# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1855707'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H28 Cl2 N0 O2 P2 Pd2'
_chemical_formula_weight         838.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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                   16.503(5)
_cell_length_b                   10.164(5)
_cell_length_c                   19.571(5)
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 95.459(5)
_cell_angle_gamma                90.000(5)
_cell_volume                     3268(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1987
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      23.26

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.394
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.7696
_exptl_absorpt_correction_T_max  0.8878
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27307
_diffrn_reflns_av_unetI/netI     0.0808
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.543
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_full        25.240
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6677
_reflns_number_gt                4628
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0354P)²+0.8254P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6677
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.0979
_refine_ls_wR_factor_gt          0.0875
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.0204(3) 1.1542(4) 0.6582(2) 0.0205(11) Uani 1 1 d . . . . .
C2 C -0.0106(3) 1.2811(4) 0.6478(2) 0.0258(12) Uani 1 1 d . . . . .
H2 H -0.023094 1.311948 0.603311 0.031 Uiso 1 1 calc R U . . .
C3 C -0.0230(3) 1.3613(5) 0.7027(2) 0.0306(13) Uani 1 1 d . . . . .
H3 H -0.043458 1.445774 0.694826 0.037 Uiso 1 1 calc R U . . .
C4 C -0.0055(3) 1.3177(5) 0.7693(2) 0.0299(13) Uani 1 1 d . . . . .
H4 H -0.014881 1.372241 0.805873 0.036 Uiso 1 1 calc R U . . .
C5 C 0.0259(3) 1.1936(5) 0.7814(2) 0.0270(12) Uani 1 1 d . . . . .
H5 H 0.037628 1.163887 0.826224 0.032 Uiso 1 1 calc R U . . .
C6 C 0.0399(3) 1.1127(4) 0.7262(2) 0.0188(11) Uani 1 1 d . . . . .
C7 C 0.0151(3) 0.8389(4) 0.7704(2) 0.0218(11) Uani 1 1 d . . . . .
C8 C -0.0363(3) 0.7640(5) 0.7262(3) 0.0297(13) Uani 1 1 d . . . . .
H8 H -0.032246 0.769047 0.679215 0.036 Uiso 1 1 calc R U . . .
C9 C -0.0931(3) 0.6824(5) 0.7506(3) 0.0394(15) Uani 1 1 d . . . . .
H9 H -0.127921 0.633497 0.720286 0.047 Uiso 1 1 calc R U . . .
C10 C -0.0981(4) 0.6735(5) 0.8201(3) 0.0458(16) Uani 1 1 d . . . . .
H10 H -0.135758 0.616837 0.836835 0.055 Uiso 1 1 calc R U . . .
C11 C -0.0485(4) 0.7468(5) 0.8647(3) 0.0474(17) Uani 1 1 d . . . . .
H11 H -0.053044 0.740659 0.911613 0.057 Uiso 1 1 calc R U . . .
C12 C 0.0091(4) 0.8311(5) 0.8406(3) 0.0343(14) Uani 1 1 d . . . . .
H12 H 0.043032 0.881210 0.871116 0.041 Uiso 1 1 calc R U . . .
C13 C 0.1771(3) 0.9576(5) 0.7857(2) 0.0241(11) Uani 1 1 d . . . . .
C14 C 0.2092(4) 0.8462(5) 0.8199(3) 0.0359(14) Uani 1 1 d . . . . .
H14 H 0.179358 0.768459 0.818825 0.043 Uiso 1 1 calc R U . . .
C15 C 0.2857(4) 0.8519(6) 0.8553(3) 0.0420(16) Uani 1 1 d . . . . .
H15 H 0.307406 0.777846 0.878179 0.050 Uiso 1 1 calc R U . . .
C16 C 0.3299(4) 0.9675(6) 0.8566(3) 0.0442(16) Uani 1 1 d . . . . .
H16 H 0.381933 0.970092 0.879512 0.053 Uiso 1 1 calc R U . . .
C17 C 0.2981(4) 1.0776(6) 0.8249(3) 0.0416(15) Uani 1 1 d . . . . .
H17 H 0.327777 1.155577 0.827143 0.050 Uiso 1 1 calc R U . . .
C18 C 0.2214(3) 1.0736(5) 0.7891(2) 0.0316(13) Uani 1 1 d . . . . .
H18 H 0.199726 1.148825 0.767392 0.038 Uiso 1 1 calc R U . . .
C19 C 0.7068(3) 0.5578(4) 0.5354(2) 0.0239(12) Uani 1 1 d . . . . .
C20 C 0.7487(4) 0.4417(5) 0.5217(2) 0.0336(14) Uani 1 1 d . . . . .
H20 H 0.719796 0.365142 0.509887 0.040 Uiso 1 1 calc R U . . .
C21 C 0.8330(4) 0.4412(5) 0.5260(3) 0.0405(15) Uani 1 1 d . . . . .
H21 H 0.859500 0.363341 0.516725 0.049 Uiso 1 1 calc R U . . .
C22 C 0.8797(4) 0.5522(5) 0.5434(3) 0.0384(15) Uani 1 1 d . . . . .
H22 H 0.936168 0.549493 0.545001 0.046 Uiso 1 1 calc R U . . .
C23 C 0.8393(3) 0.6681(5) 0.5586(2) 0.0315(13) Uani 1 1 d . . . . .
H23 H 0.868804 0.743824 0.570954 0.038 Uiso 1 1 calc R U . . .
C24 C 0.7548(3) 0.6692(4) 0.5550(2) 0.0253(12) Uani 1 1 d . . . . .
C25 C 0.7391(3) 0.8905(4) 0.6495(2) 0.0216(11) Uani 1 1 d . . . . .
C26 C 0.7163(3) 0.8536(4) 0.7131(2) 0.0284(13) Uani 1 1 d . . . . .
H26 H 0.676979 0.788634 0.715561 0.034 Uiso 1 1 calc R U . . .
C27 C 0.7506(3) 0.9113(5) 0.7726(3) 0.0331(13) Uani 1 1 d . . . . .
H27 H 0.734357 0.885952 0.814902 0.040 Uiso 1 1 calc R U . . .
C28 C 0.8094(3) 1.0072(5) 0.7688(3) 0.0329(13) Uani 1 1 d . . . . .
H28 H 0.834201 1.044733 0.808815 0.039 Uiso 1 1 calc R U . . .
C29 C 0.8312(3) 1.0470(5) 0.7058(3) 0.0346(14) Uani 1 1 d . . . . .
H29 H 0.869480 1.113617 0.703556 0.042 Uiso 1 1 calc R U . . .
C30 C 0.7968(3) 0.9893(5) 0.6460(3) 0.0293(13) Uani 1 1 d . . . . .
H30 H 0.812176 1.016432 0.603719 0.035 Uiso 1 1 calc R U . . .
C31 C 0.6844(3) 0.9172(5) 0.5042(2) 0.0252(12) Uani 1 1 d . . . . .
C32 C 0.7490(4) 0.9532(6) 0.4680(3) 0.0456(16) Uani 1 1 d . . . . .
H32 H 0.800045 0.916651 0.479978 0.055 Uiso 1 1 calc R U . . .
C33 C 0.7390(4) 1.0433(6) 0.4140(3) 0.0516(18) Uani 1 1 d . . . . .
H33 H 0.782753 1.067188 0.389954 0.062 Uiso 1 1 calc R U . . .
C34 C 0.6646(4) 1.0945(6) 0.3976(3) 0.0553(18) Uani 1 1 d . . . . .
H34 H 0.656702 1.151803 0.360502 0.066 Uiso 1 1 calc R U . . .
C35 C 0.5995(4) 1.0646(6) 0.4343(3) 0.0554(18) Uani 1 1 d . . . . .
H35 H 0.549196 1.104253 0.423273 0.066 Uiso 1 1 calc R U . . .
C36 C 0.6100(4) 0.9753(5) 0.4875(3) 0.0402(15) Uani 1 1 d . . . . .
H36 H 0.566341 0.954265 0.512257 0.048 Uiso 1 1 calc R U . . .
O1 O 0.0927(2) 0.9093(3) 0.66033(14) 0.0236(8) Uani 1 1 d . . . . .
O2 O 0.6122(2) 0.7502(3) 0.58944(15) 0.0232(8) Uani 1 1 d . . . . .
P1 P 0.08205(8) 0.95140(12) 0.73340(6) 0.0207(3) Uani 1 1 d . . . . .
P2 P 0.69391(9) 0.80612(12) 0.57526(6) 0.0239(3) Uani 1 1 d . . . . .
CL1 Cl -0.03743(11) 1.14759(13) 0.50073(6) 0.0501(5) Uani 1 1 d . . . . .
CL2 Cl 0.55968(9) 0.39428(12) 0.46737(6) 0.0338(3) Uani 1 1 d . . . . .
PD1 Pd 0.03090(3) 1.02332(4) 0.58601(2) 0.02449(12) Uani 1 1 d . . . . .
PD2 Pd 0.58853(3) 0.57906(4) 0.53349(2) 0.02554(12) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.396(6) . ?
C1 C6 1.404(6) . ?
C1 PD1 1.960(4) . ?
C2 C3 1.380(6) . ?
C3 C4 1.380(6) . ?
C4 C5 1.375(6) . ?
C5 C6 1.395(6) . ?
C6 P1 1.781(5) . ?
C7 C8 1.381(6) . ?
C7 C12 1.389(6) . ?
C7 P1 1.790(5) . ?
C8 C9 1.371(7) . ?
C9 C10 1.374(8) . ?
C10 C11 1.360(8) . ?
C11 C12 1.395(7) . ?
C13 C18 1.385(7) . ?
C13 C14 1.394(7) . ?
C13 P1 1.791(5) . ?
C14 C15 1.382(7) . ?
C15 C16 1.383(8) . ?
C16 C17 1.361(8) . ?
C17 C18 1.387(7) . ?
C19 C20 1.406(7) . ?
C19 C24 1.414(7) . ?
C19 PD2 1.961(5) . ?
C20 C21 1.386(8) . ?
C21 C22 1.390(8) . ?
C22 C23 1.399(7) . ?
C23 C24 1.390(7) . ?
C24 P2 1.783(5) . ?
C25 C26 1.386(6) . ?
C25 C30 1.390(7) . ?
C25 P2 1.787(5) . ?
C26 C27 1.377(6) . ?
C27 C28 1.382(7) . ?
C28 C29 1.378(7) . ?
C29 C30 1.383(7) . ?
C31 C36 1.373(7) . ?
C31 C32 1.384(7) . ?
C31 P2 1.787(5) . ?
C32 C33 1.397(7) . ?
C33 C34 1.345(8) . ?
C34 C35 1.382(8) . ?
C35 C36 1.380(7) . ?
O1 P1 1.519(3) . ?
O1 PD1 2.053(3) . ?
O2 P2 1.514(3) . ?
O2 PD2 2.073(3) . ?
P2 PD2 2.9577(17) . ?
CL1 PD1 2.3008(14) . ?
CL1 PD1 2.4384(14) 3_576 ?
CL2 PD2 2.3047(14) . ?
CL2 PD2 2.4593(17) 3_666 ?
PD1 CL1 2.4383(14) 3_576 ?
PD2 CL2 2.4594(17) 3_666 ?

