# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_8d
_database_code_depnum_ccdc_archive 'CCDC 1825947'
_audit_update_record             
;
2018-02-26 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C33 H37 N8 O4 Pd, B F4'
_chemical_formula_sum            'C33 H37 B F4 N8 O4 Pd'
_chemical_formula_weight         802.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -1.0140 0.9845 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0015 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   8.200(2)
_cell_length_b                   13.605(3)
_cell_length_c                   30.666(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.85(3)
_cell_angle_gamma                90
_cell_volume                     3396.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5416
_cell_measurement_theta_min      1.317
_cell_measurement_theta_max      25.944

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             1640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.588
_shelx_estimated_absorpt_T_min   0.843
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700

_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_measurement_device_type  
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            77120
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.317
_diffrn_reflns_theta_max         25.771
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6783
_reflns_number_gt                6042
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'

_refine_special_details          
;
Hydrogen atoms were included at calculated positions with isotropic 
Ufactors=1.2Ueq (Ufactors=1.5Ueq for methyl groups). Anisotropic 
thermal motion modeling has been applied to all atoms with full
occupancies. Thermal parameters restrains (SIMU and ISOR) have been 
used to compensate for electron density noise caused by radiation
damage. Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+174.9742P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6783
_refine_ls_number_parameters     407
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.1325
_refine_ls_wR_factor_ref         0.3219
_refine_ls_wR_factor_gt          0.3163
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_restrained_S_all      1.139
_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
Pd_1 Pd 0.47981(11) 0.70027(8) 0.72143(3) 0.0224(3) Uani 1 1 d . . . . .
C19A_2 C 0.474(2) 0.7895(14) 0.6628(6) 0.051(4) Uiso 0.5 1 d D . P A 1
H19A_2 H 0.580759 0.815759 0.655963 0.061 Uiso 0.5 1 calc R U P A 1
H19B_2 H 0.402500 0.766025 0.636572 0.061 Uiso 0.5 1 calc R U P A 1
C21A_2 C 0.399(3) 0.8397(17) 0.6932(5) 0.020(2) Uiso 0.5 1 d D . P A 1
H21A_2 H 0.296380 0.868751 0.682948 0.024 Uiso 0.5 1 calc DR U P A 1
C20A_2 C 0.4524(14) 0.8533(9) 0.7359(4) 0.020(2) Uiso 0.5 1 d D . P A 1
H20A_2 H 0.367691 0.870016 0.755162 0.024 Uiso 0.5 1 calc R U P A 1
H20B_2 H 0.555112 0.891495 0.742593 0.024 Uiso 0.5 1 calc R U P A 1
C19B_2 C 0.474(2) 0.7895(14) 0.6628(6) 0.051(4) Uiso 0.5 1 d D . P A 2
H19C_2 H 0.565855 0.779612 0.644975 0.061 Uiso 0.5 1 calc R U P A 2
H19D_2 H 0.366076 0.795571 0.644773 0.061 Uiso 0.5 1 calc R U P A 2
C21B_2 C 0.502(3) 0.8508(16) 0.6960(5) 0.019(5) Uiso 0.5 1 d D . P A 2
H21B_2 H 0.571333 0.904188 0.690428 0.023 Uiso 0.5 1 calc R U P A 2
C20B_2 C 0.4524(14) 0.8533(9) 0.7359(4) 0.020(2) Uiso 0.5 1 d D . P A 2
H20C_2 H 0.338600 0.876397 0.737297 0.024 Uiso 0.5 1 calc R U P A 2
H20D_2 H 0.531881 0.880538 0.759677 0.024 Uiso 0.5 1 calc R U P A 2
C11_4 C 0.2334(17) 0.3143(10) 0.6356(6) 0.037(3) Uani 1 1 d . . . . .
H11A_4 H 0.150212 0.354188 0.618072 0.055 Uiso 1 1 calc R U . . .
H11B_4 H 0.216452 0.318093 0.666634 0.055 Uiso 1 1 calc R U . . .
H11C_4 H 0.223889 0.245800 0.625751 0.055 Uiso 1 1 calc R U . . .
N1_4 N 0.6558(8) 0.3258(6) 0.6005(3) 0.029(3) Uani 1 1 d G . . . .
C2_4 C 0.4931(8) 0.2999(5) 0.6028(3) 0.034(3) Uani 1 1 d G . . . .
N3_4 N 0.4000(7) 0.3521(6) 0.6299(3) 0.027(2) Uani 1 1 d G . . . .
C4_4 C 0.4696(8) 0.4303(5) 0.6547(3) 0.023(3) Uani 1 1 d G . . . .
C5_4 C 0.6324(8) 0.4562(5) 0.6524(3) 0.023(3) Uani 1 1 d G . . . .
C6_4 C 0.7254(7) 0.4040(6) 0.6253(3) 0.029(3) Uani 1 1 d G . . . .
O2_4 O 0.4334(13) 0.2306(8) 0.5809(3) 0.038(2) Uani 1 1 d . . . . .
C10_4 C 0.7383(17) 0.2832(9) 0.5656(5) 0.028(3) Uani 1 1 d . . . . .
H10A_4 H 0.713765 0.211957 0.563406 0.034 Uiso 1 1 calc R U . . .
H10B_4 H 0.858564 0.290912 0.572800 0.034 Uiso 1 1 calc R U . . .
C14_4 C 0.6842(14) 0.3316(8) 0.5218(3) 0.044(3) Uani 1 1 d G U . . .
C19_4 C 0.5765(15) 0.2821(8) 0.4909(4) 0.059(5) Uani 1 1 d G . . . .
H19_4 H 0.540080 0.217818 0.497072 0.071 Uiso 1 1 calc R U . . .
C18_4 C 0.5222(16) 0.3265(11) 0.4510(3) 0.071(5) Uani 1 1 d G U . . .
H18_4 H 0.448558 0.292560 0.429869 0.086 Uiso 1 1 calc R U . . .
C17_4 C 0.5755(18) 0.4204(11) 0.4419(3) 0.074(4) Uani 1 1 d G U . . .
H17_4 H 0.538324 0.450783 0.414643 0.089 Uiso 1 1 calc R U . . .
C16_4 C 0.6832(18) 0.4700(8) 0.4728(4) 0.069(4) Uani 1 1 d G U . . .
H16_4 H 0.719614 0.534265 0.466618 0.083 Uiso 1 1 calc R U . . .
C15_4 C 0.7375(15) 0.4256(8) 0.5127(4) 0.057(4) Uani 1 1 d G U . . .
H15_4 H 0.811138 0.459525 0.533821 0.069 Uiso 1 1 calc R U . . .
O6_4 O 0.8781(11) 0.4268(8) 0.6215(4) 0.037(2) Uani 1 1 d . . . . .
N9_4 N 0.3997(13) 0.5027(9) 0.6759(4) 0.026(2) Uani 1 1 d . . . . .
C13_4 C 0.2256(16) 0.5157(13) 0.6823(5) 0.040(4) Uani 1 1 d . . . . .
H13A_4 H 0.157428 0.511742 0.653881 0.059 Uiso 1 1 calc R U . . .
H13B_4 H 0.210644 0.580010 0.695658 0.059 Uiso 1 1 calc R U . . .
H13C_4 H 0.193026 0.463812 0.701726 0.059 Uiso 1 1 calc R U . . .
C8_4 C 0.5186(14) 0.5725(8) 0.6901(4) 0.020(2) Uani 1 1 d . . . . .
