0.7225(2) 0.19003(16) 0.53261(7) 0.0215(5) Uani 1 1 d . . . . .
H24 H 0.7990 0.1761 0.5244 0.026 Uiso 1 1 calc R U . . .
C25 C 0.63224(19) 0.12302(17) 0.52260(7) 0.0213(5) Uani 1 1 d . . . . .
H25 H 0.6465 0.0624 0.5075 0.026 Uiso 1 1 calc R U . . .
C26 C 0.52074(19) 0.14457(16) 0.53470(7) 0.0178(5) Uani 1 1 d . . . . .
H26 H 0.4602 0.0977 0.5272 0.021 Uiso 1 1 calc R U . . .
C27 C 0.26204(18) 0.19994(16) 0.53942(7) 0.0192(5) Uani 1 1 d . . . . .
C28 C 0.18947(19) 0.24899(16) 0.50682(8) 0.0222(5) Uani 1 1 d . . . . .
H28 H 0.1955 0.3196 0.5043 0.027 Uiso 1 1 calc R U . . .
C29 C 0.1088(2) 0.19868(18) 0.47796(8) 0.0278(6) Uani 1 1 d . . . . .
H29 H 0.0614 0.2352 0.4562 0.033 Uiso 1 1 calc R U . . .
C30 C 0.0969(2) 0.09626(18) 0.48053(8) 0.0282(6) Uani 1 1 d . . . . .
H30 H 0.0427 0.0617 0.4605 0.034 Uiso 1 1 calc R U . . .
C31 C 0.1653(2) 0.04495(17) 0.51284(9) 0.0277(6) Uani 1 1 d . . . . .
H31 H 0.1575 -0.0255 0.5155 0.033 Uiso 1 1 calc R U . . .
C32 C 0.24542(19) 0.09617(17) 0.54135(8) 0.0249(5) Uani 1 1 d . . . . .
H32 H 0.2914 0.0591 0.5633 0.030 Uiso 1 1 calc R U . . .
C33 C 0.35499(19) 0.21368(16) 0.62485(8) 0.0210(5) Uani 1 1 d . . . . .
C34 C 0.2519(2) 0.1757(2) 0.63994(8) 0.0321(6) Uani 1 1 d . . . . .
H34 H 0.1853 0.1694 0.6192 0.038 Uiso 1 1 calc R U . . .
C35 C 0.2423(2) 0.1469(2) 0.68375(9) 0.0382(7) Uani 1 1 d . . . . .
H35 H 0.1703 0.1211 0.6924 0.046 Uiso 1 1 calc R U . . .
C36 C 0.3367(2) 0.15545(18) 0.71499(8) 0.0316(6) Uani 1 1 d . . . . .
H36 H 0.3305 0.1356 0.7451 0.038 Uiso 1 1 calc R U . . .
C37 C 0.4400(2) 0.19317(17) 0.70180(8) 0.0281(6) Uani 1 1 d . . . . .
H37 H 0.5056 0.2002 0.7230 0.034 Uiso 1 1 calc R U . . .
C38 C 0.4485(2) 0.22108(17) 0.65750(8) 0.0235(5) Uani 1 1 d . . . . .
H38 H 0.5209 0.2462 0.6491 0.028 Uiso 1 1 calc R U . . .
C39 C 0.33848(18) 0.37660(16) 0.57289(7) 0.0178(5) Uani 1 1 d . . . . .
C40 C 0.28796(19) 0.42766(17) 0.60693(8) 0.0221(5) Uani 1 1 d . . . . .
H40 H 0.2716 0.3919 0.6331 0.027 Uiso 1 1 calc R U . . .
C41 C 0.2606(2) 0.52869(18) 0.60412(9) 0.0282(6) Uani 1 1 d . . . . .
H41 H 0.2272 0.5607 0.6283 0.034 Uiso 1 1 calc R U . . .
C42 C 0.2813(2) 0.58296(17) 0.56657(9) 0.0294(6) Uani 1 1 d . . . . .
H42 H 0.2606 0.6517 0.5643 0.035 Uiso 1 1 calc R U . . .
C43 C 0.3331(2) 0.53566(17) 0.53213(8) 0.0257(5) Uani 1 1 d . . . . .
H43 H 0.3488 0.5719 0.5060 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3618(2) 0.43520(16) 0.53595(8) 0.0217(5) Uani 1 1 d . . . . .
H44 H 0.3991 0.4045 0.5124 0.026 Uiso 1 1 calc R U . . .
C45 C 0.2590(2) 0.7644(2) 0.67645(9) 0.0338(6) Uani 1 1 d . . . . .
H45A H 0.2758 0.8087 0.7026 0.041 Uiso 1 1 calc R U . . .
H45B H 0.2914 0.6972 0.6838 0.041 Uiso 1 1 calc R U . . .
C46 C 0.1288(2) 0.7582(2) 0.66419(10) 0.0376(7) Uani 1 1 d . . . . .
H46A H 0.0842 0.7652 0.6909 0.045 Uiso 1 1 calc R U . . .
H46B H 0.1073 0.6944 0.6489 0.045 Uiso 1 1 calc R U . . .
C47 C 0.1084(3) 0.8465(3) 0.63289(12) 0.0728(12) Uani 1 1 d . . . . .
H47A H 0.0471 0.8308 0.6088 0.087 Uiso 1 1 calc R U . . .
H47B H 0.0842 0.9061 0.6494 0.087 Uiso 1 1 calc R U . . .
C48 C 0.2207(3) 0.8642(2) 0.61429(11) 0.0538(8) Uani 1 1 d . . . . .
H48A H 0.2148 0.8464 0.5822 0.065 Uiso 1 1 calc R U . . .
H48B H 0.2418 0.9358 0.6172 0.065 Uiso 1 1 calc R U . . .
B1 B 0.3619(2) 0.25552(18) 0.57355(8) 0.0183(5) Uani 1 1 d . . . . .
N2 N 0.64756(15) 0.92898(13) 0.66022(6) 0.0173(4) Uani 1 1 d . . . . .
N3 N 0.53695(16) 0.79403(13) 0.60067(6) 0.0172(4) Uani 1 1 d D . . . .
N4 N 0.67171(15) 0.62899(12) 0.62865(6) 0.0153(4) Uani 1 1 d . . . . .
O3 O 0.30847(15) 0.80430(13) 0.63802(6) 0.0336(4) Uani 1 1 d . . . . .
Pd1 Pd 0.65839(2) 0.77518(2) 0.65200(2) 0.01548(5) Uani 1 1 d . . . . .
N1 N 0.7783(2) 0.73222(15) 0.73899(7) 0.0322(5) Uani 1 1 d . . . . .
O1 O 0.79712(14) 0.76057(11) 0.69857(5) 0.0265(4) Uani 1 1 d . . . . .
O2 O 0.67696(17) 0.71795(14) 0.74542(6) 0.0369(4) Uani 1 1 d . . . . .
H3 H 0.4620(17) 0.785(2) 0.6105(9) 0.044 Uiso 1 1 d D 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
C1 N2 1.505(3) . ?
C1 C2 1.511(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.489(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.486(3) . ?
C3 C4 1.514(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.510(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.502(3) . ?
C5 C6 1.522(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.519(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.519(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.504(3) . ?
C9 C10 1.511(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.523(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.520(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.504(3) . ?
C13 C14 1.524(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.522(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.523(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.499(3) . ?
C17 C18 1.511(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.519(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.509(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.397(3) . ?
C21 C22 1.400(3) . ?
C21 B1 1.652(3) . ?
C22 C23 1.391(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.380(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.397(3) . ?
C27 C32 1.402(3) . ?
C27 B1 1.651(3) . ?
C28 C29 1.390(3) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.380(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.386(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.397(3) . ?
C33 C38 1.397(3) . ?
C33 B1 1.646(3) . ?
C34 C35 1.383(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.376(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(3) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.394(3) . ?
C39 C44 1.401(3) . ?
C39 B1 1.641(3) . ?
C40 C41 1.388(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.386(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(3) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.430(3) . ?
C45 C46 1.513(3) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.514(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.465(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.431(3) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N2 Pd1 2.0759(17) . ?
N3 Pd1 2.0087(17) . ?
N3 H3 0.940(17) . ?
N4 Pd1 2.0861(17) . ?
Pd1 O1 2.0421(15) . ?
N1 O2 1.211(3) . ?
N1 O1 1.305(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
N2 C1 C2 109.70(17) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.82(18) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.36(17) . . ?
N3 C3 H3A 110.5 . . ?
C4 C3 H3A 110.5 . . ?
N3 C3 H3B 110.5 . . ?
C4 C3 H3B 110.5 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 110.66(17) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 116.96(18) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.13(19) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 111.6(2) . . ?
C8 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
C8 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.88(17) . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.14(18) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.3(2) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.07(17) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.20(18) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.27(19) . . ?
C14 C15 H15A 108.9 . . ?
C16 C15 H15A 108.9 . . ?
C14 C15 H15B 108.9 . . ?
C16 C15 H15B 108.9 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.25(17) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.24(19) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 112.8(2) . . ?
C20 C19 H19A 109.0 . . ?
C18 C19 H19A 109.0 . . ?
C20 C19 H19B 109.0 . . ?
C18 C19 H19B 109.0 . . ?
H19A C19 H19B 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.63(19) . . ?
C26 C21 B1 123.56(19) . . ?
C22 C21 B1 121.78(19) . . ?
C23 C22 C21 123.0(2) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 118.8(2) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
C24 C25 C26 119.9(2) . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 123.4(2) . . ?
C25 C26 H26 118.3 . . ?
C21 C26 H26 118.3 . . ?
C28 C27 C32 114.7(2) . . ?
C28 C27 B1 124.65(19) . . ?
C32 C27 B1 120.6(2) . . ?
C29 C28 C27 122.7(2) . . ?
C29 C28 H28 118.7 . . ?
C27 C28 H28 118.7 . . ?
C30 C29 C28 120.7(2) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 118.6(2) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C30 C31 C32 120.0(2) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 123.3(2) . . ?
C31 C32 H32 118.3 . . ?
C27 C32 H32 118.3 . . ?
C34 C33 C38 115.0(2) . . ?
C34 C33 B1 122.2(2) . . ?
C38 C33 B1 122.6(2) . . ?
C35 C34 C33 123.0(2) . . ?
C35 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C36 C35 C34 120.3(2) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 118.9(2) . . ?
C37 C36 H36 120.5 . . ?
C35 C36 H36 120.5 . . ?
C36 C37 C38 120.1(2) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 122.8(2) . . ?
C37 C38 H38 118.6 . . ?
C33 C38 H38 118.6 . . ?
C40 C39 C44 115.1(2) . . ?
C40 C39 B1 123.5(2) . . ?
C44 C39 B1 121.32(19) . . ?
C41 C40 C39 122.5(2) . . ?
C41 C40 H40 118.7 . . ?
C39 C40 H40 118.7 . . ?
C42 C41 C40 120.6(2) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 118.9(2) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C44 C43 C42 119.6(2) . . ?
C44 C43 H43 120.2 . . ?
C42 C43 H43 120.2 . . ?
C43 C44 C39 123.3(2) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 105.9(2) . . ?
O3 C45 H45A 110.6 . . ?
C46 C45 H45A 110.6 . . ?
O3 C45 H45B 110.6 . . ?
C46 C45 H45B 110.6 . . ?
H45A C45 H45B 108.7 . . ?
C45 C46 C47 102.0(2) . . ?
C45 C46 H46A 111.4 . . ?
C47 C46 H46A 111.4 . . ?
C45 C46 H46B 111.4 . . ?
C47 C46 H46B 111.4 . . ?
H46A C46 H46B 109.2 . . ?
C48 C47 C46 105.4(3) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
O3 C48 C47 109.1(3) . . ?
O3 C48 H48A 109.9 . . ?
C47 C48 H48A 109.9 . . ?
O3 C48 H48B 109.9 . . ?
C47 C48 H48B 109.9 . . ?
H48A C48 H48B 108.3 . . ?
C39 B1 C33 109.05(18) . . ?
C39 B1 C27 109.37(18) . . ?
C33 B1 C27 110.10(18) . . ?
C39 B1 C21 109.85(17) . . ?
C33 B1 C21 108.90(18) . . ?
C27 B1 C21 109.56(17) . . ?
C5 N2 C9 109.33(16) . . ?
C5 N2 C1 111.48(17) . . ?
C9 N2 C1 110.41(16) . . ?
C5 N2 Pd1 104.56(12) . . ?
C9 N2 Pd1 114.90(13) . . ?
C1 N2 Pd1 106.03(12) . . ?
C3 N3 C2 115.75(17) . . ?
C3 N3 Pd1 107.27(13) . . ?
C2 N3 Pd1 107.15(13) . . ?
C3 N3 H3 110.2(17) . . ?
C2 N3 H3 106.6(17) . . ?
Pd1 N3 H3 109.8(17) . . ?
C17 N4 C13 109.86(16) . . ?
C17 N4 C4 110.42(16) . . ?
C13 N4 C4 111.53(16) . . ?
C17 N4 Pd1 115.39(13) . . ?
C13 N4 Pd1 104.21(12) . . ?
C4 N4 Pd1 105.26(12) . . ?
C45 O3 C48 107.5(2) . . ?
N3 Pd1 O1 172.70(7) . . ?
N3 Pd1 N2 85.55(7) . . ?
O1 Pd1 N2 93.69(6) . . ?
N3 Pd1 N4 85.70(7) . . ?
O1 Pd1 N4 93.78(6) . . ?
N2 Pd1 N4 167.08(7) . . ?
O2 N1 O1 115.29(19) . . ?
N1 O1 Pd1 119.04(14) . . ?

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
N2 C1 C2 N3 54.6(2) . . . . ?
N3 C3 C4 N4 -54.4(2) . . . . ?
N2 C5 C6 C7 -179.14(19) . . . . ?
C5 C6 C7 C8 -171.9(2) . . . . ?
N2 C9 C10 C11 170.52(18) . . . . ?
C9 C10 C11 C12 172.7(2) . . . . ?
N4 C13 C14 C15 178.12(18) . . . . ?
C13 C14 C15 C16 179.33(19) . . . . ?
N4 C17 C18 C19 -167.80(19) . . . . ?
C17 C18 C19 C20 -169.3(2) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?
B1 C21 C22 C23 178.1(2) . . . . ?
C21 C22 C23 C24 -0.6(4) . . . . ?
C22 C23 C24 C25 0.4(3) . . . . ?
C23 C24 C25 C26 0.2(3) . . . . ?
C24 C25 C26 C21 -0.6(3) . . . . ?
C22 C21 C26 C25 0.4(3) . . . . ?
B1 C21 C26 C25 -177.5(2) . . . . ?
C32 C27 C28 C29 -1.2(3) . . . . ?
B1 C27 C28 C29 178.1(2) . . . . ?
C27 C28 C29 C30 0.1(4) . . . . ?
C28 C29 C30 C31 1.1(4) . . . . ?
C29 C30 C31 C32 -1.1(4) . . . . ?
C30 C31 C32 C27 0.0(4) . . . . ?
C28 C27 C32 C31 1.2(3) . . . . ?
B1 C27 C32 C31 -178.2(2) . . . . ?
C38 C33 C34 C35 -0.3(4) . . . . ?
B1 C33 C34 C35 -175.2(2) . . . . ?
C33 C34 C35 C36 0.4(4) . . . . ?
C34 C35 C36 C37 0.1(4) . . . . ?
C35 C36 C37 C38 -0.7(4) . . . . ?
C36 C37 C38 C33 0.7(3) . . . . ?
C34 C33 C38 C37 -0.2(3) . . . . ?
B1 C33 C38 C37 174.7(2) . . . . ?
C44 C39 C40 C41 1.2(3) . . . . ?
B1 C39 C40 C41 -174.8(2) . . . . ?
C39 C40 C41 C42 0.9(3) . . . . ?
C40 C41 C42 C43 -1.8(3) . . . . ?
C41 C42 C43 C44 0.5(3) . . . . ?
C42 C43 C44 C39 1.7(3) . . . . ?
C40 C39 C44 C43 -2.5(3) . . . . ?
B1 C39 C44 C43 173.6(2) . . . . ?
O3 C45 C46 C47 -32.1(3) . . . . ?
C45 C46 C47 C48 25.0(3) . . . . ?
C46 C47 C48 O3 -9.7(4) . . . . ?
C40 C39 B1 C33 -17.0(3) . . . . ?
C44 C39 B1 C33 167.18(19) . . . . ?
C40 C39 B1 C27 103.4(2) . . . . ?
C44 C39 B1 C27 -72.4(2) . . . . ?
C40 C39 B1 C21 -136.3(2) . . . . ?
C44 C39 B1 C21 47.9(3) . . . . ?
C34 C33 B1 C39 93.3(2) . . . . ?
C38 C33 B1 C39 -81.2(2) . . . . ?
C34 C33 B1 C27 -26.7(3) . . . . ?
C38 C33 B1 C27 158.80(19) . . . . ?
C34 C33 B1 C21 -146.8(2) . . . . ?
C38 C33 B1 C21 38.7(3) . . . . ?
C28 C27 B1 C39 15.4(3) . . . . ?
C32 C27 B1 C39 -165.23(19) . . . . ?
C28 C27 B1 C33 135.2(2) . . . . ?
C32 C27 B1 C33 -45.4(3) . . . . ?
C28 C27 B1 C21 -105.0(2) . . . . ?
C32 C27 B1 C21 74.3(2) . . . . ?
C26 C21 B1 C39 -149.0(2) . . . . ?
C22 C21 B1 C39 33.2(3) . . . . ?
C26 C21 B1 C33 91.6(2) . . . . ?
C22 C21 B1 C33 -86.1(2) . . . . ?
C26 C21 B1 C27 -28.8(3) . . . . ?
C22 C21 B1 C27 153.4(2) . . . . ?
C6 C5 N2 C9 -55.9(2) . . . . ?
C6 C5 N2 C1 66.5(2) . . . . ?
C6 C5 N2 Pd1 -179.41(16) . . . . ?
C10 C9 N2 C5 -174.57(18) . . . . ?
C10 C9 N2 C1 62.4(2) . . . . ?
C10 C9 N2 Pd1 -57.4(2) . . . . ?
C2 C1 N2 C5 78.9(2) . . . . ?
C2 C1 N2 C9 -159.42(18) . . . . ?
C2 C1 N2 Pd1 -34.4(2) . . . . ?
C4 C3 N3 C2 166.62(17) . . . . ?
C4 C3 N3 Pd1 47.09(18) . . . . ?
C1 C2 N3 C3 -166.15(18) . . . . ?
C1 C2 N3 Pd1 -46.6(2) . . . . ?
C18 C17 N4 C13 176.62(18) . . . . ?
C18 C17 N4 C4 -60.0(2) . . . . ?
C18 C17 N4 Pd1 59.2(2) . . . . ?
C14 C13 N4 C17 58.2(2) . . . . ?
C14 C13 N4 C4 -64.6(2) . . . . ?
C14 C13 N4 Pd1 -177.65(15) . . . . ?
C3 C4 N4 C17 158.47(17) . . . . ?
C3 C4 N4 C13 -79.1(2) . . . . ?
C3 C4 N4 Pd1 33.33(19) . . . . ?
C46 C45 O3 C48 27.3(3) . . . . ?
C47 C48 O3 C45 -11.0(4) . . . . ?
O2 N1 O1 Pd1 -0.9(3) . . . . ?

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
C5 H5B O1 0.99 2.55 3.180(3) 121.1 .
C10 H10A O2 0.99 2.57 3.278(3) 128.7 .
C13 H13A O1 0.99 2.56 3.172(3) 119.8 .
C18 H18B O2 0.99 2.60 3.215(3) 120.2 .
N3 H3 O3 0.940(17) 2.023(18) 2.939(3) 164(2) .

_refine_diff_density_max         0.768
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.063

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-150K
_database_code_depnum_ccdc_archive 'CCDC 1441786'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-150K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5322(4)
_cell_length_b                   13.4261(5)
_cell_length_c                   30.0361(11)
_cell_angle_alpha                90
_cell_angle_beta                 94.162(4)
_cell_angle_gamma                90
_cell_volume                     4638.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4437
_cell_measurement_theta_min      3.5480
_cell_measurement_theta_max      26.6080

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.88257
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20443
_diffrn_reflns_av_unetI/netI     0.0927
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.034
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9474
_reflns_number_gt                6319
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0350P)²+1.5001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9474
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0902
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
C1 C 0.5515(3) 0.9629(3) 0.62798(12) 0.0324(9) Uani 1 1 d . . . . .
H1A H 0.4769 0.9574 0.6422 0.039 Uiso 1 1 calc R U . . .
H1B H 0.5631 1.0337 0.6202 0.039 Uiso 1 1 calc R U . . .
C2 C 0.5465(3) 0.9006(3) 0.58642(12) 0.0293(9) Uani 1 1 d . . . . .
H2A H 0.4776 0.9186 0.5665 0.035 Uiso 1 1 calc R U . . .
H2B H 0.6171 0.9112 0.5701 0.035 Uiso 1 1 calc R U . . .
C3 C 0.5606(3) 0.7193(3) 0.56669(11) 0.0243(8) Uani 1 1 d . . . . .
H3A H 0.6309 0.7368 0.5513 0.029 Uiso 1 1 calc R U . . .
H3B H 0.4936 0.7154 0.5442 0.029 Uiso 1 1 calc R U . . .
C4 C 0.5777(3) 0.6206(3) 0.59065(11) 0.0246(8) Uani 1 1 d . . . . .
H4A H 0.5038 0.5997 0.6027 0.030 Uiso 1 1 calc R U . . .
H4B H 0.6002 0.5691 0.5693 0.030 Uiso 1 1 calc R U . . .
C5 C 0.7647(3) 0.9674(3) 0.64724(13) 0.0310(9) Uani 1 1 d . . . . .
H5A H 0.7749 0.9460 0.6162 0.037 Uiso 1 1 calc R U . . .
H5B H 0.8268 0.9350 0.6666 0.037 Uiso 1 1 calc R U . . .
C6 C 0.7834(3) 1.0790(3) 0.64990(13) 0.0337(9) Uani 1 1 d . . . . .
H6A H 0.7220 1.1130 0.6308 0.040 Uiso 1 1 calc R U . . .
H6B H 0.7772 1.1015 0.6810 0.040 Uiso 1 1 calc R U . . .
C7 C 0.9013(4) 1.1073(3) 0.63492(15) 0.0438(11) Uani 1 1 d . . . . .
H7A H 0.9034 1.0931 0.6026 0.053 Uiso 1 1 calc R U . . .
H7B H 0.9617 1.0661 0.6511 0.053 Uiso 1 1 calc R U . . .
C8 C 0.9285(4) 1.2164(3) 0.64326(16) 0.0537(12) Uani 1 1 d . . . . .
H8A H 0.9312 1.2299 0.6754 0.081 Uiso 1 1 calc R U . . .
H8B H 0.8680 1.2575 0.6278 0.081 Uiso 1 1 calc R U . . .
H8C H 1.0041 1.2324 0.6320 0.081 Uiso 1 1 calc R U . . .
C9 C 0.6304(3) 0.9618(3) 0.70673(12) 0.0288(9) Uani 1 1 d . . . . .
H9A H 0.6255 1.0354 0.7070 0.035 Uiso 1 1 calc R U . . .
H9B H 0.6993 0.9426 0.7264 0.035 Uiso 1 1 calc R U . . .
C10 C 0.5240(3) 0.9208(3) 0.72630(12) 0.0301(9) Uani 1 1 d . . . . .
H10A H 0.5212 0.8476 0.7222 0.036 Uiso 1 1 calc R U . . .
H10B H 0.4535 0.9496 0.7105 0.036 Uiso 1 1 calc R U . . .
C11 C 0.5256(3) 0.9454(3) 0.77591(13) 0.0363(10) Uani 1 1 d . . . . .
H11A H 0.5911 0.9097 0.7920 0.044 Uiso 1 1 calc R U . . .
H11B H 0.5394 1.0178 0.7800 0.044 Uiso 1 1 calc R U . . .
C12 C 0.4136(4) 0.9176(3) 0.79641(15) 0.0485(12) Uani 1 1 d . . . . .
H12A H 0.4213 0.9315 0.8285 0.073 Uiso 1 1 calc R U . . .
H12B H 0.3979 0.8466 0.7916 0.073 Uiso 1 1 calc R U . . .
H12C H 0.3493 0.9568 0.7824 0.073 Uiso 1 1 calc R U . . .
C13 C 0.7910(3) 0.6243(2) 0.61161(12) 0.0245(8) Uani 1 1 d . . . . .
H13A H 0.8482 0.6387 0.6370 0.029 Uiso 1 1 calc R U . . .
H13B H 0.7975 0.6782 0.5894 0.029 Uiso 1 1 calc R U . . .
C14 C 0.8259(3) 0.5272(3) 0.59033(13) 0.0304(9) Uani 1 1 d . . . . .
H14A H 0.8231 0.4727 0.6124 0.036 Uiso 1 1 calc R U . . .
H14B H 0.7697 0.5114 0.5648 0.036 Uiso 1 1 calc R U . . .
C15 C 0.9472(3) 0.5330(3) 0.57410(14) 0.0340(9) Uani 1 1 d . . . . .
H15A H 0.9493 0.5874 0.5519 0.041 Uiso 1 1 calc R U . . .
H15B H 1.0027 0.5502 0.5996 0.041 Uiso 1 1 calc R U . . .
C16 C 0.9867(3) 0.4375(3) 0.55312(14) 0.0372(10) Uani 1 1 d . . . . .
H16A H 1.0631 0.4478 0.5415 0.056 Uiso 1 1 calc R U . . .
H16B H 0.9305 0.4182 0.5286 0.056 Uiso 1 1 calc R U . . .
H16C H 0.9922 0.3845 0.5756 0.056 Uiso 1 1 calc R U . . .
C17 C 0.6582(3) 0.5496(3) 0.66224(12) 0.0267(9) Uani 1 1 d . . . . .
H17A H 0.7231 0.5552 0.6856 0.032 Uiso 1 1 calc R U . . .
H17B H 0.6655 0.4842 0.6475 0.032 Uiso 1 1 calc R U . . .
C18 C 0.5453(3) 0.5514(3) 0.68454(12) 0.0324(9) Uani 1 1 d . . . . .
H18A H 0.4807 0.5331 0.6625 0.039 Uiso 1 1 calc R U . . .
H18B H 0.5307 0.6197 0.6952 0.039 Uiso 1 1 calc R U . . .
C19 C 0.5480(4) 0.4795(3) 0.72376(14) 0.0448(11) Uani 1 1 d . . . . .
H19A H 0.5762 0.4139 0.7140 0.054 Uiso 1 1 calc R U . . .
H19B H 0.6041 0.5044 0.7477 0.054 Uiso 1 1 calc R U . . .
C20 C 0.4322(4) 0.4660(4) 0.74233(17) 0.0615(14) Uani 1 1 d . . . . .
H20A H 0.4419 0.4281 0.7703 0.092 Uiso 1 1 calc R U . . .
H20B H 0.3803 0.4296 0.7208 0.092 Uiso 1 1 calc R U . . .
H20C H 0.3986 0.5313 0.7481 0.092 Uiso 1 1 calc R U . . .
C21 C 0.4930(3) 0.2311(3) 0.55685(11) 0.0215(7) Uani 1 1 d . . . . .
C22 C 0.5873(3) 0.2962(3) 0.56628(13) 0.0300(9) Uani 1 1 d . . . . .
H22 H 0.5742 0.3563 0.5819 0.036 Uiso 1 1 calc R U . . .
C23 C 0.6982(3) 0.2765(3) 0.55384(13) 0.0328(9) Uani 1 1 d . . . . .
H23 H 0.7588 0.3231 0.5608 0.039 Uiso 1 1 calc R U . . .
C24 C 0.7216(3) 0.1900(3) 0.53146(13) 0.0315(9) Uani 1 1 d . . . . .
H24 H 0.7975 0.1764 0.5227 0.038 Uiso 1 1 calc R U . . .
C25 C 0.6312(3) 0.1235(3) 0.52215(12) 0.0280(9) Uani 1 1 d . . . . .
H25 H 0.6454 0.0627 0.5073 0.034 Uiso 1 1 calc R U . . .
C26 C 0.5212(3) 0.1449(2) 0.53422(11) 0.0232(8) Uani 1 1 d . . . . .
H26 H 0.4611 0.0983 0.5267 0.028 Uiso 1 1 calc R U . . .
C27 C 0.2629(3) 0.2003(2) 0.53993(12) 0.0235(8) Uani 1 1 d . . . . .
C28 C 0.1900(3) 0.2494(3) 0.50797(12) 0.0306(9) Uani 1 1 d . . . . .
H28 H 0.1959 0.3198 0.5056 0.037 Uiso 1 1 calc R U . . .
C29 C 0.1093(3) 0.1999(3) 0.47943(14) 0.0393(10) Uani 1 1 d . . . . .
H29 H 0.0622 0.2367 0.4580 0.047 Uiso 1 1 calc R U . . .
C30 C 0.0968(3) 0.0986(3) 0.48180(14) 0.0391(10) Uani 1 1 d . . . . .
H30 H 0.0420 0.0648 0.4621 0.047 Uiso 1 1 calc R U . . .
C31 C 0.1654(3) 0.0467(3) 0.51346(15) 0.0390(11) Uani 1 1 d . . . . .
H31 H 0.1574 -0.0235 0.5159 0.047 Uiso 1 1 calc R U . . .
C32 C 0.2458(3) 0.0969(3) 0.54164(14) 0.0317(9) Uani 1 1 d . . . . .
H32 H 0.2917 0.0595 0.5632 0.038 Uiso 1 1 calc R U . . .
C33 C 0.3568(3) 0.2130(3) 0.62481(12) 0.0268(8) Uani 1 1 d . . . . .
C34 C 0.2542(4) 0.1756(3) 0.64031(14) 0.0441(11) Uani 1 1 d . . . . .
H34 H 0.1877 0.1694 0.6199 0.053 Uiso 1 1 calc R U . . .
C35 C 0.2452(4) 0.1472(4) 0.68421(15) 0.0557(13) Uani 1 1 d . . . . .
H35 H 0.1736 0.1219 0.6932 0.067 Uiso 1 1 calc R U . . .
C36 C 0.3389(4) 0.1552(3) 0.71494(14) 0.0465(11) Uani 1 1 d . . . . .
H36 H 0.3331 0.1355 0.7451 0.056 Uiso 1 1 calc R U . . .
C37 C 0.4412(4) 0.1924(3) 0.70112(13) 0.0383(10) Uani 1 1 d . . . . .
H37 H 0.5068 0.1991 0.7219 0.046 Uiso 1 1 calc R U . . .
C38 C 0.4493(3) 0.2200(3) 0.65705(12) 0.0320(9) Uani 1 1 d . . . . .
H38 H 0.5214 0.2450 0.6484 0.038 Uiso 1 1 calc R U . . .
C39 C 0.3398(3) 0.3756(3) 0.57309(12) 0.0238(8) Uani 1 1 d . . . . .
C40 C 0.2883(3) 0.4268(3) 0.60689(13) 0.0302(9) Uani 1 1 d . . . . .
H40 H 0.2712 0.3912 0.6330 0.036 Uiso 1 1 calc R U . . .
C41 C 0.2609(3) 0.5269(3) 0.60418(16) 0.0396(11) Uani 1 1 d . . . . .
H41 H 0.2270 0.5587 0.6283 0.048 Uiso 1 1 calc R U . . .
C42 C 0.2825(3) 0.5809(3) 0.56670(16) 0.0407(11) Uani 1 1 d . . . . .
H42 H 0.2615 0.6492 0.5644 0.049 Uiso 1 1 calc R U . . .
C43 C 0.3351(3) 0.5345(3) 0.53259(14) 0.0355(10) Uani 1 1 d . . . . .
H43 H 0.3518 0.5709 0.5067 0.043 Uiso 1 1 calc R U . . .
C44 C 0.3636(3) 0.4342(3) 0.53618(12) 0.0288(9) Uani 1 1 d . . . . .
H44 H 0.4010 0.4038 0.5125 0.035 Uiso 1 1 calc R U . . .
C45 C 0.2606(4) 0.7653(4) 0.67609(17) 0.0589(9) Uani 1 1 d . . . . .
H45A H 0.2771 0.8098 0.7021 0.071 Uiso 1 1 calc R U . . .
H45B H 0.2930 0.6986 0.6835 0.071 Uiso 1 1 calc R U . . .
C46 C 0.1310(4) 0.7587(4) 0.66436(18) 0.0707(11) Uani 1 1 d . . . . .
H46A H 0.1093 0.6935 0.6507 0.085 Uiso 1 1 calc R U . . .
H46B H 0.0865 0.7693 0.6909 0.085 Uiso 1 1 calc R U . . .
C47 C 0.1120(4) 0.8411(4) 0.63167(18) 0.0707(11) Uani 1 1 d . . . . .
H47A H 0.0553 0.8208 0.6070 0.085 Uiso 1 1 calc R U . . .
H47B H 0.0812 0.9005 0.6464 0.085 Uiso 1 1 calc R U . . .
C48 C 0.2240(4) 0.8636(4) 0.61448(17) 0.0589(9) Uani 1 1 d . . . . .
H48A H 0.2214 0.8488 0.5821 0.071 Uiso 1 1 calc R U . . .
H48B H 0.2424 0.9351 0.6188 0.071 Uiso 1 1 calc R U . . .
B1 B 0.3631(3) 0.2550(3) 0.57357(13) 0.0230(9) Uani 1 1 d . . . . .
N1A N 0.7801(4) 0.7316(3) 0.73851(12) 0.0500(10) Uani 1 1 d . . . . .
N2 N 0.6496(2) 0.9288(2) 0.66018(9) 0.0246(7) Uani 1 1 d . . . . .
N3 N 0.5390(2) 0.7950(2) 0.60072(9) 0.0232(7) Uani 1 1 d D . . . .
N4 N 0.6713(2) 0.6295(2) 0.62845(9) 0.0215(6) Uani 1 1 d . . . . .
O1A O 0.7973(2) 0.75977(19) 0.69797(9) 0.0381(7) Uani 1 1 d . . . . .
O2A O 0.6795(3) 0.7187(2) 0.74553(10) 0.0559(8) Uani 1 1 d . . . . .
O3 O 0.3101(2) 0.8044(2) 0.63779(10) 0.0463(7) Uani 1 1 d . . . . .
Pd1 Pd 0.65952(2) 0.77519(2) 0.65189(2) 0.02215(9) Uani 1 1 d . . . . .
H3 H 0.4638(19) 0.785(2) 0.6122(10) 0.027 Uiso 1 1 d D 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
C1 C2 1.501(5) . ?
C1 N2 1.506(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.486(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.475(4) . ?
C3 C4 1.514(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.513(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.502(5) . ?
C5 C6 1.515(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.512(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.515(5) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.498(4) . ?
C9 C10 1.502(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.525(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.517(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.506(4) . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.516(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.514(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.492(4) . ?
C17 C18 1.507(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.521(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.495(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.392(5) . ?
C21 C22 1.408(5) . ?
C21 B1 1.646(5) . ?
C22 C23 1.384(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.385(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.375(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.395(5) . ?
C27 C32 1.404(5) . ?
C27 B1 1.651(5) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.371(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.391(5) . ?
C33 C34 1.396(5) . ?
C33 B1 1.646(5) . ?
C34 C35 1.384(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.374(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.372(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.385(5) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.394(5) . ?
C39 C44 1.403(5) . ?
C39 B1 1.641(5) . ?
C40 C41 1.382(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.376(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.376(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.388(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.421(5) . ?
C45 C46 1.513(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.485(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.457(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.417(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1A O2A 1.206(5) . ?
N1A O1A 1.304(4) . ?
N2 Pd1 2.081(3) . ?
N3 Pd1 2.014(3) . ?
N3 H3 0.966(18) . ?
N4 Pd1 2.087(3) . ?
O1A Pd1 2.041(2) . ?