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 C6 117.6(4) . . ?
C2 C1 PD1 125.3(3) . . ?
C6 C1 PD1 116.9(3) . . ?
C3 C2 C1 120.8(4) . . ?
C2 C3 C4 120.8(4) . . ?
C5 C4 C3 120.0(4) . . ?
C4 C5 C6 119.6(4) . . ?
C5 C6 C1 121.1(4) . . ?
C5 C6 P1 125.0(3) . . ?
C1 C6 P1 113.8(3) . . ?
C8 C7 C12 119.4(5) . . ?
C8 C7 P1 117.7(4) . . ?
C12 C7 P1 122.8(4) . . ?
C9 C8 C7 121.0(5) . . ?
C8 C9 C10 119.5(5) . . ?
C11 C10 C9 120.7(5) . . ?
C10 C11 C12 120.5(5) . . ?
C7 C12 C11 119.0(5) . . ?
C18 C13 C14 119.6(5) . . ?
C18 C13 P1 119.2(4) . . ?
C14 C13 P1 121.2(4) . . ?
C15 C14 C13 119.6(5) . . ?
C14 C15 C16 120.0(5) . . ?
C17 C16 C15 120.7(6) . . ?
C16 C17 C18 120.0(6) . . ?
C13 C18 C17 120.1(5) . . ?
C20 C19 C24 116.8(5) . . ?
C20 C19 PD2 126.5(4) . . ?
C24 C19 PD2 116.6(3) . . ?
C21 C20 C19 120.0(5) . . ?
C20 C21 C22 122.8(5) . . ?
C21 C22 C23 118.1(5) . . ?
C24 C23 C22 119.4(5) . . ?
C23 C24 C19 122.7(4) . . ?
C23 C24 P2 125.4(4) . . ?
C19 C24 P2 111.9(4) . . ?
C26 C25 C30 119.0(4) . . ?
C26 C25 P2 118.2(4) . . ?
C30 C25 P2 122.8(4) . . ?
C27 C26 C25 121.3(5) . . ?
C26 C27 C28 119.3(5) . . ?
C29 C28 C27 120.0(5) . . ?
C28 C29 C30 120.8(5) . . ?
C29 C30 C25 119.5(5) . . ?
C36 C31 C32 118.7(5) . . ?
C36 C31 P2 117.8(4) . . ?
C32 C31 P2 123.3(4) . . ?
C31 C32 C33 121.3(5) . . ?
C34 C33 C32 118.2(6) . . ?
C33 C34 C35 121.9(6) . . ?
C34 C35 C36 119.3(6) . . ?
C31 C36 C35 120.4(5) . . ?
P1 O1 PD1 114.45(17) . . ?
P2 O2 PD2 110.14(17) . . ?
O1 P1 C6 105.31(19) . . ?
O1 P1 C7 109.4(2) . . ?
C6 P1 C7 111.6(2) . . ?
O1 P1 C13 112.0(2) . . ?
C6 P1 C13 109.1(2) . . ?
C7 P1 C13 109.4(2) . . ?
O2 P2 C24 106.2(2) . . ?
O2 P2 C31 111.5(2) . . ?
C24 P2 C31 109.3(2) . . ?
O2 P2 C25 110.0(2) . . ?
C24 P2 C25 110.8(2) . . ?
C31 P2 C25 109.2(2) . . ?
O2 P2 PD2 41.14(11) . . ?
C24 P2 PD2 70.03(18) . . ?
C31 P2 PD2 105.77(17) . . ?
C25 P2 PD2 141.99(16) . . ?
PD1 CL1 PD1 93.60(5) . 3_576 ?
PD2 CL2 PD2 93.80(5) . 3_666 ?
C1 PD1 O1 86.79(16) . . ?
C1 PD1 CL1 94.58(14) . . ?
O1 PD1 CL1 178.61(9) . . ?
C1 PD1 CL1 176.40(14) . 3_576 ?
O1 PD1 CL1 92.26(9) . 3_576 ?
CL1 PD1 CL1 86.40(5) . 3_576 ?
C19 PD2 O2 86.89(16) . . ?
C19 PD2 CL2 94.17(13) . . ?
O2 PD2 CL2 177.49(9) . . ?
C19 PD2 CL2 179.31(12) . 3_666 ?
O2 PD2 CL2 92.76(10) . 3_666 ?
CL2 PD2 CL2 86.20(5) . 3_666 ?
C19 PD2 P2 61.50(13) . . ?
O2 PD2 P2 28.72(9) . . ?
CL2 PD2 P2 151.13(5) . . ?
CL2 PD2 P2 118.30(4) 3_666 . ?