N7_4 N 0.6571(12) 0.5421(8) 0.6759(4) 0.024(2) Uani 1 1 d . . . . .
C12_4 C 0.8116(16) 0.5964(11) 0.6825(5) 0.032(3) Uani 1 1 d . . . . .
H12A_4 H 0.857763 0.601362 0.654553 0.048 Uiso 1 1 calc R U . . .
H12B_4 H 0.889231 0.561863 0.703996 0.048 Uiso 1 1 calc R U . . .
H12C_4 H 0.791520 0.662526 0.693402 0.048 Uiso 1 1 calc R U . . .
C11_3 C 0.7682(14) 0.4887(11) 0.8916(5) 0.033(3) Uani 1 1 d . . . . .
H11A_3 H 0.800376 0.458934 0.864791 0.049 Uiso 1 1 calc DR U . . .
H11C_3 H 0.785390 0.441245 0.915752 0.049 Uiso 1 1 calc R U . . .
H11B_3 H 0.835078 0.547341 0.899065 0.049 Uiso 1 1 calc R U . . .
O2_3 O 0.5581(11) 0.4514(8) 0.9508(3) 0.034(2) Uani 1 1 d . . . . .
N1_3 N 0.3310(7) 0.5205(6) 0.9128(2) 0.027(2) Uani 1 1 d G U . . .
C2_3 C 0.4958(8) 0.4938(6) 0.9172(2) 0.027(3) Uani 1 1 d G . . . .
N3_3 N 0.5920(6) 0.5167(6) 0.8843(2) 0.022(2) Uani 1 1 d G U . . .
C4_3 C 0.5234(7) 0.5663(6) 0.8469(2) 0.020(2) Uani 1 1 d G U . . .
C5_3 C 0.3586(8) 0.5930(6) 0.8425(2) 0.018(2) Uani 1 1 d G U . . .
C6_3 C 0.2624(6) 0.5701(6) 0.8754(2) 0.025(3) Uani 1 1 d G U . . .
C10_3 C 0.2397(16) 0.5000(12) 0.9488(4) 0.031(3) Uani 1 1 d . . . . .
H10B_3 H 0.145607 0.545950 0.947742 0.037 Uiso 1 1 calc R U . . .
H10A_3 H 0.310865 0.511479 0.976776 0.037 Uiso 1 1 calc R U . . .
C14_3 C 0.1758(11) 0.3947(6) 0.9480(3) 0.033(3) Uani 1 1 d G U . . .
C15_3 C 0.1091(11) 0.3505(7) 0.9091(3) 0.033(3) Uani 1 1 d G U . . .
H15_3 H 0.112581 0.383448 0.881901 0.039 Uiso 1 1 calc R U . . .
C16_3 C 0.0374(12) 0.2580(7) 0.9099(3) 0.040(3) Uani 1 1 d G U . . .
H16_3 H -0.008199 0.227823 0.883286 0.047 Uiso 1 1 calc R U . . .
C17_3 C 0.0323(13) 0.2098(6) 0.9497(4) 0.053(3) Uani 1 1 d G U . . .
H17_3 H -0.016741 0.146643 0.950247 0.064 Uiso 1 1 calc R U . . .
C18_3 C 0.0990(15) 0.2540(9) 0.9886(3) 0.060(4) Uani 1 1 d G U . . .
H18_3 H 0.095497 0.221086 1.015823 0.072 Uiso 1 1 calc R U . . .
C19_3 C 0.1707(14) 0.3465(9) 0.9878(3) 0.052(5) Uani 1 1 d G . . . .
H19_3 H 0.216278 0.376711 1.014439 0.063 Uiso 1 1 calc R U . . .
O6_3 O 0.1078(10) 0.5958(7) 0.8734(3) 0.028(2) Uani 1 1 d . . . . .
N9_3 N 0.5876(13) 0.6006(10) 0.8113(4) 0.029(2) Uani 1 1 d . U . . .
C13_3 C 0.7543(14) 0.5926(11) 0.7999(4) 0.029(3) Uani 1 1 d . U . . .
H13A_3 H 0.779153 0.523605 0.794457 0.043 Uiso 1 1 calc R U . . .
H13B_3 H 0.831666 0.617622 0.824224 0.043 Uiso 1 1 calc R U . . .
H13C_3 H 0.764253 0.631363 0.773435 0.043 Uiso 1 1 calc R U . . .
C8_3 C 0.4653(14) 0.6442(10) 0.7822(4) 0.021(2) Uani 1 1 d . U . . .
N7_3 N 0.3294(11) 0.6387(8) 0.8029(3) 0.023(2) Uani 1 1 d . U . . .
C12_3 C 0.1680(14) 0.6769(10) 0.7840(4) 0.025(3) Uani 1 1 d . U . . .
H12A_3 H 0.137419 0.732618 0.801604 0.037 Uiso 1 1 calc R U . . .
H12C_3 H 0.085300 0.624965 0.784105 0.037 Uiso 1 1 calc R U . . .
H12B_3 H 0.174068 0.698628 0.753769 0.037 Uiso 1 1 calc R U . . .
B_5 B 0.9444(19) 0.8641(11) 0.7293(6) 0.032(3) Uani 1 1 d . U . . .
F1_5 F 1.0773(10) 0.9097(7) 0.7560(3) 0.047(2) Uani 1 1 d . U . . .
F2_5 F 0.8601(10) 0.8076(7) 0.7556(3) 0.042(2) Uani 1 1 d . U . . .
F3_5 F 0.8441(13) 0.9386(8) 0.7095(4) 0.064(3) Uani 1 1 d . U . . .
F4_5 F 1.0086(12) 0.8082(8) 0.6979(3) 0.047(2) Uani 1 1 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
Pd_1 C8_3 2.030(12) . ?
Pd_1 C8_4 2.029(12) . ?
Pd_1 C20B_2 2.147(12) . ?
Pd_1 C20A_2 2.147(12) . ?
Pd_1 C21A_2 2.16(2) . ?
Pd_1 C19A_2 2.165(18) . ?
Pd_1 C19B_2 2.165(18) . ?
Pd_1 C21B_2 2.21(2) . ?
C19A_2 C21A_2 1.361(17) . ?
C19A_2 H19A_2 0.9900 . ?
C19A_2 H19B_2 0.9900 . ?
C21A_2 C20A_2 1.343(16) . ?
C21A_2 H21A_2 0.9500 . ?
C20A_2 H20A_2 0.9900 . ?
C20A_2 H20B_2 0.9900 . ?
C19B_2 C21B_2 1.315(17) . ?
C19B_2 H19C_2 0.9900 . ?
C19B_2 H19D_2 0.9900 . ?
C21B_2 C20B_2 1.336(16) . ?
C21B_2 H21B_2 0.9500 . ?
C20B_2 H20C_2 0.9900 . ?
C20B_2 H20D_2 0.9900 . ?
C11_4 N3_4 1.489(14) . ?
C11_4 H11A_4 0.9800 . ?
C11_4 H11B_4 0.9800 . ?
C11_4 H11C_4 0.9800 . ?
N1_4 C2_4 1.3900 . ?
N1_4 C6_4 1.3900 . ?
N1_4 C10_4 1.453(14) . ?
C2_4 O2_4 1.225(12) . ?
C2_4 N3_4 1.3900 . ?
N3_4 C4_4 1.3900 . ?
C4_4 N9_4 1.346(12) . ?
C4_4 C5_4 1.3900 . ?
C5_4 N7_4 1.376(12) . ?
C5_4 C6_4 1.3900 . ?
C6_4 O6_4 1.308(10) . ?
C10_4 C14_4 1.515(16) . ?
C10_4 H10A_4 0.9900 . ?
C10_4 H10B_4 0.9900 . ?
C14_4 C19_4 1.3900 . ?
C14_4 C15_4 1.3900 . ?
C19_4 C18_4 1.3900 . ?
C19_4 H19_4 0.9500 . ?
C18_4 C17_4 1.3900 . ?
C18_4 H18_4 0.9500 . ?
C17_4 C16_4 1.3900 . ?
C17_4 H17_4 0.9500 . ?
C16_4 C15_4 1.3900 . ?
C16_4 H16_4 0.9500 . ?
C15_4 H15_4 0.9500 . ?
N9_4 C8_4 1.393(15) . ?
N9_4 C13_4 1.475(16) . ?
C13_4 H13A_4 0.9800 . ?
C13_4 H13B_4 0.9800 . ?
C13_4 H13C_4 0.9800 . ?
C8_4 N7_4 1.329(16) . ?
N7_4 C12_4 1.460(17) . ?
C12_4 H12A_4 0.9800 . ?
C12_4 H12B_4 0.9800 . ?
C12_4 H12C_4 0.9800 . ?
C11_3 N3_3 1.486(12) . ?
C11_3 H11A_3 0.9800 . ?
C11_3 H11C_3 0.9800 . ?
C11_3 H11B_3 0.9800 . ?
O2_3 C2_3 1.235(11) . ?
N1_3 C2_3 1.3900 . ?
N1_3 C6_3 1.3900 . ?
N1_3 C10_3 1.434(14) . ?
C2_3 N3_3 1.3900 . ?
N3_3 C4_3 1.3900 . ?
C4_3 N9_3 1.348(12) . ?
C4_3 C5_3 1.3900 . ?
C5_3 N7_3 1.360(12) . ?
C5_3 C6_3 1.3900 . ?
C6_3 O6_3 1.309(9) . ?
C10_3 C14_3 1.525(17) . ?
C10_3 H10B_3 0.9900 . ?
C10_3 H10A_3 0.9900 . ?
C14_3 C15_3 1.3900 . ?
C14_3 C19_3 1.3900 . ?
C15_3 C16_3 1.3900 . ?
C15_3 H15_3 0.9500 . ?
C16_3 C17_3 1.3900 . ?
C16_3 H16_3 0.9500 . ?
C17_3 C18_3 1.3900 . ?
C17_3 H17_3 0.9500 . ?
C18_3 C19_3 1.3900 . ?
C18_3 H18_3 0.9500 . ?
C19_3 H19_3 0.9500 . ?
N9_3 C8_3 1.394(16) . ?
N9_3 C13_3 1.455(15) . ?
C13_3 H13A_3 0.9800 . ?
C13_3 H13B_3 0.9800 . ?
C13_3 H13C_3 0.9800 . ?
C8_3 N7_3 1.349(15) . ?
N7_3 C12_3 1.474(14) . ?
C12_3 H12A_3 0.9800 . ?
C12_3 H12C_3 0.9800 . ?
C12_3 H12B_3 0.9800 . ?
B_5 F2_5 1.360(17) . ?
B_5 F4_5 1.381(19) . ?
B_5 F3_5 1.398(18) . ?
B_5 F1_5 1.426(18) . ?