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
C2 C1 N2 110.2(3) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.9(3) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 107.2(3) . . ?
N3 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
N3 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
N4 C4 C3 110.4(3) . . ?
N4 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N4 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 116.9(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.1(3) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 112.0(4) . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7B 109.2 . . ?
C8 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.9(3) . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.5(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.1(3) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.3(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.7(3) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C14 113.7(3) . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15B 108.8 . . ?
C14 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.1(3) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.3(3) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.4(3) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.1(3) . . ?
C26 C21 B1 124.2(3) . . ?
C22 C21 B1 121.6(3) . . ?
C23 C22 C21 122.9(3) . . ?
C23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C24 C23 C22 120.7(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 118.1(3) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C26 C25 C24 120.5(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 123.8(3) . . ?
C25 C26 H26 118.1 . . ?
C21 C26 H26 118.1 . . ?
C28 C27 C32 114.4(3) . . ?
C28 C27 B1 124.8(3) . . ?
C32 C27 B1 120.8(3) . . ?
C29 C28 C27 122.8(3) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 120.8(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 C31 118.6(4) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C30 C31 C32 120.0(4) . . ?
C30 C31 H31 120.0 . . ?
C32 C31 H31 120.0 . . ?
C31 C32 C27 123.3(4) . . ?
C31 C32 H32 118.4 . . ?
C27 C32 H32 118.4 . . ?
C38 C33 C34 114.7(3) . . ?
C38 C33 B1 122.9(3) . . ?
C34 C33 B1 122.1(3) . . ?
C35 C34 C33 122.7(4) . . ?
C35 C34 H34 118.6 . . ?
C33 C34 H34 118.6 . . ?
C36 C35 C34 120.6(4) . . ?
C36 C35 H35 119.7 . . ?
C34 C35 H35 119.7 . . ?
C37 C36 C35 118.5(4) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C36 C37 C38 120.4(4) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C37 C38 C33 123.1(4) . . ?
C37 C38 H38 118.5 . . ?
C33 C38 H38 118.5 . . ?
C40 C39 C44 114.6(3) . . ?
C40 C39 B1 123.9(3) . . ?
C44 C39 B1 121.3(3) . . ?
C41 C40 C39 123.0(4) . . ?
C41 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C42 C41 C40 120.4(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 119.1(4) . . ?
C41 C42 H42 120.5 . . ?
C43 C42 H42 120.5 . . ?
C42 C43 C44 119.7(4) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C39 123.1(4) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 106.3(4) . . ?
O3 C45 H45A 110.5 . . ?
C46 C45 H45A 110.5 . . ?
O3 C45 H45B 110.5 . . ?
C46 C45 H45B 110.5 . . ?
H45A C45 H45B 108.7 . . ?
C47 C46 C45 101.9(4) . . ?
C47 C46 H46A 111.4 . . ?
C45 C46 H46A 111.4 . . ?
C47 C46 H46B 111.4 . . ?
C45 C46 H46B 111.4 . . ?
H46A C46 H46B 109.3 . . ?
C48 C47 C46 107.3(4) . . ?
C48 C47 H47A 110.3 . . ?
C46 C47 H47A 110.3 . . ?
C48 C47 H47B 110.3 . . ?
C46 C47 H47B 110.3 . . ?
H47A C47 H47B 108.5 . . ?
O3 C48 C47 108.4(4) . . ?
O3 C48 H48A 110.0 . . ?
C47 C48 H48A 110.0 . . ?
O3 C48 H48B 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.4 . . ?
C39 B1 C21 110.0(3) . . ?
C39 B1 C33 109.2(3) . . ?
C21 B1 C33 108.8(3) . . ?
C39 B1 C27 109.1(3) . . ?
C21 B1 C27 109.8(3) . . ?
C33 B1 C27 110.1(3) . . ?
O2A N1A O1A 114.8(3) . . ?
C9 N2 C5 109.5(3) . . ?
C9 N2 C1 110.7(3) . . ?
C5 N2 C1 111.5(3) . . ?
C9 N2 Pd1 114.7(2) . . ?
C5 N2 Pd1 104.7(2) . . ?
C1 N2 Pd1 105.66(19) . . ?
C3 N3 C2 116.1(3) . . ?
C3 N3 Pd1 107.19(19) . . ?
C2 N3 Pd1 107.18(19) . . ?
C3 N3 H3 111(2) . . ?
C2 N3 H3 108(2) . . ?
Pd1 N3 H3 107(2) . . ?
C17 N4 C13 109.6(2) . . ?
C17 N4 C4 110.6(2) . . ?
C13 N4 C4 111.4(3) . . ?
C17 N4 Pd1 115.6(2) . . ?
C13 N4 Pd1 103.89(19) . . ?
C4 N4 Pd1 105.49(19) . . ?
N1A O1A Pd1 119.9(3) . . ?
C48 O3 C45 107.4(3) . . ?
N3 Pd1 O1A 172.51(12) . . ?
N3 Pd1 N2 85.39(11) . . ?
O1A Pd1 N2 93.79(10) . . ?
N3 Pd1 N4 85.67(10) . . ?
O1A Pd1 N4 93.86(10) . . ?
N2 Pd1 N4 167.06(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C1 C2 N3 54.6(4) . . . . ?
N3 C3 C4 N4 -53.7(4) . . . . ?
N2 C5 C6 C7 -178.6(3) . . . . ?
C5 C6 C7 C8 -172.2(3) . . . . ?
N2 C9 C10 C11 170.4(3) . . . . ?
C9 C10 C11 C12 172.7(3) . . . . ?
N4 C13 C14 C15 178.9(3) . . . . ?
C13 C14 C15 C16 179.3(3) . . . . ?
N4 C17 C18 C19 -170.1(3) . . . . ?
C17 C18 C19 C20 -170.5(4) . . . . ?
C26 C21 C22 C23 0.5(5) . . . . ?
B1 C21 C22 C23 178.0(3) . . . . ?
C21 C22 C23 C24 -0.5(6) . . . . ?
C22 C23 C24 C25 -0.4(6) . . . . ?
C23 C24 C25 C26 1.3(5) . . . . ?
C24 C25 C26 C21 -1.4(5) . . . . ?
C22 C21 C26 C25 0.5(5) . . . . ?
B1 C21 C26 C25 -176.9(3) . . . . ?
C32 C27 C28 C29 -1.6(5) . . . . ?
B1 C27 C28 C29 178.0(4) . . . . ?
C27 C28 C29 C30 0.7(6) . . . . ?
C28 C29 C30 C31 0.6(6) . . . . ?
C29 C30 C31 C32 -0.8(6) . . . . ?
C30 C31 C32 C27 -0.2(6) . . . . ?
C28 C27 C32 C31 1.4(5) . . . . ?
B1 C27 C32 C31 -178.2(4) . . . . ?
C38 C33 C34 C35 -0.4(6) . . . . ?
B1 C33 C34 C35 -174.9(4) . . . . ?
C33 C34 C35 C36 0.3(7) . . . . ?
C34 C35 C36 C37 0.2(7) . . . . ?
C35 C36 C37 C38 -0.6(6) . . . . ?
C36 C37 C38 C33 0.5(6) . . . . ?
C34 C33 C38 C37 0.0(5) . . . . ?
B1 C33 C38 C37 174.5(3) . . . . ?
C44 C39 C40 C41 0.9(5) . . . . ?
B1 C39 C40 C41 -174.6(3) . . . . ?
C39 C40 C41 C42 1.0(5) . . . . ?
C40 C41 C42 C43 -2.0(5) . . . . ?
C41 C42 C43 C44 1.0(5) . . . . ?
C42 C43 C44 C39 1.0(5) . . . . ?
C40 C39 C44 C43 -2.0(5) . . . . ?
B1 C39 C44 C43 173.7(3) . . . . ?
O3 C45 C46 C47 -29.3(5) . . . . ?
C45 C46 C47 C48 20.3(6) . . . . ?
C46 C47 C48 O3 -4.6(6) . . . . ?
C40 C39 B1 C21 -137.3(3) . . . . ?
C44 C39 B1 C21 47.4(4) . . . . ?
C40 C39 B1 C33 -18.1(4) . . . . ?
C44 C39 B1 C33 166.6(3) . . . . ?
C40 C39 B1 C27 102.3(4) . . . . ?
C44 C39 B1 C27 -73.0(4) . . . . ?
C26 C21 B1 C39 -149.1(3) . . . . ?
C22 C21 B1 C39 33.6(4) . . . . ?
C26 C21 B1 C33 91.4(4) . . . . ?
C22 C21 B1 C33 -85.9(4) . . . . ?
C26 C21 B1 C27 -29.1(4) . . . . ?
C22 C21 B1 C27 153.6(3) . . . . ?
C38 C33 B1 C39 -81.1(4) . . . . ?
C34 C33 B1 C39 93.0(4) . . . . ?
C38 C33 B1 C21 38.9(4) . . . . ?
C34 C33 B1 C21 -147.0(3) . . . . ?
C38 C33 B1 C27 159.2(3) . . . . ?
C34 C33 B1 C27 -26.7(5) . . . . ?
C28 C27 B1 C39 15.2(5) . . . . ?
C32 C27 B1 C39 -165.3(3) . . . . ?
C28 C27 B1 C21 -105.4(4) . . . . ?
C32 C27 B1 C21 74.1(4) . . . . ?
C28 C27 B1 C33 134.9(3) . . . . ?
C32 C27 B1 C33 -45.6(4) . . . . ?
C10 C9 N2 C5 -174.3(3) . . . . ?
C10 C9 N2 C1 62.4(4) . . . . ?
C10 C9 N2 Pd1 -57.0(3) . . . . ?
C6 C5 N2 C9 -56.7(4) . . . . ?
C6 C5 N2 C1 66.1(4) . . . . ?
C6 C5 N2 Pd1 179.9(3) . . . . ?
C2 C1 N2 C9 -159.0(3) . . . . ?
C2 C1 N2 C5 78.9(4) . . . . ?
C2 C1 N2 Pd1 -34.3(3) . . . . ?
C4 C3 N3 C2 166.5(3) . . . . ?
C4 C3 N3 Pd1 46.8(3) . . . . ?
C1 C2 N3 C3 -166.2(3) . . . . ?
C1 C2 N3 Pd1 -46.4(3) . . . . ?
C18 C17 N4 C13 175.4(3) . . . . ?
C18 C17 N4 C4 -61.4(4) . . . . ?
C18 C17 N4 Pd1 58.4(3) . . . . ?
C14 C13 N4 C17 58.1(4) . . . . ?
C14 C13 N4 C4 -64.6(4) . . . . ?
C14 C13 N4 Pd1 -177.7(2) . . . . ?
C3 C4 N4 C17 158.1(3) . . . . ?
C3 C4 N4 C13 -79.7(3) . . . . ?
C3 C4 N4 Pd1 32.4(3) . . . . ?
O2A N1A O1A Pd1 -1.5(5) . . . . ?
C47 C48 O3 C45 -14.5(5) . . . . ?
C46 C45 O3 C48 27.7(5) . . . . ?

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
C5 H5B O1A 0.99 2.57 3.186(5) 120.7 .
C10 H10A O2A 0.99 2.57 3.280(5) 128.1 .
C13 H13A O1A 0.99 2.55 3.165(4) 120.1 .
C18 H18B O2A 0.99 2.57 3.223(5) 123.2 .
N3 H3 O3 0.966(18) 2.00(2) 2.941(4) 164(3) .

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-180K
_database_code_depnum_ccdc_archive 'CCDC 1441787'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-180K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5569(5)
_cell_length_b                   13.4632(5)
_cell_length_c                   30.0545(13)
_cell_angle_alpha                90
_cell_angle_beta                 93.906(4)
_cell_angle_gamma                90
_cell_volume                     4665.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    3920
_cell_measurement_theta_min      3.5420
_cell_measurement_theta_max      25.2240