_refine_diff_density_max         0.854
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.122

####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1855708'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43.50 H36 N O1.50 P2 Pd'
_chemical_formula_weight         765.07

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   17.7768(7)
_cell_length_b                   9.4520(4)
_cell_length_c                   42.7751(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.266(2)
_cell_angle_gamma                90
_cell_volume                     7112.7(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1987
_cell_measurement_theta_min      2.315
_cell_measurement_theta_max      28.185

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_F_000             3136
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    0.649
_shelx_estimated_absorpt_T_min   0.829
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.8095
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48007
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_theta_min         0.962
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8896
_reflns_number_gt                7841
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0006P)²+153.3228P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8896
_refine_ls_number_parameters     444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   0.748
_refine_ls_restrained_S_all      0.748
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
PD1 Pd 0.28402(2) 0.50401(2) 0.12779(2) 0.00796(6) Uani 1 1 d . . . . .
P1 P 0.22472(4) 0.28258(8) 0.08122(2) 0.00844(14) Uani 1 1 d . . . . .
P2 P 0.25879(4) 0.67019(8) 0.16192(2) 0.00823(14) Uani 1 1 d . . . . .
C25 C 0.19760(16) 0.3820(3) 0.13763(7) 0.0100(5) Uani 1 1 d . . . . .
C20 C 0.17599(16) 0.2765(3) 0.11473(6) 0.0092(5) Uani 1 1 d . . . . .
C24 C 0.15693(17) 0.3815(3) 0.16348(7) 0.0106(6) Uani 1 1 d . . . . .
H24 H 0.169726 0.448396 0.179971 0.013 Uiso 1 1 calc R U . . .
C21 C 0.11818(17) 0.1789(3) 0.11673(7) 0.0124(6) Uani 1 1 d . . . . .
H21 H 0.106122 0.109384 0.100760 0.015 Uiso 1 1 calc R U . . .
C23 C 0.09837(17) 0.2857(3) 0.16556(7) 0.0130(6) Uani 1 1 d . . . . .
H23 H 0.071613 0.289671 0.183230 0.016 Uiso 1 1 calc R U . . .
C22 C 0.07829(17) 0.1846(3) 0.14242(7) 0.0146(6) Uani 1 1 d . . . . .
H22 H 0.037975 0.120322 0.144045 0.018 Uiso 1 1 calc R U . . .
C14 C 0.16849(17) 0.3895(3) 0.05166(7) 0.0109(6) Uani 1 1 d . . . . .
C15 C 0.10841(18) 0.4696(3) 0.06002(7) 0.0162(6) Uani 1 1 d . . . . .
H15 H 0.094200 0.459931 0.080489 0.019 Uiso 1 1 calc R U . . .
C17 C 0.08957(19) 0.5771(4) 0.00861(8) 0.0177(7) Uani 1 1 d . . . . .
H17 H 0.062611 0.640842 -0.006111 0.021 Uiso 1 1 calc R U . . .
C19 C 0.18864(18) 0.4054(3) 0.02146(7) 0.0147(6) Uani 1 1 d . . . . .
H19 H 0.229724 0.352255 0.015565 0.018 Uiso 1 1 calc R U . . .
C16 C 0.06939(19) 0.5632(4) 0.03850(8) 0.0196(7) Uani 1 1 d . . . . .
H16 H 0.028735 0.617768 0.044318 0.024 Uiso 1 1 calc R U . . .
C18 C 0.14905(18) 0.4981(4) 0.00013(7) 0.0177(6) Uani 1 1 d . . . . .
H18 H 0.162725 0.507706 -0.020438 0.021 Uiso 1 1 calc R U . . .
C8 C 0.23100(17) 0.1061(3) 0.06608(7) 0.0109(6) Uani 1 1 d . . . . .
C9 C 0.28261(17) 0.0145(3) 0.08318(7) 0.0133(6) Uani 1 1 d . . . . .
H9 H 0.316967 0.049115 0.100568 0.016 Uiso 1 1 calc R U . . .
C11 C 0.23348(19) -0.1771(4) 0.04925(8) 0.0188(7) Uani 1 1 d . . . . .
H11 H 0.233793 -0.274358 0.043694 0.023 Uiso 1 1 calc R U . . .
C10 C 0.28403(18) -0.1278(3) 0.07486(7) 0.0151(6) Uani 1 1 d . . . . .
H10 H 0.319134 -0.190655 0.086541 0.018 Uiso 1 1 calc R U . . .
C13 C 0.18109(18) 0.0554(3) 0.04044(7) 0.0138(6) Uani 1 1 d . . . . .
H13 H 0.145692 0.117962 0.028816 0.017 Uiso 1 1 calc R U . . .
C12 C 0.18280(19) -0.0859(4) 0.03179(8) 0.0182(7) Uani 1 1 d . . . . .
H12 H 0.149444 -0.119935 0.014031 0.022 Uiso 1 1 calc R U . . .
C4 C 0.46822(17) 0.5167(4) 0.04300(7) 0.0165(6) Uani 1 1 d . . . . .
H4 H 0.504582 0.556303 0.031276 0.020 Uiso 1 1 calc R U . . .
C7 C 0.35969(16) 0.4027(3) 0.07671(7) 0.0096(5) Uani 1 1 d . . . . .
C2 C 0.39227(16) 0.5355(3) 0.08588(7) 0.0107(6) Uani 1 1 d . . . . .
C5 C 0.43803(17) 0.3846(4) 0.03514(7) 0.0154(6) Uani 1 1 d . . . . .
H5 H 0.454307 0.332789 0.018304 0.018 Uiso 1 1 calc R U . . .