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
C8_3 Pd_1 C8_4 98.1(5) . . ?
C8_3 Pd_1 C20B_2 99.0(5) . . ?
C8_4 Pd_1 C20B_2 162.8(5) . . ?
C8_3 Pd_1 C20A_2 99.0(5) . . ?
C8_4 Pd_1 C20A_2 162.8(5) . . ?
C8_3 Pd_1 C21A_2 130.6(5) . . ?
C8_4 Pd_1 C21A_2 128.4(5) . . ?
C20A_2 Pd_1 C21A_2 36.4(4) . . ?
C8_3 Pd_1 C19A_2 167.2(6) . . ?
C8_4 Pd_1 C19A_2 94.4(6) . . ?
C20A_2 Pd_1 C19A_2 68.6(6) . . ?
C21A_2 Pd_1 C19A_2 36.7(5) . . ?
C8_3 Pd_1 C19B_2 167.2(6) . . ?
C8_4 Pd_1 C19B_2 94.4(6) . . ?
C20B_2 Pd_1 C19B_2 68.6(6) . . ?
C8_3 Pd_1 C21B_2 133.6(5) . . ?
C8_4 Pd_1 C21B_2 127.1(5) . . ?
C20B_2 Pd_1 C21B_2 35.7(4) . . ?
C19B_2 Pd_1 C21B_2 35.0(4) . . ?
C21A_2 C19A_2 Pd_1 71.3(12) . . ?
C21A_2 C19A_2 H19A_2 116.5 . . ?
Pd_1 C19A_2 H19A_2 116.5 . . ?
C21A_2 C19A_2 H19B_2 116.5 . . ?
Pd_1 C19A_2 H19B_2 116.5 . . ?
H19A_2 C19A_2 H19B_2 113.5 . . ?
C20A_2 C21A_2 C19A_2 128.1(17) . . ?
C20A_2 C21A_2 Pd_1 71.4(11) . . ?
C19A_2 C21A_2 Pd_1 72.0(12) . . ?
C20A_2 C21A_2 H21A_2 115.9 . . ?
C19A_2 C21A_2 H21A_2 115.9 . . ?
Pd_1 C21A_2 H21A_2 135.8 . . ?
C21A_2 C20A_2 Pd_1 72.2(11) . . ?
C21A_2 C20A_2 H20A_2 116.4 . . ?
Pd_1 C20A_2 H20A_2 116.4 . . ?
C21A_2 C20A_2 H20B_2 116.4 . . ?
Pd_1 C20A_2 H20B_2 116.4 . . ?
H20A_2 C20A_2 H20B_2 113.3 . . ?
C21B_2 C19B_2 Pd_1 74.2(12) . . ?
C21B_2 C19B_2 H19C_2 116.1 . . ?
Pd_1 C19B_2 H19C_2 116.1 . . ?
C21B_2 C19B_2 H19D_2 116.1 . . ?
Pd_1 C19B_2 H19D_2 116.1 . . ?
H19C_2 C19B_2 H19D_2 113.1 . . ?
C19B_2 C21B_2 C20B_2 133.0(19) . . ?
C19B_2 C21B_2 Pd_1 70.8(13) . . ?
C20B_2 C21B_2 Pd_1 69.7(10) . . ?
C19B_2 C21B_2 H21B_2 113.5 . . ?
C20B_2 C21B_2 H21B_2 113.5 . . ?
Pd_1 C21B_2 H21B_2 148.1 . . ?
C21B_2 C20B_2 Pd_1 74.6(11) . . ?
C21B_2 C20B_2 H20C_2 116.0 . . ?
Pd_1 C20B_2 H20C_2 116.0 . . ?
C21B_2 C20B_2 H20D_2 116.0 . . ?
Pd_1 C20B_2 H20D_2 116.0 . . ?
H20C_2 C20B_2 H20D_2 113.0 . . ?
N3_4 C11_4 H11A_4 109.5 . . ?
N3_4 C11_4 H11B_4 109.5 . . ?
H11A_4 C11_4 H11B_4 109.5 . . ?
N3_4 C11_4 H11C_4 109.5 . . ?
H11A_4 C11_4 H11C_4 109.5 . . ?
H11B_4 C11_4 H11C_4 109.5 . . ?
C2_4 N1_4 C6_4 120.0 . . ?
C2_4 N1_4 C10_4 118.1(7) . . ?
C6_4 N1_4 C10_4 120.8(7) . . ?
O2_4 C2_4 N1_4 119.4(7) . . ?
O2_4 C2_4 N3_4 120.6(7) . . ?
N1_4 C2_4 N3_4 120.0 . . ?
C4_4 N3_4 C2_4 120.0 . . ?
C4_4 N3_4 C11_4 121.5(7) . . ?
C2_4 N3_4 C11_4 118.0(7) . . ?
N9_4 C4_4 N3_4 130.8(7) . . ?
N9_4 C4_4 C5_4 107.8(7) . . ?
N3_4 C4_4 C5_4 120.0 . . ?
N7_4 C5_4 C6_4 133.7(6) . . ?
N7_4 C5_4 C4_4 105.7(6) . . ?
C6_4 C5_4 C4_4 120.0 . . ?
O6_4 C6_4 C5_4 122.0(7) . . ?
O6_4 C6_4 N1_4 118.0(7) . . ?
C5_4 C6_4 N1_4 120.0 . . ?
N1_4 C10_4 C14_4 111.5(10) . . ?
N1_4 C10_4 H10A_4 109.3 . . ?
C14_4 C10_4 H10A_4 109.3 . . ?
N1_4 C10_4 H10B_4 109.3 . . ?
C14_4 C10_4 H10B_4 109.3 . . ?
H10A_4 C10_4 H10B_4 108.0 . . ?
C19_4 C14_4 C15_4 120.0 . . ?
C19_4 C14_4 C10_4 119.2(9) . . ?
C15_4 C14_4 C10_4 120.8(9) . . ?
C14_4 C19_4 C18_4 120.0 . . ?
C14_4 C19_4 H19_4 120.0 . . ?
C18_4 C19_4 H19_4 120.0 . . ?
C19_4 C18_4 C17_4 120.0 . . ?
C19_4 C18_4 H18_4 120.0 . . ?
C17_4 C18_4 H18_4 120.0 . . ?
C18_4 C17_4 C16_4 120.0 . . ?
C18_4 C17_4 H17_4 120.0 . . ?
C16_4 C17_4 H17_4 120.0 . . ?
C15_4 C16_4 C17_4 120.0 . . ?
C15_4 C16_4 H16_4 120.0 . . ?
C17_4 C16_4 H16_4 120.0 . . ?
C16_4 C15_4 C14_4 120.0 . . ?
C16_4 C15_4 H15_4 120.0 . . ?
C14_4 C15_4 H15_4 120.0 . . ?
C4_4 N9_4 C8_4 109.1(9) . . ?
C4_4 N9_4 C13_4 128.8(11) . . ?
C8_4 N9_4 C13_4 122.0(12) . . ?
N9_4 C13_4 H13A_4 109.5 . . ?
N9_4 C13_4 H13B_4 109.5 . . ?
H13A_4 C13_4 H13B_4 109.5 . . ?
N9_4 C13_4 H13C_4 109.5 . . ?
H13A_4 C13_4 H13C_4 109.5 . . ?
H13B_4 C13_4 H13C_4 109.5 . . ?
N7_4 C8_4 N9_4 106.2(10) . . ?
N7_4 C8_4 Pd_1 127.6(9) . . ?
N9_4 C8_4 Pd_1 126.0(9) . . ?
C8_4 N7_4 C5_4 110.9(9) . . ?
C8_4 N7_4 C12_4 123.9(11) . . ?
C5_4 N7_4 C12_4 125.0(10) . . ?
N7_4 C12_4 H12A_4 109.5 . . ?
N7_4 C12_4 H12B_4 109.5 . . ?
H12A_4 C12_4 H12B_4 109.5 . . ?
N7_4 C12_4 H12C_4 109.5 . . ?
H12A_4 C12_4 H12C_4 109.5 . . ?
H12B_4 C12_4 H12C_4 109.5 . . ?
N3_3 C11_3 H11A_3 109.5 . . ?
N3_3 C11_3 H11C_3 109.5 . . ?
H11A_3 C11_3 H11C_3 109.5 . . ?
N3_3 C11_3 H11B_3 109.5 . . ?
H11A_3 C11_3 H11B_3 109.5 . . ?
H11C_3 C11_3 H11B_3 109.5 . . ?
C2_3 N1_3 C6_3 120.0 . . ?
C2_3 N1_3 C10_3 117.7(7) . . ?
C6_3 N1_3 C10_3 122.2(7) . . ?
O2_3 C2_3 N1_3 120.3(6) . . ?
O2_3 C2_3 N3_3 119.7(6) . . ?
N1_3 C2_3 N3_3 120.0 . . ?
C4_3 N3_3 C2_3 120.0 . . ?
C4_3 N3_3 C11_3 122.7(7) . . ?
C2_3 N3_3 C11_3 117.3(7) . . ?
N9_3 C4_3 N3_3 132.5(6) . . ?
N9_3 C4_3 C5_3 107.5(6) . . ?
N3_3 C4_3 C5_3 120.0 . . ?
N7_3 C5_3 C4_3 105.8(6) . . ?
N7_3 C5_3 C6_3 134.2(6) . . ?
C4_3 C5_3 C6_3 120.0 . . ?
O6_3 C6_3 C5_3 122.3(6) . . ?
O6_3 C6_3 N1_3 117.6(6) . . ?
C5_3 C6_3 N1_3 120.0 . . ?
N1_3 C10_3 C14_3 112.3(11) . . ?
N1_3 C10_3 H10B_3 109.1 . . ?
C14_3 C10_3 H10B_3 109.1 . . ?
N1_3 C10_3 H10A_3 109.1 . . ?
C14_3 C10_3 H10A_3 109.1 . . ?
H10B_3 C10_3 H10A_3 107.9 . . ?
C15_3 C14_3 C19_3 120.0 . . ?
C15_3 C14_3 C10_3 121.3(8) . . ?
C19_3 C14_3 C10_3 118.4(8) . . ?
C14_3 C15_3 C16_3 120.0 . . ?
C14_3 C15_3 H15_3 120.0 . . ?
C16_3 C15_3 H15_3 120.0 . . ?
C15_3 C16_3 C17_3 120.0 . . ?
C15_3 C16_3 H16_3 120.0 . . ?
C17_3 C16_3 H16_3 120.0 . . ?
C18_3 C17_3 C16_3 120.0 . . ?
C18_3 C17_3 H17_3 120.0 . . ?
C16_3 C17_3 H17_3 120.0 . . ?
C17_3 C18_3 C19_3 120.0 . . ?
C17_3 C18_3 H18_3 120.0 . . ?