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.441
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.82210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20542
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.026
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9519
_reflns_number_gt                5973
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0367P)²+0.6887P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9519
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1115
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1090
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.011
_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
C1 C 0.5531(4) 0.9627(3) 0.62844(13) 0.0373(10) Uani 1 1 d . . . . .
H1A H 0.5645 1.0335 0.6209 0.045 Uiso 1 1 calc R U . . .
H1B H 0.4788 0.9566 0.6428 0.045 Uiso 1 1 calc R U . . .
C2 C 0.5485(4) 0.9011(3) 0.58655(13) 0.0365(10) Uani 1 1 d . . . . .
H2A H 0.4801 0.9194 0.5666 0.044 Uiso 1 1 calc R U . . .
H2B H 0.6193 0.9115 0.5704 0.044 Uiso 1 1 calc R U . . .
C3 C 0.5616(3) 0.7199(3) 0.56682(12) 0.0300(8) Uani 1 1 d . . . . .
H3A H 0.6317 0.7371 0.5513 0.036 Uiso 1 1 calc R U . . .
H3B H 0.4947 0.7161 0.5445 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5784(3) 0.6216(3) 0.59081(12) 0.0298(9) Uani 1 1 d . . . . .
H4A H 0.5046 0.6011 0.6030 0.036 Uiso 1 1 calc R U . . .
H4B H 0.6006 0.5701 0.5695 0.036 Uiso 1 1 calc R U . . .
C5 C 0.7654(3) 0.9669(3) 0.64709(14) 0.0380(10) Uani 1 1 d . . . . .
H5A H 0.7754 0.9452 0.6161 0.046 Uiso 1 1 calc R U . . .
H5B H 0.8272 0.9346 0.6664 0.046 Uiso 1 1 calc R U . . .
C6 C 0.7851(4) 1.0777(3) 0.64935(14) 0.0435(11) Uani 1 1 d . . . . .
H6A H 0.7244 1.1115 0.6301 0.052 Uiso 1 1 calc R U . . .
H6B H 0.7781 1.1006 0.6803 0.052 Uiso 1 1 calc R U . . .
C7 C 0.9025(4) 1.1061(3) 0.63474(17) 0.0558(13) Uani 1 1 d . . . . .
H7A H 0.9060 1.0902 0.6027 0.067 Uiso 1 1 calc R U . . .
H7B H 0.9626 1.0662 0.6516 0.067 Uiso 1 1 calc R U . . .
C8 C 0.9289(4) 1.2147(4) 0.64185(19) 0.0718(16) Uani 1 1 d . . . . .
H8A H 0.9360 1.2291 0.6739 0.108 Uiso 1 1 calc R U . . .
H8B H 0.8660 1.2547 0.6275 0.108 Uiso 1 1 calc R U . . .
H8C H 1.0019 1.2311 0.6288 0.108 Uiso 1 1 calc R U . . .
C9 C 0.6318(3) 0.9615(3) 0.70670(12) 0.0330(9) Uani 1 1 d . . . . .
H9A H 0.6267 1.0349 0.7069 0.040 Uiso 1 1 calc R U . . .
H9B H 0.7006 0.9426 0.7263 0.040 Uiso 1 1 calc R U . . .
C10 C 0.5255(3) 0.9203(3) 0.72636(13) 0.0374(10) Uani 1 1 d . . . . .
H10A H 0.5230 0.8473 0.7222 0.045 Uiso 1 1 calc R U . . .
H10B H 0.4552 0.9490 0.7106 0.045 Uiso 1 1 calc R U . . .
C11 C 0.5264(4) 0.9443(3) 0.77584(14) 0.0456(11) Uani 1 1 d . . . . .
H11A H 0.5919 0.9088 0.7918 0.055 Uiso 1 1 calc R U . . .
H11B H 0.5397 1.0164 0.7800 0.055 Uiso 1 1 calc R U . . .
C12 C 0.4155(4) 0.9162(4) 0.79646(16) 0.0632(14) Uani 1 1 d . . . . .
H12A H 0.4226 0.9313 0.8284 0.095 Uiso 1 1 calc R U . . .
H12B H 0.4012 0.8449 0.7922 0.095 Uiso 1 1 calc R U . . .
H12C H 0.3508 0.9539 0.7821 0.095 Uiso 1 1 calc R U . . .
C13 C 0.7909(3) 0.6242(3) 0.61129(13) 0.0302(9) Uani 1 1 d . . . . .
H13A H 0.8480 0.6383 0.6365 0.036 Uiso 1 1 calc R U . . .
H13B H 0.7979 0.6778 0.5891 0.036 Uiso 1 1 calc R U . . .
C14 C 0.8246(3) 0.5273(3) 0.59014(14) 0.0353(10) Uani 1 1 d . . . . .
H14A H 0.7692 0.5122 0.5645 0.042 Uiso 1 1 calc R U . . .
H14B H 0.8204 0.4728 0.6121 0.042 Uiso 1 1 calc R U . . .
C15 C 0.9463(3) 0.5328(3) 0.57447(15) 0.0415(10) Uani 1 1 d . . . . .
H15A H 1.0008 0.5492 0.6003 0.050 Uiso 1 1 calc R U . . .
H15B H 0.9497 0.5874 0.5525 0.050 Uiso 1 1 calc R U . . .
C16 C 0.9860(4) 0.4374(3) 0.55329(15) 0.0466(11) Uani 1 1 d . . . . .
H16A H 1.0634 0.4473 0.5425 0.070 Uiso 1 1 calc R U . . .
H16B H 0.9314 0.4195 0.5282 0.070 Uiso 1 1 calc R U . . .
H16C H 0.9890 0.3840 0.5755 0.070 Uiso 1 1 calc R U . . .
C17 C 0.6564(3) 0.5501(3) 0.66203(12) 0.0320(10) Uani 1 1 d . . . . .
H17A H 0.6623 0.4849 0.6471 0.038 Uiso 1 1 calc R U . . .
H17B H 0.7214 0.5544 0.6852 0.038 Uiso 1 1 calc R U . . .
C18 C 0.5451(3) 0.5529(3) 0.68456(13) 0.0392(10) Uani 1 1 d . . . . .
H18A H 0.4799 0.5363 0.6627 0.047 Uiso 1 1 calc R U . . .
H18B H 0.5322 0.6208 0.6959 0.047 Uiso 1 1 calc R U . . .
C19 C 0.5473(4) 0.4796(4) 0.72312(16) 0.0557(13) Uani 1 1 d . . . . .
H19A H 0.5734 0.4141 0.7126 0.067 Uiso 1 1 calc R U . . .
H19B H 0.6046 0.5025 0.7469 0.067 Uiso 1 1 calc R U . . .
C20 C 0.4321(5) 0.4676(4) 0.74231(19) 0.0800(17) Uani 1 1 d . . . . .
H20A H 0.4414 0.4280 0.7697 0.120 Uiso 1 1 calc R U . . .
H20B H 0.3785 0.4337 0.7207 0.120 Uiso 1 1 calc R U . . .
H20C H 0.4010 0.5331 0.7492 0.120 Uiso 1 1 calc R U . . .
C21 C 0.4931(3) 0.2313(3) 0.55660(11) 0.0259(8) Uani 1 1 d . . . . .
C22 C 0.5866(3) 0.2953(3) 0.56559(14) 0.0370(10) Uani 1 1 d . . . . .
H22 H 0.5735 0.3553 0.5811 0.044 Uiso 1 1 calc R U . . .
C23 C 0.6969(3) 0.2761(3) 0.55321(14) 0.0393(10) Uani 1 1 d . . . . .
H23 H 0.7570 0.3229 0.5601 0.047 Uiso 1 1 calc R U . . .
C24 C 0.7212(3) 0.1902(3) 0.53097(14) 0.0376(10) Uani 1 1 d . . . . .
H24 H 0.7971 0.1766 0.5223 0.045 Uiso 1 1 calc R U . . .
C25 C 0.6305(3) 0.1240(3) 0.52169(13) 0.0347(10) Uani 1 1 d . . . . .
H25 H 0.6444 0.0634 0.5068 0.042 Uiso 1 1 calc R U . . .
C26 C 0.5210(3) 0.1454(3) 0.53391(12) 0.0285(9) Uani 1 1 d . . . . .
H26 H 0.4608 0.0990 0.5265 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2634(3) 0.1999(3) 0.54009(13) 0.0292(9) Uani 1 1 d . . . . .
C28 C 0.1905(3) 0.2493(3) 0.50889(13) 0.0359(10) Uani 1 1 d . . . . .
H28 H 0.1963 0.3196 0.5069 0.043 Uiso 1 1 calc R U . . .
C29 C 0.1094(4) 0.2009(3) 0.48045(15) 0.0461(12) Uani 1 1 d . . . . .
H29 H 0.0622 0.2380 0.4593 0.055 Uiso 1 1 calc R U . . .
C30 C 0.0970(3) 0.0992(3) 0.48264(15) 0.0461(12) Uani 1 1 d . . . . .
H30 H 0.0419 0.0655 0.4632 0.055 Uiso 1 1 calc R U . . .
C31 C 0.1659(3) 0.0478(3) 0.51360(16) 0.0459(12) Uani 1 1 d . . . . .
H31 H 0.1583 -0.0223 0.5159 0.055 Uiso 1 1 calc R U . . .
C32 C 0.2462(3) 0.0975(3) 0.54137(15) 0.0377(10) Uani 1 1 d . . . . .
H32 H 0.2925 0.0598 0.5626 0.045 Uiso 1 1 calc R U . . .
C33 C 0.3574(3) 0.2131(3) 0.62480(12) 0.0328(9) Uani 1 1 d . . . . .
C34 C 0.2556(4) 0.1753(4) 0.64048(15) 0.0543(13) Uani 1 1 d . . . . .
H34 H 0.1895 0.1687 0.6201 0.065 Uiso 1 1 calc R U . . .
C35 C 0.2465(5) 0.1472(4) 0.68415(17) 0.0690(15) Uani 1 1 d . . . . .
H35 H 0.1748 0.1226 0.6933 0.083 Uiso 1 1 calc R U . . .
C36 C 0.3401(5) 0.1545(3) 0.71452(16) 0.0584(13) Uani 1 1 d . . . . .
H36 H 0.3344 0.1341 0.7446 0.070 Uiso 1 1 calc R U . . .
C37 C 0.4413(4) 0.1913(3) 0.70090(15) 0.0489(12) Uani 1 1 d . . . . .
H37 H 0.5067 0.1975 0.7216 0.059 Uiso 1 1 calc R U . . .
C38 C 0.4495(4) 0.2199(3) 0.65668(13) 0.0403(10) Uani 1 1 d . . . . .
H38 H 0.5213 0.2453 0.6480 0.048 Uiso 1 1 calc R U . . .
C39 C 0.3399(3) 0.3755(3) 0.57301(13) 0.0300(9) Uani 1 1 d . . . . .
C40 C 0.2889(3) 0.4256(3) 0.60701(14) 0.0353(10) Uani 1 1 d . . . . .
H40 H 0.2724 0.3900 0.6331 0.042 Uiso 1 1 calc R U . . .
C41 C 0.2612(3) 0.5259(3) 0.60414(17) 0.0471(12) Uani 1 1 d . . . . .
H41 H 0.2268 0.5575 0.6282 0.057 Uiso 1 1 calc R U . . .
C42 C 0.2830(3) 0.5798(3) 0.56689(18) 0.0497(13) Uani 1 1 d . . . . .
H42 H 0.2616 0.6478 0.5645 0.060 Uiso 1 1 calc R U . . .
C43 C 0.3362(3) 0.5335(3) 0.53309(15) 0.0423(11) Uani 1 1 d . . . . .
H43 H 0.3537 0.5700 0.5073 0.051 Uiso 1 1 calc R U . . .
C44 C 0.3646(3) 0.4334(3) 0.53647(13) 0.0323(9) Uani 1 1 d . . . . .
H44 H 0.4024 0.4032 0.5129 0.039 Uiso 1 1 calc R U . . .
C45 C 0.2607(4) 0.7655(4) 0.67542(18) 0.0702(11) Uani 1 1 d . . . . .
H45A H 0.2774 0.8095 0.7014 0.084 Uiso 1 1 calc R U . . .
H45B H 0.2928 0.6989 0.6827 0.084 Uiso 1 1 calc R U . . .
C46 C 0.1322(4) 0.7590(5) 0.6644(2) 0.0865(14) Uani 1 1 d . . . . .
H46A H 0.1100 0.6931 0.6520 0.104 Uiso 1 1 calc R U . . .
H46B H 0.0885 0.7718 0.6911 0.104 Uiso 1 1 calc R U . . .
C47 C 0.1121(5) 0.8374(5) 0.6311(2) 0.0865(14) Uani 1 1 d . . . . .
H47A H 0.0783 0.8967 0.6447 0.104 Uiso 1 1 calc R U . . .
H47B H 0.0575 0.8141 0.6064 0.104 Uiso 1 1 calc R U . . .
C48 C 0.2245(4) 0.8618(4) 0.61414(18) 0.0702(11) Uani 1 1 d . . . . .
H48A H 0.2233 0.8472 0.5818 0.084 Uiso 1 1 calc R U . . .
H48B H 0.2413 0.9334 0.6186 0.084 Uiso 1 1 calc R U . . .
B1 B 0.3638(4) 0.2549(3) 0.57349(14) 0.0293(10) Uani 1 1 d . . . . .
N1A N 0.7809(4) 0.7309(3) 0.73780(14) 0.0624(12) Uani 1 1 d . . . . .
N2 N 0.6510(3) 0.9285(2) 0.66022(10) 0.0295(8) Uani 1 1 d . . . . .
N3 N 0.5403(3) 0.7956(2) 0.60090(10) 0.0288(7) Uani 1 1 d D . . . .
N4 N 0.6715(2) 0.6302(2) 0.62826(10) 0.0270(7) Uani 1 1 d . . . . .
O1A O 0.7976(2) 0.7595(2) 0.69740(10) 0.0462(8) Uani 1 1 d . . . . .
O2A O 0.6816(4) 0.7194(3) 0.74561(11) 0.0721(10) Uani 1 1 d . . . . .
O3 O 0.3107(2) 0.8045(2) 0.63748(11) 0.0547(8) Uani 1 1 d . . . . .
Pd1 Pd 0.66006(2) 0.77537(2) 0.65180(2) 0.02721(10) Uani 1 1 d . . . . .
H3 H 0.4651(19) 0.787(3) 0.6127(11) 0.033 Uiso 1 1 d D 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
C1 N2 1.502(4) . ?
C1 C2 1.506(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.489(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.478(5) . ?
C3 C4 1.513(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.498(5) . ?
C5 C6 1.509(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.503(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.506(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.497(5) . ?
C9 C10 1.505(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.521(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.509(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.505(4) . ?
C13 C14 1.514(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.515(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.518(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.495(5) . ?
C17 N4 1.500(4) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.521(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.496(6) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.392(5) . ?
C21 C22 1.393(5) . ?
C21 B1 1.642(5) . ?
C22 C23 1.376(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.390(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.372(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.387(5) . ?
C27 C32 1.394(5) . ?
C27 B1 1.656(5) . ?
C28 C29 1.388(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.370(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.379(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.386(5) . ?
C33 C34 1.393(6) . ?
C33 B1 1.648(6) . ?
C34 C35 1.377(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.371(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.358(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.393(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.389(5) . ?
C39 C44 1.392(5) . ?
C39 B1 1.647(5) . ?
C40 C41 1.390(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.372(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.373(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.389(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.414(6) . ?
C45 C46 1.502(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.464(7) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.465(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.409(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1A O2A 1.197(5) . ?
N1A O1A 1.300(5) . ?
N2 Pd1 2.080(3) . ?
N3 Pd1 2.010(3) . ?
N3 H3 0.967(18) . ?
N4 Pd1 2.085(3) . ?
O1A Pd1 2.038(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 110.2(3) . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.4(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 107.2(3) . . ?
N3 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
N3 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
N4 C4 C3 110.5(3) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 117.6(3) . . ?
N2 C5 H5A 107.9 . . ?
C6 C5 H5A 107.9 . . ?
N2 C5 H5B 107.9 . . ?
C6 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
C7 C6 C5 112.0(4) . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 C8 112.6(4) . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7B 109.1 . . ?
C8 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.7(3) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.7(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 113.5(4) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.2(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 C15 111.1(3) . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14B 109.4 . . ?
C15 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 113.8(3) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N4 115.6(3) . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17B 108.4 . . ?
N4 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.0(3) . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18B 109.4 . . ?
C19 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.2(4) . . ?
C20 C19 H19A 108.9 . . ?
C18 C19 H19A 108.9 . . ?
C20 C19 H19B 108.9 . . ?
C18 C19 H19B 108.9 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 114.0(3) . . ?
C26 C21 B1 123.9(3) . . ?
C22 C21 B1 122.0(3) . . ?
C23 C22 C21 123.5(4) . . ?
C23 C22 H22 118.3 . . ?
C21 C22 H22 118.3 . . ?
C24 C23 C22 120.9(4) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 117.4(4) . . ?
C23 C24 H24 121.3 . . ?
C25 C24 H24 121.3 . . ?
C26 C25 C24 120.5(4) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C21 123.7(3) . . ?
C25 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C28 C27 C32 114.3(3) . . ?
C28 C27 B1 124.3(3) . . ?
C32 C27 B1 121.4(3) . . ?
C27 C28 C29 123.0(4) . . ?
C27 C28 H28 118.5 . . ?
C29 C28 H28 118.5 . . ?
C30 C29 C28 120.4(4) . . ?
C30 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
C31 C30 C29 118.4(4) . . ?
C31 C30 H30 120.8 . . ?
C29 C30 H30 120.8 . . ?
C30 C31 C32 120.2(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 123.7(4) . . ?
C31 C32 H32 118.1 . . ?
C27 C32 H32 118.1 . . ?
C38 C33 C34 114.7(4) . . ?
C38 C33 B1 122.9(3) . . ?
C34 C33 B1 122.3(3) . . ?
C35 C34 C33 122.9(4) . . ?
C35 C34 H34 118.5 . . ?
C33 C34 H34 118.5 . . ?
C36 C35 C34 120.5(5) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C37 C36 C35 118.8(4) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C36 C37 C38 120.3(4) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 H37 119.8 . . ?
C33 C38 C37 122.8(4) . . ?
C33 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C40 C39 C44 115.4(3) . . ?
C40 C39 B1 123.5(4) . . ?
C44 C39 B1 121.1(3) . . ?
C39 C40 C41 122.3(4) . . ?
C39 C40 H40 118.9 . . ?
C41 C40 H40 118.9 . . ?
C42 C41 C40 120.7(4) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C41 C42 C43 118.7(4) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 120.1(4) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C39 122.8(4) . . ?
C43 C44 H44 118.6 . . ?
C39 C44 H44 118.6 . . ?
O3 C45 C46 107.3(4) . . ?
O3 C45 H45A 110.3 . . ?
C46 C45 H45A 110.3 . . ?
O3 C45 H45B 110.3 . . ?
C46 C45 H45B 110.3 . . ?
H45A C45 H45B 108.5 . . ?
C47 C46 C45 102.5(5) . . ?
C47 C46 H46A 111.3 . . ?
C45 C46 H46A 111.3 . . ?
C47 C46 H46B 111.3 . . ?
C45 C46 H46B 111.3 . . ?
H46A C46 H46B 109.2 . . ?
C46 C47 C48 107.2(4) . . ?
C46 C47 H47A 110.3 . . ?
C48 C47 H47A 110.3 . . ?
C46 C47 H47B 110.3 . . ?
C48 C47 H47B 110.3 . . ?
H47A C47 H47B 108.5 . . ?
O3 C48 C47 108.5(4) . . ?
O3 C48 H48A 110.0 . . ?
C47 C48 H48A 110.0 . . ?
O3 C48 H48B 110.0 . . ?
C47 C48 H48B 110.0 . . ?
H48A C48 H48B 108.4 . . ?
C21 B1 C39 110.1(3) . . ?
C21 B1 C33 108.9(3) . . ?
C39 B1 C33 109.1(3) . . ?
C21 B1 C27 109.9(3) . . ?
C39 B1 C27 109.0(3) . . ?
C33 B1 C27 109.9(3) . . ?
O2A N1A O1A 115.2(4) . . ?
C9 N2 C5 109.4(3) . . ?
C9 N2 C1 110.4(3) . . ?
C5 N2 C1 111.5(3) . . ?
C9 N2 Pd1 114.8(2) . . ?
C5 N2 Pd1 104.9(2) . . ?
C1 N2 Pd1 105.6(2) . . ?
C3 N3 C2 116.1(3) . . ?
C3 N3 Pd1 107.2(2) . . ?
C2 N3 Pd1 107.2(2) . . ?
C3 N3 H3 112(2) . . ?
C2 N3 H3 107(2) . . ?
Pd1 N3 H3 107(2) . . ?
C17 N4 C13 110.0(3) . . ?
C17 N4 C4 109.9(3) . . ?
C13 N4 C4 111.5(3) . . ?
C17 N4 Pd1 115.6(2) . . ?
C13 N4 Pd1 104.2(2) . . ?
C4 N4 Pd1 105.5(2) . . ?
N1A O1A Pd1 120.0(3) . . ?
C48 O3 C45 106.9(4) . . ?
N3 Pd1 O1A 172.25(13) . . ?
N3 Pd1 N2 85.44(11) . . ?
O1A Pd1 N2 93.76(11) . . ?
N3 Pd1 N4 85.70(11) . . ?
O1A Pd1 N4 93.75(10) . . ?
N2 Pd1 N4 167.07(12) . . ?

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
N2 C1 C2 N3 55.2(4) . . . . ?
N3 C3 C4 N4 -53.7(4) . . . . ?
N2 C5 C6 C7 -179.2(3) . . . . ?
C5 C6 C7 C8 -173.3(4) . . . . ?
N2 C9 C10 C11 170.2(3) . . . . ?
C9 C10 C11 C12 172.9(4) . . . . ?
N4 C13 C14 C15 179.6(3) . . . . ?
C13 C14 C15 C16 179.4(3) . . . . ?
N4 C17 C18 C19 -170.7(3) . . . . ?
C17 C18 C19 C20 -171.0(4) . . . . ?
C26 C21 C22 C23 0.1(6) . . . . ?
B1 C21 C22 C23 177.8(4) . . . . ?
C21 C22 C23 C24 -0.4(6) . . . . ?
C22 C23 C24 C25 -0.2(6) . . . . ?
C23 C24 C25 C26 1.0(6) . . . . ?
C24 C25 C26 C21 -1.3(6) . . . . ?
C22 C21 C26 C25 0.7(5) . . . . ?
B1 C21 C26 C25 -176.9(3) . . . . ?
C32 C27 C28 C29 -1.7(6) . . . . ?
B1 C27 C28 C29 178.1(4) . . . . ?
C27 C28 C29 C30 0.9(7) . . . . ?
C28 C29 C30 C31 0.3(7) . . . . ?
C29 C30 C31 C32 -0.6(7) . . . . ?
C30 C31 C32 C27 -0.3(7) . . . . ?
C28 C27 C32 C31 1.4(6) . . . . ?
B1 C27 C32 C31 -178.4(4) . . . . ?
C38 C33 C34 C35 0.2(7) . . . . ?
B1 C33 C34 C35 -174.9(5) . . . . ?
C33 C34 C35 C36 -0.8(8) . . . . ?
C34 C35 C36 C37 1.0(8) . . . . ?
C35 C36 C37 C38 -0.8(7) . . . . ?
C34 C33 C38 C37 0.1(6) . . . . ?
B1 C33 C38 C37 175.1(4) . . . . ?
C36 C37 C38 C33 0.2(6) . . . . ?
C44 C39 C40 C41 1.9(5) . . . . ?
B1 C39 C40 C41 -174.7(3) . . . . ?
C39 C40 C41 C42 0.4(6) . . . . ?
C40 C41 C42 C43 -2.1(6) . . . . ?
C41 C42 C43 C44 1.5(6) . . . . ?
C42 C43 C44 C39 0.9(6) . . . . ?
C40 C39 C44 C43 -2.5(5) . . . . ?
B1 C39 C44 C43 174.1(3) . . . . ?
O3 C45 C46 C47 -27.1(6) . . . . ?
C45 C46 C47 C48 17.6(7) . . . . ?
C46 C47 C48 O3 -2.6(7) . . . . ?
C26 C21 B1 C39 -149.0(3) . . . . ?
C22 C21 B1 C39 33.7(5) . . . . ?
C26 C21 B1 C33 91.5(4) . . . . ?
C22 C21 B1 C33 -85.9(4) . . . . ?
C26 C21 B1 C27 -28.9(5) . . . . ?
C22 C21 B1 C27 153.7(3) . . . . ?
C40 C39 B1 C21 -137.0(3) . . . . ?
C44 C39 B1 C21 46.6(4) . . . . ?
C40 C39 B1 C33 -17.6(5) . . . . ?
C44 C39 B1 C33 166.0(3) . . . . ?
C40 C39 B1 C27 102.4(4) . . . . ?
C44 C39 B1 C27 -74.0(4) . . . . ?
C38 C33 B1 C21 38.6(5) . . . . ?
C34 C33 B1 C21 -146.8(4) . . . . ?
C38 C33 B1 C39 -81.6(4) . . . . ?
C34 C33 B1 C39 93.1(4) . . . . ?
C38 C33 B1 C27 159.0(3) . . . . ?
C34 C33 B1 C27 -26.3(5) . . . . ?
C28 C27 B1 C21 -106.1(4) . . . . ?
C32 C27 B1 C21 73.7(4) . . . . ?
C28 C27 B1 C39 14.7(5) . . . . ?
C32 C27 B1 C39 -165.6(3) . . . . ?
C28 C27 B1 C33 134.1(4) . . . . ?
C32 C27 B1 C33 -46.1(5) . . . . ?
C10 C9 N2 C5 -174.2(3) . . . . ?
C10 C9 N2 C1 62.7(4) . . . . ?
C10 C9 N2 Pd1 -56.6(4) . . . . ?
C6 C5 N2 C9 -56.7(4) . . . . ?
C6 C5 N2 C1 65.7(4) . . . . ?
C6 C5 N2 Pd1 179.5(3) . . . . ?
C2 C1 N2 C9 -159.7(3) . . . . ?
C2 C1 N2 C5 78.5(4) . . . . ?
C2 C1 N2 Pd1 -34.9(4) . . . . ?
C4 C3 N3 C2 166.3(3) . . . . ?
C4 C3 N3 Pd1 46.5(3) . . . . ?
C1 C2 N3 C3 -166.5(3) . . . . ?
C1 C2 N3 Pd1 -46.7(3) . . . . ?
C18 C17 N4 C13 174.9(3) . . . . ?
C18 C17 N4 C4 -61.9(4) . . . . ?
C18 C17 N4 Pd1 57.3(4) . . . . ?
C14 C13 N4 C17 57.7(4) . . . . ?
C14 C13 N4 C4 -64.5(4) . . . . ?
C14 C13 N4 Pd1 -177.8(3) . . . . ?
C3 C4 N4 C17 157.8(3) . . . . ?
C3 C4 N4 C13 -79.9(4) . . . . ?
C3 C4 N4 Pd1 32.6(3) . . . . ?
O2A N1A O1A Pd1 -2.8(6) . . . . ?
C47 C48 O3 C45 -14.9(6) . . . . ?
C46 C45 O3 C48 26.4(6) . . . . ?

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
C5 H5B O1A 0.99 2.57 3.186(5) 120.6 .
C10 H10A O2A 0.99 2.58 3.280(6) 127.8 .
C13 H13A O1A 0.99 2.55 3.161(5) 120.0 .
C18 H18B O2A 0.99 2.57 3.239(6) 124.4 .
N3 H3 O3 0.967(18) 1.99(2) 2.943(5) 167(3) .

_refine_diff_density_max         0.774
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.081

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-200K
_database_code_depnum_ccdc_archive 'CCDC 1441788'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-200K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.5703(5)
_cell_length_b                   13.4876(6)
_cell_length_c                   30.0621(14)
_cell_angle_alpha                90
_cell_angle_beta                 93.739(5)
_cell_angle_gamma                90
_cell_volume                     4681.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    3604
_cell_measurement_theta_min      3.5420
_cell_measurement_theta_max      24.4030