C6 C 0.38370(16) 0.3275(3) 0.05193(7) 0.0124(6) Uani 1 1 d . . . . .
H6 H 0.362899 0.236710 0.046462 0.015 Uiso 1 1 calc R U . . .
C3 C 0.44555(17) 0.5924(4) 0.06809(7) 0.0143(6) Uani 1 1 d . . . . .
H3 H 0.466424 0.683430 0.073195 0.017 Uiso 1 1 calc R U . . .
C26 C 0.15912(16) 0.7209(3) 0.15607(7) 0.0091(5) Uani 1 1 d . . . . .
C31 C 0.11537(17) 0.7444(3) 0.18009(7) 0.0113(6) Uani 1 1 d . . . . .
H31 H 0.135590 0.722731 0.201327 0.014 Uiso 1 1 calc R U . . .
C30 C 0.04226(17) 0.7993(3) 0.17319(7) 0.0146(6) Uani 1 1 d . . . . .
H30 H 0.013039 0.816376 0.189733 0.018 Uiso 1 1 calc R U . . .
C28 C 0.05417(18) 0.8034(4) 0.11794(7) 0.0164(6) Uani 1 1 d . . . . .
H28 H 0.033086 0.822592 0.096685 0.020 Uiso 1 1 calc R U . . .
C29 C 0.01198(18) 0.8291(4) 0.14213(8) 0.0163(6) Uani 1 1 d . . . . .
H29 H -0.037806 0.867314 0.137480 0.020 Uiso 1 1 calc R U . . .
C27 C 0.12731(17) 0.7494(3) 0.12476(7) 0.0130(6) Uani 1 1 d . . . . .
H27 H 0.156064 0.731643 0.108091 0.016 Uiso 1 1 calc R U . . .
C38 C 0.30478(16) 0.8421(3) 0.16140(7) 0.0097(5) Uani 1 1 d . . . . .
C39 C 0.26663(17) 0.9644(3) 0.16783(7) 0.0124(6) Uani 1 1 d . . . . .
H39 H 0.214441 0.959368 0.170306 0.015 Uiso 1 1 calc R U . . .
C40 C 0.30373(18) 1.0936(3) 0.17070(7) 0.0147(6) Uani 1 1 d . . . . .
H40 H 0.277192 1.176562 0.175297 0.018 Uiso 1 1 calc R U . . .
C43 C 0.38147(17) 0.8508(3) 0.15739(7) 0.0144(6) Uani 1 1 d . . . . .
H43 H 0.408307 0.767971 0.152955 0.017 Uiso 1 1 calc R U . . .
C41 C 0.37932(19) 1.1015(4) 0.16686(8) 0.0182(7) Uani 1 1 d . . . . .
H41 H 0.405011 1.189824 0.168949 0.022 Uiso 1 1 calc R U . . .
C42 C 0.41795(18) 0.9802(4) 0.15993(8) 0.0186(7) Uani 1 1 d . . . . .
H42 H 0.469762 0.986417 0.156913 0.022 Uiso 1 1 calc R U . . .
C37 C 0.27890(17) 0.7128(3) 0.22797(7) 0.0132(6) Uani 1 1 d . . . . .
H37 H 0.253592 0.800647 0.223676 0.016 Uiso 1 1 calc R U . . .
C36 C 0.30708(19) 0.6763(4) 0.25891(7) 0.0178(7) Uani 1 1 d . . . . .
H36 H 0.299122 0.737430 0.275760 0.021 Uiso 1 1 calc R U . . .
C32 C 0.28756(16) 0.6211(3) 0.20317(7) 0.0104(5) Uani 1 1 d . . . . .
C34 C 0.35692(19) 0.4596(4) 0.24078(8) 0.0185(7) Uani 1 1 d . . . . .
H34 H 0.384574 0.374149 0.245197 0.022 Uiso 1 1 calc R U . . .
C33 C 0.32662(18) 0.4932(4) 0.20988(7) 0.0157(6) Uani 1 1 d . . . . .
H33 H 0.332385 0.429312 0.193239 0.019 Uiso 1 1 calc R U . . .
C35 C 0.34660(19) 0.5514(4) 0.26521(8) 0.0189(7) Uani 1 1 d . . . . .
H35 H 0.366869 0.528058 0.286347 0.023 Uiso 1 1 calc R U . . .
N1 N 0.30498(14) 0.3546(3) 0.09533(6) 0.0096(5) Uani 1 1 d . . . . .
O1 O 0.37276(12) 0.6038(2) 0.11058(5) 0.0115(4) Uani 1 1 d . . . . .
O2 O 0.500000 0.1988(4) 0.250000 0.0389(10) Uani 1 2 d S T P . .
C44 C 0.500000 0.0716(6) 0.250000 0.0269(11) Uani 1 2 d S T P . .
C45 C 0.4284(3) -0.0105(6) 0.25035(11) 0.0462(12) Uani 1 1 d . . . . .
H45A H 0.430967 -0.061646 0.270406 0.069 Uiso 1 1 calc R U . . .
H45B H 0.422343 -0.078337 0.232830 0.069 Uiso 1 1 calc R U . . .
H45C H 0.385014 0.054381 0.248034 0.069 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
PD1 C25 2.013(3) . ?
PD1 N1 2.052(2) . ?
PD1 O1 2.063(2) . ?
PD1 P2 2.2335(8) . ?
PD1 P1 2.9758(8) . ?
P1 N1 1.617(3) . ?
P1 C20 1.779(3) . ?
P1 C8 1.799(3) . ?
P1 C14 1.804(3) . ?
P2 C26 1.818(3) . ?
P2 C38 1.821(3) . ?
P2 C32 1.825(3) . ?
C25 C24 1.406(4) . ?
C25 C20 1.412(4) . ?
C20 C21 1.392(4) . ?
C24 C23 1.393(4) . ?
C21 C22 1.392(4) . ?
C23 C22 1.385(4) . ?
C14 C15 1.397(4) . ?
C14 C19 1.397(4) . ?
C15 C16 1.388(4) . ?
C17 C16 1.383(5) . ?
C17 C18 1.385(5) . ?
C19 C18 1.383(4) . ?
C8 C9 1.390(4) . ?
C8 C13 1.393(4) . ?
C9 C10 1.392(4) . ?
C11 C12 1.385(5) . ?
C11 C10 1.394(5) . ?
C13 C12 1.388(4) . ?
C4 C5 1.382(5) . ?
C4 C3 1.397(4) . ?
C7 C6 1.394(4) . ?
C7 C2 1.414(4) . ?
C7 N1 1.418(4) . ?
C2 O1 1.326(3) . ?
C2 C3 1.404(4) . ?
C5 C6 1.393(4) . ?
C26 C31 1.393(4) . ?
C26 C27 1.403(4) . ?
C31 C30 1.391(4) . ?
C30 C29 1.389(4) . ?
C28 C29 1.384(4) . ?
C28 C27 1.388(4) . ?
C38 C39 1.387(4) . ?
C38 C43 1.401(4) . ?
C39 C40 1.385(4) . ?
C40 C41 1.379(5) . ?
C43 C42 1.382(4) . ?
C41 C42 1.389(5) . ?
C37 C36 1.390(4) . ?
C37 C32 1.395(4) . ?
C36 C35 1.380(5) . ?
C32 C33 1.403(4) . ?
C34 C35 1.391(5) . ?
C34 C33 1.391(4) . ?
O2 C44 1.202(7) . ?
C44 C45 1.492(5) . ?
C44 C45 1.492(5) 2_655 ?