C19_3 C18_3 H18_3 120.0 . . ?
C18_3 C19_3 C14_3 120.0 . . ?
C18_3 C19_3 H19_3 120.0 . . ?
C14_3 C19_3 H19_3 120.0 . . ?
C4_3 N9_3 C8_3 110.2(9) . . ?
C4_3 N9_3 C13_3 129.6(10) . . ?
C8_3 N9_3 C13_3 120.1(11) . . ?
N9_3 C13_3 H13A_3 109.5 . . ?
N9_3 C13_3 H13B_3 109.5 . . ?
H13A_3 C13_3 H13B_3 109.5 . . ?
N9_3 C13_3 H13C_3 109.5 . . ?
H13A_3 C13_3 H13C_3 109.5 . . ?
H13B_3 C13_3 H13C_3 109.5 . . ?
N7_3 C8_3 N9_3 104.2(10) . . ?
N7_3 C8_3 Pd_1 126.5(9) . . ?
N9_3 C8_3 Pd_1 129.2(9) . . ?
C8_3 N7_3 C5_3 112.2(9) . . ?
C8_3 N7_3 C12_3 123.3(10) . . ?
C5_3 N7_3 C12_3 124.5(9) . . ?
N7_3 C12_3 H12A_3 109.5 . . ?
N7_3 C12_3 H12C_3 109.5 . . ?
H12A_3 C12_3 H12C_3 109.5 . . ?
N7_3 C12_3 H12B_3 109.5 . . ?
H12A_3 C12_3 H12B_3 109.5 . . ?
H12C_3 C12_3 H12B_3 109.5 . . ?
F2_5 B_5 F4_5 111.5(12) . . ?
F2_5 B_5 F3_5 110.7(12) . . ?
F4_5 B_5 F3_5 110.4(14) . . ?
F2_5 B_5 F1_5 108.2(14) . . ?
F4_5 B_5 F1_5 108.2(12) . . ?
F3_5 B_5 F1_5 107.7(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
Pd_1 C19A_2 C21A_2 C20A_2 47(2) . . . . ?
C19A_2 C21A_2 C20A_2 Pd_1 -47(2) . . . . ?
Pd_1 C19B_2 C21B_2 C20B_2 -34(2) . . . . ?
C19B_2 C21B_2 C20B_2 Pd_1 34(3) . . . . ?
C6_4 N1_4 C2_4 O2_4 -179.6(10) . . . . ?
C10_4 N1_4 C2_4 O2_4 12.6(11) . . . . ?
C6_4 N1_4 C2_4 N3_4 0.0 . . . . ?
C10_4 N1_4 C2_4 N3_4 -167.8(9) . . . . ?
O2_4 C2_4 N3_4 C4_4 179.6(10) . . . . ?
N1_4 C2_4 N3_4 C4_4 0.0 . . . . ?
O2_4 C2_4 N3_4 C11_4 7.0(11) . . . . ?
N1_4 C2_4 N3_4 C11_4 -172.6(10) . . . . ?
C2_4 N3_4 C4_4 N9_4 164.9(11) . . . . ?
C11_4 N3_4 C4_4 N9_4 -22.8(13) . . . . ?
C2_4 N3_4 C4_4 C5_4 0.0 . . . . ?
C11_4 N3_4 C4_4 C5_4 172.4(10) . . . . ?
N9_4 C4_4 C5_4 N7_4 4.6(9) . . . . ?
N3_4 C4_4 C5_4 N7_4 172.6(8) . . . . ?
N9_4 C4_4 C5_4 C6_4 -168.0(8) . . . . ?
N3_4 C4_4 C5_4 C6_4 0.0 . . . . ?
N7_4 C5_4 C6_4 O6_4 8.7(12) . . . . ?
C4_4 C5_4 C6_4 O6_4 178.9(10) . . . . ?
N7_4 C5_4 C6_4 N1_4 -170.2(11) . . . . ?
C4_4 C5_4 C6_4 N1_4 0.0 . . . . ?
C2_4 N1_4 C6_4 O6_4 -178.9(10) . . . . ?
C10_4 N1_4 C6_4 O6_4 -11.4(11) . . . . ?
C2_4 N1_4 C6_4 C5_4 0.0 . . . . ?
C10_4 N1_4 C6_4 C5_4 167.5(9) . . . . ?
C2_4 N1_4 C10_4 C14_4 76.1(11) . . . . ?
C6_4 N1_4 C10_4 C14_4 -91.6(11) . . . . ?
N1_4 C10_4 C14_4 C19_4 -104.5(10) . . . . ?
N1_4 C10_4 C14_4 C15_4 73.8(12) . . . . ?
C15_4 C14_4 C19_4 C18_4 0.0 . . . . ?
C10_4 C14_4 C19_4 C18_4 178.3(11) . . . . ?
C14_4 C19_4 C18_4 C17_4 0.0 . . . . ?
C19_4 C18_4 C17_4 C16_4 0.0 . . . . ?
C18_4 C17_4 C16_4 C15_4 0.0 . . . . ?
C17_4 C16_4 C15_4 C14_4 0.0 . . . . ?
C19_4 C14_4 C15_4 C16_4 0.0 . . . . ?
C10_4 C14_4 C15_4 C16_4 -178.3(11) . . . . ?
N3_4 C4_4 N9_4 C8_4 -170.4(8) . . . . ?
C5_4 C4_4 N9_4 C8_4 -4.1(11) . . . . ?
N3_4 C4_4 N9_4 C13_4 6.1(19) . . . . ?
C5_4 C4_4 N9_4 C13_4 172.4(12) . . . . ?
C4_4 N9_4 C8_4 N7_4 2.0(14) . . . . ?
C13_4 N9_4 C8_4 N7_4 -174.8(12) . . . . ?
C4_4 N9_4 C8_4 Pd_1 177.1(8) . . . . ?
C13_4 N9_4 C8_4 Pd_1 0.3(18) . . . . ?
N9_4 C8_4 N7_4 C5_4 1.0(14) . . . . ?
Pd_1 C8_4 N7_4 C5_4 -174.0(8) . . . . ?
N9_4 C8_4 N7_4 C12_4 177.7(12) . . . . ?
Pd_1 C8_4 N7_4 C12_4 2.7(19) . . . . ?
C6_4 C5_4 N7_4 C8_4 167.7(8) . . . . ?
C4_4 C5_4 N7_4 C8_4 -3.5(11) . . . . ?
C6_4 C5_4 N7_4 C12_4 -9.0(17) . . . . ?
C4_4 C5_4 N7_4 C12_4 179.9(11) . . . . ?
C6_3 N1_3 C2_3 O2_3 178.6(10) . . . . ?
C10_3 N1_3 C2_3 O2_3 2.0(11) . . . . ?
C6_3 N1_3 C2_3 N3_3 0.0 . . . . ?
C10_3 N1_3 C2_3 N3_3 -176.6(10) . . . . ?
O2_3 C2_3 N3_3 C4_3 -178.6(10) . . . . ?
N1_3 C2_3 N3_3 C4_3 0.0 . . . . ?
O2_3 C2_3 N3_3 C11_3 -0.3(11) . . . . ?
N1_3 C2_3 N3_3 C11_3 178.3(10) . . . . ?
C2_3 N3_3 C4_3 N9_3 177.0(11) . . . . ?
C11_3 N3_3 C4_3 N9_3 -1.2(13) . . . . ?
C2_3 N3_3 C4_3 C5_3 0.0 . . . . ?
C11_3 N3_3 C4_3 C5_3 -178.2(10) . . . . ?
N9_3 C4_3 C5_3 N7_3 2.8(9) . . . . ?
N3_3 C4_3 C5_3 N7_3 -179.5(8) . . . . ?
N9_3 C4_3 C5_3 C6_3 -177.7(9) . . . . ?
N3_3 C4_3 C5_3 C6_3 0.0 . . . . ?
N7_3 C5_3 C6_3 O6_3 -2.5(12) . . . . ?
C4_3 C5_3 C6_3 O6_3 178.2(9) . . . . ?
N7_3 C5_3 C6_3 N1_3 179.3(11) . . . . ?
C4_3 C5_3 C6_3 N1_3 0.0 . . . . ?
C2_3 N1_3 C6_3 O6_3 -178.3(9) . . . . ?
C10_3 N1_3 C6_3 O6_3 -1.9(11) . . . . ?
C2_3 N1_3 C6_3 C5_3 0.0 . . . . ?
C10_3 N1_3 C6_3 C5_3 176.4(10) . . . . ?
C2_3 N1_3 C10_3 C14_3 -83.5(10) . . . . ?
C6_3 N1_3 C10_3 C14_3 100.0(11) . . . . ?
N1_3 C10_3 C14_3 C15_3 -42.0(13) . . . . ?
N1_3 C10_3 C14_3 C19_3 144.2(8) . . . . ?
C19_3 C14_3 C15_3 C16_3 0.0 . . . . ?
C10_3 C14_3 C15_3 C16_3 -173.7(10) . . . . ?
C14_3 C15_3 C16_3 C17_3 0.0 . . . . ?
C15_3 C16_3 C17_3 C18_3 0.0 . . . . ?
C16_3 C17_3 C18_3 C19_3 0.0 . . . . ?
C17_3 C18_3 C19_3 C14_3 0.0 . . . . ?
C15_3 C14_3 C19_3 C18_3 0.0 . . . . ?
C10_3 C14_3 C19_3 C18_3 173.9(10) . . . . ?
N3_3 C4_3 N9_3 C8_3 179.0(8) . . . . ?
C5_3 C4_3 N9_3 C8_3 -3.7(12) . . . . ?
N3_3 C4_3 N9_3 C13_3 3(2) . . . . ?
C5_3 C4_3 N9_3 C13_3 -180.0(12) . . . . ?
C4_3 N9_3 C8_3 N7_3 3.1(14) . . . . ?
C13_3 N9_3 C8_3 N7_3 179.7(12) . . . . ?
C4_3 N9_3 C8_3 Pd_1 -175.2(9) . . . . ?
C13_3 N9_3 C8_3 Pd_1 1.4(19) . . . . ?
N9_3 C8_3 N7_3 C5_3 -1.2(14) . . . . ?
Pd_1 C8_3 N7_3 C5_3 177.1(8) . . . . ?
N9_3 C8_3 N7_3 C12_3 179.6(12) . . . . ?
Pd_1 C8_3 N7_3 C12_3 -2.0(19) . . . . ?
C4_3 C5_3 N7_3 C8_3 -1.0(12) . . . . ?
C6_3 C5_3 N7_3 C8_3 179.7(8) . . . . ?
C4_3 C5_3 N7_3 C12_3 178.2(10) . . . . ?
C6_3 C5_3 N7_3 C12_3 -1.2(17) . . . . ?