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.439
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83416
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20675
_diffrn_reflns_av_unetI/netI     0.1096
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9555
_reflns_number_gt                5746
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0368P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9555
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1202
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1101
_refine_ls_wR_factor_gt          0.0914
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
C1 C 0.5539(4) 0.9631(3) 0.62834(13) 0.0422(11) Uani 1 1 d . . . . .
H1A H 0.4795 0.9574 0.6427 0.051 Uiso 1 1 calc R U . . .
H1B H 0.5657 1.0336 0.6206 0.051 Uiso 1 1 calc R U . . .
C2 C 0.5498(4) 0.9011(3) 0.58683(13) 0.0414(11) Uani 1 1 d . . . . .
H2A H 0.4818 0.9195 0.5668 0.050 Uiso 1 1 calc R U . . .
H2B H 0.6207 0.9114 0.5707 0.050 Uiso 1 1 calc R U . . .
C3 C 0.5617(3) 0.7204(3) 0.56684(12) 0.0333(9) Uani 1 1 d . . . . .
H3A H 0.6315 0.7374 0.5510 0.040 Uiso 1 1 calc R U . . .
H3B H 0.4946 0.7167 0.5447 0.040 Uiso 1 1 calc R U . . .
C4 C 0.5785(3) 0.6226(3) 0.59063(12) 0.0320(9) Uani 1 1 d . . . . .
H4A H 0.6009 0.5714 0.5692 0.038 Uiso 1 1 calc R U . . .
H4B H 0.5047 0.6019 0.6027 0.038 Uiso 1 1 calc R U . . .
C5 C 0.7665(4) 0.9664(3) 0.64707(14) 0.0442(11) Uani 1 1 d . . . . .
H5A H 0.7770 0.9446 0.6162 0.053 Uiso 1 1 calc R U . . .
H5B H 0.8279 0.9343 0.6665 0.053 Uiso 1 1 calc R U . . .
C6 C 0.7856(4) 1.0772(3) 0.64933(15) 0.0494(12) Uani 1 1 d . . . . .
H6A H 0.7246 1.1108 0.6302 0.059 Uiso 1 1 calc R U . . .
H6B H 0.7790 1.1001 0.6804 0.059 Uiso 1 1 calc R U . . .
C7 C 0.9025(4) 1.1056(3) 0.63426(18) 0.0621(14) Uani 1 1 d . . . . .
H7A H 0.9628 1.0657 0.6509 0.075 Uiso 1 1 calc R U . . .
H7B H 0.9055 1.0897 0.6022 0.075 Uiso 1 1 calc R U . . .
C8 C 0.9288(5) 1.2135(4) 0.6413(2) 0.0875(19) Uani 1 1 d . . . . .
H8A H 0.9363 1.2278 0.6733 0.131 Uiso 1 1 calc R U . . .
H8B H 0.8657 1.2533 0.6271 0.131 Uiso 1 1 calc R U . . .
H8C H 1.0014 1.2299 0.6279 0.131 Uiso 1 1 calc R U . . .
C9 C 0.6324(3) 0.9609(3) 0.70672(13) 0.0382(10) Uani 1 1 d . . . . .
H9A H 0.6270 1.0342 0.7070 0.046 Uiso 1 1 calc R U . . .
H9B H 0.7011 0.9421 0.7262 0.046 Uiso 1 1 calc R U . . .
C10 C 0.5266(4) 0.9195(3) 0.72651(13) 0.0430(11) Uani 1 1 d . . . . .
H10A H 0.5245 0.8466 0.7224 0.052 Uiso 1 1 calc R U . . .
H10B H 0.4562 0.9477 0.7108 0.052 Uiso 1 1 calc R U . . .
C11 C 0.5274(4) 0.9439(3) 0.77601(14) 0.0517(12) Uani 1 1 d . . . . .
H11A H 0.5930 0.9090 0.7920 0.062 Uiso 1 1 calc R U . . .
H11B H 0.5400 1.0160 0.7801 0.062 Uiso 1 1 calc R U . . .
C12 C 0.4167(4) 0.9151(4) 0.79625(17) 0.0745(16) Uani 1 1 d . . . . .
H12A H 0.4227 0.9306 0.8282 0.112 Uiso 1 1 calc R U . . .
H12B H 0.4035 0.8438 0.7922 0.112 Uiso 1 1 calc R U . . .
H12C H 0.3519 0.9520 0.7816 0.112 Uiso 1 1 calc R U . . .
C13 C 0.7902(3) 0.6246(3) 0.61133(13) 0.0350(10) Uani 1 1 d . . . . .
H13A H 0.8469 0.6383 0.6367 0.042 Uiso 1 1 calc R U . . .
H13B H 0.7975 0.6784 0.5893 0.042 Uiso 1 1 calc R U . . .
C14 C 0.8247(3) 0.5279(3) 0.58985(14) 0.0403(10) Uani 1 1 d . . . . .
H14A H 0.8199 0.4733 0.6116 0.048 Uiso 1 1 calc R U . . .
H14B H 0.7697 0.5133 0.5641 0.048 Uiso 1 1 calc R U . . .
C15 C 0.9459(3) 0.5325(3) 0.57431(16) 0.0466(11) Uani 1 1 d . . . . .
H15A H 1.0003 0.5487 0.6001 0.056 Uiso 1 1 calc R U . . .
H15B H 0.9500 0.5869 0.5524 0.056 Uiso 1 1 calc R U . . .
C16 C 0.9849(4) 0.4373(3) 0.55330(16) 0.0553(12) Uani 1 1 d . . . . .
H16A H 1.0627 0.4462 0.5429 0.083 Uiso 1 1 calc R U . . .
H16B H 0.9310 0.4201 0.5280 0.083 Uiso 1 1 calc R U . . .
H16C H 0.9861 0.3838 0.5754 0.083 Uiso 1 1 calc R U . . .
C17 C 0.6556(3) 0.5510(3) 0.66169(13) 0.0373(10) Uani 1 1 d . . . . .
H17A H 0.7210 0.5547 0.6846 0.045 Uiso 1 1 calc R U . . .
H17B H 0.6604 0.4860 0.6466 0.045 Uiso 1 1 calc R U . . .
C18 C 0.5449(3) 0.5542(3) 0.68482(14) 0.0444(11) Uani 1 1 d . . . . .
H18A H 0.4792 0.5400 0.6630 0.053 Uiso 1 1 calc R U . . .
H18B H 0.5339 0.6217 0.6969 0.053 Uiso 1 1 calc R U . . .
C19 C 0.5456(4) 0.4795(4) 0.72259(17) 0.0667(14) Uani 1 1 d . . . . .
H19A H 0.5683 0.4139 0.7112 0.080 Uiso 1 1 calc R U . . .
H19B H 0.6049 0.4995 0.7461 0.080 Uiso 1 1 calc R U . . .
C20 C 0.4326(5) 0.4696(5) 0.7427(2) 0.096(2) Uani 1 1 d . . . . .
H20A H 0.4425 0.4300 0.7700 0.144 Uiso 1 1 calc R U . . .
H20B H 0.3772 0.4366 0.7215 0.144 Uiso 1 1 calc R U . . .
H20C H 0.4034 0.5355 0.7498 0.144 Uiso 1 1 calc R U . . .
C21 C 0.4932(3) 0.2309(3) 0.55660(12) 0.0310(9) Uani 1 1 d . . . . .
C22 C 0.5867(3) 0.2949(3) 0.56542(14) 0.0424(11) Uani 1 1 d . . . . .
H22 H 0.5736 0.3549 0.5809 0.051 Uiso 1 1 calc R U . . .
C23 C 0.6969(3) 0.2758(3) 0.55286(15) 0.0458(11) Uani 1 1 d . . . . .
H23 H 0.7571 0.3224 0.5597 0.055 Uiso 1 1 calc R U . . .
C24 C 0.7206(3) 0.1900(3) 0.53055(14) 0.0426(11) Uani 1 1 d . . . . .
H24 H 0.7964 0.1765 0.5218 0.051 Uiso 1 1 calc R U . . .
C25 C 0.6310(3) 0.1241(3) 0.52125(13) 0.0383(10) Uani 1 1 d . . . . .
H25 H 0.6451 0.0638 0.5062 0.046 Uiso 1 1 calc R U . . .
C26 C 0.5214(3) 0.1454(3) 0.53376(12) 0.0312(9) Uani 1 1 d . . . . .
H26 H 0.4614 0.0990 0.5264 0.037 Uiso 1 1 calc R U . . .
C27 C 0.2639(3) 0.2001(3) 0.54049(13) 0.0314(9) Uani 1 1 d . . . . .
C28 C 0.1905(3) 0.2498(3) 0.50934(13) 0.0408(11) Uani 1 1 d . . . . .
H28 H 0.1968 0.3199 0.5073 0.049 Uiso 1 1 calc R U . . .
C29 C 0.1085(4) 0.2019(3) 0.48117(15) 0.0510(12) Uani 1 1 d . . . . .
H29 H 0.0602 0.2392 0.4606 0.061 Uiso 1 1 calc R U . . .
C30 C 0.0970(4) 0.0997(3) 0.48305(16) 0.0506(12) Uani 1 1 d . . . . .
H30 H 0.0428 0.0661 0.4633 0.061 Uiso 1 1 calc R U . . .
C31 C 0.1652(4) 0.0484(3) 0.51379(18) 0.0538(13) Uani 1 1 d . . . . .
H31 H 0.1572 -0.0215 0.5161 0.065 Uiso 1 1 calc R U . . .
C32 C 0.2459(3) 0.0978(3) 0.54165(15) 0.0432(11) Uani 1 1 d . . . . .
H32 H 0.2917 0.0599 0.5628 0.052 Uiso 1 1 calc R U . . .
C33 C 0.3575(3) 0.2125(3) 0.62472(13) 0.0385(10) Uani 1 1 d . . . . .
C34 C 0.2569(4) 0.1751(4) 0.64077(16) 0.0641(14) Uani 1 1 d . . . . .
H34 H 0.1906 0.1687 0.6206 0.077 Uiso 1 1 calc R U . . .
C35 C 0.2477(5) 0.1465(4) 0.68437(17) 0.0783(17) Uani 1 1 d . . . . .
H35 H 0.1763 0.1218 0.6936 0.094 Uiso 1 1 calc R U . . .
C36 C 0.3416(5) 0.1536(4) 0.71444(16) 0.0656(15) Uani 1 1 d . . . . .
H36 H 0.3363 0.1329 0.7444 0.079 Uiso 1 1 calc R U . . .
C37 C 0.4417(5) 0.1906(3) 0.70070(16) 0.0573(14) Uani 1 1 d . . . . .
H37 H 0.5070 0.1970 0.7213 0.069 Uiso 1 1 calc R U . . .
C38 C 0.4501(4) 0.2193(3) 0.65655(13) 0.0453(11) Uani 1 1 d . . . . .
H38 H 0.5218 0.2445 0.6478 0.054 Uiso 1 1 calc R U . . .
C39 C 0.3407(3) 0.3749(3) 0.57313(13) 0.0320(9) Uani 1 1 d . . . . .
C40 C 0.2888(3) 0.4251(3) 0.60688(14) 0.0405(10) Uani 1 1 d . . . . .
H40 H 0.2713 0.3894 0.6328 0.049 Uiso 1 1 calc R U . . .
C41 C 0.2613(3) 0.5251(3) 0.60438(17) 0.0508(12) Uani 1 1 d . . . . .
H41 H 0.2271 0.5567 0.6285 0.061 Uiso 1 1 calc R U . . .
C42 C 0.2836(4) 0.5783(3) 0.56704(19) 0.0531(13) Uani 1 1 d . . . . .
H42 H 0.2627 0.6464 0.5647 0.064 Uiso 1 1 calc R U . . .
C43 C 0.3361(4) 0.5325(3) 0.53327(16) 0.0466(12) Uani 1 1 d . . . . .
H43 H 0.3531 0.5689 0.5074 0.056 Uiso 1 1 calc R U . . .
C44 C 0.3646(3) 0.4332(3) 0.53666(14) 0.0373(10) Uani 1 1 d . . . . .
H44 H 0.4024 0.4032 0.5130 0.045 Uiso 1 1 calc R U . . .
C45 C 0.2610(5) 0.7660(4) 0.67509(19) 0.0769(11) Uani 1 1 d . . . . .
H45A H 0.2783 0.8097 0.7011 0.092 Uiso 1 1 calc R U . . .
H45B H 0.2926 0.6992 0.6822 0.092 Uiso 1 1 calc R U . . .
C46 C 0.1334(5) 0.7603(5) 0.6646(2) 0.0974(15) Uani 1 1 d . . . . .
H46A H 0.1102 0.6938 0.6532 0.117 Uiso 1 1 calc R U . . .
H46B H 0.0903 0.7756 0.6911 0.117 Uiso 1 1 calc R U . . .
C47 C 0.1143(5) 0.8354(5) 0.6305(2) 0.0974(15) Uani 1 1 d . . . . .
H47A H 0.0780 0.8947 0.6431 0.117 Uiso 1 1 calc R U . . .
H47B H 0.0619 0.8097 0.6058 0.117 Uiso 1 1 calc R U . . .
C48 C 0.2260(5) 0.8619(4) 0.61388(19) 0.0769(11) Uani 1 1 d . . . . .
H48A H 0.2258 0.8480 0.5815 0.092 Uiso 1 1 calc R U . . .
H48B H 0.2416 0.9333 0.6187 0.092 Uiso 1 1 calc R U . . .
B1 B 0.3641(4) 0.2547(3) 0.57347(15) 0.0322(11) Uani 1 1 d . . . . .
N1A N 0.7830(5) 0.7316(4) 0.73721(17) 0.0762(15) Uani 1 1 d . . . . .
N2 N 0.6517(3) 0.9283(2) 0.66011(10) 0.0348(8) Uani 1 1 d . . . . .
N3 N 0.5412(3) 0.7961(2) 0.60090(10) 0.0306(8) Uani 1 1 d D . . . .
N4 N 0.6710(2) 0.6304(2) 0.62818(10) 0.0312(8) Uani 1 1 d . . . . .
O1A O 0.7976(3) 0.7591(2) 0.69735(11) 0.0573(9) Uani 1 1 d . . . . .
O2A O 0.6849(4) 0.7202(3) 0.74543(12) 0.0834(12) Uani 1 1 d . . . . .
O3 O 0.3114(3) 0.8046(2) 0.63729(11) 0.0625(9) Uani 1 1 d . . . . .
Pd1 Pd 0.66040(3) 0.77550(2) 0.65178(2) 0.03129(10) Uani 1 1 d . . . . .
H3 H 0.4649(19) 0.787(3) 0.6120(11) 0.038 Uiso 1 1 d D 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
C1 C2 1.500(5) . ?
C1 N2 1.507(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N3 1.484(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 N3 1.476(5) . ?
C3 C4 1.507(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N4 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 N2 1.500(5) . ?
C5 C6 1.512(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.504(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.499(6) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 N2 1.499(5) . ?
C9 C10 1.503(6) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.524(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.505(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N4 1.502(5) . ?
C13 C14 1.520(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.508(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.513(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 N4 1.489(5) . ?
C17 C18 1.497(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.518(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.481(7) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C26 1.392(5) . ?
C21 C22 1.396(5) . ?
C21 B1 1.640(6) . ?
C22 C23 1.378(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.374(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.380(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.377(5) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.394(5) . ?
C27 C32 1.396(5) . ?
C27 B1 1.649(6) . ?
C28 C29 1.390(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.364(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.384(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.384(6) . ?
C33 C38 1.392(5) . ?
C33 B1 1.649(6) . ?
C34 C35 1.377(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.370(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.351(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.388(5) . ?
C39 C44 1.391(5) . ?
C39 B1 1.644(5) . ?
C40 C41 1.387(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.371(6) . ?
C41 H41 0.9500 . ?
C42 C43 1.365(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.382(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 O3 1.410(6) . ?
C45 C46 1.492(7) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.448(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.459(7) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 O3 1.406(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
N1A O2A 1.186(6) . ?
N1A O1A 1.276(6) . ?
N2 Pd1 2.079(3) . ?
N3 Pd1 2.011(3) . ?
N3 H3 0.972(18) . ?
N4 Pd1 2.087(3) . ?
O1A Pd1 2.040(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
C2 C1 N2 109.6(3) . . ?
C2 C1 H1A 109.8 . . ?
N2 C1 H1A 109.8 . . ?
C2 C1 H1B 109.8 . . ?
N2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 107.1(3) . . ?
N3 C2 H2A 110.3 . . ?
C1 C2 H2A 110.3 . . ?
N3 C2 H2B 110.3 . . ?
C1 C2 H2B 110.3 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 107.3(3) . . ?
N3 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
N3 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
C3 C4 N4 110.9(3) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 117.2(3) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.7(4) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
C8 C7 C6 112.5(4) . . ?
C8 C7 H7A 109.1 . . ?
C6 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C6 C7 H7B 109.1 . . ?
H7A C7 H7B 107.8 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.8(3) . . ?
N2 C9 H9A 108.3 . . ?
C10 C9 H9A 108.3 . . ?
N2 C9 H9B 108.3 . . ?
C10 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.6(3) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.8(4) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.5(3) . . ?
N4 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
N4 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.8(3) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 113.7(3) . . ?
C14 C15 H15A 108.8 . . ?
C16 C15 H15A 108.8 . . ?
C14 C15 H15B 108.8 . . ?
C16 C15 H15B 108.8 . . ?
H15A C15 H15B 107.7 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.9(3) . . ?
N4 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
N4 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C17 C18 C19 111.4(3) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 113.8(4) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.7(3) . . ?
C26 C21 B1 124.2(3) . . ?
C22 C21 B1 122.1(3) . . ?
C23 C22 C21 123.5(4) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.6(4) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 118.1(4) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C21 123.9(3) . . ?
C25 C26 H26 118.1 . . ?
C21 C26 H26 118.1 . . ?
C28 C27 C32 114.0(3) . . ?
C28 C27 B1 124.3(3) . . ?
C32 C27 B1 121.7(3) . . ?
C29 C28 C27 123.2(4) . . ?
C29 C28 H28 118.4 . . ?
C27 C28 H28 118.4 . . ?
C30 C29 C28 120.1(4) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C31 C30 C29 118.7(4) . . ?
C31 C30 H30 120.7 . . ?
C29 C30 H30 120.7 . . ?
C30 C31 C32 120.2(4) . . ?
C30 C31 H31 119.9 . . ?
C32 C31 H31 119.9 . . ?
C31 C32 C27 123.8(4) . . ?
C31 C32 H32 118.1 . . ?
C27 C32 H32 118.1 . . ?
C34 C33 C38 114.3(4) . . ?
C34 C33 B1 122.9(4) . . ?
C38 C33 B1 122.6(4) . . ?
C35 C34 C33 123.5(5) . . ?
C35 C34 H34 118.2 . . ?
C33 C34 H34 118.2 . . ?
C36 C35 C34 120.1(5) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C37 C36 C35 118.9(5) . . ?
C37 C36 H36 120.6 . . ?
C35 C36 H36 120.6 . . ?
C36 C37 C38 120.6(4) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C37 C38 C33 122.6(4) . . ?
C37 C38 H38 118.7 . . ?
C33 C38 H38 118.7 . . ?
C40 C39 C44 114.7(4) . . ?
C40 C39 B1 123.7(4) . . ?
C44 C39 B1 121.4(4) . . ?
C41 C40 C39 122.9(4) . . ?
C41 C40 H40 118.5 . . ?
C39 C40 H40 118.5 . . ?
C42 C41 C40 119.9(4) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C43 C42 C41 119.2(4) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C43 C44 120.0(4) . . ?
C42 C43 H43 120.0 . . ?
C44 C43 H43 120.0 . . ?
C43 C44 C39 123.1(4) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 107.7(4) . . ?
O3 C45 H45A 110.2 . . ?
C46 C45 H45A 110.2 . . ?
O3 C45 H45B 110.2 . . ?
C46 C45 H45B 110.2 . . ?
H45A C45 H45B 108.5 . . ?
C47 C46 C45 102.5(5) . . ?
C47 C46 H46A 111.3 . . ?
C45 C46 H46A 111.3 . . ?
C47 C46 H46B 111.3 . . ?
C45 C46 H46B 111.3 . . ?
H46A C46 H46B 109.2 . . ?
C46 C47 C48 108.4(5) . . ?
C46 C47 H47A 110.0 . . ?
C48 C47 H47A 110.0 . . ?
C46 C47 H47B 110.0 . . ?
C48 C47 H47B 110.0 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 107.7(5) . . ?
O3 C48 H48A 110.2 . . ?
C47 C48 H48A 110.2 . . ?
O3 C48 H48B 110.2 . . ?
C47 C48 H48B 110.2 . . ?
H48A C48 H48B 108.5 . . ?
C21 B1 C39 110.1(3) . . ?
C21 B1 C33 108.7(3) . . ?
C39 B1 C33 109.2(3) . . ?
C21 B1 C27 110.2(3) . . ?
C39 B1 C27 109.1(3) . . ?
C33 B1 C27 109.5(3) . . ?
O2A N1A O1A 114.9(4) . . ?
C9 N2 C5 109.4(3) . . ?
C9 N2 C1 110.5(3) . . ?
C5 N2 C1 111.6(3) . . ?
C9 N2 Pd1 114.5(2) . . ?
C5 N2 Pd1 104.9(2) . . ?
C1 N2 Pd1 105.8(2) . . ?
C3 N3 C2 116.5(3) . . ?
C3 N3 Pd1 107.4(2) . . ?
C2 N3 Pd1 107.0(2) . . ?
C3 N3 H3 110(2) . . ?
C2 N3 H3 107(2) . . ?
Pd1 N3 H3 108(2) . . ?
C17 N4 C13 110.0(3) . . ?
C17 N4 C4 110.2(3) . . ?
C13 N4 C4 111.5(3) . . ?
C17 N4 Pd1 115.6(2) . . ?
C13 N4 Pd1 103.9(2) . . ?
C4 N4 Pd1 105.4(2) . . ?
N1A O1A Pd1 121.1(3) . . ?
C48 O3 C45 107.0(4) . . ?
N3 Pd1 O1A 172.23(14) . . ?
N3 Pd1 N2 85.33(11) . . ?
O1A Pd1 N2 93.92(12) . . ?
N3 Pd1 N4 85.60(11) . . ?
O1A Pd1 N4 93.81(11) . . ?
N2 Pd1 N4 166.98(12) . . ?

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
N2 C1 C2 N3 55.1(4) . . . . ?
N3 C3 C4 N4 -53.1(4) . . . . ?
N2 C5 C6 C7 -178.5(4) . . . . ?
C5 C6 C7 C8 -173.3(4) . . . . ?
N2 C9 C10 C11 170.5(3) . . . . ?
C9 C10 C11 C12 173.0(4) . . . . ?
N4 C13 C14 C15 179.7(3) . . . . ?
C13 C14 C15 C16 179.1(4) . . . . ?
N4 C17 C18 C19 -172.0(3) . . . . ?
C17 C18 C19 C20 -172.1(4) . . . . ?
C26 C21 C22 C23 0.0(6) . . . . ?
B1 C21 C22 C23 178.1(4) . . . . ?
C21 C22 C23 C24 -0.3(7) . . . . ?
C22 C23 C24 C25 -0.1(6) . . . . ?
C23 C24 C25 C26 0.7(6) . . . . ?
C24 C25 C26 C21 -1.1(6) . . . . ?
C22 C21 C26 C25 0.8(5) . . . . ?
B1 C21 C26 C25 -177.3(4) . . . . ?
C32 C27 C28 C29 -1.5(6) . . . . ?
B1 C27 C28 C29 178.4(4) . . . . ?
C27 C28 C29 C30 -0.3(7) . . . . ?
C28 C29 C30 C31 1.9(7) . . . . ?
C29 C30 C31 C32 -1.6(7) . . . . ?
C30 C31 C32 C27 -0.3(7) . . . . ?
C28 C27 C32 C31 1.8(6) . . . . ?
B1 C27 C32 C31 -178.1(4) . . . . ?
C38 C33 C34 C35 -0.1(7) . . . . ?
B1 C33 C34 C35 -175.0(5) . . . . ?
C33 C34 C35 C36 -0.5(9) . . . . ?
C34 C35 C36 C37 1.2(8) . . . . ?
C35 C36 C37 C38 -1.1(7) . . . . ?
C36 C37 C38 C33 0.5(7) . . . . ?
C34 C33 C38 C37 0.1(6) . . . . ?
B1 C33 C38 C37 175.0(4) . . . . ?
C44 C39 C40 C41 0.9(5) . . . . ?
B1 C39 C40 C41 -174.7(3) . . . . ?
C39 C40 C41 C42 1.1(6) . . . . ?
C40 C41 C42 C43 -2.1(6) . . . . ?
C41 C42 C43 C44 1.0(6) . . . . ?
C42 C43 C44 C39 1.1(6) . . . . ?
C40 C39 C44 C43 -2.0(5) . . . . ?
B1 C39 C44 C43 173.7(3) . . . . ?
O3 C45 C46 C47 -25.0(6) . . . . ?
C45 C46 C47 C48 15.0(7) . . . . ?
C46 C47 C48 O3 -0.2(7) . . . . ?
C26 C21 B1 C39 -148.9(3) . . . . ?
C22 C21 B1 C39 33.2(5) . . . . ?
C26 C21 B1 C33 91.6(4) . . . . ?
C22 C21 B1 C33 -86.3(4) . . . . ?
C26 C21 B1 C27 -28.5(5) . . . . ?
C22 C21 B1 C27 153.6(3) . . . . ?
C40 C39 B1 C21 -137.5(4) . . . . ?
C44 C39 B1 C21 47.2(4) . . . . ?
C40 C39 B1 C33 -18.3(5) . . . . ?
C44 C39 B1 C33 166.4(3) . . . . ?
C40 C39 B1 C27 101.4(4) . . . . ?
C44 C39 B1 C27 -73.9(4) . . . . ?
C34 C33 B1 C21 -146.9(4) . . . . ?
C38 C33 B1 C21 38.7(5) . . . . ?
C34 C33 B1 C39 93.0(5) . . . . ?
C38 C33 B1 C39 -81.4(4) . . . . ?
C34 C33 B1 C27 -26.4(5) . . . . ?
C38 C33 B1 C27 159.2(3) . . . . ?
C28 C27 B1 C21 -106.4(4) . . . . ?
C32 C27 B1 C21 73.5(5) . . . . ?
C28 C27 B1 C39 14.6(5) . . . . ?
C32 C27 B1 C39 -165.5(4) . . . . ?
C28 C27 B1 C33 134.1(4) . . . . ?
C32 C27 B1 C33 -46.0(5) . . . . ?
C10 C9 N2 C5 -173.7(3) . . . . ?
C10 C9 N2 C1 63.0(4) . . . . ?
C10 C9 N2 Pd1 -56.3(4) . . . . ?
C6 C5 N2 C9 -57.3(4) . . . . ?
C6 C5 N2 C1 65.3(4) . . . . ?
C6 C5 N2 Pd1 179.4(3) . . . . ?
C2 C1 N2 C9 -159.2(3) . . . . ?
C2 C1 N2 C5 78.8(4) . . . . ?
C2 C1 N2 Pd1 -34.8(4) . . . . ?
C4 C3 N3 C2 166.0(3) . . . . ?
C4 C3 N3 Pd1 46.1(3) . . . . ?
C1 C2 N3 C3 -167.0(3) . . . . ?
C1 C2 N3 Pd1 -46.9(3) . . . . ?
C18 C17 N4 C13 174.0(3) . . . . ?
C18 C17 N4 C4 -62.7(4) . . . . ?
C18 C17 N4 Pd1 56.8(4) . . . . ?
C14 C13 N4 C17 58.0(4) . . . . ?
C14 C13 N4 C4 -64.6(4) . . . . ?
C14 C13 N4 Pd1 -177.7(3) . . . . ?
C3 C4 N4 C17 157.5(3) . . . . ?
C3 C4 N4 C13 -79.9(4) . . . . ?
C3 C4 N4 Pd1 32.1(3) . . . . ?
O2A N1A O1A Pd1 -2.5(6) . . . . ?
C47 C48 O3 C45 -15.9(6) . . . . ?
C46 C45 O3 C48 25.8(6) . . . . ?

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
C5 H5B O1A 0.99 2.57 3.188(5) 120.4 .
C10 H10A O2A 0.99 2.58 3.281(6) 127.7 .
C13 H13A O1A 0.99 2.54 3.156(5) 120.3 .
C18 H18B O2A 0.99 2.57 3.251(6) 125.7 .
N3 H3 O3 0.972(18) 1.99(2) 2.942(5) 166(3) .

_refine_diff_density_max         0.740
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.079

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-220K
_database_code_depnum_ccdc_archive 'CCDC 1441789'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT201_SS-220K             
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          3 Report
RESPONSE: The disordered fragments of the partially decayed nitrite 
ligand are modelled isotropically as this was deemed the best model to fit 
the available data.
;
_vrf_PLAT910_SS-220K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         14 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6115(7)
_cell_length_b                   13.5033(7)
_cell_length_c                   29.9820(17)
_cell_angle_alpha                90
_cell_angle_beta                 93.955(5)
_cell_angle_gamma                90
_cell_volume                     4689.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    220(2)
_cell_measurement_reflns_used    3411
_cell_measurement_theta_min      3.5280
_cell_measurement_theta_max      23.4320

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.438
_shelx_estimated_absorpt_T_min   0.929
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.79232
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      220(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20694
_diffrn_reflns_av_unetI/netI     0.1383
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.008
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9574
_reflns_number_gt                5369
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0360P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9574
_refine_ls_number_parameters     504
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.0628
_refine_ls_wR_factor_ref         0.1333
_refine_ls_wR_factor_gt          0.1065
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.001
_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
C1 C 0.5546(5) 0.9626(3) 0.62930(16) 0.0477(14) Uani 1 1 d . . . . .
H1A H 0.4810 0.9563 0.6432 0.057 Uiso 1 1 calc R U . . .
H1B H 0.5657 1.0325 0.6219 0.057 Uiso 1 1 calc R U . . .
C2 C 0.5516(5) 0.9013(3) 0.58728(16) 0.0452(14) Uani 1 1 d . . . . .
H2A H 0.4850 0.9197 0.5671 0.054 Uiso 1 1 calc R U . . .
H2B H 0.6221 0.9116 0.5717 0.054 Uiso 1 1 calc R U . . .
C3 C 0.5635(4) 0.7214(3) 0.56708(15) 0.0395(12) Uani 1 1 d . . . . .
H3A H 0.6334 0.7378 0.5520 0.047 Uiso 1 1 calc R U . . .
H3B H 0.4982 0.7185 0.5446 0.047 Uiso 1 1 calc R U . . .
C4 C 0.5781(4) 0.6235(3) 0.59101(15) 0.0364(12) Uani 1 1 d . . . . .
H4A H 0.5989 0.5724 0.5698 0.044 Uiso 1 1 calc R U . . .
H4B H 0.5048 0.6043 0.6029 0.044 Uiso 1 1 calc R U . . .
C5 C 0.7661(4) 0.9665(4) 0.64928(17) 0.0467(13) Uani 1 1 d . . . . .
H5A H 0.7770 0.9452 0.6186 0.056 Uiso 1 1 calc R U . . .
H5B H 0.8265 0.9346 0.6687 0.056 Uiso 1 1 calc R U . . .
C6 C 0.7854(5) 1.0768(4) 0.6517(2) 0.0601(16) Uani 1 1 d . . . . .
H6A H 0.7795 1.0991 0.6826 0.072 Uiso 1 1 calc R U . . .
H6B H 0.7251 1.1103 0.6329 0.072 Uiso 1 1 calc R U . . .
C7 C 0.9024(6) 1.1049(4) 0.6365(2) 0.079(2) Uani 1 1 d . . . . .
H7A H 0.9047 1.0909 0.6045 0.095 Uiso 1 1 calc R U . . .
H7B H 0.9621 1.0648 0.6526 0.095 Uiso 1 1 calc R U . . .
C8 C 0.9271(6) 1.2135(5) 0.6450(3) 0.111(3) Uani 1 1 d . . . . .
H8A H 0.9433 1.2244 0.6768 0.167 Uiso 1 1 calc R U . . .
H8B H 0.8604 1.2524 0.6345 0.167 Uiso 1 1 calc R U . . .
H8C H 0.9933 1.2334 0.6292 0.167 Uiso 1 1 calc R U . . .
C9 C 0.6321(4) 0.9612(4) 0.70850(16) 0.0425(13) Uani 1 1 d . . . . .
H9A H 0.7006 0.9446 0.7280 0.051 Uiso 1 1 calc R U . . .
H9B H 0.6244 1.0335 0.7085 0.051 Uiso 1 1 calc R U . . .
C10 C 0.5282(4) 0.9176(4) 0.72826(16) 0.0459(14) Uani 1 1 d . . . . .
H10A H 0.5297 0.8454 0.7252 0.055 Uiso 1 1 calc R U . . .
H10B H 0.4580 0.9423 0.7119 0.055 Uiso 1 1 calc R U . . .
C11 C 0.5260(5) 0.9445(4) 0.77699(18) 0.0617(16) Uani 1 1 d . . . . .
H11A H 0.5910 0.9122 0.7937 0.074 Uiso 1 1 calc R U . . .
H11B H 0.5362 1.0162 0.7803 0.074 Uiso 1 1 calc R U . . .
C12 C 0.4161(6) 0.9147(5) 0.7967(2) 0.085(2) Uani 1 1 d . . . . .
H12A H 0.4202 0.9319 0.8282 0.127 Uiso 1 1 calc R U . . .
H12B H 0.4051 0.8438 0.7934 0.127 Uiso 1 1 calc R U . . .
H12C H 0.3517 0.9492 0.7813 0.127 Uiso 1 1 calc R U . . .
C13 C 0.7891(4) 0.6242(3) 0.61195(16) 0.0383(12) Uani 1 1 d . . . . .
H13A H 0.8453 0.6378 0.6371 0.046 Uiso 1 1 calc R U . . .
H13B H 0.7963 0.6773 0.5900 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8226(4) 0.5276(4) 0.59058(18) 0.0456(13) Uani 1 1 d . . . . .
H14A H 0.8173 0.4737 0.6122 0.055 Uiso 1 1 calc R U . . .
H14B H 0.7682 0.5134 0.5649 0.055 Uiso 1 1 calc R U . . .
C15 C 0.9436(4) 0.5313(4) 0.57518(19) 0.0507(14) Uani 1 1 d . . . . .
H15A H 0.9480 0.5852 0.5535 0.061 Uiso 1 1 calc R U . . .
H15B H 0.9971 0.5469 0.6009 0.061 Uiso 1 1 calc R U . . .
C16 C 0.9827(5) 0.4372(4) 0.5542(2) 0.0604(16) Uani 1 1 d . . . . .
H16A H 1.0609 0.4454 0.5453 0.091 Uiso 1 1 calc R U . . .
H16B H 0.9318 0.4219 0.5281 0.091 Uiso 1 1 calc R U . . .
H16C H 0.9806 0.3835 0.5756 0.091 Uiso 1 1 calc R U . . .
C17 C 0.6545(4) 0.5505(3) 0.66142(16) 0.0410(13) Uani 1 1 d . . . . .
H17A H 0.7215 0.5499 0.6832 0.049 Uiso 1 1 calc R U . . .
H17B H 0.6532 0.4869 0.6456 0.049 Uiso 1 1 calc R U . . .
C18 C 0.5472(4) 0.5579(4) 0.68649(17) 0.0479(14) Uani 1 1 d . . . . .
H18A H 0.4793 0.5541 0.6653 0.058 Uiso 1 1 calc R U . . .
H18B H 0.5459 0.6223 0.7015 0.058 Uiso 1 1 calc R U . . .
C19 C 0.5411(6) 0.4765(5) 0.7208(2) 0.0767(19) Uani 1 1 d . . . . .
H19A H 0.5519 0.4127 0.7060 0.092 Uiso 1 1 calc R U . . .
H19B H 0.6050 0.4849 0.7435 0.092 Uiso 1 1 calc R U . . .
C20 C 0.4321(6) 0.4731(6) 0.7432(3) 0.106(3) Uani 1 1 d . . . . .
H20A H 0.4360 0.4206 0.7653 0.159 Uiso 1 1 calc R U . . .
H20B H 0.3685 0.4605 0.7212 0.159 Uiso 1 1 calc R U . . .
H20C H 0.4201 0.5360 0.7578 0.159 Uiso 1 1 calc R U . . .
C21 C 0.4931(4) 0.2304(3) 0.55650(14) 0.0307(10) Uani 1 1 d . . . . .
C22 C 0.5867(4) 0.2938(4) 0.56550(18) 0.0476(14) Uani 1 1 d . . . . .
H22 H 0.5739 0.3531 0.5808 0.057 Uiso 1 1 calc R U . . .
C23 C 0.6964(4) 0.2748(4) 0.55339(19) 0.0525(14) Uani 1 1 d . . . . .
H23 H 0.7558 0.3207 0.5605 0.063 Uiso 1 1 calc R U . . .
C24 C 0.7196(4) 0.1896(4) 0.53110(18) 0.0491(14) Uani 1 1 d . . . . .
H24 H 0.7945 0.1758 0.5228 0.059 Uiso 1 1 calc R U . . .
C25 C 0.6295(4) 0.1243(3) 0.52118(16) 0.0420(13) Uani 1 1 d . . . . .
H25 H 0.6430 0.0653 0.5058 0.050 Uiso 1 1 calc R U . . .
C26 C 0.5207(4) 0.1451(3) 0.53364(15) 0.0348(11) Uani 1 1 d . . . . .
H26 H 0.4616 0.0992 0.5263 0.042 Uiso 1 1 calc R U . . .
C27 C 0.2645(4) 0.2006(3) 0.54040(15) 0.0346(11) Uani 1 1 d . . . . .
C28 C 0.1910(4) 0.2503(3) 0.50949(16) 0.0434(13) Uani 1 1 d . . . . .
H28 H 0.1972 0.3195 0.5075 0.052 Uiso 1 1 calc R U . . .
C29 C 0.1090(5) 0.2025(4) 0.48139(19) 0.0569(16) Uani 1 1 d . . . . .
H29 H 0.0612 0.2396 0.4610 0.068 Uiso 1 1 calc R U . . .
C30 C 0.0970(5) 0.1011(4) 0.4831(2) 0.0584(16) Uani 1 1 d . . . . .
H30 H 0.0428 0.0681 0.4636 0.070 Uiso 1 1 calc R U . . .
C31 C 0.1660(5) 0.0495(4) 0.5138(2) 0.0589(17) Uani 1 1 d . . . . .
H31 H 0.1579 -0.0195 0.5161 0.071 Uiso 1 1 calc R U . . .
C32 C 0.2473(4) 0.0983(4) 0.54144(19) 0.0493(14) Uani 1 1 d . . . . .
H32 H 0.2935 0.0607 0.5621 0.059 Uiso 1 1 calc R U . . .
C33 C 0.3590(5) 0.2127(3) 0.62487(16) 0.0438(13) Uani 1 1 d . . . . .
C34 C 0.2578(6) 0.1749(5) 0.6407(2) 0.0698(18) Uani 1 1 d . . . . .
H34 H 0.1920 0.1684 0.6209 0.084 Uiso 1 1 calc R U . . .
C35 C 0.2517(7) 0.1469(5) 0.6846(2) 0.094(2) Uani 1 1 d . . . . .
H35 H 0.1818 0.1219 0.6940 0.113 Uiso 1 1 calc R U . . .
C36 C 0.3449(8) 0.1545(5) 0.7149(2) 0.082(2) Uani 1 1 d . . . . .
H36 H 0.3397 0.1348 0.7447 0.098 Uiso 1 1 calc R U . . .
C37 C 0.4455(7) 0.1913(5) 0.7007(2) 0.070(2) Uani 1 1 d . . . . .
H37 H 0.5103 0.1981 0.7211 0.083 Uiso 1 1 calc R U . . .
C38 C 0.4526(5) 0.2188(4) 0.65626(17) 0.0516(14) Uani 1 1 d . . . . .
H38 H 0.5233 0.2425 0.6471 0.062 Uiso 1 1 calc R U . . .
C39 C 0.3420(4) 0.3749(3) 0.57290(16) 0.0358(12) Uani 1 1 d . . . . .
C40 C 0.2904(4) 0.4245(4) 0.60655(18) 0.0454(13) Uani 1 1 d . . . . .
H40 H 0.2739 0.3892 0.6324 0.054 Uiso 1 1 calc R U . . .
C41 C 0.2619(4) 0.5242(4) 0.6038(2) 0.0571(16) Uani 1 1 d . . . . .
H41 H 0.2269 0.5550 0.6275 0.068 Uiso 1 1 calc R U . . .
C42 C 0.2843(5) 0.5776(4) 0.5669(2) 0.0601(17) Uani 1 1 d . . . . .
H42 H 0.2636 0.6448 0.5647 0.072 Uiso 1 1 calc R U . . .
C43 C 0.3370(5) 0.5329(4) 0.5332(2) 0.0545(16) Uani 1 1 d . . . . .
H43 H 0.3534 0.5694 0.5077 0.065 Uiso 1 1 calc R U . . .
C44 C 0.3667(4) 0.4331(4) 0.53633(17) 0.0440(13) Uani 1 1 d . . . . .
H44 H 0.4049 0.4040 0.5130 0.053 Uiso 1 1 calc R U . . .
C45 C 0.2650(6) 0.7661(5) 0.6743(2) 0.0849(15) Uani 1 1 d . . . . .
H45A H 0.2829 0.8083 0.7004 0.102 Uiso 1 1 calc R U . . .
H45B H 0.2958 0.6997 0.6809 0.102 Uiso 1 1 calc R U . . .
C46 C 0.1385(6) 0.7608(6) 0.6644(3) 0.112(2) Uani 1 1 d . . . . .
H46A H 0.1149 0.6954 0.6530 0.135 Uiso 1 1 calc R U . . .
H46B H 0.0972 0.7757 0.6911 0.135 Uiso 1 1 calc R U . . .
C47 C 0.1185(6) 0.8366(6) 0.6305(3) 0.112(2) Uani 1 1 d . . . . .
H47A H 0.0838 0.8952 0.6435 0.135 Uiso 1 1 calc R U . . .
H47B H 0.0654 0.8118 0.6062 0.135 Uiso 1 1 calc R U . . .
C48 C 0.2305(6) 0.8632(5) 0.6130(2) 0.0849(15) Uani 1 1 d . . . . .
H48A H 0.2295 0.8487 0.5809 0.102 Uiso 1 1 calc R U . . .
H48B H 0.2465 0.9339 0.6175 0.102 Uiso 1 1 calc R U . . .
B1 B 0.3651(5) 0.2551(4) 0.57324(18) 0.0365(14) Uani 1 1 d . . . . .
N2 N 0.6524(3) 0.9281(3) 0.66175(13) 0.0396(10) Uani 1 1 d . . . . .
N3 N 0.5425(3) 0.7964(3) 0.60132(12) 0.0336(9) Uani 1 1 d D . . . .
N4 N 0.6706(3) 0.6301(3) 0.62876(12) 0.0320(9) Uani 1 1 d . . . . .
O3 O 0.3153(3) 0.8054(3) 0.63691(14) 0.0685(12) Uani 1 1 d . . . . .
Pd1 Pd 0.65939(3) 0.77505(3) 0.65340(2) 0.03345(12) Uani 1 1 d . . . . .
N1_a N 0.7749(7) 0.7489(7) 0.7061(3) 0.043(2) Uiso 0.708(7) 1 d D . P A 1
O1_a O 0.8736(6) 0.7602(5) 0.7024(2) 0.0796(15) Uiso 0.708(7) 1 d D . P A 1
O2_a O 0.7368(6) 0.7327(6) 0.7429(3) 0.0796(15) Uiso 0.708(7) 1 d D . P A 1
N1A_b N 0.7823(12) 0.7099(11) 0.7366(5) 0.043(2) Uiso 0.292(7) 1 d D . P A 2
O1A_b O 0.798(2) 0.7654(16) 0.7020(7) 0.076(7) Uiso 0.292(7) 1 d D . P A 2
O2A_b O 0.6808(13) 0.7131(12) 0.7445(6) 0.0796(15) Uiso 0.292(7) 1 d D . P A 2
H3 H 0.469(3) 0.790(4) 0.6146(18) 0.095 Uiso 1 1 d D 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
C1 C2 1.506(6) . ?
C1 N2 1.517(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.484(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.474(6) . ?
C3 C4 1.508(6) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.509(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.490(6) . ?
C5 C6 1.507(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.511(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.513(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 C10 1.501(7) . ?
C9 N2 1.506(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.507(7) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.499(8) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.499(6) . ?
C13 C14 1.516(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.510(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.502(7) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 N4 1.475(6) . ?
C17 C18 1.502(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.510(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.473(9) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C26 1.389(6) . ?
C21 C22 1.395(6) . ?
C21 B1 1.635(7) . ?
C22 C23 1.372(7) . ?
C22 H22 0.9400 . ?
C23 C24 1.367(7) . ?
C23 H23 0.9400 . ?
C24 C25 1.385(6) . ?
C24 H24 0.9400 . ?
C25 C26 1.371(6) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.388(6) . ?
C27 C32 1.396(6) . ?
C27 B1 1.648(7) . ?
C28 C29 1.387(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.378(7) . ?
C29 H29 0.9400 . ?
C30 C31 1.368(7) . ?
C30 H30 0.9400 . ?
C31 C32 1.380(7) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.390(7) . ?
C33 C34 1.394(8) . ?
C33 B1 1.656(7) . ?
C34 C35 1.374(8) . ?
C34 H34 0.9400 . ?
C35 C36 1.368(9) . ?
C35 H35 0.9400 . ?
C36 C37 1.364(9) . ?
C36 H36 0.9400 . ?
C37 C38 1.392(8) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C40 1.382(7) . ?
C39 C44 1.395(7) . ?
C39 B1 1.640(7) . ?
C40 C41 1.387(7) . ?
C40 H40 0.9400 . ?
C41 C42 1.362(8) . ?
C41 H41 0.9400 . ?
C42 C43 1.358(8) . ?
C42 H42 0.9400 . ?
C43 C44 1.392(7) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.403(7) . ?
C45 C46 1.479(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.450(10) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.480(9) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.412(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N2 Pd1 2.083(4) . ?
N3 Pd1 2.018(3) . ?
N3 H3 0.97(2) . ?
N4 Pd1 2.099(4) . ?
Pd1 N1_a 2.031(8) . ?
Pd1 O1A_b 2.10(2) . ?
N1_a O1_a 1.170(11) . ?
N1_a O2_a 1.237(10) . ?
N1A_b O2A_b 1.219(16) . ?
N1A_b O1A_b 1.301(17) . ?