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
C25 PD1 N1 88.02(11) . . ?
C25 PD1 O1 169.21(10) . . ?
N1 PD1 O1 81.40(9) . . ?
C25 PD1 P2 92.03(9) . . ?
N1 PD1 P2 178.19(7) . . ?
O1 PD1 P2 98.48(6) . . ?
C25 PD1 P1 61.93(8) . . ?
N1 PD1 P1 31.16(7) . . ?
O1 PD1 P1 107.35(6) . . ?
P2 PD1 P1 147.89(3) . . ?
N1 P1 C20 102.63(13) . . ?
N1 P1 C8 115.31(14) . . ?
C20 P1 C8 108.82(14) . . ?
N1 P1 C14 113.31(14) . . ?
C20 P1 C14 107.34(14) . . ?
C8 P1 C14 108.91(14) . . ?
N1 P1 PD1 41.02(9) . . ?
C20 P1 PD1 69.53(10) . . ?
C8 P1 PD1 149.19(10) . . ?
C14 P1 PD1 100.51(10) . . ?
C26 P2 C38 101.17(14) . . ?
C26 P2 C32 109.41(13) . . ?
C38 P2 C32 100.08(13) . . ?
C26 P2 PD1 112.25(9) . . ?
C38 P2 PD1 119.14(10) . . ?
C32 P2 PD1 113.48(10) . . ?
C24 C25 C20 115.1(3) . . ?
C24 C25 PD1 131.3(2) . . ?
C20 C25 PD1 113.5(2) . . ?
C21 C20 C25 123.7(3) . . ?
C21 C20 P1 121.3(2) . . ?
C25 C20 P1 114.9(2) . . ?
C23 C24 C25 121.7(3) . . ?
C22 C21 C20 119.1(3) . . ?
C22 C23 C24 121.4(3) . . ?
C23 C22 C21 118.9(3) . . ?
C15 C14 C19 119.0(3) . . ?
C15 C14 P1 119.4(2) . . ?
C19 C14 P1 121.2(2) . . ?
C16 C15 C14 120.2(3) . . ?
C16 C17 C18 120.0(3) . . ?
C18 C19 C14 120.3(3) . . ?
C17 C16 C15 120.2(3) . . ?
C19 C18 C17 120.3(3) . . ?
C9 C8 C13 119.9(3) . . ?
C9 C8 P1 117.3(2) . . ?
C13 C8 P1 122.5(2) . . ?
C8 C9 C10 120.1(3) . . ?
C12 C11 C10 120.8(3) . . ?
C9 C10 C11 119.4(3) . . ?
C12 C13 C8 120.3(3) . . ?
C11 C12 C13 119.5(3) . . ?
C5 C4 C3 120.3(3) . . ?
C6 C7 C2 120.4(3) . . ?
C6 C7 N1 125.0(3) . . ?
C2 C7 N1 114.6(3) . . ?
O1 C2 C3 121.3(3) . . ?
O1 C2 C7 120.6(3) . . ?
C3 C2 C7 118.1(3) . . ?
C4 C5 C6 119.9(3) . . ?
C5 C6 C7 120.3(3) . . ?
C4 C3 C2 120.8(3) . . ?
C31 C26 C27 118.8(3) . . ?
C31 C26 P2 125.2(2) . . ?
C27 C26 P2 115.7(2) . . ?
C30 C31 C26 120.5(3) . . ?
C29 C30 C31 120.0(3) . . ?
C29 C28 C27 120.0(3) . . ?
C28 C29 C30 120.1(3) . . ?
C28 C27 C26 120.5(3) . . ?
C39 C38 C43 119.2(3) . . ?
C39 C38 P2 120.5(2) . . ?
C43 C38 P2 120.0(2) . . ?
C40 C39 C38 120.8(3) . . ?
C41 C40 C39 119.8(3) . . ?
C42 C43 C38 119.7(3) . . ?
C40 C41 C42 120.1(3) . . ?
C43 C42 C41 120.4(3) . . ?
C36 C37 C32 120.4(3) . . ?
C35 C36 C37 120.1(3) . . ?
C37 C32 C33 119.0(3) . . ?
C37 C32 P2 122.1(2) . . ?
C33 C32 P2 118.6(2) . . ?
C35 C34 C33 119.8(3) . . ?
C34 C33 C32 120.3(3) . . ?
C36 C35 C34 120.4(3) . . ?
C7 N1 P1 124.4(2) . . ?
C7 N1 PD1 111.43(19) . . ?
P1 N1 PD1 107.82(13) . . ?
C2 O1 PD1 111.27(18) . . ?
O2 C44 C45 121.4(3) . . ?
O2 C44 C45 121.4(3) . 2_655 ?
C45 C44 C45 117.3(6) . 2_655 ?