_refine_diff_density_max         3.950
_refine_diff_density_min         -4.426
_refine_diff_density_rms         0.262

####################################################################### 
# 
# 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_4a
_database_code_depnum_ccdc_archive 'CCDC 1825948'
_audit_update_record             
;
2018-02-26 deposited with the CCDC.
2018-08-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H32 N4 O2 P Pd, B F4, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C30.50 H33 B Cl F4 N4 O2 P Pd'
_chemical_formula_weight         747.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0015 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1001 0.0923 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -1.0140 0.9845 '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'
Cl Cl 0.1456 0.1550 '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                   8.818(2)
_cell_length_b                   15.614(3)
_cell_length_c                   23.329(5)
_cell_angle_alpha                90
_cell_angle_beta                 94.90(3)
_cell_angle_gamma                90
_cell_volume                     3200.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7063
_cell_measurement_theta_min      1.547
_cell_measurement_theta_max      29.085

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_F_000             1516
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.731
_shelx_estimated_absorpt_T_min   0.810
_shelx_estimated_absorpt_T_max   0.964
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.700

_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_measurement_device_type  
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38281
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.547
_diffrn_reflns_theta_max         29.085
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             8782
_reflns_number_gt                8453
_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.
;

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_decay_%        0

_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_molecular_graphics    'Ortep3 for Windows - Coot'
_computing_publication_material  'enCIFer - publCIF'

_refine_special_details          
;
Hydrogen atoms were included at calculated positions with isotropic 
Ufactors=1.2Ueq (Ufactors=1.5Ueq for methyl groups). Anisotropic 
thermal motion modeling has been applied to all atoms. Geometric 
restrains (DFIX, DANG, SADI) have been used to model disordered BF4 ion
and DCM solvent molecule.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0357P)²+3.1753P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8782
_refine_ls_number_parameters     449
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0276
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0706
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      1.000
_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
Pd_1 Pd 0.83983(2) 0.52433(2) 0.36456(2) 0.01409(4) Uani 1 1 d . . . . .
C19A_2 C 0.8465(4) 0.66047(12) 0.34468(10) 0.0515(7) Uani 0.5 1 d D . P A 1
H19A_2 H 0.945261 0.683390 0.334396 0.062 Uiso 0.5 1 calc R U P A 1
H19B_2 H 0.758017 0.683747 0.320655 0.062 Uiso 0.5 1 calc R U P A 1
C21A_2 C 0.8309(5) 0.6525(2) 0.39793(17) 0.0341(9) Uani 0.5 1 d D . P A 1
H21A_2 H 0.753287 0.686943 0.411947 0.041 Uiso 0.5 1 calc R U P A 1
C20A_2 C 0.9097(2) 0.60109(11) 0.43890(7) 0.0280(3) Uani 0.5 1 d D . P A 1
H20A_2 H 0.858716 0.589105 0.474241 0.034 Uiso 0.5 1 calc R U P A 1
H20B_2 H 1.020198 0.612146 0.446263 0.034 Uiso 0.5 1 calc R U P A 1
C19B_2 C 0.8465(4) 0.66047(12) 0.34468(10) 0.0515(7) Uani 0.5 1 d D . P A 2
H19C_2 H 0.893550 0.676360 0.309142 0.062 Uiso 0.5 1 calc R U P A 2
H19D_2 H 0.753377 0.693654 0.350530 0.062 Uiso 0.5 1 calc R U P A 2
C21B_2 C 0.9395(4) 0.64700(19) 0.39026(14) 0.0218(6) Uani 0.5 1 d D . P A 2
H21B_2 H 1.038335 0.671230 0.390127 0.026 Uiso 0.5 1 calc R U P A 2
C20B_2 C 0.9097(2) 0.60109(11) 0.43890(7) 0.0280(3) Uani 0.5 1 d D . P A 2
H20C_2 H 0.827383 0.623414 0.461074 0.034 Uiso 0.5 1 calc R U P A 2
H20D_2 H 0.999347 0.580448 0.463480 0.034 Uiso 0.5 1 calc R U P A 2
C18_4 C 1.03990(18) 0.48412(10) 0.23874(7) 0.0208(3) Uani 1 1 d . . . . .
H18_4 H 1.048836 0.531170 0.264626 0.025 Uiso 1 1 calc R U . . .
C17_4 C 1.1587(2) 0.46449(12) 0.20528(8) 0.0293(4) Uani 1 1 d . . . . .
H17_4 H 1.247743 0.499030 0.207817 0.035 Uiso 1 1 calc R U . . .
C16_4 C 1.1478(2) 0.39496(14) 0.16838(8) 0.0326(4) Uani 1 1 d . . . . .
H16_4 H 1.229826 0.381624 0.146017 0.039 Uiso 1 1 calc R U . . .
C15_4 C 1.0178(2) 0.34467(12) 0.16391(7) 0.0293(3) Uani 1 1 d . . . . .
H15_4 H 1.010929 0.296718 0.138754 0.035 Uiso 1 1 calc R U . . .
C14_4 C 0.89707(19) 0.36464(10) 0.19639(6) 0.0212(3) Uani 1 1 d . . . . .
H14_4 H 0.807323 0.330722 0.192878 0.025 Uiso 1 1 calc R U . . .
C13_4 C 0.90746(16) 0.43446(9) 0.23417(6) 0.0157(2) Uani 1 1 d . . . . .
P_4 P 0.75435(4) 0.46437(2) 0.27750(2) 0.01281(7) Uani 1 1 d . . . . .
C7_4 C 0.62592(17) 0.53030(8) 0.23075(6) 0.0151(2) Uani 1 1 d . . . . .
C8_4 C 0.54498(18) 0.59487(10) 0.25548(7) 0.0211(3) Uani 1 1 d . . . . .
H8_4 H 0.558412 0.604086 0.295847 0.025 Uiso 1 1 calc R U . . .
C9_4 C 0.4443(2) 0.64616(11) 0.22149(8) 0.0263(3) Uani 1 1 d . . . . .
H9_4 H 0.389917 0.690414 0.238747 0.032 Uiso 1 1 calc R U . . .
C10_4 C 0.42312(19) 0.63301(11) 0.16281(7) 0.0256(3) Uani 1 1 d . . . . .
H10_4 H 0.354350 0.668071 0.139694 0.031 Uiso 1 1 calc R U . . .
C11_4 C 0.5026(2) 0.56848(13) 0.13789(7) 0.0297(4) Uani 1 1 d . . . . .
H11_4 H 0.488097 0.559203 0.097546 0.036 Uiso 1 1 calc R U . . .
C12_4 C 0.6040(2) 0.51699(11) 0.17163(7) 0.0244(3) Uani 1 1 d . . . . .
H12_4 H 0.658131 0.472765 0.154240 0.029 Uiso 1 1 calc R U . . .
C1_4 C 0.64872(16) 0.36542(9) 0.28535(6) 0.0149(2) Uani 1 1 d . . . . .
C2_4 C 0.72571(18) 0.29169(9) 0.30579(6) 0.0179(3) Uani 1 1 d . . . . .
H2_4 H 0.833508 0.292328 0.312440 0.021 Uiso 1 1 calc R U . . .
C3_4 C 0.6455(2) 0.21749(10) 0.31645(7) 0.0242(3) Uani 1 1 d . . . . .
H3_4 H 0.698489 0.167734 0.330449 0.029 Uiso 1 1 calc R U . . .
C4_4 C 0.4882(2) 0.21617(11) 0.30662(8) 0.0302(4) Uani 1 1 d . . . . .
H4_4 H 0.433230 0.165517 0.313768 0.036 Uiso 1 1 calc R U . . .
C5_4 C 0.4115(2) 0.28907(12) 0.28632(9) 0.0325(4) Uani 1 1 d . . . . .
H5_4 H 0.303780 0.288061 0.279465 0.039 Uiso 1 1 calc R U . . .
C6_4 C 0.49093(18) 0.36365(10) 0.27591(8) 0.0241(3) Uani 1 1 d . . . . .
H6_4 H 0.437297 0.413427 0.262346 0.029 Uiso 1 1 calc R U . . .
C11_3 C 0.6161(3) 0.22376(15) 0.50295(12) 0.0553(7) Uani 1 1 d . . . . .
H11A_3 H 0.587874 0.273878 0.524978 0.083 Uiso 1 1 calc R U . . .
H11B_3 H 0.599469 0.171594 0.524911 0.083 Uiso 1 1 calc R U . . .
H11C_3 H 0.553425 0.221845 0.466207 0.083 Uiso 1 1 calc R U . . .
N3_3 N 0.7777(2) 0.22972(10) 0.49206(6) 0.0334(4) Uani 1 1 d . . . . .
C2_3 C 0.8770(3) 0.16804(12) 0.51616(8) 0.0407(5) Uani 1 1 d . . . . .
O2_3 O 0.8337(3) 0.11063(11) 0.54638(7) 0.0622(6) Uani 1 1 d . . . . .
N1_3 N 1.0282(2) 0.17356(10) 0.50452(7) 0.0376(4) Uani 1 1 d . . . . .
C10_3 C 1.1324(4) 0.10974(15) 0.53269(12) 0.0639(9) Uani 1 1 d . . . . .
H10A_3 H 1.235406 0.133721 0.537909 0.096 Uiso 1 1 calc R U . . .
H10B_3 H 1.133127 0.058308 0.508637 0.096 Uiso 1 1 calc R U . . .
H10C_3 H 1.098191 0.094708 0.570272 0.096 Uiso 1 1 calc R U . . .
C6_3 C 1.0931(2) 0.23374(11) 0.46933(7) 0.0280(4) Uani 1 1 d . . . . .
O6_3 O 1.22786(18) 0.23214(9) 0.46123(6) 0.0377(3) Uani 1 1 d . . . . .
C5_3 C 0.98198(19) 0.29397(9) 0.44629(6) 0.0207(3) Uani 1 1 d . . . . .
C4_3 C 0.8346(2) 0.29272(10) 0.45904(6) 0.0228(3) Uani 1 1 d . . . . .
N9_3 N 0.76524(16) 0.36445(9) 0.43460(5) 0.0203(2) Uani 1 1 d . . . . .
C13_3 C 0.6058(2) 0.39217(13) 0.43411(8) 0.0298(4) Uani 1 1 d . . . . .
H13A_3 H 0.539814 0.350065 0.413210 0.045 Uiso 1 1 calc R U . . .
H13B_3 H 0.593624 0.447984 0.415058 0.045 Uiso 1 1 calc R U . . .
H13C_3 H 0.577775 0.396950 0.473737 0.045 Uiso 1 1 calc R U . . .
C8_3 C 0.86928(17) 0.41062(9) 0.40671(6) 0.0167(3) Uani 1 1 d . . . . .
N7_3 N 1.00066(15) 0.36747(8) 0.41403(5) 0.0172(2) Uani 1 1 d . . . . .
C12_3 C 1.14281(19) 0.39472(11) 0.39182(7) 0.0252(3) Uani 1 1 d . . . . .
H12A_3 H 1.181924 0.348514 0.368769 0.038 Uiso 1 1 calc R U . . .
H12B_3 H 1.217701 0.408208 0.424034 0.038 Uiso 1 1 calc R U . . .
H12C_3 H 1.124217 0.445719 0.367763 0.038 Uiso 1 1 calc R U . . .
BA_5 B 0.3537(4) 0.5951(2) 0.38457(15) 0.0345(7) Uani 0.8 1 d D . P B 1
F1A_5 F 0.2774(4) 0.6500(2) 0.34803(14) 0.1137(14) Uani 0.8 1 d D . P B 1
F2A_5 F 0.3769(2) 0.51887(11) 0.35812(9) 0.0520(5) Uani 0.8 1 d D . P B 1
F3A_5 F 0.4902(4) 0.6323(3) 0.40006(19) 0.1085(19) Uani 0.8 1 d D . P B 1
F4A_5 F 0.2726(3) 0.58498(18) 0.43375(11) 0.0367(5) Uani 0.8 1 d D . P B 1
BB_5 B 0.3294(15) 0.6156(9) 0.3901(6) 0.034(4) Uiso 0.2 1 d D . P C 2
F1B_5 F 0.2543(9) 0.6918(5) 0.3871(4) 0.0582(19) Uiso 0.2 1 d D . P C 2
F2B_5 F 0.2758(8) 0.5679(5) 0.3430(3) 0.0457(15) Uiso 0.2 1 d D . P C 2
F3B_5 F 0.4956(12) 0.6195(8) 0.3942(5) 0.047(2) Uiso 0.2 1 d D . P C 2
F4B_5 F 0.2977(12) 0.5668(6) 0.4389(4) 0.030(2) Uiso 0.2 1 d D . P C 2
C1A_11 C 1.0701(4) 0.5386(2) 0.04397(13) 0.0293(7) Uani 0.5 1 d D . P D -1
H1A1_11 H 1.139652 0.494898 0.062357 0.035 Uiso 0.5 1 calc R U P D -1
H1A2_11 H 1.124022 0.594238 0.045586 0.035 Uiso 0.5 1 calc R U P D -1
Cl2A_11 Cl 1.02063(12) 0.50994(6) -0.02920(4) 0.03425(19) Uani 0.5 1 d D . P D
-1
Cl1A_11 Cl 0.90419(11) 0.54622(6) 0.08218(4) 0.03010(17) Uani 0.5 1 d D . P D
-1