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
C2 C1 N2 109.9(4) . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1B 109.7 . . ?
N2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.6(4) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.8(4) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
C3 C4 N4 110.8(3) . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
N4 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 117.6(4) . . ?
N2 C5 H5A 107.9 . . ?
C6 C5 H5A 107.9 . . ?
N2 C5 H5B 107.9 . . ?
C6 C5 H5B 107.9 . . ?
H5A C5 H5B 107.2 . . ?
C5 C6 C7 111.5(5) . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C6 C7 C8 110.9(6) . . ?
C6 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 115.6(4) . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9B 108.4 . . ?
N2 C9 H9B 108.4 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 110.8(4) . . ?
C9 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.9(5) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.1(4) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.3 . . ?
C15 C14 C13 111.9(4) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C16 C15 C14 114.5(4) . . ?
C16 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
C16 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.6(4) . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.8(4) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 114.5(5) . . ?
C20 C19 H19A 108.6 . . ?
C18 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.6(4) . . ?
C26 C21 B1 124.4(4) . . ?
C22 C21 B1 121.9(4) . . ?
C23 C22 C21 124.0(5) . . ?
C23 C22 H22 118.0 . . ?
C21 C22 H22 118.0 . . ?
C24 C23 C22 120.3(5) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.0(5) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C26 C25 C24 120.5(5) . . ?
C26 C25 H25 119.7 . . ?
C24 C25 H25 119.7 . . ?
C25 C26 C21 123.5(4) . . ?
C25 C26 H26 118.2 . . ?
C21 C26 H26 118.2 . . ?
C28 C27 C32 114.2(4) . . ?
C28 C27 B1 124.1(4) . . ?
C32 C27 B1 121.7(4) . . ?
C29 C28 C27 123.0(5) . . ?
C29 C28 H28 118.5 . . ?
C27 C28 H28 118.5 . . ?
C30 C29 C28 120.5(5) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C31 C30 C29 118.3(5) . . ?
C31 C30 H30 120.9 . . ?
C29 C30 H30 120.9 . . ?
C30 C31 C32 120.4(5) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.5(5) . . ?
C31 C32 H32 118.3 . . ?
C27 C32 H32 118.3 . . ?
C38 C33 C34 115.4(5) . . ?
C38 C33 B1 122.0(5) . . ?
C34 C33 B1 122.5(4) . . ?
C35 C34 C33 121.8(6) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C36 C35 C34 121.6(7) . . ?
C36 C35 H35 119.2 . . ?
C34 C35 H35 119.2 . . ?
C37 C36 C35 118.5(6) . . ?
C37 C36 H36 120.8 . . ?
C35 C36 H36 120.8 . . ?
C36 C37 C38 120.2(6) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 122.5(6) . . ?
C33 C38 H38 118.7 . . ?
C37 C38 H38 118.7 . . ?
C40 C39 C44 115.1(4) . . ?
C40 C39 B1 123.6(5) . . ?
C44 C39 B1 121.2(4) . . ?
C39 C40 C41 122.7(5) . . ?
C39 C40 H40 118.7 . . ?
C41 C40 H40 118.7 . . ?
C42 C41 C40 120.3(6) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C43 C42 C41 119.3(5) . . ?
C43 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C42 C43 C44 120.2(6) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C39 122.3(5) . . ?
C43 C44 H44 118.8 . . ?
C39 C44 H44 118.8 . . ?
O3 C45 C46 108.8(6) . . ?
O3 C45 H45A 109.9 . . ?
C46 C45 H45A 109.9 . . ?
O3 C45 H45B 109.9 . . ?
C46 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
C47 C46 C45 102.4(7) . . ?
C47 C46 H46A 111.3 . . ?
C45 C46 H46A 111.3 . . ?
C47 C46 H46B 111.3 . . ?
C45 C46 H46B 111.3 . . ?
H46A C46 H46B 109.2 . . ?
C46 C47 C48 108.5(6) . . ?
C46 C47 H47A 110.0 . . ?
C48 C47 H47A 110.0 . . ?
C46 C47 H47B 110.0 . . ?
C48 C47 H47B 110.0 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 106.6(6) . . ?
O3 C48 H48A 110.4 . . ?
C47 C48 H48A 110.4 . . ?
O3 C48 H48B 110.4 . . ?
C47 C48 H48B 110.4 . . ?
H48A C48 H48B 108.6 . . ?
C21 B1 C39 110.5(4) . . ?
C21 B1 C27 110.3(4) . . ?
C39 B1 C27 109.1(4) . . ?
C21 B1 C33 108.4(4) . . ?
C39 B1 C33 109.2(4) . . ?
C27 B1 C33 109.3(4) . . ?
C5 N2 C9 109.1(4) . . ?
C5 N2 C1 111.7(4) . . ?
C9 N2 C1 110.3(4) . . ?
C5 N2 Pd1 105.8(3) . . ?
C9 N2 Pd1 114.6(3) . . ?
C1 N2 Pd1 105.2(3) . . ?
C3 N3 C2 116.1(4) . . ?
C3 N3 Pd1 107.8(3) . . ?
C2 N3 Pd1 107.4(3) . . ?
C3 N3 H3 115(4) . . ?
C2 N3 H3 107(4) . . ?
Pd1 N3 H3 104(3) . . ?
C17 N4 C13 110.2(3) . . ?
C17 N4 C4 109.8(3) . . ?
C13 N4 C4 111.5(4) . . ?
C17 N4 Pd1 115.6(3) . . ?
C13 N4 Pd1 104.4(2) . . ?
C4 N4 Pd1 105.1(2) . . ?
C45 O3 C48 107.5(5) . . ?
N3 Pd1 N1_a 178.0(3) . . ?
N3 Pd1 N2 85.52(14) . . ?
N1_a Pd1 N2 96.2(3) . . ?
N3 Pd1 O1A_b 171.5(6) . . ?
N2 Pd1 O1A_b 90.7(6) . . ?
N3 Pd1 N4 85.15(13) . . ?
N1_a Pd1 N4 93.3(3) . . ?
N2 Pd1 N4 166.10(15) . . ?
O1A_b Pd1 N4 97.1(7) . . ?
O1_a N1_a O2_a 121.3(8) . . ?
O1_a N1_a Pd1 120.2(6) . . ?
O2_a N1_a Pd1 117.9(7) . . ?
O2A_b N1A_b O1A_b 108.7(19) . . ?
N1A_b O1A_b Pd1 116.8(16) . . ?

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
N2 C1 C2 N3 55.6(5) . . . . ?
N3 C3 C4 N4 -54.3(5) . . . . ?
N2 C5 C6 C7 -177.9(5) . . . . ?
C5 C6 C7 C8 -172.4(5) . . . . ?
N2 C9 C10 C11 172.0(4) . . . . ?
C9 C10 C11 C12 172.1(5) . . . . ?
N4 C13 C14 C15 -179.9(4) . . . . ?
C13 C14 C15 C16 179.3(4) . . . . ?
N4 C17 C18 C19 -177.1(4) . . . . ?
C17 C18 C19 C20 -173.8(6) . . . . ?
C26 C21 C22 C23 -0.3(7) . . . . ?
B1 C21 C22 C23 177.9(5) . . . . ?
C21 C22 C23 C24 0.0(8) . . . . ?
C22 C23 C24 C25 0.3(8) . . . . ?
C23 C24 C25 C26 -0.2(7) . . . . ?
C24 C25 C26 C21 -0.1(7) . . . . ?
C22 C21 C26 C25 0.3(7) . . . . ?
B1 C21 C26 C25 -177.8(4) . . . . ?
C32 C27 C28 C29 -1.2(8) . . . . ?
B1 C27 C28 C29 178.3(5) . . . . ?
C27 C28 C29 C30 -0.1(9) . . . . ?
C28 C29 C30 C31 1.5(9) . . . . ?
C29 C30 C31 C32 -1.6(9) . . . . ?
C30 C31 C32 C27 0.3(9) . . . . ?
C28 C27 C32 C31 1.1(8) . . . . ?
B1 C27 C32 C31 -178.4(5) . . . . ?
C38 C33 C34 C35 0.7(9) . . . . ?
B1 C33 C34 C35 -175.1(6) . . . . ?
C33 C34 C35 C36 -0.2(11) . . . . ?
C34 C35 C36 C37 0.3(11) . . . . ?
C35 C36 C37 C38 -1.0(10) . . . . ?
C34 C33 C38 C37 -1.4(8) . . . . ?
B1 C33 C38 C37 174.4(5) . . . . ?
C36 C37 C38 C33 1.6(9) . . . . ?
C44 C39 C40 C41 1.9(7) . . . . ?
B1 C39 C40 C41 -173.9(4) . . . . ?
C39 C40 C41 C42 0.1(8) . . . . ?
C40 C41 C42 C43 -1.3(8) . . . . ?
C41 C42 C43 C44 0.5(8) . . . . ?
C42 C43 C44 C39 1.6(7) . . . . ?
C40 C39 C44 C43 -2.7(7) . . . . ?
B1 C39 C44 C43 173.2(4) . . . . ?
O3 C45 C46 C47 -24.6(8) . . . . ?
C45 C46 C47 C48 15.2(9) . . . . ?
C46 C47 C48 O3 -1.2(9) . . . . ?
C26 C21 B1 C39 -148.7(4) . . . . ?
C22 C21 B1 C39 33.3(6) . . . . ?
C26 C21 B1 C27 -27.9(6) . . . . ?
C22 C21 B1 C27 154.1(4) . . . . ?
C26 C21 B1 C33 91.7(5) . . . . ?
C22 C21 B1 C33 -86.3(5) . . . . ?
C40 C39 B1 C21 -137.8(4) . . . . ?
C44 C39 B1 C21 46.7(5) . . . . ?
C40 C39 B1 C27 100.7(5) . . . . ?
C44 C39 B1 C27 -74.8(5) . . . . ?
C40 C39 B1 C33 -18.7(6) . . . . ?
C44 C39 B1 C33 165.8(4) . . . . ?
C28 C27 B1 C21 -107.1(5) . . . . ?
C32 C27 B1 C21 72.3(6) . . . . ?
C28 C27 B1 C39 14.6(7) . . . . ?
C32 C27 B1 C39 -166.0(5) . . . . ?
C28 C27 B1 C33 133.9(5) . . . . ?
C32 C27 B1 C33 -46.7(6) . . . . ?
C38 C33 B1 C21 38.3(6) . . . . ?
C34 C33 B1 C21 -146.2(5) . . . . ?
C38 C33 B1 C39 -82.2(5) . . . . ?
C34 C33 B1 C39 93.3(6) . . . . ?
C38 C33 B1 C27 158.5(4) . . . . ?
C34 C33 B1 C27 -26.0(7) . . . . ?
C6 C5 N2 C9 -56.7(6) . . . . ?
C6 C5 N2 C1 65.5(5) . . . . ?
C6 C5 N2 Pd1 179.4(4) . . . . ?
C10 C9 N2 C5 -172.4(4) . . . . ?
C10 C9 N2 C1 64.6(5) . . . . ?
C10 C9 N2 Pd1 -53.9(5) . . . . ?
C2 C1 N2 C5 78.5(5) . . . . ?
C2 C1 N2 C9 -159.9(4) . . . . ?
C2 C1 N2 Pd1 -35.8(5) . . . . ?
C4 C3 N3 C2 166.8(4) . . . . ?
C4 C3 N3 Pd1 46.4(4) . . . . ?
C1 C2 N3 C3 -167.1(4) . . . . ?
C1 C2 N3 Pd1 -46.4(4) . . . . ?
C18 C17 N4 C13 170.3(4) . . . . ?
C18 C17 N4 C4 -66.5(5) . . . . ?
C18 C17 N4 Pd1 52.2(5) . . . . ?
C14 C13 N4 C17 56.9(5) . . . . ?
C14 C13 N4 C4 -65.3(5) . . . . ?
C14 C13 N4 Pd1 -178.4(3) . . . . ?
C3 C4 N4 C17 158.7(4) . . . . ?
C3 C4 N4 C13 -78.8(5) . . . . ?
C3 C4 N4 Pd1 33.7(4) . . . . ?
C46 C45 O3 C48 24.9(7) . . . . ?
C47 C48 O3 C45 -14.4(8) . . . . ?
O2A_b N1A_b O1A_b Pd1 -32(2) . . . . ?

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
C5 H5B O1_a 0.98 2.60 3.402(8) 138.6 .
C5 H5B O1A_b 0.98 2.52 3.15(2) 121.6 .
C10 H10A O2A_b 0.98 2.54 3.299(17) 133.9 .
C13 H13A O1_a 0.98 2.57 3.365(8) 138.7 .
C18 H18B O2A_b 0.98 2.31 3.073(17) 134.1 .
C46 H46B O1_a 0.98 2.65 3.352(11) 128.9 1_455
N3 H3 O3 0.97(2) 1.96(2) 2.915(6) 168(5) .

_refine_diff_density_max         0.762
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.084

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-240K
_database_code_depnum_ccdc_archive 'CCDC 1441790'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-240K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6460(6)
_cell_length_b                   13.5277(7)
_cell_length_c                   30.0138(15)
_cell_angle_alpha                90
_cell_angle_beta                 93.953(5)
_cell_angle_gamma                90
_cell_volume                     4717.2(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    3334
_cell_measurement_theta_min      3.5270
_cell_measurement_theta_max      23.4400