_refine_diff_density_max         0.489
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.097

####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1855709'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H37 Cl N2 O2 P2 Pd2'
_chemical_formula_weight         983.98

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 '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                   13.6607(5)
_cell_length_b                   16.4857(6)
_cell_length_c                   19.0403(8)
_cell_angle_alpha                90
_cell_angle_beta                 108.269(2)
_cell_angle_gamma                90
_cell_volume                     4071.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1968
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      27.32

_exptl_crystal_description       Prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    1.070
_shelx_estimated_absorpt_T_min   0.754
_shelx_estimated_absorpt_T_max   0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            67644
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.672
_diffrn_reflns_theta_max         30.583
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12435
_reflns_number_gt                9307
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0137P)²+9.5322P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12435
_refine_ls_number_parameters     560
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0463
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0878
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
PD1 Pd 0.56671(2) 0.38539(2) 0.22256(2) 0.01403(6) Uani 0.8765(6) 1 d . U P A 1
PD2 Pd 0.36538(2) 0.50419(2) 0.22930(2) 0.01413(6) Uani 0.8765(6) 1 d . U P A 1
PD1' Pd 0.58698(14) 0.36093(12) 0.27861(11) 0.0168(5) Uani 0.1235(6) 1 d . U P
A 2
PD2' Pd 0.37461(14) 0.48425(13) 0.28935(11) 0.0190(5) Uani 0.1235(6) 1 d . U P
A 2
P1 P 0.79512(7) 0.35542(6) 0.25355(5) 0.01565(18) Uani 0.8765(6) 1 d . U P A 1
P1' P 0.8119(5) 0.3261(4) 0.2954(4) 0.0194(11) Uani 0.1235(6) 1 d . U P A 2
P2' P 0.2965(5) 0.6449(4) 0.3319(4) 0.0180(11) Uani 0.1235(6) 1 d . U P A 2
P2 P 0.29348(7) 0.66361(6) 0.27974(5) 0.01483(18) Uani 0.8765(6) 1 d . U P A 1
CL1 Cl 0.39950(6) 0.41269(5) 0.14580(5) 0.01728(17) Uani 0.8765(6) 1 d . . P A
1
CL1' Cl 0.4341(5) 0.3503(4) 0.3075(4) 0.0264(15) Uani 0.1235(6) 1 d . . P A 2
O2 O 0.38439(18) 0.41761(15) 0.31508(14) 0.0178(4) Uani 0.8765(6) 1 d . . P A 1
O2H H 0.443842 0.384175 0.324094 0.021 Uiso 1 1 d R U . A 1
O2' O 0.3725(13) 0.4923(11) 0.1758(10) 0.0178(4) Uani 0.1235(6) 1 d . . P A 2
O1 O 0.51921(18) 0.32834(15) 0.30601(14) 0.0178(4) Uani 0.8765(6) 1 d . . P A 1
O1' O 0.5189(13) 0.4249(11) 0.1758(10) 0.0178(4) Uani 0.1235(6) 1 d . . P A 2
N1 N 0.7063(2) 0.35823(18) 0.29323(16) 0.0163(4) Uani 0.8765(6) 1 d . . P A 1
N2 N 0.3491(2) 0.57805(18) 0.30775(17) 0.0163(4) Uani 0.8765(6) 1 d . . P A 1
N1' N 0.7155(16) 0.3815(13) 0.2543(12) 0.0163(4) Uani 0.1235(6) 1 d . . P A 2
N2' N 0.3307(16) 0.5962(13) 0.2708(12) 0.0163(4) Uani 0.1235(6) 1 d . . P A 2
C2 C 0.6030(3) 0.2983(2) 0.3605(2) 0.0268(8) Uani 1 1 d . . . . .
C3 C 0.5935(3) 0.2558(2) 0.4204(2) 0.0331(9) Uani 1 1 d . . . . .
H3 H 0.527093 0.247894 0.425336 0.040 Uiso 1 1 calc R U . . .
C4 C 0.6800(3) 0.2242(2) 0.4738(2) 0.0344(9) Uani 1 1 d . . . . .
H4 H 0.671793 0.195538 0.514919 0.041 Uiso 1 1 calc R U . . .
C5 C 0.7768(3) 0.2340(2) 0.4677(2) 0.0364(9) Uani 1 1 d . . . . .
H5 H 0.835526 0.211587 0.503607 0.044 Uiso 1 1 calc R U . . .
C6 C 0.7871(3) 0.2784(2) 0.4065(2) 0.0325(9) Uani 1 1 d . . . . .
H6 H 0.853293 0.286279 0.401278 0.039 Uiso 1 1 calc R U . . .
C7 C 0.7007(3) 0.3103(2) 0.35453(19) 0.0248(7) Uani 1 1 d . . . . .
C8 C 0.8165(2) 0.2540(2) 0.2244(2) 0.0225(7) Uani 1 1 d . . . . .
C9 C 0.7499(3) 0.2276(2) 0.1573(2) 0.0247(7) Uani 1 1 d . . . . .
H9 H 0.700653 0.263979 0.126921 0.030 Uiso 1 1 calc R U . . .
C10 C 0.7550(3) 0.1483(2) 0.1343(2) 0.0277(8) Uani 1 1 d . . . . .
H10 H 0.709571 0.130614 0.088027 0.033 Uiso 1 1 calc R U . . .
C11 C 0.8259(3) 0.0951(2) 0.1784(2) 0.0303(8) Uani 1 1 d . . . . .
H11 H 0.828675 0.040557 0.162949 0.036 Uiso 1 1 calc R U . . .
C12 C 0.8926(3) 0.1211(2) 0.2447(2) 0.0297(8) Uani 1 1 d . . . . .
H12 H 0.941373 0.084369 0.275031 0.036 Uiso 1 1 calc R U . . .
C13 C 0.8891(3) 0.2003(2) 0.2678(2) 0.0279(8) Uani 1 1 d . . . . .
H13 H 0.936378 0.218131 0.313288 0.033 Uiso 1 1 calc R U . . .
C14 C 0.9183(2) 0.3948(2) 0.3098(2) 0.0250(7) Uani 1 1 d . . . . .
C15 C 1.0066(2) 0.3824(2) 0.2895(2) 0.0271(8) Uani 1 1 d . . . . .
H15 H 1.005721 0.345089 0.251249 0.033 Uiso 1 1 calc R U . . .
C16 C 1.0961(3) 0.4250(2) 0.3257(2) 0.0308(8) Uani 1 1 d . . . . .
H16 H 1.155767 0.418331 0.310747 0.037 Uiso 1 1 calc R U . . .
C17 C 1.0989(3) 0.4764(2) 0.3824(2) 0.0322(9) Uani 1 1 d . . . . .
H17 H 1.160882 0.504263 0.407497 0.039 Uiso 1 1 calc R U . . .
C18 C 1.0116(3) 0.4881(2) 0.4038(2) 0.0318(8) Uani 1 1 d . . . . .
H18 H 1.014063 0.523728 0.443570 0.038 Uiso 1 1 calc R U . . .
C19 C 0.9208(3) 0.4478(2) 0.3673(2) 0.0293(8) Uani 1 1 d . . . . .
H19 H 0.860700 0.456346 0.381300 0.035 Uiso 1 1 calc R U . . .
C20 C 0.7427(3) 0.4216(2) 0.17681(19) 0.0251(7) Uani 1 1 d . . . . .
C21 C 0.8035(3) 0.4564(2) 0.1395(2) 0.0312(8) Uani 1 1 d . . . . .
H21 H 0.874893 0.444045 0.152896 0.037 Uiso 1 1 calc R U . . .
C22 C 0.7596(3) 0.5091(2) 0.0826(2) 0.0310(8) Uani 1 1 d . . . . .
H22 H 0.801049 0.533830 0.056819 0.037 Uiso 1 1 calc R U . . .
C23 C 0.6553(3) 0.5265(2) 0.06266(19) 0.0266(8) Uani 1 1 d . . . . .
H23 H 0.626015 0.563389 0.023342 0.032 Uiso 1 1 calc R U . . .
C24 C 0.5928(3) 0.4909(2) 0.09920(19) 0.0250(7) Uani 1 1 d . . . . .