_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
Pd_1 C8_3 2.0354(15) . ?
Pd_1 C21A_2 2.151(3) . ?
Pd_1 C20B_2 2.1543(16) . ?
Pd_1 C20A_2 2.1543(16) . ?
Pd_1 C21B_2 2.171(3) . ?
Pd_1 C19A_2 2.178(2) . ?
Pd_1 C19B_2 2.178(2) . ?
Pd_1 P_4 2.3041(6) . ?
C19A_2 C21A_2 1.268(5) . ?
C19A_2 H19A_2 0.9900 . ?
C19A_2 H19B_2 0.9900 . ?
C21A_2 C20A_2 1.388(4) . ?
C21A_2 H21A_2 0.9500 . ?
C20A_2 H20A_2 0.9900 . ?
C20A_2 H20B_2 0.9900 . ?
C19B_2 C21B_2 1.303(4) . ?
C19B_2 H19C_2 0.9900 . ?
C19B_2 H19D_2 0.9900 . ?
C21B_2 C20B_2 1.386(4) . ?
C21B_2 H21B_2 0.9500 . ?
C20B_2 H20C_2 0.9900 . ?
C20B_2 H20D_2 0.9900 . ?
C18_4 C17_4 1.393(2) . ?
C18_4 C13_4 1.398(2) . ?
C18_4 H18_4 0.9500 . ?
C17_4 C16_4 1.384(3) . ?
C17_4 H17_4 0.9500 . ?
C16_4 C15_4 1.387(3) . ?
C16_4 H16_4 0.9500 . ?
C15_4 C14_4 1.393(2) . ?
C15_4 H15_4 0.9500 . ?
C14_4 C13_4 1.400(2) . ?
C14_4 H14_4 0.9500 . ?
C13_4 P_4 1.8153(16) . ?
P_4 C1_4 1.8214(14) . ?
P_4 C7_4 1.8223(15) . ?
C7_4 C8_4 1.389(2) . ?
C7_4 C12_4 1.392(2) . ?
C8_4 C9_4 1.392(2) . ?
C8_4 H8_4 0.9500 . ?
C9_4 C10_4 1.381(2) . ?
C9_4 H9_4 0.9500 . ?
C10_4 C11_4 1.384(3) . ?
C10_4 H10_4 0.9500 . ?
C11_4 C12_4 1.394(2) . ?
C11_4 H11_4 0.9500 . ?
C12_4 H12_4 0.9500 . ?
C1_4 C6_4 1.390(2) . ?
C1_4 C2_4 1.3995(19) . ?
C2_4 C3_4 1.391(2) . ?
C2_4 H2_4 0.9500 . ?
C3_4 C4_4 1.386(3) . ?
C3_4 H3_4 0.9500 . ?
C4_4 C5_4 1.387(3) . ?
C4_4 H4_4 0.9500 . ?
C5_4 C6_4 1.391(2) . ?
C5_4 H5_4 0.9500 . ?
C6_4 H6_4 0.9500 . ?
C11_3 N3_3 1.472(3) . ?
C11_3 H11A_3 0.9800 . ?
C11_3 H11B_3 0.9800 . ?
C11_3 H11C_3 0.9800 . ?
N3_3 C4_3 1.371(2) . ?
N3_3 C2_3 1.388(3) . ?
C2_3 O2_3 1.222(2) . ?
C2_3 N1_3 1.386(3) . ?
N1_3 C6_3 1.402(3) . ?
N1_3 C10_3 1.472(3) . ?
C10_3 H10A_3 0.9800 . ?
C10_3 H10B_3 0.9800 . ?
C10_3 H10C_3 0.9800 . ?
C6_3 O6_3 1.219(3) . ?
C6_3 C5_3 1.430(2) . ?
C5_3 C4_3 1.358(2) . ?
C5_3 N7_3 1.3898(19) . ?
C4_3 N9_3 1.376(2) . ?
N9_3 C8_3 1.3736(19) . ?
N9_3 C13_3 1.470(2) . ?
C13_3 H13A_3 0.9800 . ?
C13_3 H13B_3 0.9800 . ?
C13_3 H13C_3 0.9800 . ?
C8_3 N7_3 1.3384(19) . ?
N7_3 C12_3 1.460(2) . ?
C12_3 H12A_3 0.9800 . ?
C12_3 H12B_3 0.9800 . ?
C12_3 H12C_3 0.9800 . ?
BA_5 F1A_5 1.348(4) . ?
BA_5 F2A_5 1.364(4) . ?
BA_5 F3A_5 1.357(4) . ?
BA_5 F4A_5 1.412(4) . ?
BB_5 F1B_5 1.362(13) . ?
BB_5 F2B_5 1.378(14) . ?
BB_5 F4B_5 1.415(13) . ?
BB_5 F3B_5 1.462(14) . ?
C1A_11 Cl1A_11 1.781(3) . ?
C1A_11 Cl2A_11 1.782(3) . ?
C1A_11 H1A1_11 0.9900 . ?
C1A_11 H1A2_11 0.9900 . ?