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.436
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      240(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20802
_diffrn_reflns_av_unetI/netI     0.1194
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.012
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9632
_reflns_number_gt                5444
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0326P)²+0.8603P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9632
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1120
_refine_ls_wR_factor_gt          0.0903
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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
C1 C 0.5567(4) 0.9629(3) 0.62986(14) 0.0488(12) Uani 1 1 d . . . . .
H1A H 0.4828 0.9567 0.6434 0.059 Uiso 1 1 calc R U . . .
H1B H 0.5685 1.0327 0.6228 0.059 Uiso 1 1 calc R U . . .
C2 C 0.5541(4) 0.9027(3) 0.58774(14) 0.0465(12) Uani 1 1 d . . . . .
H2A H 0.4881 0.9217 0.5675 0.056 Uiso 1 1 calc R U . . .
H2B H 0.6247 0.9131 0.5724 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5652(3) 0.7226(3) 0.56706(13) 0.0401(10) Uani 1 1 d . . . . .
H3A H 0.6351 0.7386 0.5521 0.048 Uiso 1 1 calc R U . . .
H3B H 0.5002 0.7200 0.5445 0.048 Uiso 1 1 calc R U . . .
C4 C 0.5788(3) 0.6251(3) 0.59108(13) 0.0403(11) Uani 1 1 d . . . . .
H4A H 0.5053 0.6065 0.6028 0.048 Uiso 1 1 calc R U . . .
H4B H 0.5994 0.5739 0.5700 0.048 Uiso 1 1 calc R U . . .
C5 C 0.7672(4) 0.9659(3) 0.64942(16) 0.0502(12) Uani 1 1 d . . . . .
H5A H 0.7771 0.9450 0.6187 0.060 Uiso 1 1 calc R U . . .
H5B H 0.8280 0.9341 0.6685 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7857(4) 1.0768(3) 0.65207(18) 0.0655(15) Uani 1 1 d . . . . .
H6A H 0.7253 1.1101 0.6333 0.079 Uiso 1 1 calc R U . . .
H6B H 0.7797 1.0989 0.6829 0.079 Uiso 1 1 calc R U . . .
C7 C 0.9020(5) 1.1055(4) 0.6369(2) 0.089(2) Uani 1 1 d . . . . .
H7A H 0.9615 1.0654 0.6529 0.107 Uiso 1 1 calc R U . . .
H7B H 0.9041 1.0912 0.6049 0.107 Uiso 1 1 calc R U . . .
C8 C 0.9280(6) 1.2126(5) 0.6448(3) 0.133(3) Uani 1 1 d . . . . .
H8A H 0.9340 1.2256 0.6767 0.199 Uiso 1 1 calc R U . . .
H8B H 0.8667 1.2524 0.6306 0.199 Uiso 1 1 calc R U . . .
H8C H 1.0002 1.2292 0.6324 0.199 Uiso 1 1 calc R U . . .
C9 C 0.6322(4) 0.9606(3) 0.70882(14) 0.0474(12) Uani 1 1 d . . . . .
H9A H 0.6231 1.0326 0.7086 0.057 Uiso 1 1 calc R U . . .
H9B H 0.7007 0.9451 0.7284 0.057 Uiso 1 1 calc R U . . .
C10 C 0.5298(4) 0.9159(4) 0.72846(15) 0.0537(13) Uani 1 1 d . . . . .
H10A H 0.5328 0.8438 0.7256 0.064 Uiso 1 1 calc R U . . .
H10B H 0.4594 0.9393 0.7120 0.064 Uiso 1 1 calc R U . . .
C11 C 0.5263(5) 0.9435(4) 0.77752(17) 0.0687(15) Uani 1 1 d . . . . .
H11A H 0.5908 0.9114 0.7946 0.082 Uiso 1 1 calc R U . . .
H11B H 0.5364 1.0151 0.7807 0.082 Uiso 1 1 calc R U . . .
C12 C 0.4161(5) 0.9139(5) 0.7968(2) 0.099(2) Uani 1 1 d . . . . .
H12A H 0.4213 0.9275 0.8287 0.149 Uiso 1 1 calc R U . . .
H12B H 0.4028 0.8439 0.7919 0.149 Uiso 1 1 calc R U . . .
H12C H 0.3529 0.9513 0.7825 0.149 Uiso 1 1 calc R U . . .
C13 C 0.7884(3) 0.6236(3) 0.61210(14) 0.0408(11) Uani 1 1 d . . . . .
H13A H 0.8445 0.6362 0.6373 0.049 Uiso 1 1 calc R U . . .
H13B H 0.7965 0.6769 0.5904 0.049 Uiso 1 1 calc R U . . .
C14 C 0.8211(3) 0.5278(3) 0.59046(15) 0.0465(12) Uani 1 1 d . . . . .
H14A H 0.7673 0.5148 0.5646 0.056 Uiso 1 1 calc R U . . .
H14B H 0.8146 0.4735 0.6117 0.056 Uiso 1 1 calc R U . . .
C15 C 0.9424(4) 0.5308(3) 0.57555(18) 0.0578(13) Uani 1 1 d . . . . .
H15A H 0.9954 0.5457 0.6015 0.069 Uiso 1 1 calc R U . . .
H15B H 0.9480 0.5848 0.5540 0.069 Uiso 1 1 calc R U . . .
C16 C 0.9805(4) 0.4358(4) 0.55436(18) 0.0654(15) Uani 1 1 d . . . . .
H16A H 1.0582 0.4436 0.5452 0.098 Uiso 1 1 calc R U . . .
H16B H 0.9290 0.4206 0.5285 0.098 Uiso 1 1 calc R U . . .
H16C H 0.9787 0.3823 0.5758 0.098 Uiso 1 1 calc R U . . .
C17 C 0.6524(4) 0.5500(3) 0.66144(14) 0.0440(12) Uani 1 1 d . . . . .
H17A H 0.7202 0.5469 0.6826 0.053 Uiso 1 1 calc R U . . .
H17B H 0.6478 0.4871 0.6452 0.053 Uiso 1 1 calc R U . . .
C18 C 0.5477(4) 0.5597(3) 0.68729(16) 0.0559(13) Uani 1 1 d . . . . .
H18A H 0.4792 0.5613 0.6664 0.067 Uiso 1 1 calc R U . . .
H18B H 0.5514 0.6225 0.7036 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5364(5) 0.4766(4) 0.7197(2) 0.0879(19) Uani 1 1 d . . . . .
H19A H 0.5429 0.4141 0.7036 0.105 Uiso 1 1 calc R U . . .
H19B H 0.6014 0.4801 0.7422 0.105 Uiso 1 1 calc R U . . .
C20 C 0.4307(6) 0.4744(5) 0.7427(2) 0.110(2) Uani 1 1 d . . . . .
H20A H 0.4297 0.4157 0.7612 0.165 Uiso 1 1 calc R U . . .
H20B H 0.3652 0.4733 0.7209 0.165 Uiso 1 1 calc R U . . .
H20C H 0.4266 0.5328 0.7613 0.165 Uiso 1 1 calc R U . . .
C21 C 0.4933(3) 0.2308(3) 0.55627(12) 0.0345(9) Uani 1 1 d . . . . .
C22 C 0.5871(4) 0.2939(3) 0.56504(16) 0.0511(12) Uani 1 1 d . . . . .
H22 H 0.5749 0.3534 0.5802 0.061 Uiso 1 1 calc R U . . .
C23 C 0.6963(4) 0.2737(4) 0.55271(17) 0.0592(13) Uani 1 1 d . . . . .
H23 H 0.7561 0.3190 0.5596 0.071 Uiso 1 1 calc R U . . .
C24 C 0.7183(4) 0.1880(3) 0.53051(16) 0.0521(13) Uani 1 1 d . . . . .
H24 H 0.7927 0.1740 0.5219 0.063 Uiso 1 1 calc R U . . .
C25 C 0.6294(4) 0.1229(3) 0.52115(15) 0.0464(12) Uani 1 1 d . . . . .
H25 H 0.6427 0.0632 0.5063 0.056 Uiso 1 1 calc R U . . .
C26 C 0.5207(4) 0.1454(3) 0.53352(13) 0.0387(10) Uani 1 1 d . . . . .
H26 H 0.4612 0.1000 0.5261 0.046 Uiso 1 1 calc R U . . .
C27 C 0.2647(3) 0.2012(3) 0.54040(14) 0.0376(10) Uani 1 1 d . . . . .
C28 C 0.1908(4) 0.2506(3) 0.50978(14) 0.0491(12) Uani 1 1 d . . . . .
H28 H 0.1963 0.3198 0.5079 0.059 Uiso 1 1 calc R U . . .
C29 C 0.1093(4) 0.2024(4) 0.48184(17) 0.0617(14) Uani 1 1 d . . . . .
H29 H 0.0617 0.2393 0.4614 0.074 Uiso 1 1 calc R U . . .
C30 C 0.0971(4) 0.1022(4) 0.48356(18) 0.0639(15) Uani 1 1 d . . . . .
H30 H 0.0424 0.0697 0.4643 0.077 Uiso 1 1 calc R U . . .
C31 C 0.1665(4) 0.0500(4) 0.5141(2) 0.0651(15) Uani 1 1 d . . . . .
H31 H 0.1585 -0.0190 0.5163 0.078 Uiso 1 1 calc R U . . .
C32 C 0.2479(4) 0.0991(3) 0.54136(17) 0.0521(13) Uani 1 1 d . . . . .
H32 H 0.2947 0.0616 0.5618 0.062 Uiso 1 1 calc R U . . .
C33 C 0.3609(4) 0.2130(3) 0.62461(14) 0.0461(11) Uani 1 1 d . . . . .
C34 C 0.2610(5) 0.1754(4) 0.64118(18) 0.0789(17) Uani 1 1 d . . . . .
H34 H 0.1950 0.1691 0.6215 0.095 Uiso 1 1 calc R U . . .
C35 C 0.2540(7) 0.1472(5) 0.6849(2) 0.103(2) Uani 1 1 d . . . . .
H35 H 0.1841 0.1226 0.6943 0.124 Uiso 1 1 calc R U . . .
C36 C 0.3471(8) 0.1544(5) 0.7149(2) 0.097(2) Uani 1 1 d . . . . .
H36 H 0.3425 0.1342 0.7447 0.116 Uiso 1 1 calc R U . . .
C37 C 0.4471(6) 0.1917(4) 0.70074(18) 0.0710(17) Uani 1 1 d . . . . .
H37 H 0.5118 0.1988 0.7210 0.085 Uiso 1 1 calc R U . . .
C38 C 0.4539(4) 0.2194(3) 0.65603(14) 0.0556(13) Uani 1 1 d . . . . .
H38 H 0.5243 0.2434 0.6469 0.067 Uiso 1 1 calc R U . . .
C39 C 0.3422(3) 0.3747(3) 0.57321(14) 0.0390(11) Uani 1 1 d . . . . .
C40 C 0.2904(4) 0.4244(3) 0.60674(16) 0.0492(12) Uani 1 1 d . . . . .
H40 H 0.2736 0.3894 0.6326 0.059 Uiso 1 1 calc R U . . .
C41 C 0.2622(4) 0.5236(4) 0.6037(2) 0.0654(16) Uani 1 1 d . . . . .
H41 H 0.2274 0.5546 0.6274 0.078 Uiso 1 1 calc R U . . .
C42 C 0.2849(4) 0.5773(4) 0.5664(2) 0.0626(16) Uani 1 1 d . . . . .
H42 H 0.2639 0.6442 0.5641 0.075 Uiso 1 1 calc R U . . .
C43 C 0.3386(4) 0.5317(3) 0.53272(18) 0.0568(14) Uani 1 1 d . . . . .
H43 H 0.3556 0.5676 0.5072 0.068 Uiso 1 1 calc R U . . .
C44 C 0.3676(4) 0.4323(3) 0.53650(15) 0.0445(12) Uani 1 1 d . . . . .
H44 H 0.4059 0.4026 0.5134 0.053 Uiso 1 1 calc R U . . .
C45 C 0.2666(5) 0.7656(5) 0.6739(2) 0.0909(13) Uani 1 1 d . . . . .
H45A H 0.2858 0.8065 0.7004 0.109 Uiso 1 1 calc R U . . .
H45B H 0.2962 0.6987 0.6799 0.109 Uiso 1 1 calc R U . . .
C46 C 0.1409(5) 0.7625(6) 0.6644(2) 0.123(2) Uani 1 1 d . . . . .
H46A H 0.1156 0.6968 0.6541 0.148 Uiso 1 1 calc R U . . .
H46B H 0.1006 0.7803 0.6909 0.148 Uiso 1 1 calc R U . . .
C47 C 0.1215(6) 0.8347(6) 0.6297(3) 0.123(2) Uani 1 1 d . . . . .
H47A H 0.0847 0.8934 0.6415 0.148 Uiso 1 1 calc R U . . .
H47B H 0.0704 0.8075 0.6055 0.148 Uiso 1 1 calc R U . . .
C48 C 0.2324(5) 0.8617(5) 0.6128(2) 0.0909(13) Uani 1 1 d . . . . .
H48A H 0.2325 0.8470 0.5808 0.109 Uiso 1 1 calc R U . . .
H48B H 0.2474 0.9324 0.6172 0.109 Uiso 1 1 calc R U . . .
B1 B 0.3657(4) 0.2542(3) 0.57319(16) 0.0398(13) Uani 1 1 d . . . . .
N2 N 0.6529(3) 0.9275(2) 0.66259(11) 0.0415(9) Uani 1 1 d . . . . .
N3 N 0.5443(3) 0.7977(2) 0.60136(11) 0.0378(9) Uani 1 1 d D . . . .
N4 N 0.6701(3) 0.6307(2) 0.62888(11) 0.0359(8) Uani 1 1 d . . . . .
O3 O 0.3165(3) 0.8054(3) 0.63699(13) 0.0730(10) Uani 1 1 d . . . . .
Pd1 Pd 0.65961(3) 0.77493(2) 0.65379(2) 0.03515(11) Uani 1 1 d . . . . .
N1 N 0.7722(3) 0.7512(3) 0.70655(13) 0.0497(10) Uani 1 1 d . . . . .
O1 O 0.8748(3) 0.7605(3) 0.70288(12) 0.0934(14) Uani 1 1 d . . . . .
O2 O 0.7391(3) 0.7257(3) 0.74185(13) 0.1002(14) Uani 1 1 d . . . . .
H3 H 0.469(3) 0.789(4) 0.6137(18) 0.120 Uiso 1 1 d D 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
C1 C2 1.502(6) . ?
C1 N2 1.515(5) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.485(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.478(5) . ?
C3 C4 1.506(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.502(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.507(5) . ?
C5 C6 1.517(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.510(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.496(7) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N2 1.493(5) . ?
C9 C10 1.494(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.522(6) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.498(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.503(5) . ?
C13 C14 1.510(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.511(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.515(6) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 N4 1.489(5) . ?
C17 C18 1.495(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.499(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.452(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C26 1.390(5) . ?
C21 C22 1.397(5) . ?
C21 B1 1.634(6) . ?
C22 C23 1.376(6) . ?
C22 H22 0.9400 . ?
C23 C24 1.371(6) . ?
C23 H23 0.9400 . ?
C24 C25 1.373(6) . ?
C24 H24 0.9400 . ?
C25 C26 1.377(6) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.386(5) . ?
C27 C32 1.397(5) . ?
C27 B1 1.646(6) . ?
C28 C29 1.386(6) . ?
C28 H28 0.9400 . ?
C29 C30 1.364(6) . ?
C29 H29 0.9400 . ?
C30 C31 1.374(7) . ?
C30 H30 0.9400 . ?
C31 C32 1.380(6) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.389(6) . ?
C33 C34 1.393(7) . ?
C33 B1 1.646(6) . ?
C34 C35 1.374(7) . ?
C34 H34 0.9400 . ?
C35 C36 1.365(8) . ?
C35 H35 0.9400 . ?
C36 C37 1.364(8) . ?
C36 H36 0.9400 . ?
C37 C38 1.401(7) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C40 1.383(6) . ?
C39 C44 1.398(6) . ?
C39 B1 1.653(6) . ?
C40 C41 1.383(6) . ?
C40 H40 0.9400 . ?
C41 C42 1.375(7) . ?
C41 H41 0.9400 . ?
C42 C43 1.372(7) . ?
C42 H42 0.9400 . ?
C43 C44 1.389(6) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.395(6) . ?
C45 C46 1.473(8) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.433(9) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.466(8) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.403(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N2 Pd1 2.083(3) . ?
N3 Pd1 2.021(3) . ?
N3 H3 0.99(2) . ?
N4 Pd1 2.096(3) . ?
Pd1 N1 2.011(3) . ?
N1 O2 1.203(5) . ?
N1 O1 1.214(5) . ?

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
C2 C1 N2 110.2(3) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.5(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.6(3) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 111.3(3) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.9(4) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.4(4) . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 112.1(6) . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 115.5(4) . . ?
N2 C9 H9A 108.4 . . ?
C10 C9 H9A 108.4 . . ?
N2 C9 H9B 108.4 . . ?
C10 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 111.0(4) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 112.9(5) . . ?
C12 C11 H11A 109.0 . . ?
C10 C11 H11A 109.0 . . ?
C12 C11 H11B 109.0 . . ?
C10 C11 H11B 109.0 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.6(3) . . ?
N4 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
N4 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C13 C14 C15 111.9(4) . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14B 109.2 . . ?
C15 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 114.1(4) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.5(3) . . ?
N4 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
N4 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 112.5(4) . . ?
C17 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
C17 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C18 116.1(5) . . ?
C20 C19 H19A 108.3 . . ?
C18 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
C18 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.4(4) . . ?
C26 C21 B1 123.9(4) . . ?
C22 C21 B1 122.6(4) . . ?
C23 C22 C21 123.6(4) . . ?
C23 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.5(4) . . ?
C23 C24 H24 120.7 . . ?
C25 C24 H24 120.7 . . ?
C24 C25 C26 119.9(4) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C21 124.2(4) . . ?
C25 C26 H26 117.9 . . ?
C21 C26 H26 117.9 . . ?
C28 C27 C32 114.2(4) . . ?
C28 C27 B1 124.9(4) . . ?
C32 C27 B1 120.9(4) . . ?
C29 C28 C27 122.8(4) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 120.9(5) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 118.6(4) . . ?
C29 C30 H30 120.7 . . ?
C31 C30 H30 120.7 . . ?
C30 C31 C32 119.8(5) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C27 123.7(4) . . ?
C31 C32 H32 118.1 . . ?
C27 C32 H32 118.1 . . ?
C38 C33 C34 114.4(4) . . ?
C38 C33 B1 122.7(4) . . ?
C34 C33 B1 122.8(4) . . ?
C35 C34 C33 123.2(6) . . ?
C35 C34 H34 118.4 . . ?
C33 C34 H34 118.4 . . ?
C36 C35 C34 120.9(7) . . ?
C36 C35 H35 119.6 . . ?
C34 C35 H35 119.6 . . ?
C37 C36 C35 118.5(6) . . ?
C37 C36 H36 120.7 . . ?
C35 C36 H36 120.7 . . ?
C36 C37 C38 120.3(5) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 122.7(5) . . ?
C33 C38 H38 118.6 . . ?
C37 C38 H38 118.6 . . ?
C40 C39 C44 115.4(4) . . ?
C40 C39 B1 124.0(4) . . ?
C44 C39 B1 120.4(4) . . ?
C39 C40 C41 122.5(5) . . ?
C39 C40 H40 118.8 . . ?
C41 C40 H40 118.8 . . ?
C42 C41 C40 120.5(5) . . ?
C42 C41 H41 119.7 . . ?
C40 C41 H41 119.7 . . ?
C43 C42 C41 119.1(5) . . ?
C43 C42 H42 120.5 . . ?
C41 C42 H42 120.5 . . ?
C42 C43 C44 119.7(5) . . ?
C42 C43 H43 120.2 . . ?
C44 C43 H43 120.2 . . ?
C43 C44 C39 122.7(5) . . ?
C43 C44 H44 118.6 . . ?
C39 C44 H44 118.6 . . ?
O3 C45 C46 108.6(5) . . ?
O3 C45 H45A 110.0 . . ?
C46 C45 H45A 110.0 . . ?
O3 C45 H45B 110.0 . . ?
C46 C45 H45B 110.0 . . ?
H45A C45 H45B 108.4 . . ?
C47 C46 C45 103.1(6) . . ?
C47 C46 H46A 111.1 . . ?
C45 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
C45 C46 H46B 111.1 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 108.8(5) . . ?
C46 C47 H47A 109.9 . . ?
C48 C47 H47A 109.9 . . ?
C46 C47 H47B 109.9 . . ?
C48 C47 H47B 109.9 . . ?
H47A C47 H47B 108.3 . . ?
O3 C48 C47 106.5(5) . . ?
O3 C48 H48A 110.4 . . ?
C47 C48 H48A 110.4 . . ?
O3 C48 H48B 110.4 . . ?
C47 C48 H48B 110.4 . . ?
H48A C48 H48B 108.6 . . ?
C21 B1 C27 111.0(3) . . ?
C21 B1 C33 108.4(3) . . ?
C27 B1 C33 110.1(3) . . ?
C21 B1 C39 110.2(3) . . ?
C27 B1 C39 108.6(3) . . ?
C33 B1 C39 108.5(4) . . ?
C9 N2 C5 110.0(3) . . ?
C9 N2 C1 110.4(3) . . ?
C5 N2 C1 110.4(3) . . ?
C9 N2 Pd1 115.1(3) . . ?
C5 N2 Pd1 105.5(2) . . ?
C1 N2 Pd1 105.3(2) . . ?
C3 N3 C2 116.5(3) . . ?
C3 N3 Pd1 107.8(2) . . ?
C2 N3 Pd1 107.5(2) . . ?
C3 N3 H3 112(3) . . ?
C2 N3 H3 108(3) . . ?
Pd1 N3 H3 105(3) . . ?
C17 N4 C4 109.7(3) . . ?
C17 N4 C13 110.2(3) . . ?
C4 N4 C13 111.2(3) . . ?
C17 N4 Pd1 115.8(3) . . ?
C4 N4 Pd1 105.1(2) . . ?
C13 N4 Pd1 104.8(2) . . ?
C45 O3 C48 107.9(4) . . ?
N1 Pd1 N3 179.00(17) . . ?
N1 Pd1 N2 94.97(13) . . ?
N3 Pd1 N2 85.35(13) . . ?
N1 Pd1 N4 94.67(13) . . ?
N3 Pd1 N4 85.18(12) . . ?
N2 Pd1 N4 166.23(13) . . ?
O2 N1 O1 119.1(4) . . ?
O2 N1 Pd1 120.5(3) . . ?
O1 N1 Pd1 120.3(3) . . ?

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
N2 C1 C2 N3 55.4(5) . . . . ?
N3 C3 C4 N4 -54.2(4) . . . . ?
N2 C5 C6 C7 -178.5(4) . . . . ?
C5 C6 C7 C8 -172.5(5) . . . . ?
N2 C9 C10 C11 172.1(4) . . . . ?
C9 C10 C11 C12 171.0(4) . . . . ?
N4 C13 C14 C15 -179.5(4) . . . . ?
C13 C14 C15 C16 178.9(4) . . . . ?
N4 C17 C18 C19 -179.3(4) . . . . ?
C17 C18 C19 C20 -173.5(5) . . . . ?
C26 C21 C22 C23 -0.4(6) . . . . ?
B1 C21 C22 C23 177.3(4) . . . . ?
C21 C22 C23 C24 0.1(8) . . . . ?
C22 C23 C24 C25 -0.3(7) . . . . ?
C23 C24 C25 C26 0.9(7) . . . . ?
C24 C25 C26 C21 -1.3(7) . . . . ?
C22 C21 C26 C25 1.0(6) . . . . ?
B1 C21 C26 C25 -176.6(4) . . . . ?
C32 C27 C28 C29 -1.4(7) . . . . ?
B1 C27 C28 C29 177.9(4) . . . . ?
C27 C28 C29 C30 0.6(8) . . . . ?
C28 C29 C30 C31 0.8(8) . . . . ?
C29 C30 C31 C32 -1.4(8) . . . . ?
C30 C31 C32 C27 0.5(8) . . . . ?
C28 C27 C32 C31 0.9(7) . . . . ?
B1 C27 C32 C31 -178.5(5) . . . . ?
C38 C33 C34 C35 0.1(8) . . . . ?
B1 C33 C34 C35 -175.3(6) . . . . ?
C33 C34 C35 C36 -0.2(11) . . . . ?
C34 C35 C36 C37 0.9(10) . . . . ?
C35 C36 C37 C38 -1.5(9) . . . . ?
C34 C33 C38 C37 -0.8(7) . . . . ?
B1 C33 C38 C37 174.7(4) . . . . ?
C36 C37 C38 C33 1.5(8) . . . . ?
C44 C39 C40 C41 1.9(6) . . . . ?
B1 C39 C40 C41 -173.8(4) . . . . ?
C39 C40 C41 C42 0.3(7) . . . . ?
C40 C41 C42 C43 -1.7(7) . . . . ?
C41 C42 C43 C44 0.9(7) . . . . ?
C42 C43 C44 C39 1.4(6) . . . . ?
C40 C39 C44 C43 -2.7(6) . . . . ?
B1 C39 C44 C43 173.1(4) . . . . ?
O3 C45 C46 C47 -21.5(8) . . . . ?
C45 C46 C47 C48 12.4(9) . . . . ?
C46 C47 C48 O3 0.5(8) . . . . ?
C26 C21 B1 C27 -29.2(5) . . . . ?
C22 C21 B1 C27 153.5(4) . . . . ?
C26 C21 B1 C33 91.9(4) . . . . ?
C22 C21 B1 C33 -85.5(5) . . . . ?
C26 C21 B1 C39 -149.4(4) . . . . ?
C22 C21 B1 C39 33.2(5) . . . . ?
C28 C27 B1 C21 -106.6(5) . . . . ?
C32 C27 B1 C21 72.7(5) . . . . ?
C28 C27 B1 C33 133.4(4) . . . . ?
C32 C27 B1 C33 -47.4(5) . . . . ?
C28 C27 B1 C39 14.7(6) . . . . ?
C32 C27 B1 C39 -166.0(4) . . . . ?
C38 C33 B1 C21 37.8(5) . . . . ?
C34 C33 B1 C21 -147.0(5) . . . . ?
C38 C33 B1 C27 159.4(4) . . . . ?
C34 C33 B1 C27 -25.5(6) . . . . ?
C38 C33 B1 C39 -81.9(5) . . . . ?
C34 C33 B1 C39 93.2(5) . . . . ?
C40 C39 B1 C21 -138.1(4) . . . . ?
C44 C39 B1 C21 46.5(5) . . . . ?
C40 C39 B1 C27 100.1(4) . . . . ?
C44 C39 B1 C27 -75.3(5) . . . . ?
C40 C39 B1 C33 -19.5(5) . . . . ?
C44 C39 B1 C33 165.1(4) . . . . ?
C10 C9 N2 C5 -171.7(4) . . . . ?
C10 C9 N2 C1 66.3(5) . . . . ?
C10 C9 N2 Pd1 -52.7(4) . . . . ?
C6 C5 N2 C9 -56.0(5) . . . . ?
C6 C5 N2 C1 66.0(5) . . . . ?
C6 C5 N2 Pd1 179.2(3) . . . . ?
C2 C1 N2 C9 -160.5(4) . . . . ?
C2 C1 N2 C5 77.7(4) . . . . ?
C2 C1 N2 Pd1 -35.6(4) . . . . ?
C4 C3 N3 C2 166.7(3) . . . . ?
C4 C3 N3 Pd1 45.9(3) . . . . ?
C1 C2 N3 C3 -167.2(3) . . . . ?
C1 C2 N3 Pd1 -46.3(4) . . . . ?
C18 C17 N4 C4 -68.7(4) . . . . ?
C18 C17 N4 C13 168.6(4) . . . . ?
C18 C17 N4 Pd1 49.9(4) . . . . ?
C3 C4 N4 C17 159.0(3) . . . . ?
C3 C4 N4 C13 -78.9(4) . . . . ?
C3 C4 N4 Pd1 34.0(4) . . . . ?
C14 C13 N4 C17 56.8(5) . . . . ?
C14 C13 N4 C4 -65.0(4) . . . . ?
C14 C13 N4 Pd1 -178.1(3) . . . . ?
C46 C45 O3 C48 22.7(7) . . . . ?
C47 C48 O3 C45 -14.3(7) . . . . ?

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
C5 H5B O1 0.98 2.61 3.405(6) 138.6 .
C13 H13A O1 0.98 2.59 3.389(6) 138.4 .
N3 H3 O3 0.99(2) 1.96(2) 2.930(5) 166(5) .

_refine_diff_density_max         0.605
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.077

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-250K
_database_code_depnum_ccdc_archive 'CCDC 1441791'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-250K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         18 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6422(5)
_cell_length_b                   13.5412(6)
_cell_length_c                   30.0467(11)
_cell_angle_alpha                90
_cell_angle_beta                 93.985(4)
_cell_angle_gamma                90
_cell_volume                     4725.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    5167
_cell_measurement_theta_min      3.4830
_cell_measurement_theta_max      26.3800