H24 H 0.521271 0.503044 0.084447 0.030 Uiso 1 1 calc R U . . .
C25 C 0.6353(3) 0.4370(2) 0.15787(19) 0.0235(7) Uani 1 1 d . . . . .
C26 C 0.3331(2) 0.5967(2) 0.16096(19) 0.0261(8) Uani 1 1 d . . . . .
C27 C 0.3372(3) 0.5993(2) 0.0883(2) 0.0280(8) Uani 1 1 d . . . . .
H27 H 0.356865 0.552373 0.067106 0.034 Uiso 1 1 calc R U . . .
C28 C 0.3126(3) 0.6702(2) 0.04732(19) 0.0300(8) Uani 1 1 d . . . . .
H28 H 0.316971 0.671270 -0.001501 0.036 Uiso 1 1 calc R U . . .
C29 C 0.2821(3) 0.7392(2) 0.0756(2) 0.0321(8) Uani 1 1 d . . . . .
H29 H 0.266229 0.787204 0.046671 0.039 Uiso 1 1 calc R U . . .
C30 C 0.2748(3) 0.7379(2) 0.1457(2) 0.0308(8) Uani 1 1 d . . . . .
H30 H 0.252183 0.784775 0.165241 0.037 Uiso 1 1 calc R U . . .
C31 C 0.3005(3) 0.6685(2) 0.18783(19) 0.0262(8) Uani 1 1 d . . . . .
C32 C 0.3612(2) 0.7481(2) 0.3346(2) 0.0237(7) Uani 1 1 d . . . . .
C33 C 0.4634(2) 0.7376(2) 0.3785(2) 0.0277(8) Uani 1 1 d . . . . .
H33 H 0.495119 0.685806 0.381888 0.033 Uiso 1 1 calc R U . . .
C34 C 0.5185(3) 0.8028(2) 0.4170(2) 0.0291(8) Uani 1 1 d . . . . .
H34 H 0.587378 0.795604 0.448209 0.035 Uiso 1 1 calc R U . . .
C35 C 0.4728(3) 0.8789(2) 0.4098(2) 0.0280(8) Uani 1 1 d . . . . .
H35 H 0.510901 0.923795 0.435825 0.034 Uiso 1 1 calc R U . . .
C36 C 0.3724(3) 0.8897(2) 0.36516(19) 0.0247(7) Uani 1 1 d . . . . .
H36 H 0.341788 0.942075 0.359866 0.030 Uiso 1 1 calc R U . . .
C37 C 0.3161(3) 0.8238(2) 0.32798(19) 0.0225(7) Uani 1 1 d . . . . .
H37 H 0.246581 0.830922 0.297981 0.027 Uiso 1 1 calc R U . . .
C38 C 0.1608(2) 0.6655(2) 0.2786(2) 0.0252(7) Uani 1 1 d . . . . .
C39 C 0.1289(3) 0.6964(2) 0.3363(2) 0.0266(8) Uani 1 1 d . . . . .
H39 H 0.177273 0.722029 0.377404 0.032 Uiso 1 1 calc R U . . .
C40 C 0.0259(3) 0.6895(2) 0.3334(2) 0.0293(8) Uani 1 1 d . . . . .
H40 H 0.003977 0.711248 0.372207 0.035 Uiso 1 1 calc R U . . .
C41 C -0.0441(3) 0.6513(2) 0.2744(2) 0.0309(9) Uani 1 1 d . . . . .
H41 H -0.114214 0.646568 0.272473 0.037 Uiso 1 1 calc R U . . .
C42 C -0.0117(3) 0.6198(2) 0.2181(2) 0.0309(8) Uani 1 1 d . . . . .
H42 H -0.059781 0.593062 0.177625 0.037 Uiso 1 1 calc R U . . .
C43 C 0.0897(3) 0.6269(2) 0.2200(2) 0.0289(8) Uani 1 1 d . . . . .
H43 H 0.110820 0.605144 0.180873 0.035 Uiso 1 1 calc R U . . .
C44 C 0.3555(2) 0.5372(2) 0.37569(19) 0.0229(7) Uani 1 1 d . . . . .
C45 C 0.3442(2) 0.5763(2) 0.4364(2) 0.0247(7) Uani 1 1 d . . . . .
H45 H 0.328389 0.632573 0.433859 0.030 Uiso 1 1 calc R U . A 2
C46 C 0.3563(3) 0.5325(2) 0.5034(2) 0.0262(7) Uani 1 1 d . . . . .
H46 H 0.348495 0.559119 0.545605 0.031 Uiso 1 1 calc R U . . .
C47 C 0.3795(2) 0.4511(2) 0.50559(19) 0.0210(7) Uani 1 1 d . . . . .
H47 H 0.388344 0.420786 0.549577 0.025 Uiso 1 1 calc R U . . .
C48 C 0.3897(2) 0.4136(2) 0.44273(19) 0.0243(7) Uani 1 1 d . . . . .
H48 H 0.405993 0.357431 0.444801 0.029 Uiso 1 1 calc R U . . .
C49 C 0.3771(2) 0.4549(2) 0.37786(19) 0.0229(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
PD1a C25 1.960(3) . ?
PD1a N1 2.010(3) . ?
PD1a O1 2.116(2) . ?
PD1a CL1 2.3373(9) . ?
PD2a C26 1.963(3) . ?
PD2a N2 1.993(3) . ?
PD2a O2 2.123(2) . ?
PD2a CL1 2.3421(9) . ?
PD1'b C2 1.826(4) . ?
PD1'b C7 1.947(4) . ?
PD1'b N1' 1.98(2) . ?
PD1'b O1' 2.160(18) . ?
PD1'b CL1' 2.328(7) . ?
PD2'b C49 1.743(4) . ?
PD2'b N2' 1.94(2) . ?
PD2'b C44 1.950(4) . ?
PD2'b O2' 2.157(17) . ?
PD2'b CL1' 2.341(7) . ?
P1a N1 1.619(3) . ?
P1a C20 1.783(4) . ?
P1a C14 1.808(3) . ?
P1a C8 1.814(3) . ?
P1'b N1' 1.59(2) . ?
P1'b C14 1.795(8) . ?
P1'b C8 1.817(8) . ?
P1'b C7 2.171(8) . ?
P2'b N2' 1.60(2) . ?
P2'b C38 1.844(7) . ?
P2'b C32 1.911(8) . ?
P2'b C44 2.019(8) . ?
P2'b C45 2.201(8) . ?
P2a N2 1.612(3) . ?
P2a C31 1.784(4) . ?
P2a C38 1.805(3) . ?
P2a C32 1.811(3) . ?
O2a C49 1.375(4) . ?
O2a O2H 0.9516 . ?
O2'b C26 1.799(18) . ?
O1a C2 1.374(4) . ?
O1'b C25 1.739(17) . ?
N1a C7 1.431(4) . ?
N2a C44 1.436(5) . ?
N1'b C20 1.76(2) . ?
N2'b C31 1.92(2) . ?
C2 C3 1.378(5) . ?
C2 C7 1.389(5) . ?
C3 C4 1.397(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.420(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(5) . ?
C6 H6 0.9500 . ?
C8 C9 1.386(5) . ?
C8 C13 1.391(5) . ?
C9 C10 1.388(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.374(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.392(5) . ?
C14 C15 1.393(5) . ?
C15 C16 1.392(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.364(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.386(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.376(5) . ?
C20 C25 1.420(5) . ?
C21 C22 1.370(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.385(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.389(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.403(5) . ?
C24 H24 0.9500 . ?
C26 C27 1.402(5) . ?
C26 C31 1.415(5) . ?
C27 C28 1.387(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.376(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.379(5) . ?
C30 H30 0.9500 . ?
C32 C37 1.380(4) . ?
C32 C33 1.396(4) . ?
C33 C34 1.384(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.388(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.381(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.389(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C43 1.383(5) . ?
C38 C39 1.400(5) . ?
C39 C40 1.395(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.378(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.383(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.379(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.374(5) . ?
C44 C49 1.386(5) . ?
C45 C46 1.430(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.377(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.393(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.374(5) . ?
C48 H48 0.9500 . ?