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
C8_3 Pd_1 C21A_2 130.08(12) . . ?
C8_3 Pd_1 C20B_2 94.62(7) . . ?
C8_3 Pd_1 C20A_2 94.62(7) . . ?
C21A_2 Pd_1 C20A_2 37.63(11) . . ?
C8_3 Pd_1 C21B_2 127.19(10) . . ?
C20B_2 Pd_1 C21B_2 37.39(10) . . ?
C8_3 Pd_1 C19A_2 161.76(7) . . ?
C21A_2 Pd_1 C19A_2 34.05(13) . . ?
C20A_2 Pd_1 C19A_2 67.50(8) . . ?
C8_3 Pd_1 C19B_2 161.76(7) . . ?
C20B_2 Pd_1 C19B_2 67.50(8) . . ?
C21B_2 Pd_1 C19B_2 34.89(10) . . ?
C8_3 Pd_1 P_4 95.17(4) . . ?
C21A_2 Pd_1 P_4 132.66(11) . . ?
C20B_2 Pd_1 P_4 170.14(5) . . ?
C20A_2 Pd_1 P_4 170.14(5) . . ?
C21B_2 Pd_1 P_4 134.13(9) . . ?
C19A_2 Pd_1 P_4 102.80(6) . . ?
C19B_2 Pd_1 P_4 102.80(6) . . ?
C21A_2 C19A_2 Pd_1 71.82(18) . . ?
C21A_2 C19A_2 H19A_2 116.4 . . ?
Pd_1 C19A_2 H19A_2 116.4 . . ?
C21A_2 C19A_2 H19B_2 116.4 . . ?
Pd_1 C19A_2 H19B_2 116.4 . . ?
H19A_2 C19A_2 H19B_2 113.4 . . ?
C19A_2 C21A_2 C20A_2 129.9(3) . . ?
C19A_2 C21A_2 Pd_1 74.13(17) . . ?
C20A_2 C21A_2 Pd_1 71.32(16) . . ?
C19A_2 C21A_2 H21A_2 115.0 . . ?
C20A_2 C21A_2 H21A_2 115.0 . . ?
Pd_1 C21A_2 H21A_2 134.5 . . ?
C21A_2 C20A_2 Pd_1 71.05(15) . . ?
C21A_2 C20A_2 H20A_2 116.5 . . ?
Pd_1 C20A_2 H20A_2 116.5 . . ?
C21A_2 C20A_2 H20B_2 116.5 . . ?
Pd_1 C20A_2 H20B_2 116.5 . . ?
H20A_2 C20A_2 H20B_2 113.5 . . ?
C21B_2 C19B_2 Pd_1 72.26(16) . . ?
C21B_2 C19B_2 H19C_2 116.3 . . ?
Pd_1 C19B_2 H19C_2 116.3 . . ?
C21B_2 C19B_2 H19D_2 116.3 . . ?
Pd_1 C19B_2 H19D_2 116.3 . . ?
H19C_2 C19B_2 H19D_2 113.3 . . ?
C19B_2 C21B_2 C20B_2 126.9(3) . . ?
C19B_2 C21B_2 Pd_1 72.85(15) . . ?
C20B_2 C21B_2 Pd_1 70.67(14) . . ?
C19B_2 C21B_2 H21B_2 116.5 . . ?
C20B_2 C21B_2 H21B_2 116.5 . . ?
Pd_1 C21B_2 H21B_2 134.5 . . ?
C21B_2 C20B_2 Pd_1 71.94(13) . . ?
C21B_2 C20B_2 H20C_2 116.4 . . ?
Pd_1 C20B_2 H20C_2 116.4 . . ?
C21B_2 C20B_2 H20D_2 116.4 . . ?
Pd_1 C20B_2 H20D_2 116.4 . . ?
H20C_2 C20B_2 H20D_2 113.4 . . ?
C17_4 C18_4 C13_4 119.91(15) . . ?
C17_4 C18_4 H18_4 120.0 . . ?
C13_4 C18_4 H18_4 120.0 . . ?
C16_4 C17_4 C18_4 120.37(16) . . ?
C16_4 C17_4 H17_4 119.8 . . ?
C18_4 C17_4 H17_4 119.8 . . ?
C17_4 C16_4 C15_4 120.27(16) . . ?
C17_4 C16_4 H16_4 119.9 . . ?
C15_4 C16_4 H16_4 119.9 . . ?
C16_4 C15_4 C14_4 119.84(17) . . ?
C16_4 C15_4 H15_4 120.1 . . ?
C14_4 C15_4 H15_4 120.1 . . ?
C15_4 C14_4 C13_4 120.31(15) . . ?
C15_4 C14_4 H14_4 119.8 . . ?
C13_4 C14_4 H14_4 119.8 . . ?
C18_4 C13_4 C14_4 119.28(14) . . ?
C18_4 C13_4 P_4 118.10(11) . . ?
C14_4 C13_4 P_4 122.62(11) . . ?
C13_4 P_4 C1_4 104.41(7) . . ?
C13_4 P_4 C7_4 105.42(7) . . ?
C1_4 P_4 C7_4 104.02(7) . . ?
C13_4 P_4 Pd_1 113.11(5) . . ?
C1_4 P_4 Pd_1 112.81(5) . . ?
C7_4 P_4 Pd_1 115.97(5) . . ?
C8_4 C7_4 C12_4 119.16(13) . . ?
C8_4 C7_4 P_4 118.46(11) . . ?
C12_4 C7_4 P_4 122.37(12) . . ?
C7_4 C8_4 C9_4 120.42(14) . . ?
C7_4 C8_4 H8_4 119.8 . . ?
C9_4 C8_4 H8_4 119.8 . . ?
C10_4 C9_4 C8_4 120.31(16) . . ?
C10_4 C9_4 H9_4 119.8 . . ?
C8_4 C9_4 H9_4 119.8 . . ?
C9_4 C10_4 C11_4 119.62(15) . . ?
C9_4 C10_4 H10_4 120.2 . . ?
C11_4 C10_4 H10_4 120.2 . . ?
C10_4 C11_4 C12_4 120.39(15) . . ?
C10_4 C11_4 H11_4 119.8 . . ?
C12_4 C11_4 H11_4 119.8 . . ?
C7_4 C12_4 C11_4 120.09(15) . . ?
C7_4 C12_4 H12_4 120.0 . . ?
C11_4 C12_4 H12_4 120.0 . . ?
C6_4 C1_4 C2_4 119.17(13) . . ?
C6_4 C1_4 P_4 120.96(11) . . ?
C2_4 C1_4 P_4 119.65(11) . . ?
C3_4 C2_4 C1_4 120.46(15) . . ?
C3_4 C2_4 H2_4 119.8 . . ?
C1_4 C2_4 H2_4 119.8 . . ?
C4_4 C3_4 C2_4 119.97(15) . . ?
C4_4 C3_4 H3_4 120.0 . . ?
C2_4 C3_4 H3_4 120.0 . . ?
C5_4 C4_4 C3_4 119.75(15) . . ?
C5_4 C4_4 H4_4 120.1 . . ?
C3_4 C4_4 H4_4 120.1 . . ?
C4_4 C5_4 C6_4 120.58(17) . . ?
C4_4 C5_4 H5_4 119.7 . . ?
C6_4 C5_4 H5_4 119.7 . . ?
C1_4 C6_4 C5_4 120.07(15) . . ?
C1_4 C6_4 H6_4 120.0 . . ?
C5_4 C6_4 H6_4 120.0 . . ?
N3_3 C11_3 H11A_3 109.5 . . ?
N3_3 C11_3 H11B_3 109.5 . . ?
H11A_3 C11_3 H11B_3 109.5 . . ?
N3_3 C11_3 H11C_3 109.5 . . ?
H11A_3 C11_3 H11C_3 109.5 . . ?
H11B_3 C11_3 H11C_3 109.5 . . ?
C4_3 N3_3 C2_3 118.52(18) . . ?
C4_3 N3_3 C11_3 123.26(18) . . ?
C2_3 N3_3 C11_3 118.22(18) . . ?
O2_3 C2_3 N1_3 120.8(2) . . ?
O2_3 C2_3 N3_3 121.7(3) . . ?
N1_3 C2_3 N3_3 117.49(17) . . ?
C2_3 N1_3 C6_3 127.17(16) . . ?
C2_3 N1_3 C10_3 116.4(2) . . ?
C6_3 N1_3 C10_3 116.4(2) . . ?
N1_3 C10_3 H10A_3 109.5 . . ?
N1_3 C10_3 H10B_3 109.5 . . ?
H10A_3 C10_3 H10B_3 109.5 . . ?
N1_3 C10_3 H10C_3 109.5 . . ?
H10A_3 C10_3 H10C_3 109.5 . . ?
H10B_3 C10_3 H10C_3 109.5 . . ?
O6_3 C6_3 N1_3 121.95(16) . . ?
O6_3 C6_3 C5_3 126.94(17) . . ?
N1_3 C6_3 C5_3 111.11(17) . . ?
C4_3 C5_3 N7_3 106.89(14) . . ?
C4_3 C5_3 C6_3 123.12(15) . . ?
N7_3 C5_3 C6_3 129.61(16) . . ?
C5_3 C4_3 N3_3 122.44(16) . . ?
C5_3 C4_3 N9_3 107.29(14) . . ?
N3_3 C4_3 N9_3 130.25(17) . . ?
C8_3 N9_3 C4_3 109.41(14) . . ?
C8_3 N9_3 C13_3 121.24(14) . . ?
C4_3 N9_3 C13_3 129.32(15) . . ?
N9_3 C13_3 H13A_3 109.5 . . ?
N9_3 C13_3 H13B_3 109.5 . . ?
H13A_3 C13_3 H13B_3 109.5 . . ?
N9_3 C13_3 H13C_3 109.5 . . ?
H13A_3 C13_3 H13C_3 109.5 . . ?
H13B_3 C13_3 H13C_3 109.5 . . ?
N7_3 C8_3 N9_3 106.33(13) . . ?
N7_3 C8_3 Pd_1 125.03(11) . . ?
N9_3 C8_3 Pd_1 128.60(11) . . ?
C8_3 N7_3 C5_3 110.08(13) . . ?
C8_3 N7_3 C12_3 124.62(13) . . ?
C5_3 N7_3 C12_3 125.30(13) . . ?
N7_3 C12_3 H12A_3 109.5 . . ?
N7_3 C12_3 H12B_3 109.5 . . ?
H12A_3 C12_3 H12B_3 109.5 . . ?
N7_3 C12_3 H12C_3 109.5 . . ?
H12A_3 C12_3 H12C_3 109.5 . . ?
H12B_3 C12_3 H12C_3 109.5 . . ?
F1A_5 BA_5 F2A_5 110.8(3) . . ?
F1A_5 BA_5 F3A_5 106.2(4) . . ?
F2A_5 BA_5 F3A_5 109.2(3) . . ?
F1A_5 BA_5 F4A_5 109.0(3) . . ?
F2A_5 BA_5 F4A_5 112.1(3) . . ?
F3A_5 BA_5 F4A_5 109.3(3) . . ?
F1B_5 BB_5 F2B_5 107.3(9) . . ?
F1B_5 BB_5 F4B_5 112.6(11) . . ?
F2B_5 BB_5 F4B_5 105.9(10) . . ?
F1B_5 BB_5 F3B_5 116.5(11) . . ?
F2B_5 BB_5 F3B_5 110.4(11) . . ?
F4B_5 BB_5 F3B_5 103.7(10) . . ?
Cl1A_11 C1A_11 Cl2A_11 110.60(18) . . ?
Cl1A_11 C1A_11 H1A1_11 109.5 . . ?
Cl2A_11 C1A_11 H1A1_11 109.5 . . ?
Cl1A_11 C1A_11 H1A2_11 109.5 . . ?
Cl2A_11 C1A_11 H1A2_11 109.5 . . ?
H1A1_11 C1A_11 H1A2_11 108.1 . . ?