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.435
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20071
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         3.161
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             9638
_reflns_number_gt                6377
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0410P)²+0.7086P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9638
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1029
_refine_ls_wR_factor_gt          0.0889
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.001
_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
C1 C 0.5567(3) 0.9632(2) 0.63027(11) 0.0506(9) Uani 1 1 d . . . . .
H1A H 0.5686 1.0329 0.6233 0.061 Uiso 1 1 calc R U . . .
H1B H 0.4830 0.9570 0.6439 0.061 Uiso 1 1 calc R U . . .
C2 C 0.5540(3) 0.9025(2) 0.58792(11) 0.0469(9) Uani 1 1 d . . . . .
H2A H 0.4879 0.9214 0.5677 0.056 Uiso 1 1 calc R U . . .
H2B H 0.6246 0.9129 0.5726 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5650(3) 0.7223(2) 0.56713(10) 0.0410(8) Uani 1 1 d . . . . .
H3A H 0.6348 0.7382 0.5521 0.049 Uiso 1 1 calc R U . . .
H3B H 0.4999 0.7197 0.5447 0.049 Uiso 1 1 calc R U . . .
C4 C 0.5788(3) 0.6249(2) 0.59102(10) 0.0403(8) Uani 1 1 d . . . . .
H4A H 0.5053 0.6060 0.6026 0.048 Uiso 1 1 calc R U . . .
H4B H 0.5998 0.5739 0.5699 0.048 Uiso 1 1 calc R U . . .
C5 C 0.7674(3) 0.9658(2) 0.64953(12) 0.0501(9) Uani 1 1 d . . . . .
H5A H 0.7779 0.9449 0.6189 0.060 Uiso 1 1 calc R U . . .
H5B H 0.8279 0.9339 0.6688 0.060 Uiso 1 1 calc R U . . .
C6 C 0.7857(4) 1.0765(3) 0.65228(14) 0.0688(12) Uani 1 1 d . . . . .
H6A H 0.7251 1.1099 0.6336 0.083 Uiso 1 1 calc R U . . .
H6B H 0.7801 1.0984 0.6831 0.083 Uiso 1 1 calc R U . . .
C7 C 0.9020(4) 1.1051(3) 0.63688(17) 0.0904(15) Uani 1 1 d . . . . .
H7A H 0.9617 1.0650 0.6528 0.108 Uiso 1 1 calc R U . . .
H7B H 0.9037 1.0907 0.6050 0.108 Uiso 1 1 calc R U . . .
C8 C 0.9284(5) 1.2119(4) 0.6447(2) 0.138(3) Uani 1 1 d . . . . .
H8A H 0.9501 1.2225 0.6761 0.208 Uiso 1 1 calc R U . . .
H8B H 0.8609 1.2511 0.6359 0.208 Uiso 1 1 calc R U . . .
H8C H 0.9915 1.2314 0.6271 0.208 Uiso 1 1 calc R U . . .
C9 C 0.6327(3) 0.9616(3) 0.70888(11) 0.0483(9) Uani 1 1 d . . . . .
H9A H 0.6231 1.0335 0.7085 0.058 Uiso 1 1 calc R U . . .
H9B H 0.7016 0.9465 0.7283 0.058 Uiso 1 1 calc R U . . .
C10 C 0.5295(3) 0.9157(3) 0.72868(11) 0.0552(10) Uani 1 1 d . . . . .
H10A H 0.5333 0.8436 0.7259 0.066 Uiso 1 1 calc R U . . .
H10B H 0.4588 0.9384 0.7122 0.066 Uiso 1 1 calc R U . . .
C11 C 0.5267(4) 0.9437(3) 0.77755(13) 0.0693(12) Uani 1 1 d . . . . .
H11A H 0.5912 0.9117 0.7946 0.083 Uiso 1 1 calc R U . . .
H11B H 0.5368 1.0153 0.7806 0.083 Uiso 1 1 calc R U . . .
C12 C 0.4162(4) 0.9143(4) 0.79685(15) 0.1006(17) Uani 1 1 d . . . . .
H12A H 0.4200 0.9306 0.8283 0.151 Uiso 1 1 calc R U . . .
H12B H 0.4046 0.8437 0.7931 0.151 Uiso 1 1 calc R U . . .
H12C H 0.3525 0.9494 0.7815 0.151 Uiso 1 1 calc R U . . .
C13 C 0.7885(3) 0.6239(2) 0.61178(11) 0.0419(8) Uani 1 1 d . . . . .
H13A H 0.8449 0.6369 0.6368 0.050 Uiso 1 1 calc R U . . .
H13B H 0.7961 0.6768 0.5900 0.050 Uiso 1 1 calc R U . . .
C14 C 0.8209(3) 0.5276(3) 0.59030(12) 0.0500(9) Uani 1 1 d . . . . .
H14A H 0.8144 0.4735 0.6117 0.060 Uiso 1 1 calc R U . . .
H14B H 0.7672 0.5144 0.5644 0.060 Uiso 1 1 calc R U . . .
C15 C 0.9417(3) 0.5310(3) 0.57563(13) 0.0588(10) Uani 1 1 d . . . . .
H15A H 0.9945 0.5458 0.6016 0.071 Uiso 1 1 calc R U . . .
H15B H 0.9472 0.5852 0.5543 0.071 Uiso 1 1 calc R U . . .
C16 C 0.9804(3) 0.4367(3) 0.55435(14) 0.0683(12) Uani 1 1 d . . . . .
H16A H 1.0581 0.4450 0.5452 0.102 Uiso 1 1 calc R U . . .
H16B H 0.9290 0.4214 0.5285 0.102 Uiso 1 1 calc R U . . .
H16C H 0.9791 0.3831 0.5757 0.102 Uiso 1 1 calc R U . . .
C17 C 0.6531(3) 0.5499(2) 0.66143(11) 0.0459(9) Uani 1 1 d . . . . .
H17A H 0.7208 0.5471 0.6827 0.055 Uiso 1 1 calc R U . . .
H17B H 0.6485 0.4870 0.6453 0.055 Uiso 1 1 calc R U . . .
C18 C 0.5474(3) 0.5605(3) 0.68714(12) 0.0558(10) Uani 1 1 d . . . . .
H18A H 0.5513 0.6229 0.7037 0.067 Uiso 1 1 calc R U . . .
H18B H 0.4789 0.5623 0.6663 0.067 Uiso 1 1 calc R U . . .
C19 C 0.5371(4) 0.4763(4) 0.71926(16) 0.0889(15) Uani 1 1 d . . . . .
H19A H 0.5418 0.4142 0.7028 0.107 Uiso 1 1 calc R U . . .
H19B H 0.6032 0.4785 0.7413 0.107 Uiso 1 1 calc R U . . .
C20 C 0.4316(5) 0.4753(4) 0.74302(18) 0.113(2) Uani 1 1 d . . . . .
H20A H 0.4334 0.4197 0.7634 0.170 Uiso 1 1 calc R U . . .
H20B H 0.3655 0.4692 0.7217 0.170 Uiso 1 1 calc R U . . .
H20C H 0.4259 0.5362 0.7597 0.170 Uiso 1 1 calc R U . . .
C21 C 0.4943(3) 0.2308(2) 0.55611(10) 0.0368(7) Uani 1 1 d . . . . .
C22 C 0.5871(3) 0.2938(2) 0.56502(12) 0.0520(9) Uani 1 1 d . . . . .
H22 H 0.5747 0.3532 0.5802 0.062 Uiso 1 1 calc R U . . .
C23 C 0.6963(3) 0.2735(3) 0.55270(14) 0.0606(10) Uani 1 1 d . . . . .
H23 H 0.7562 0.3187 0.5597 0.073 Uiso 1 1 calc R U . . .
C24 C 0.7186(3) 0.1885(3) 0.53041(13) 0.0543(9) Uani 1 1 d . . . . .
H24 H 0.7929 0.1747 0.5218 0.065 Uiso 1 1 calc R U . . .
C25 C 0.6297(3) 0.1236(3) 0.52096(11) 0.0474(9) Uani 1 1 d . . . . .
H25 H 0.6431 0.0644 0.5059 0.057 Uiso 1 1 calc R U . . .
C26 C 0.5205(3) 0.1449(2) 0.53353(10) 0.0397(8) Uani 1 1 d . . . . .
H26 H 0.4612 0.0993 0.5265 0.048 Uiso 1 1 calc R U . . .
C27 C 0.2652(3) 0.2017(2) 0.54074(10) 0.0384(8) Uani 1 1 d . . . . .
C28 C 0.1909(3) 0.2513(3) 0.50990(11) 0.0481(9) Uani 1 1 d . . . . .
H28 H 0.1967 0.3204 0.5079 0.058 Uiso 1 1 calc R U . . .
C29 C 0.1089(3) 0.2032(3) 0.48218(13) 0.0633(11) Uani 1 1 d . . . . .
H29 H 0.0612 0.2398 0.4618 0.076 Uiso 1 1 calc R U . . .
C30 C 0.0967(3) 0.1029(3) 0.48414(14) 0.0668(11) Uani 1 1 d . . . . .
H30 H 0.0412 0.0703 0.4653 0.080 Uiso 1 1 calc R U . . .
C31 C 0.1664(3) 0.0511(3) 0.51387(16) 0.0645(11) Uani 1 1 d . . . . .
H31 H 0.1592 -0.0179 0.5155 0.077 Uiso 1 1 calc R U . . .
C32 C 0.2476(3) 0.0992(3) 0.54160(13) 0.0536(9) Uani 1 1 d . . . . .
H32 H 0.2935 0.0614 0.5621 0.064 Uiso 1 1 calc R U . . .
C33 C 0.3617(3) 0.2131(2) 0.62502(11) 0.0456(8) Uani 1 1 d . . . . .
C34 C 0.2623(4) 0.1761(4) 0.64116(14) 0.0831(14) Uani 1 1 d . . . . .
H34 H 0.1965 0.1702 0.6214 0.100 Uiso 1 1 calc R U . . .
C35 C 0.2546(6) 0.1470(4) 0.68523(17) 0.1087(19) Uani 1 1 d . . . . .
H35 H 0.1849 0.1221 0.6946 0.130 Uiso 1 1 calc R U . . .
C36 C 0.3481(6) 0.1548(4) 0.71459(16) 0.0955(17) Uani 1 1 d . . . . .
H36 H 0.3436 0.1349 0.7444 0.115 Uiso 1 1 calc R U . . .
C37 C 0.4486(5) 0.1915(3) 0.70078(14) 0.0782(14) Uani 1 1 d . . . . .
H37 H 0.5134 0.1980 0.7210 0.094 Uiso 1 1 calc R U . . .
C38 C 0.4541(4) 0.2197(3) 0.65590(11) 0.0590(10) Uani 1 1 d . . . . .
H38 H 0.5241 0.2441 0.6466 0.071 Uiso 1 1 calc R U . . .
C39 C 0.3432(3) 0.3745(2) 0.57298(10) 0.0399(8) Uani 1 1 d . . . . .
C40 C 0.2910(3) 0.4242(3) 0.60664(12) 0.0508(9) Uani 1 1 d . . . . .
H40 H 0.2744 0.3893 0.6325 0.061 Uiso 1 1 calc R U . . .
C41 C 0.2626(3) 0.5233(3) 0.60345(15) 0.0643(11) Uani 1 1 d . . . . .
H41 H 0.2276 0.5542 0.6271 0.077 Uiso 1 1 calc R U . . .
C42 C 0.2845(3) 0.5769(3) 0.56657(17) 0.0645(12) Uani 1 1 d . . . . .
H42 H 0.2629 0.6437 0.5642 0.077 Uiso 1 1 calc R U . . .
C43 C 0.3387(3) 0.5314(3) 0.53294(14) 0.0563(10) Uani 1 1 d . . . . .
H43 H 0.3563 0.5674 0.5075 0.068 Uiso 1 1 calc R U . . .
C44 C 0.3673(3) 0.4323(2) 0.53660(11) 0.0466(9) Uani 1 1 d . . . . .
H44 H 0.4048 0.4027 0.5133 0.056 Uiso 1 1 calc R U . . .
C45 C 0.2671(4) 0.7663(4) 0.67412(17) 0.0955(11) Uani 1 1 d . . . . .
H45A H 0.2858 0.8081 0.7003 0.115 Uiso 1 1 calc R U . . .
H45B H 0.2968 0.6997 0.6806 0.115 Uiso 1 1 calc R U . . .
C46 C 0.1411(5) 0.7630(5) 0.6640(2) 0.1212(15) Uani 1 1 d . . . . .
H46A H 0.1163 0.6979 0.6528 0.145 Uiso 1 1 calc R U . . .
H46B H 0.0999 0.7789 0.6904 0.145 Uiso 1 1 calc R U . . .
C47 C 0.1227(4) 0.8372(5) 0.6302(2) 0.1212(15) Uani 1 1 d . . . . .
H47A H 0.0898 0.8966 0.6430 0.145 Uiso 1 1 calc R U . . .
H47B H 0.0687 0.8129 0.6062 0.145 Uiso 1 1 calc R U . . .
C48 C 0.2317(4) 0.8604(4) 0.61275(17) 0.0955(11) Uani 1 1 d . . . . .
H48A H 0.2297 0.8438 0.5810 0.115 Uiso 1 1 calc R U . . .
H48B H 0.2478 0.9312 0.6161 0.115 Uiso 1 1 calc R U . . .
B1 B 0.3653(3) 0.2549(3) 0.57336(12) 0.0383(9) Uani 1 1 d . . . . .
N2 N 0.6524(2) 0.92759(19) 0.66232(8) 0.0414(7) Uani 1 1 d . . . . .
N3 N 0.5444(2) 0.79790(19) 0.60145(8) 0.0362(6) Uani 1 1 d D . . . .
N4 N 0.6698(2) 0.63086(18) 0.62884(8) 0.0364(6) Uani 1 1 d . . . . .
O3 O 0.3173(2) 0.8054(2) 0.63661(10) 0.0748(8) Uani 1 1 d . . . . .
Pd1 Pd 0.65958(2) 0.77488(2) 0.65377(2) 0.03485(9) Uani 1 1 d . . . . .
N1 N 0.7725(3) 0.7507(2) 0.70648(10) 0.0488(7) Uani 1 1 d . . . . .
O1 O 0.8746(3) 0.7599(3) 0.70278(10) 0.0982(11) Uani 1 1 d . . . . .
O2 O 0.7392(3) 0.7249(3) 0.74174(10) 0.1033(12) Uani 1 1 d . . . . .
H3 H 0.469(2) 0.787(3) 0.6128(15) 0.124 Uiso 1 1 d D 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
C1 N2 1.501(4) . ?
C1 C2 1.513(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 N3 1.480(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C3 N3 1.484(4) . ?
C3 C4 1.505(4) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C4 N4 1.501(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 N2 1.510(4) . ?
C5 C6 1.516(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C6 C7 1.512(5) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.494(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 H8C 0.9700 . ?
C9 N2 1.505(4) . ?
C9 C10 1.511(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C10 C11 1.519(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C11 C12 1.502(5) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 H12C 0.9700 . ?
C13 N4 1.510(4) . ?
C13 C14 1.514(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C14 C15 1.503(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C15 C16 1.511(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 H16C 0.9700 . ?
C17 N4 1.492(4) . ?
C17 C18 1.504(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C18 C19 1.504(5) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C19 C20 1.463(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C20 H20C 0.9700 . ?
C21 C22 1.388(4) . ?
C21 C26 1.390(4) . ?
C21 B1 1.655(5) . ?
C22 C23 1.377(5) . ?
C22 H22 0.9400 . ?
C23 C24 1.366(5) . ?
C23 H23 0.9400 . ?
C24 C25 1.372(5) . ?
C24 H24 0.9400 . ?
C25 C26 1.381(4) . ?
C25 H25 0.9400 . ?
C26 H26 0.9400 . ?
C27 C28 1.396(5) . ?
C27 C32 1.403(4) . ?
C27 B1 1.637(5) . ?
C28 C29 1.385(5) . ?
C28 H28 0.9400 . ?
C29 C30 1.367(5) . ?
C29 H29 0.9400 . ?
C30 C31 1.359(6) . ?
C30 H30 0.9400 . ?
C31 C32 1.379(5) . ?
C31 H31 0.9400 . ?
C32 H32 0.9400 . ?
C33 C38 1.374(5) . ?
C33 C34 1.379(5) . ?
C33 B1 1.655(5) . ?
C34 C35 1.391(6) . ?
C34 H34 0.9400 . ?
C35 C36 1.357(7) . ?
C35 H35 0.9400 . ?
C36 C37 1.362(7) . ?
C36 H36 0.9400 . ?
C37 C38 1.407(5) . ?
C37 H37 0.9400 . ?
C38 H38 0.9400 . ?
C39 C44 1.389(4) . ?
C39 C40 1.389(4) . ?
C39 B1 1.640(5) . ?
C40 C41 1.384(5) . ?
C40 H40 0.9400 . ?
C41 C42 1.363(6) . ?
C41 H41 0.9400 . ?
C42 C43 1.374(5) . ?
C42 H42 0.9400 . ?
C43 C44 1.386(5) . ?
C43 H43 0.9400 . ?
C44 H44 0.9400 . ?
C45 O3 1.408(5) . ?
C45 C46 1.478(7) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C46 C47 1.434(7) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C47 C48 1.441(6) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C48 O3 1.402(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
N2 Pd1 2.086(3) . ?
N3 Pd1 2.019(2) . ?
N3 H3 0.972(19) . ?
N4 Pd1 2.095(2) . ?
Pd1 N1 2.014(3) . ?
N1 O2 1.205(4) . ?
N1 O1 1.208(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 C1 C2 109.7(3) . . ?
N2 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N2 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N3 C2 C1 106.6(3) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 106.8(2) . . ?
N3 C3 H3A 110.4 . . ?
C4 C3 H3A 110.4 . . ?
N3 C3 H3B 110.4 . . ?
C4 C3 H3B 110.4 . . ?
H3A C3 H3B 108.6 . . ?
N4 C4 C3 111.1(2) . . ?
N4 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N4 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C5 C6 116.7(3) . . ?
N2 C5 H5A 108.1 . . ?
C6 C5 H5A 108.1 . . ?
N2 C5 H5B 108.1 . . ?
C6 C5 H5B 108.1 . . ?
H5A C5 H5B 107.3 . . ?
C7 C6 C5 111.2(3) . . ?
C7 C6 H6A 109.4 . . ?
C5 C6 H6A 109.4 . . ?
C7 C6 H6B 109.4 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 112.2(5) . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 114.6(3) . . ?
N2 C9 H9A 108.6 . . ?
C10 C9 H9A 108.6 . . ?
N2 C9 H9B 108.6 . . ?
C10 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 C11 110.4(3) . . ?
C9 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
C9 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
C12 C11 C10 112.5(4) . . ?
C12 C11 H11A 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.4(3) . . ?
N4 C13 H13A 108.0 . . ?
C14 C13 H13A 108.0 . . ?
N4 C13 H13B 108.0 . . ?
C14 C13 H13B 108.0 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.4(3) . . ?
C15 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C14 C15 C16 114.2(3) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 114.6(3) . . ?
N4 C17 H17A 108.6 . . ?
C18 C17 H17A 108.6 . . ?
N4 C17 H17B 108.6 . . ?
C18 C17 H17B 108.6 . . ?
H17A C17 H17B 107.6 . . ?
C19 C18 C17 111.2(3) . . ?
C19 C18 H18A 109.4 . . ?
C17 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
C17 C18 H18B 109.4 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 115.3(4) . . ?
C20 C19 H19A 108.5 . . ?
C18 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 C26 114.5(3) . . ?
C22 C21 B1 122.0(3) . . ?
C26 C21 B1 123.5(3) . . ?
C23 C22 C21 123.1(3) . . ?
C23 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
C24 C23 C22 120.7(3) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 118.4(3) . . ?
C23 C24 H24 120.8 . . ?
C25 C24 H24 120.8 . . ?
C24 C25 C26 120.3(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C21 123.0(3) . . ?
C25 C26 H26 118.5 . . ?
C21 C26 H26 118.5 . . ?
C28 C27 C32 113.9(3) . . ?
C28 C27 B1 124.6(3) . . ?
C32 C27 B1 121.5(3) . . ?
C29 C28 C27 122.8(3) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 120.7(4) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C31 C30 C29 118.8(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.6 . . ?
C30 C31 C32 120.4(4) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 123.4(4) . . ?
C31 C32 H32 118.3 . . ?
C27 C32 H32 118.3 . . ?
C38 C33 C34 115.0(3) . . ?
C38 C33 B1 122.8(3) . . ?
C34 C33 B1 122.1(3) . . ?
C33 C34 C35 123.3(5) . . ?
C33 C34 H34 118.3 . . ?
C35 C34 H34 118.3 . . ?
C36 C35 C34 119.6(5) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C35 C36 C37 119.9(4) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C36 C37 C38 119.2(5) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C33 C38 C37 122.9(4) . . ?
C33 C38 H38 118.5 . . ?
C37 C38 H38 118.5 . . ?
C44 C39 C40 115.0(3) . . ?
C44 C39 B1 121.4(3) . . ?
C40 C39 B1 123.4(3) . . ?
C41 C40 C39 122.3(4) . . ?
C41 C40 H40 118.9 . . ?
C39 C40 H40 118.9 . . ?
C42 C41 C40 121.0(4) . . ?
C42 C41 H41 119.5 . . ?
C40 C41 H41 119.5 . . ?
C41 C42 C43 118.7(4) . . ?
C41 C42 H42 120.6 . . ?
C43 C42 H42 120.6 . . ?
C42 C43 C44 119.8(4) . . ?
C42 C43 H43 120.1 . . ?
C44 C43 H43 120.1 . . ?
C43 C44 C39 123.2(3) . . ?
C43 C44 H44 118.4 . . ?
C39 C44 H44 118.4 . . ?
O3 C45 C46 108.0(4) . . ?
O3 C45 H45A 110.1 . . ?
C46 C45 H45A 110.1 . . ?
O3 C45 H45B 110.1 . . ?
C46 C45 H45B 110.1 . . ?
H45A C45 H45B 108.4 . . ?
C47 C46 C45 102.8(5) . . ?
C47 C46 H46A 111.2 . . ?
C45 C46 H46A 111.2 . . ?
C47 C46 H46B 111.2 . . ?
C45 C46 H46B 111.2 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 108.6(5) . . ?
C46 C47 H47A 110.0 . . ?
C48 C47 H47A 110.0 . . ?
C46 C47 H47B 110.0 . . ?
C48 C47 H47B 110.0 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 108.1(4) . . ?
O3 C48 H48A 110.1 . . ?
C47 C48 H48A 110.1 . . ?
O3 C48 H48B 110.1 . . ?
C47 C48 H48B 110.1 . . ?
H48A C48 H48B 108.4 . . ?
C27 B1 C39 109.0(3) . . ?
C27 B1 C21 110.5(3) . . ?
C39 B1 C21 109.8(3) . . ?
C27 B1 C33 110.3(3) . . ?
C39 B1 C33 109.2(3) . . ?
C21 B1 C33 108.0(3) . . ?
C1 N2 C9 110.1(2) . . ?
C1 N2 C5 111.0(3) . . ?
C9 N2 C5 109.1(3) . . ?
C1 N2 Pd1 105.86(19) . . ?
C9 N2 Pd1 115.3(2) . . ?
C5 N2 Pd1 105.35(19) . . ?
C2 N3 C3 116.7(2) . . ?
C2 N3 Pd1 107.62(19) . . ?
C3 N3 Pd1 107.68(18) . . ?
C2 N3 H3 110(3) . . ?
C3 N3 H3 109(3) . . ?
Pd1 N3 H3 105(3) . . ?
C17 N4 C4 109.9(2) . . ?
C17 N4 C13 110.0(2) . . ?
C4 N4 C13 110.7(2) . . ?
C17 N4 Pd1 115.86(19) . . ?
C4 N4 Pd1 105.40(17) . . ?
C13 N4 Pd1 104.83(18) . . ?
C48 O3 C45 106.8(3) . . ?
N1 Pd1 N3 179.05(12) . . ?
N1 Pd1 N2 95.39(11) . . ?
N3 Pd1 N2 84.99(10) . . ?
N1 Pd1 N4 94.55(10) . . ?
N3 Pd1 N4 85.21(10) . . ?
N2 Pd1 N4 166.00(9) . . ?
O2 N1 O1 119.3(3) . . ?
O2 N1 Pd1 120.4(3) . . ?
O1 N1 Pd1 120.2(3) . . ?

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
N2 C1 C2 N3 55.4(3) . . . . ?
N3 C3 C4 N4 -53.8(3) . . . . ?
N2 C5 C6 C7 -177.7(3) . . . . ?
C5 C6 C7 C8 -172.7(4) . . . . ?
N2 C9 C10 C11 172.3(3) . . . . ?
C9 C10 C11 C12 170.5(4) . . . . ?
N4 C13 C14 C15 -179.1(3) . . . . ?
C13 C14 C15 C16 179.3(3) . . . . ?
N4 C17 C18 C19 -179.8(3) . . . . ?
C17 C18 C19 C20 -174.8(4) . . . . ?
C26 C21 C22 C23 -0.1(5) . . . . ?
B1 C21 C22 C23 177.2(3) . . . . ?
C21 C22 C23 C24 0.3(6) . . . . ?
C22 C23 C24 C25 -0.5(6) . . . . ?
C23 C24 C25 C26 0.5(5) . . . . ?
C24 C25 C26 C21 -0.3(5) . . . . ?
C22 C21 C26 C25 0.1(5) . . . . ?
B1 C21 C26 C25 -177.1(3) . . . . ?
C32 C27 C28 C29 -1.2(5) . . . . ?
B1 C27 C28 C29 178.5(3) . . . . ?
C27 C28 C29 C30 0.4(6) . . . . ?
C28 C29 C30 C31 0.1(6) . . . . ?
C29 C30 C31 C32 0.2(6) . . . . ?
C30 C31 C32 C27 -1.1(6) . . . . ?
C28 C27 C32 C31 1.5(5) . . . . ?
B1 C27 C32 C31 -178.2(3) . . . . ?
C38 C33 C34 C35 -0.1(7) . . . . ?
B1 C33 C34 C35 -175.3(4) . . . . ?
C33 C34 C35 C36 0.1(8) . . . . ?
C34 C35 C36 C37 0.4(8) . . . . ?
C35 C36 C37 C38 -0.8(7) . . . . ?
C34 C33 C38 C37 -0.4(5) . . . . ?
B1 C33 C38 C37 174.8(3) . . . . ?
C36 C37 C38 C33 0.9(6) . . . . ?
C44 C39 C40 C41 1.6(5) . . . . ?
B1 C39 C40 C41 -173.2(3) . . . . ?
C39 C40 C41 C42 0.3(6) . . . . ?
C40 C41 C42 C43 -1.9(6) . . . . ?
C41 C42 C43 C44 1.5(5) . . . . ?
C42 C43 C44 C39 0.5(5) . . . . ?
C40 C39 C44 C43 -2.0(5) . . . . ?
B1 C39 C44 C43 173.0(3) . . . . ?
O3 C45 C46 C47 -23.9(7) . . . . ?
C45 C46 C47 C48 15.9(7) . . . . ?
C46 C47 C48 O3 -2.8(7) . . . . ?
C28 C27 B1 C39 13.9(4) . . . . ?
C32 C27 B1 C39 -166.5(3) . . . . ?
C28 C27 B1 C21 -106.8(3) . . . . ?
C32 C27 B1 C21 72.9(4) . . . . ?
C28 C27 B1 C33 133.8(3) . . . . ?
C32 C27 B1 C33 -46.5(4) . . . . ?
C44 C39 B1 C27 -74.3(4) . . . . ?
C40 C39 B1 C27 100.3(3) . . . . ?
C44 C39 B1 C21 46.8(4) . . . . ?
C40 C39 B1 C21 -138.6(3) . . . . ?
C44 C39 B1 C33 165.1(3) . . . . ?
C40 C39 B1 C33 -20.4(4) . . . . ?
C22 C21 B1 C27 153.8(3) . . . . ?
C26 C21 B1 C27 -29.2(4) . . . . ?
C22 C21 B1 C39 33.6(4) . . . . ?
C26 C21 B1 C39 -149.4(3) . . . . ?
C22 C21 B1 C33 -85.4(4) . . . . ?
C26 C21 B1 C33 91.6(3) . . . . ?
C38 C33 B1 C27 159.1(3) . . . . ?
C34 C33 B1 C27 -26.1(5) . . . . ?
C38 C33 B1 C39 -81.1(4) . . . . ?
C34 C33 B1 C39 93.7(4) . . . . ?
C38 C33 B1 C21 38.2(4) . . . . ?
C34 C33 B1 C21 -147.0(4) . . . . ?
C2 C1 N2 C9 -161.0(3) . . . . ?
C2 C1 N2 C5 78.1(3) . . . . ?
C2 C1 N2 Pd1 -35.8(3) . . . . ?
C10 C9 N2 C1 67.0(4) . . . . ?
C10 C9 N2 C5 -171.0(3) . . . . ?
C10 C9 N2 Pd1 -52.7(3) . . . . ?
C6 C5 N2 C1 65.3(4) . . . . ?
C6 C5 N2 C9 -56.2(4) . . . . ?
C6 C5 N2 Pd1 179.5(3) . . . . ?
C1 C2 N3 C3 -167.4(3) . . . . ?
C1 C2 N3 Pd1 -46.2(3) . . . . ?
C4 C3 N3 C2 166.7(3) . . . . ?
C4 C3 N3 Pd1 45.6(3) . . . . ?
C18 C17 N4 C4 -69.0(3) . . . . ?
C18 C17 N4 C13 168.9(3) . . . . ?
C18 C17 N4 Pd1 50.3(3) . . . . ?
C3 C4 N4 C17 159.2(3) . . . . ?
C3 C4 N4 C13 -79.1(3) . . . . ?
C3 C4 N4 Pd1 33.8(3) . . . . ?
C14 C13 N4 C17 56.4(4) . . . . ?
C14 C13 N4 C4 -65.2(4) . . . . ?
C14 C13 N4 Pd1 -178.4(2) . . . . ?
C47 C48 O3 C45 -12.6(6) . . . . ?
C46 C45 O3 C48 23.0(6) . . . . ?

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
C5 H5B O1 0.98 2.61 3.408(5) 138.6 .
C13 H13A O1 0.98 2.59 3.390(5) 138.5 .
N3 H3 O3 0.972(19) 1.97(2) 2.916(4) 163(4) .

_refine_diff_density_max         0.578
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.062

_shelxl_version_number           2014-1

####################################################################### 
# 
# 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_SS-260K
_database_code_depnum_ccdc_archive 'CCDC 1441792'
_audit_update_record             
;
2015-12-10 deposited with the CCDC.
2016-02-11 downloaded from the CCDC.
;

_audit_creation_date             2015-10-30
_audit_creation_method           SHELXL-2014

# start Validation Reply Form
_vrf_PLAT910_SS-260K             
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ...         15 Report
RESPONSE: A large unit cell and weakly diffracting crystals are a likely 
cause of this problem.  Despite efforts, larger crystals could be obtained.
Crystals have also been subject to UV irradiation, leading to even weaker 
diffraction.
;
# end Validation Reply Form

_chemical_name_systematic        
"Nitro-(N,N,N',N'-tetrabutyldiethylenetriamine)palladium(II)tetraphenylborate, tetrahydrofuran solvate"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C20 H45 N4 O2 Pd, C24 H20 B, C4 H8 O
;
_chemical_formula_sum            'C48 H73 B N4 O3 Pd'
_chemical_formula_weight         871.31

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'
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                   11.6538(6)
_cell_length_b                   13.5552(7)
_cell_length_c                   30.0383(16)
_cell_angle_alpha                90
_cell_angle_beta                 93.725(5)
_cell_angle_gamma                90
_cell_volume                     4735.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    260(2)
_cell_measurement_reflns_used    3033
_cell_measurement_theta_min      3.5600
_cell_measurement_theta_max      23.3110

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_F_000             1856
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.434
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.86609
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Rigaku-Oxford Diffraction,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      260(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3795
_diffrn_reflns_number            20892
_diffrn_reflns_av_unetI/netI     0.1318
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.006
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9671
_reflns_number_gt                5082
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_molecular_graphics    
;
ORTEP-3 (Farrugia, 2012)
MERCURY (MCarae 2008)
;

_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)+(0.0346P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9671
_refine_ls_number_parameters     509
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_gt           0.0601
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_restrained_S_all      0.983
_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
C1 C 0.5575(4) 0.9624(3) 0.63011(15) 0.0563(14) Uani 1 1 d . . . . .
H1A H 0.4846 0.9559 0.6437 0.068 Uiso 1 1 calc R U . . .
H1B H 0.5685 1.0315 0.6232 0.068 Uiso 1 1 calc R U . . .
C2 C 0.5549(4) 0.9029(3) 0.58815(15) 0.0523(13) Uani 1 1 d . . . . .
H2A H 0.4896 0.9218 0.5683 0.063 Uiso 1 1 calc R U . . .
H2B H 0.6247 0.9135 0.5729 0.063 Uiso 1 1 calc R U . . .
C3 C 0.5658(4) 0.7236(3) 0.56724(13) 0.0464(11) Uani 1 1 d . . . . .
H3A H 0.6351 0.7390 0.5524 0.056 Uiso 1 1 calc R U . . .
H3B H 0.5016 0.7215 0.5450 0.056 Uiso 1 1 calc R U . . .
C4 C 0.5785(4) 0.6257(3) 0.59097(14) 0.0451(12) Uani 1 1 d . . . . .
H4A H 0.5057 0.6074 0.6025 0.054 Uiso 1 1 calc R U . . .
H4B H 0.5990 0.5753 0.5700 0.054 Uiso 1 1 calc R U . . .
C5 C 0.7670(4) 0.9655(3) 0.64931(17) 0.0597(14) Uani 1 1 d . . . . .
H5A H 0.7770 0.9443 0.6190 0.072 Uiso 1 1 calc R U . . .
H5B H 0.8269 0.9341 0.6683 0.072 Uiso 1 1 calc R U . . .
C6 C 0.7859(5) 1.0756(4) 0.6516(2) 0.0782(17) Uani 1 1 d . . . . .
H6A H 0.7800 1.0979 0.6820 0.094 Uiso 1 1 calc R U . . .
H6B H 0.7265 1.1085 0.6330 0.094 Uiso 1 1 calc R U . . .
C7 C 0.9036(5) 1.1037(4) 0.6361(2) 0.104(2) Uani 1 1 d . . . . .
H7A H 0.9624 1.0646 0.6521 0.125 Uiso 1 1 calc R U . . .
H7B H 0.9061 1.0891 0.6045 0.125 Uiso 1 1 calc R U . . .
C8 C 0.9279(6) 1.2108(5) 0.6438(3) 0.161(4) Uani 1 1 d . . . . .
H8A H 0.9482 1.2217 0.6749 0.241 Uiso 1 1 calc R U . . .
H8B H 0.8606 1.2487 0.6350 0.241 Uiso 1 1 calc R U . . .
H8C H 0.9904 1.2308 0.6266 0.241 Uiso 1 1 calc R U . . .
C9 C 0.6330(4) 0.9610(3) 0.70895(15) 0.0552(13) Uani 1 1 d . . . . .
H9A H 0.7010 0.9463 0.7282 0.066 Uiso 1 1 calc R U . . .
H9B H 0.6230 1.0320 0.7087 0.066 Uiso 1 1 calc R U . . .
C10 C 0.5316(4) 0.9153(4) 0.72864(16) 0.0608(14) Uani 1 1 d . . . . .
H10A H 0.5357 0.8441 0.7257 0.073 Uiso 1 1 calc R U . . .
H10B H 0.4617 0.9376 0.7124 0.073 Uiso 1 1 calc R U . . .
C11 C 0.5269(5) 0.9423(4) 0.77775(18) 0.0795(17) Uani 1 1 d . . . . .
H11A H 0.5903 0.9104 0.7946 0.095 Uiso 1 1 calc R U . . .
H11B H 0.5368 1.0130 0.7811 0.095 Uiso 1 1 calc R U . . .
C12 C 0.4181(5) 0.9131(5) 0.7966(2) 0.113(2) Uani 1 1 d . . . . .
H12A H 0.4224 0.9272 0.8280 0.169 Uiso 1 1 calc R U . . .
H12B H 0.4056 0.8438 0.7921 0.169 Uiso 1 1 calc R U . . .
H12C H 0.3556 0.9495 0.7821 0.169 Uiso 1 1 calc R U . . .
C13 C 0.7881(4) 0.6242(3) 0.61190(15) 0.0473(12) Uani 1 1 d . . . . .
H13A H 0.8436 0.6365 0.6368 0.057 Uiso 1 1 calc R U . . .
H13B H 0.7962 0.6768 0.5905 0.057 Uiso 1 1 calc R U . . .
C14 C 0.8205(4) 0.5283(3) 0.59016(17) 0.0562(13) Uani 1 1 d . . . . .
H14A H 0.8133 0.4745 0.6111 0.067 Uiso 1 1 calc R U . . .
H14B H 0.7678 0.5158 0.5645 0.067 Uiso 1 1 calc R U . . .
C15 C 0.9415(4) 0.5310(4) 0.57557(19) 0.0675(15) Uani 1 1 d . . . . .
H15A H 0.9934 0.5455 0.6013 0.081 Uiso 1 1 calc R U . . .
H15B H 0.9477 0.5845 0.5544 0.081 Uiso 1 1 calc R U . . .
C16 C 0.9801(4) 0.4366(4) 0.55440(19) 0.0788(17) Uani 1 1 d . . . . .
H16A H 1.0569 0.4446 0.5452 0.118 Uiso 1 1 calc R U . . .
H16B H 0.9292 0.4214 0.5289 0.118 Uiso 1 1 calc R U . . .
H16C H 0.9786 0.3838 0.5757 0.118 Uiso 1 1 calc R U . . .
C17 C 0.6521(4) 0.5509(3) 0.66113(15) 0.0511(13) Uani 1 1 d . . . . .
H17A H 0.7190 0.5476 0.6820 0.061 Uiso 1 1 calc R U . . .
H17B H 0.6473 0.4888 0.6450 0.061 Uiso 1 1 calc R U . . .
C18 C 0.5469(4) 0.5615(4) 0.68704(17) 0.0630(14) Uani 1 1 d . . . . .
H18A H 0.4792 0.5636 0.6665 0.076 Uiso 1 1 calc R U . . .
H18B H 0.5510 0.6232 0.7034 0.076 Uiso 1 1 calc R U . . .
C19 C 0.5358(5) 0.4770(5) 0.7194(2) 0.099(2) Uani 1 1 d . . . . .
H19A H 0.5408 0.4155 0.7031 0.119 Uiso 1 1 calc R U . . .
H19B H 0.6005 0.4793 0.7413 0.119 Uiso 1 1 calc R U . . .
C20 C 0.4303(6) 0.4762(5) 0.7427(3) 0.130(3) Uani 1 1 d . . . . .
H20A H 0.4191 0.4119 0.7551 0.195 Uiso 1 1 calc R U . . .
H20B H 0.3664 0.4921 0.7221 0.195 Uiso 1 1 calc R U . . .
H20C H 0.4357 0.5242 0.7662 0.195 Uiso 1 1 calc R U . . .
C21 C 0.4936(3) 0.2308(3) 0.55614(13) 0.0389(10) Uani 1 1 d . . . . .
C22 C 0.5874(4) 0.2931(3) 0.56459(17) 0.0567(13) Uani 1 1 d . . . . .
H22 H 0.5757 0.3519 0.5796 0.068 Uiso 1 1 calc R U . . .
C23 C 0.6965(4) 0.2730(4) 0.55199(19) 0.0674(15) Uani 1 1 d . . . . .
H23 H 0.7556 0.3178 0.5586 0.081 Uiso 1 1 calc R U . . .
C24 C 0.7184(4) 0.1880(4) 0.52984(17) 0.0575(13) Uani 1 1 d . . . . .
H24 H 0.7918 0.1740 0.5211 0.069 Uiso 1 1 calc R U . . .
C25 C 0.6283(4) 0.1234(3) 0.52070(15) 0.0510(12) Uani 1 1 d . . . . .
H25 H 0.6410 0.0645 0.5059 0.061 Uiso 1 1 calc R U . . .
C26 C 0.5197(4) 0.1457(3) 0.53347(14) 0.0444(11) Uani 1 1 d . . . . .
H26 H 0.4608 0.1010 0.5264 0.053 Uiso 1 1 calc R U . . .
C27 C 0.2656(3) 0.2015(3) 0.54111(14) 0.0403(11) Uani 1 1 d . . . . .
C28 C 0.1914(4) 0.2514(3) 0.51056(15) 0.0557(13) Uani 1 1 d . . . . .
H28 H 0.1974 0.3196 0.5086 0.067 Uiso 1 1 calc R U . . .
C29 C 0.1092(4) 0.2034(4) 0.48302(17) 0.0686(16) Uani 1 1 d . . . . .
H29 H 0.0614 0.2400 0.4633 0.082 Uiso 1 1 calc R U . . .
C30 C 0.0973(4) 0.1027(4) 0.4845(2) 0.0732(17) Uani 1 1 d . . . . .
H30 H 0.0435 0.0703 0.4655 0.088 Uiso 1 1 calc R U . . .
C31 C 0.1672(4) 0.0513(4) 0.5147(2) 0.0736(17) Uani 1 1 d . . . . .
H31 H 0.1596 -0.0168 0.5169 0.088 Uiso 1 1 calc R U . . .
C32 C 0.2486(4) 0.0998(3) 0.54193(18) 0.0596(14) Uani 1 1 d . . . . .
H32 H 0.2948 0.0625 0.5620 0.072 Uiso 1 1 calc R U . . .
C33 C 0.3622(4) 0.2140(3) 0.62478(15) 0.0526(12) Uani 1 1 d . . . . .
C34 C 0.2631(6) 0.1762(5) 0.64150(19) 0.0893(19) Uani 1 1 d . . . . .
H34 H 0.1979 0.1701 0.6221 0.107 Uiso 1 1 calc R U . . .
C35 C 0.2558(7) 0.1469(6) 0.6855(2) 0.119(3) Uani 1 1 d . . . . .
H35 H 0.1871 0.1220 0.6950 0.143 Uiso 1 1 calc R U . . .
C36 C 0.3500(9) 0.1548(5) 0.7147(2) 0.108(3) Uani 1 1 d . . . . .
H36 H 0.3463 0.1348 0.7442 0.129 Uiso 1 1 calc R U . . .
C37 C 0.4486(7) 0.1919(4) 0.7005(2) 0.0831(19) Uani 1 1 d . . . . .
H37 H 0.5127 0.1985 0.7204 0.100 Uiso 1 1 calc R U . . .
C38 C 0.4546(5) 0.2203(4) 0.65602(15) 0.0624(14) Uani 1 1 d . . . . .
H38 H 0.5239 0.2447 0.6470 0.075 Uiso 1 1 calc R U . . .
C39 C 0.3437(4) 0.3740(3) 0.57313(15) 0.0436(11) Uani 1 1 d . . . . .
C40 C 0.2911(4) 0.4240(4) 0.60641(18) 0.0581(14) Uani 1 1 d . . . . .
H40 H 0.2740 0.3895 0.6319 0.070 Uiso 1 1 calc R U . . .
C41 C 0.2628(4) 0.5227(4) 0.6034(2) 0.0726(17) Uani 1 1 d . . . . .
H41 H 0.2280 0.5531 0.6268 0.087 Uiso 1 1 calc R U . . .
C42 C 0.2855(4) 0.5766(4) 0.5663(3) 0.0732(18) Uani 1 1 d . . . . .
H42 H 0.2645 0.6427 0.5639 0.088 Uiso 1 1 calc R U . . .
C43 C 0.3393(4) 0.5311(4) 0.53306(19) 0.0621(15) Uani 1 1 d . . . . .
H43 H 0.3568 0.5668 0.5079 0.074 Uiso 1 1 calc R U . . .
C44 C 0.3684(4) 0.4318(3) 0.53627(16) 0.0492(13) Uani 1 1 d . . . . .
H44 H 0.4055 0.4026 0.5131 0.059 Uiso 1 1 calc R U . . .
C45 C 0.2668(6) 0.7664(5) 0.6737(2) 0.1013(15) Uani 1 1 d . . . . .
H45A H 0.2859 0.8069 0.6998 0.122 Uiso 1 1 calc R U . . .
H45B H 0.2957 0.7003 0.6798 0.122 Uiso 1 1 calc R U . . .
C46 C 0.1415(6) 0.7636(6) 0.6645(3) 0.136(2) Uani 1 1 d . . . . .
H46A H 0.1161 0.6984 0.6550 0.163 Uiso 1 1 calc R U . . .
H46B H 0.1020 0.7823 0.6907 0.163 Uiso 1 1 calc R U . . .
C47 C 0.1218(6) 0.8343(6) 0.6293(3) 0.136(2) Uani 1 1 d . . . . .
H47A H 0.0848 0.8926 0.6405 0.163 Uiso 1 1 calc R U . . .
H47B H 0.0719 0.8063 0.6055 0.163 Uiso 1 1 calc R U . . .
C48 C 0.2330(6) 0.8609(5) 0.6125(2) 0.1013(15) Uani 1 1 d . . . . .
H48A H 0.2335 0.8459 0.5809 0.122 Uiso 1 1 calc R U . . .
H48B H 0.2476 0.9308 0.6166 0.122 Uiso 1 1 calc R U . . .
B1 B 0.3670(4) 0.2545(4) 0.57334(16) 0.0430(13) Uani 1 1 d . . . . .
N2 N 0.6538(3) 0.9278(3) 0.66243(11) 0.0458(10) Uani 1 1 d . . . . .
N3 N 0.5454(3) 0.7987(3) 0.60134(11) 0.0424(9) Uani 1 1 d D . . . .
N4 N 0.6699(3) 0.6313(2) 0.62884(11) 0.0400(9) Uani 1 1 d . . . . .
O3 O 0.3171(3) 0.8054(3) 0.63671(13) 0.0817(11) Uani 1 1 d . . . . .
Pd1 Pd 0.66005(3) 0.77516(2) 0.65366(2) 0.03988(12) Uani 1 1 d . . . . .
N1 N 0.7728(4) 0.7507(3) 0.70616(14) 0.0554(11) Uani 1 1 d . . . . .
O1 O 0.8749(3) 0.7609(4) 0.70235(13) 0.1084(16) Uani 1 1 d . . . . .
O2 O 0.7396(4) 0.7247(4) 0.74112(14) 0.1127(16) Uani 1 1 d . . . . .
H3 H 0.473(3) 0.786(4) 0.6149(18) 0.135 Uiso 1 1 d D 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
C1 C2 1.495(6) . ?
C1 N2 1.510(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N3 1.474(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.474(5) . ?
C3 C4 1.509(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N4 1.508(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.492(6) . ?
C5 C6 1.509(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.525(8) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.495(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.490(6) . ?
C9 N2 1.503(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.524(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.476(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N4 1.503(5) . ?
C13 C14 1.513(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.504(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.510(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N4 1.482(5) . ?
C17 C18 1.502(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.513(7) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.454(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.384(6) . ?
C21 C22 1.392(6) . ?
C21 B1 1.626(6) . ?
C22 C23 1.376(6) . ?
C22 H22 0.9300 . ?
C23 C24 1.363(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.381(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.379(6) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C27 C32 1.394(5) . ?
C27 C28 1.394(6) . ?
C27 B1 1.644(6) . ?
C28 C29 1.386(6) . ?
C28 H28 0.9300 . ?
C29 C30 1.374(7) . ?
C29 H29 0.9300 . ?
C30 C31 1.369(7) . ?
C30 H30 0.9300 . ?
C31 C32 1.379(6) . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C33 C38 1.384(6) . ?
C33 C34 1.387(7) . ?
C33 B1 1.644(7) . ?
C34 C35 1.388(8) . ?
C34 H34 0.9300 . ?
C35 C36 1.365(9) . ?
C35 H35 0.9300 . ?
C36 C37 1.349(9) . ?
C36 H36 0.9300 . ?
C37 C38 1.397(7) . ?
C37 H37 0.9300 . ?
C38 H38 0.9300 . ?
C39 C40 1.384(6) . ?
C39 C44 1.401(6) . ?
C39 B1 1.642(6) . ?
C40 C41 1.379(6) . ?
C40 H40 0.9300 . ?
C41 C42 1.374(8) . ?
C41 H41 0.9300 . ?
C42 C43 1.360(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.390(6) . ?
C43 H43 0.9300 . ?
C44 H44 0.9300 . ?
C45 O3 1.395(7) . ?
C45 C46 1.468(8) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 C47 1.435(9) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 C48 1.467(9) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 O3 1.401(6) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
N2 Pd1 2.087(3) . ?
N3 Pd1 2.021(3) . ?
N3 H3 0.98(2) . ?
N4 Pd1 2.094(3) . ?
Pd1 N1 2.014(4) . ?
N1 O2 1.196(5) . ?
N1 O1 1.210(5) . ?

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
C2 C1 N2 110.3(3) . . ?
C2 C1 H1A 109.6 . . ?
N2 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N3 C2 C1 106.8(4) . . ?
N3 C2 H2A 110.4 . . ?
C1 C2 H2A 110.4 . . ?
N3 C2 H2B 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
N3 C3 C4 107.1(3) . . ?
N3 C3 H3A 110.3 . . ?
C4 C3 H3A 110.3 . . ?
N3 C3 H3B 110.3 . . ?
C4 C3 H3B 110.3 . . ?
H3A C3 H3B 108.5 . . ?
N4 C4 C3 110.8(3) . . ?
N4 C4 H4A 109.5 . . ?
C3 C4 H4A 109.5 . . ?
N4 C4 H4B 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
N2 C5 C6 117.1(4) . . ?
N2 C5 H5A 108.0 . . ?
C6 C5 H5A 108.0 . . ?
N2 C5 H5B 108.0 . . ?
C6 C5 H5B 108.0 . . ?
H5A C5 H5B 107.3 . . ?
C5 C6 C7 111.4(5) . . ?
C5 C6 H6A 109.3 . . ?
C7 C6 H6A 109.3 . . ?
C5 C6 H6B 109.3 . . ?
C7 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
C8 C7 C6 111.1(6) . . ?
C8 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N2 115.1(4) . . ?
C10 C9 H9A 108.5 . . ?
N2 C9 H9A 108.5 . . ?
C10 C9 H9B 108.5 . . ?
N2 C9 H9B 108.5 . . ?
H9A C9 H9B 107.5 . . ?
C9 C10 C11 111.3(4) . . ?
C9 C10 H10A 109.4 . . ?
C11 C10 H10A 109.4 . . ?
C9 C10 H10B 109.4 . . ?
C11 C10 H10B 109.4 . . ?
H10A C10 H10B 108.0 . . ?
C12 C11 C10 113.2(5) . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
C10 C11 H11B 108.9 . . ?
H11A C11 H11B 107.8 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N4 C13 C14 117.5(3) . . ?
N4 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
N4 C13 H13B 107.9 . . ?
C14 C13 H13B 107.9 . . ?
H13A C13 H13B 107.2 . . ?
C15 C14 C13 111.7(4) . . ?
C15 C14 H14A 109.3 . . ?
C13 C14 H14A 109.3 . . ?
C15 C14 H14B 109.3 . . ?
C13 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
C14 C15 C16 114.3(4) . . ?
C14 C15 H15A 108.7 . . ?
C16 C15 H15A 108.7 . . ?
C14 C15 H15B 108.7 . . ?
C16 C15 H15B 108.7 . . ?
H15A C15 H15B 107.6 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 C18 115.0(4) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C17 C18 C19 111.5(4) . . ?
C17 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
C17 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C20 C19 C18 115.1(5) . . ?
C20 C19 H19A 108.5 . . ?
C18 C19 H19A 108.5 . . ?
C20 C19 H19B 108.5 . . ?
C18 C19 H19B 108.5 . . ?
H19A C19 H19B 107.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C21 C22 113.6(4) . . ?
C26 C21 B1 123.7(4) . . ?
C22 C21 B1 122.7(4) . . ?
C23 C22 C21 123.9(4) . . ?
C23 C22 H22 118.0 . . ?
C21 C22 H22 118.0 . . ?
C24 C23 C22 120.5(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 118.0(5) . . ?
C23 C24 H24 121.0 . . ?
C25 C24 H24 121.0 . . ?
C26 C25 C24 120.3(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C21 123.7(4) . . ?
C25 C26 H26 118.1 . . ?
C21 C26 H26 118.1 . . ?
C32 C27 C28 114.1(4) . . ?
C32 C27 B1 121.3(4) . . ?
C28 C27 B1 124.6(4) . . ?
C29 C28 C27 122.7(4) . . ?
C29 C28 H28 118.6 . . ?
C27 C28 H28 118.6 . . ?
C30 C29 C28 121.0(5) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C31 C30 C29 118.0(5) . . ?
C31 C30 H30 121.0 . . ?
C29 C30 H30 121.0 . . ?
C30 C31 C32 120.5(5) . . ?
C30 C31 H31 119.7 . . ?
C32 C31 H31 119.7 . . ?
C31 C32 C27 123.7(5) . . ?
C31 C32 H32 118.2 . . ?
C27 C32 H32 118.2 . . ?
C38 C33 C34 114.0(5) . . ?
C38 C33 B1 122.9(4) . . ?
C34 C33 B1 123.0(4) . . ?
C35 C34 C33 123.7(6) . . ?
C35 C34 H34 118.2 . . ?
C33 C34 H34 118.2 . . ?
C36 C35 C34 119.6(7) . . ?
C36 C35 H35 120.2 . . ?
C34 C35 H35 120.2 . . ?
C37 C36 C35 119.5(6) . . ?
C37 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C36 C37 C38 120.1(6) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 123.1(6) . . ?
C33 C38 H38 118.4 . . ?
C37 C38 H38 118.4 . . ?
C40 C39 C44 114.9(4) . . ?
C40 C39 B1 124.2(4) . . ?
C44 C39 B1 120.8(4) . . ?
C41 C40 C39 122.9(5) . . ?
C41 C40 H40 118.6 . . ?
C39 C40 H40 118.6 . . ?
C42 C41 C40 120.8(5) . . ?
C42 C41 H41 119.6 . . ?
C40 C41 H41 119.6 . . ?
C43 C42 C41 118.4(5) . . ?
C43 C42 H42 120.8 . . ?
C41 C42 H42 120.8 . . ?
C42 C43 C44 120.7(5) . . ?
C42 C43 H43 119.6 . . ?
C44 C43 H43 119.6 . . ?
C43 C44 C39 122.3(5) . . ?
C43 C44 H44 118.8 . . ?
C39 C44 H44 118.8 . . ?
O3 C45 C46 108.9(5) . . ?
O3 C45 H45A 109.9 . . ?
C46 C45 H45A 109.9 . . ?
O3 C45 H45B 109.9 . . ?
C46 C45 H45B 109.9 . . ?
H45A C45 H45B 108.3 . . ?
C47 C46 C45 103.4(7) . . ?
C47 C46 H46A 111.1 . . ?
C45 C46 H46A 111.1 . . ?
C47 C46 H46B 111.1 . . ?
C45 C46 H46B 111.1 . . ?
H46A C46 H46B 109.1 . . ?
C46 C47 C48 108.4(6) . . ?
C46 C47 H47A 110.0 . . ?
C48 C47 H47A 110.0 . . ?
C46 C47 H47B 110.0 . . ?
C48 C47 H47B 110.0 . . ?
H47A C47 H47B 108.4 . . ?
O3 C48 C47 107.0(5) . . ?
O3 C48 H48A 110.3 . . ?
C47 C48 H48A 110.3 . . ?
O3 C48 H48B 110.3 . . ?
C47 C48 H48B 110.3 . . ?
H48A C48 H48B 108.6 . . ?
C21 B1 C39 110.3(4) . . ?
C21 B1 C27 111.0(4) . . ?
C39 B1 C27 108.4(3) . . ?
C21 B1 C33 108.7(3) . . ?
C39 B1 C33 108.5(4) . . ?
C27 B1 C33 109.9(4) . . ?
C5 N2 C9 110.0(3) . . ?
C5 N2 C1 110.9(4) . . ?
C9 N2 C1 110.3(3) . . ?
C5 N2 Pd1 105.5(3) . . ?
C9 N2 Pd1 115.0(3) . . ?
C1 N2 Pd1 105.0(2) . . ?
C3 N3 C2 117.2(4) . . ?
C3 N3 Pd1 107.7(2) . . ?
C2 N3 Pd1 107.6(2) . . ?
C3 N3 H3 110(4) . . ?
C2 N3 H3 112(4) . . ?
Pd1 N3 H3 101(4) . . ?
C17 N4 C13 110.1(3) . . ?
C17 N4 C4 109.6(3) . . ?
C13 N4 C4 111.1(3) . . ?
C17 N4 Pd1 116.0(3) . . ?
C13 N4 Pd1 104.6(2) . . ?
C4 N4 Pd1 105.2(2) . . ?
C45 O3 C48 107.6(5) . . ?
N1 Pd1 N3 179.29(18) . . ?
N1 Pd1 N2 95.21(14) . . ?
N3 Pd1 N2 85.11(13) . . ?
N1 Pd1 N4 94.45(13) . . ?
N3 Pd1 N4 85.34(13) . . ?
N2 Pd1 N4 166.25(14) . . ?
O2 N1 O1 119.5(4) . . ?
O2 N1 Pd1 120.3(4) . . ?
O1 N1 Pd1 120.2(4) . . ?

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
N2 C1 C2 N3 55.7(5) . . . . ?
N3 C3 C4 N4 -54.0(4) . . . . ?
N2 C5 C6 C7 -178.4(5) . . . . ?
C5 C6 C7 C8 -172.8(5) . . . . ?
N2 C9 C10 C11 172.2(4) . . . . ?
C9 C10 C11 C12 170.2(5) . . . . ?
N4 C13 C14 C15 -179.0(4) . . . . ?
C13 C14 C15 C16 178.8(4) . . . . ?
N4 C17 C18 C19 -179.6(4) . . . . ?
C17 C18 C19 C20 -174.2(6) . . . . ?
C26 C21 C22 C23 -0.2(7) . . . . ?
B1 C21 C22 C23 177.3(5) . . . . ?
C21 C22 C23 C24 0.0(8) . . . . ?
C22 C23 C24 C25 -0.2(8) . . . . ?
C23 C24 C25 C26 0.6(7) . . . . ?
C24 C25 C26 C21 -0.9(7) . . . . ?
C22 C21 C26 C25 0.7(6) . . . . ?
B1 C21 C26 C25 -176.8(4) . . . . ?
C32 C27 C28 C29 -0.9(7) . . . . ?
B1 C27 C28 C29 178.0(5) . . . . ?
C27 C28 C29 C30 -0.4(8) . . . . ?
C28 C29 C30 C31 1.6(9) . . . . ?
C29 C30 C31 C32 -1.6(9) . . . . ?
C30 C31 C32 C27 0.3(9) . . . . ?
C28 C27 C32 C31 0.9(7) . . . . ?
B1 C27 C32 C31 -178.0(5) . . . . ?
C38 C33 C34 C35 -0.1(9) . . . . ?
B1 C33 C34 C35 -176.2(6) . . . . ?
C33 C34 C35 C36 -0.1(11) . . . . ?
C34 C35 C36 C37 0.6(11) . . . . ?
C35 C36 C37 C38 -1.1(10) . . . . ?
C34 C33 C38 C37 -0.4(7) . . . . ?
B1 C33 C38 C37 175.7(5) . . . . ?
C36 C37 C38 C33 1.0(9) . . . . ?
C44 C39 C40 C41 1.2(6) . . . . ?
B1 C39 C40 C41 -173.7(4) . . . . ?
C39 C40 C41 C42 0.5(7) . . . . ?
C40 C41 C42 C43 -1.8(7) . . . . ?
C41 C42 C43 C44 1.4(7) . . . . ?
C42 C43 C44 C39 0.4(7) . . . . ?
C40 C39 C44 C43 -1.6(6) . . . . ?
B1 C39 C44 C43 173.5(4) . . . . ?
O3 C45 C46 C47 -20.8(8) . . . . ?
C45 C46 C47 C48 11.6(9) . . . . ?
C46 C47 C48 O3 1.1(9) . . . . ?
C26 C21 B1 C39 -149.1(4) . . . . ?
C22 C21 B1 C39 33.6(5) . . . . ?
C26 C21 B1 C27 -28.9(6) . . . . ?
C22 C21 B1 C27 153.8(4) . . . . ?
C26 C21 B1 C33 92.1(5) . . . . ?
C22 C21 B1 C33 -85.2(5) . . . . ?
C40 C39 B1 C21 -138.9(4) . . . . ?
C44 C39 B1 C21 46.4(5) . . . . ?
C40 C39 B1 C27 99.3(5) . . . . ?
C44 C39 B1 C27 -75.3(5) . . . . ?
C40 C39 B1 C33 -20.0(6) . . . . ?
C44 C39 B1 C33 165.3(4) . . . . ?
C32 C27 B1 C21 72.2(5) . . . . ?
C28 C27 B1 C21 -106.6(5) . . . . ?
C32 C27 B1 C39 -166.4(4) . . . . ?
C28 C27 B1 C39 14.7(6) . . . . ?
C32 C27 B1 C33 -48.0(6) . . . . ?
C28 C27 B1 C33 133.2(4) . . . . ?
C38 C33 B1 C21 37.8(6) . . . . ?
C34 C33 B1 C21 -146.3(5) . . . . ?
C38 C33 B1 C39 -82.1(5) . . . . ?
C34 C33 B1 C39 93.7(5) . . . . ?
C38 C33 B1 C27 159.5(4) . . . . ?
C34 C33 B1 C27 -24.7(6) . . . . ?
C6 C5 N2 C9 -56.4(5) . . . . ?
C6 C5 N2 C1 65.8(5) . . . . ?
C6 C5 N2 Pd1 178.9(4) . . . . ?
C10 C9 N2 C5 -170.9(4) . . . . ?
C10 C9 N2 C1 66.5(5) . . . . ?
C10 C9 N2 Pd1 -51.9(5) . . . . ?
C2 C1 N2 C5 77.4(5) . . . . ?
C2 C1 N2 C9 -160.6(4) . . . . ?
C2 C1 N2 Pd1 -36.1(4) . . . . ?
C4 C3 N3 C2 167.2(3) . . . . ?
C4 C3 N3 Pd1 45.8(4) . . . . ?
C1 C2 N3 C3 -167.4(4) . . . . ?
C1 C2 N3 Pd1 -46.0(4) . . . . ?
C18 C17 N4 C13 168.5(4) . . . . ?
C18 C17 N4 C4 -69.0(5) . . . . ?
C18 C17 N4 Pd1 50.0(4) . . . . ?
C14 C13 N4 C17 56.6(5) . . . . ?
C14 C13 N4 C4 -65.0(5) . . . . ?
C14 C13 N4 Pd1 -178.0(3) . . . . ?
C3 C4 N4 C17 159.1(4) . . . . ?
C3 C4 N4 C13 -79.0(4) . . . . ?
C3 C4 N4 Pd1 33.7(4) . . . . ?
C46 C45 O3 C48 22.2(7) . . . . ?
C47 C48 O3 C45 -14.3(7) . . . . ?

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
C5 H5B O1 0.97 2.61 3.399(6) 138.9 .
C13 H13A O1 0.97 2.60 3.389(6) 138.5 .
N3 H3 O3 0.98(2) 1.99(3) 2.930(5) 161(5) .

_refine_diff_density_max         0.459
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.072

_shelxl_version_number           2014-1