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
Pd_1 C19A_2 C21A_2 C20A_2 47.8(4) . . . . ?
C19A_2 C21A_2 C20A_2 Pd_1 -48.8(4) . . . . ?
Pd_1 C19B_2 C21B_2 C20B_2 -48.3(3) . . . . ?
C19B_2 C21B_2 C20B_2 Pd_1 49.1(3) . . . . ?
C13_4 C18_4 C17_4 C16_4 -1.4(3) . . . . ?
C18_4 C17_4 C16_4 C15_4 0.7(3) . . . . ?
C17_4 C16_4 C15_4 C14_4 0.5(3) . . . . ?
C16_4 C15_4 C14_4 C13_4 -1.0(3) . . . . ?
C17_4 C18_4 C13_4 C14_4 0.9(2) . . . . ?
C17_4 C18_4 C13_4 P_4 -178.56(12) . . . . ?
C15_4 C14_4 C13_4 C18_4 0.3(2) . . . . ?
C15_4 C14_4 C13_4 P_4 179.70(13) . . . . ?
C18_4 C13_4 P_4 C1_4 -155.34(11) . . . . ?
C14_4 C13_4 P_4 C1_4 25.24(14) . . . . ?
C18_4 C13_4 P_4 C7_4 95.37(12) . . . . ?
C14_4 C13_4 P_4 C7_4 -84.05(13) . . . . ?
C18_4 C13_4 P_4 Pd_1 -32.33(13) . . . . ?
C14_4 C13_4 P_4 Pd_1 148.25(11) . . . . ?
C13_4 P_4 C7_4 C8_4 -148.72(12) . . . . ?
C1_4 P_4 C7_4 C8_4 101.71(13) . . . . ?
Pd_1 P_4 C7_4 C8_4 -22.76(14) . . . . ?
C13_4 P_4 C7_4 C12_4 32.67(15) . . . . ?
C1_4 P_4 C7_4 C12_4 -76.90(15) . . . . ?
Pd_1 P_4 C7_4 C12_4 158.62(12) . . . . ?
C12_4 C7_4 C8_4 C9_4 -0.6(2) . . . . ?
P_4 C7_4 C8_4 C9_4 -179.28(13) . . . . ?
C7_4 C8_4 C9_4 C10_4 0.4(3) . . . . ?
C8_4 C9_4 C10_4 C11_4 0.0(3) . . . . ?
C9_4 C10_4 C11_4 C12_4 -0.2(3) . . . . ?
C8_4 C7_4 C12_4 C11_4 0.4(3) . . . . ?
P_4 C7_4 C12_4 C11_4 179.05(14) . . . . ?
C10_4 C11_4 C12_4 C7_4 -0.1(3) . . . . ?
C13_4 P_4 C1_4 C6_4 -132.45(13) . . . . ?
C7_4 P_4 C1_4 C6_4 -22.14(14) . . . . ?
Pd_1 P_4 C1_4 C6_4 104.35(13) . . . . ?
C13_4 P_4 C1_4 C2_4 52.95(12) . . . . ?
C7_4 P_4 C1_4 C2_4 163.26(11) . . . . ?
Pd_1 P_4 C1_4 C2_4 -70.26(12) . . . . ?
C6_4 C1_4 C2_4 C3_4 0.1(2) . . . . ?
P_4 C1_4 C2_4 C3_4 174.82(11) . . . . ?
C1_4 C2_4 C3_4 C4_4 0.2(2) . . . . ?
C2_4 C3_4 C4_4 C5_4 -0.2(3) . . . . ?
C3_4 C4_4 C5_4 C6_4 -0.2(3) . . . . ?
C2_4 C1_4 C6_4 C5_4 -0.5(2) . . . . ?
P_4 C1_4 C6_4 C5_4 -175.15(14) . . . . ?
C4_4 C5_4 C6_4 C1_4 0.6(3) . . . . ?
C4_3 N3_3 C2_3 O2_3 179.40(18) . . . . ?
C11_3 N3_3 C2_3 O2_3 -1.0(3) . . . . ?
C4_3 N3_3 C2_3 N1_3 -0.9(2) . . . . ?
C11_3 N3_3 C2_3 N1_3 178.70(18) . . . . ?
O2_3 C2_3 N1_3 C6_3 177.75(18) . . . . ?
N3_3 C2_3 N1_3 C6_3 -2.0(3) . . . . ?
O2_3 C2_3 N1_3 C10_3 -2.9(3) . . . . ?
N3_3 C2_3 N1_3 C10_3 177.33(18) . . . . ?
C2_3 N1_3 C6_3 O6_3 -178.87(17) . . . . ?
C10_3 N1_3 C6_3 O6_3 1.8(3) . . . . ?
C2_3 N1_3 C6_3 C5_3 1.5(2) . . . . ?
C10_3 N1_3 C6_3 C5_3 -177.78(16) . . . . ?
O6_3 C6_3 C5_3 C4_3 -177.82(16) . . . . ?
N1_3 C6_3 C5_3 C4_3 1.8(2) . . . . ?
O6_3 C6_3 C5_3 N7_3 -5.9(3) . . . . ?
N1_3 C6_3 C5_3 N7_3 173.64(14) . . . . ?
N7_3 C5_3 C4_3 N3_3 -178.12(14) . . . . ?
C6_3 C5_3 C4_3 N3_3 -4.6(2) . . . . ?
N7_3 C5_3 C4_3 N9_3 0.19(16) . . . . ?
C6_3 C5_3 C4_3 N9_3 173.67(14) . . . . ?
C2_3 N3_3 C4_3 C5_3 4.1(2) . . . . ?
C11_3 N3_3 C4_3 C5_3 -175.48(18) . . . . ?
C2_3 N3_3 C4_3 N9_3 -173.84(16) . . . . ?
C11_3 N3_3 C4_3 N9_3 6.6(3) . . . . ?
C5_3 C4_3 N9_3 C8_3 -0.15(16) . . . . ?
N3_3 C4_3 N9_3 C8_3 177.98(15) . . . . ?
C5_3 C4_3 N9_3 C13_3 178.03(15) . . . . ?
N3_3 C4_3 N9_3 C13_3 -3.8(3) . . . . ?
C4_3 N9_3 C8_3 N7_3 0.05(16) . . . . ?
C13_3 N9_3 C8_3 N7_3 -178.31(13) . . . . ?
C4_3 N9_3 C8_3 Pd_1 -177.81(10) . . . . ?
C13_3 N9_3 C8_3 Pd_1 3.8(2) . . . . ?
N9_3 C8_3 N7_3 C5_3 0.08(15) . . . . ?
Pd_1 C8_3 N7_3 C5_3 178.03(10) . . . . ?
N9_3 C8_3 N7_3 C12_3 -179.21(13) . . . . ?
Pd_1 C8_3 N7_3 C12_3 -1.3(2) . . . . ?
C4_3 C5_3 N7_3 C8_3 -0.17(16) . . . . ?
C6_3 C5_3 N7_3 C8_3 -173.07(15) . . . . ?
C4_3 C5_3 N7_3 C12_3 179.10(14) . . . . ?
C6_3 C5_3 N7_3 C12_3 6.2(2) . . . . ?

_refine_diff_density_max         1.203
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.078