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
C25 PD1a N1 88.71(14) . . ?
C25 PD1a O1 169.85(12) . . ?
N1a PD1a O1 81.26(11) . . ?
C25 PD1a CL1 95.13(11) . . ?
N1a PD1a CL1 176.17(9) . . ?
O1a PD1a CL1 94.91(7) . . ?
C26 PD2a N2 88.14(14) . . ?
C26 PD2a O2 168.59(13) . . ?
N2a PD2a O2 81.36(11) . . ?
C26 PD2a CL1 95.82(12) . . ?
N2a PD2a CL1 174.31(9) . . ?
O2a PD2a CL1 94.98(7) . . ?
C2 PD1'b C7 43.05(16) . . ?
C2 PD1'b N1' 114.8(6) . . ?
C7 PD1'b N1' 71.8(6) . . ?
C2 PD1'b O1' 162.3(5) . . ?
C7 PD1'b O1' 154.0(5) . . ?
N1'b PD1'b O1' 82.3(8) . . ?
C2 PD1'b CL1' 68.4(2) . . ?
C7 PD1'b CL1' 111.0(2) . . ?
N1'b PD1'b CL1' 174.5(6) . . ?
O1'b PD1'b CL1' 95.0(5) . . ?
C49 PD2'b N2' 110.6(7) . . ?
C49 PD2'b C44 43.64(16) . . ?
N2'b PD2'b C44 67.2(7) . . ?
C49 PD2'b O2' 167.4(5) . . ?
N2'b PD2'b O2' 81.5(8) . . ?
C44 PD2'b O2' 148.7(5) . . ?
C49 PD2'b CL1' 72.2(2) . . ?
N2'b PD2'b CL1' 176.6(7) . . ?
C44 PD2'b CL1' 115.4(2) . . ?
O2'b PD2'b CL1' 95.8(5) . . ?
N1a P1a C20 101.42(17) . . ?
N1a P1a C14 114.05(16) . . ?
C20 P1a C14 108.99(17) . . ?
N1a P1a C8 112.68(15) . . ?
C20 P1a C8 111.99(17) . . ?
C14 P1a C8 107.65(16) . . ?
N1'b P1'b C14 102.6(9) . . ?
N1'b P1'b C8 103.0(9) . . ?
C14 P1'b C8 108.1(4) . . ?
N1'b P1'b C7 73.7(8) . . ?
C14 P1'b C7 131.4(4) . . ?
C8 P1'b C7 120.0(4) . . ?
N2'b P2'b C38 99.4(9) . . ?
N2'b P2'b C32 103.1(9) . . ?
C38 P2'b C32 103.1(4) . . ?
N2'b P2'b C44 71.9(9) . . ?
C38 P2'b C44 126.3(4) . . ?
C32 P2'b C44 130.6(4) . . ?
N2'b P2'b C45 109.2(9) . . ?
C38 P2'b C45 123.7(4) . . ?
C32 P2'b C45 115.5(3) . . ?
C44 P2'b C45 37.70(18) . . ?
N2a P2a C31 101.48(17) . . ?
N2a P2a C38 112.73(16) . . ?
C31 P2a C38 110.45(17) . . ?
N2a P2a C32 112.32(16) . . ?
C31 P2a C32 110.86(17) . . ?
C38 P2a C32 108.86(16) . . ?
PD1a CL1a PD2 93.61(3) . . ?
PD1'b CL1'b PD2' 100.9(3) . . ?
C49 O2a PD2 110.1(2) . . ?
C49 O2a O2H 113.1 . . ?
PD2a O2a O2H 114.8 . . ?
C26 O2'b PD2' 97.2(8) . . ?
C2 O1a PD1 110.4(2) . . ?
C25 O1'b PD1' 94.2(8) . . ?
C7 N1a P1 127.2(2) . . ?
C7 N1a PD1 112.8(2) . . ?
P1a N1a PD1 112.74(16) . . ?
C44 N2a P2 126.7(2) . . ?
C44 N2a PD2 113.5(2) . . ?
P2a N2a PD2 116.01(17) . . ?
P1'b N1'b C20 105.6(12) . . ?
P1'b N1'b PD1' 116.3(12) . . ?
C20 N1'b PD1' 134.1(12) . . ?
P2'b N2'b C31 104.6(12) . . ?
P2'b N2'b PD2' 119.3(13) . . ?
C31 N2'b PD2' 135.7(12) . . ?
O1a C2 C3 122.4(3) . . ?
O1a C2 C7 118.7(3) . . ?
C3 C2 C7 118.9(3) . . ?
C3 C2 PD1' 167.7(3) . . ?
C7 C2 PD1' 73.1(2) . . ?
C2 C3 C4 121.0(4) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 120.8(4) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 120.1(4) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C2 120.8(3) . . ?
C6 C7 N1 122.8(3) . . ?
C2 C7 N1 116.4(3) . . ?
C6 C7 PD1' 175.2(3) . . ?
C2 C7 PD1' 63.8(2) . . ?
C6 C7 P1' 80.7(3) . . ?
C2 C7 P1' 155.0(3) . . ?
PD1'b C7 P1' 95.1(3) . . ?
C9 C8 C13 119.2(3) . . ?
C9 C8 P1 116.7(3) . . ?
C13 C8 P1 123.9(3) . . ?
C9 C8 P1' 136.5(3) . . ?
C13 C8 P1' 99.1(3) . . ?
C8 C9 C10 120.2(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.5(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C12 C13 C8 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
C19 C14 C15 120.1(3) . . ?
C19 C14 P1' 109.6(3) . . ?
C15 C14 P1' 126.5(4) . . ?
C19 C14 P1 118.7(3) . . ?
C15 C14 P1 120.6(3) . . ?
C16 C15 C14 119.4(3) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 120.3(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 120.1(4) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C14 119.5(3) . . ?
C18 C19 H19 120.2 . . ?
C14 C19 H19 120.2 . . ?
C21 C20 C25 122.5(3) . . ?
C21 C20 N1' 155.5(7) . . ?
C25 C20 N1' 78.8(7) . . ?
C21 C20 P1 121.8(3) . . ?
C25 C20 P1 115.8(3) . . ?
C22 C21 C20 119.2(3) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
C21 C22 C23 120.4(3) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
C22 C23 C24 121.0(3) . . ?
C22 C23 H23 119.5 . . ?
C24 C23 H23 119.5 . . ?
C23 C24 C25 120.1(3) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C20 116.9(3) . . ?
C24 C25 O1' 93.1(6) . . ?
C20 C25 O1' 149.9(6) . . ?
C24 C25 PD1 128.0(3) . . ?
C20 C25 PD1 115.0(3) . . ?
C27 C26 C31 116.4(3) . . ?
C27 C26 O2' 94.7(6) . . ?
C31 C26 O2' 148.8(6) . . ?
C27 C26 PD2 127.4(3) . . ?
C31 C26 PD2 116.1(3) . . ?
C28 C27 C26 120.3(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C29 C28 C27 121.7(3) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C30 C29 C28 119.5(4) . . ?
C30 C29 H29 120.3 . . ?
C28 C29 H29 120.3 . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C30 C31 C26 122.4(3) . . ?
C30 C31 P2 121.7(3) . . ?
C26 C31 P2 115.9(3) . . ?
C30 C31 N2' 160.9(7) . . ?
C26 C31 N2' 76.5(7) . . ?
C37 C32 C33 120.0(3) . . ?
C37 C32 P2 120.7(3) . . ?
C33 C32 P2 119.0(3) . . ?
C37 C32 P2' 127.9(3) . . ?
C33 C32 P2' 105.9(3) . . ?
C34 C33 C32 119.8(3) . . ?
C34 C33 H33 120.1 . . ?
C32 C33 H33 120.1 . . ?
C33 C34 C35 119.8(3) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 120.5(3) . . ?
C36 C35 H35 119.8 . . ?
C34 C35 H35 119.8 . . ?
C35 C36 C37 119.8(3) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C32 C37 C36 120.1(3) . . ?
C32 C37 H37 119.9 . . ?
C36 C37 H37 119.9 . . ?
C43 C38 C39 119.2(3) . . ?
C43 C38 P2 116.8(3) . . ?
C39 C38 P2 123.7(3) . . ?
C43 C38 P2' 133.7(3) . . ?
C39 C38 P2' 98.1(3) . . ?
C40 C39 C38 119.8(3) . . ?
C40 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
C41 C40 C39 120.2(4) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C40 C41 C42 119.6(3) . . ?
C40 C41 H41 120.2 . . ?
C42 C41 H41 120.2 . . ?
C43 C42 C41 120.7(3) . . ?
C43 C42 H42 119.7 . . ?
C41 C42 H42 119.7 . . ?
C42 C43 C38 120.4(4) . . ?
C42 C43 H43 119.8 . . ?
C38 C43 H43 119.8 . . ?
C45 C44 C49 120.9(3) . . ?
C45 C44 N2 123.1(3) . . ?
C49 C44 N2 116.0(3) . . ?
C45 C44 PD2' 178.2(3) . . ?
C49 C44 PD2' 60.2(2) . . ?
C45 C44 P2' 78.4(3) . . ?
C49 C44 P2' 157.9(3) . . ?
PD2'b C44 P2' 100.8(3) . . ?
C44 C45 C46 120.1(3) . . ?
C44 C45 P2' 63.9(3) . . ?
C46 C45 P2' 169.8(3) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
P2'b C45 H45 56.9 . . ?
C47 C46 C45 118.7(3) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
C46 C47 C48 119.4(3) . . ?
C46 C47 H47 120.3 . . ?
C48 C47 H47 120.3 . . ?
C49 C48 C47 122.3(3) . . ?
C49 C48 H48 118.9 . . ?
C47 C48 H48 118.9 . . ?
C48 C49 O2 122.5(3) . . ?
C48 C49 C44 118.6(3) . . ?
O2a C49 C44 119.0(3) . . ?
C48 C49 PD2' 165.0(3) . . ?
C44 C49 PD2' 76.1(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
O2a O2Ha O1a 0.95 1.50 2.406(3) 157.3 .
C24 H24 CL1a 0.95 2.75 3.300(3) 117.6 .
C27 H27 CL1a 0.95 2.71 3.287(4) 119.9 .
C30 H30 CL1'b_$1 0.95 2.96 3.736(8) 140.3 2
C37 H37 CL1a_$1 0.95 2.88 3.463(3) 120.9 2
C37 H37 CL1a_$1 0.95 2.88 3.463(3) 120.9 2

_refine_diff_density_max         1.293
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.124

####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1855711'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H42 N O P3 Pd'
_chemical_formula_weight         872.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   24.4601(12)
_cell_length_b                   14.8032(7)
_cell_length_c                   25.3318(12)
_cell_angle_alpha                90
_cell_angle_beta                 98.606(3)
_cell_angle_gamma                90
_cell_volume                     9069.1(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1817
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      26.07

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_F_000             3584
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    0.551
_shelx_estimated_absorpt_T_min   0.907
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.8869
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            63575
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.613
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             9279
_reflns_number_gt                6621
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+8.0610P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9279
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0419
_refine_ls_wR_factor_ref         0.1099
_refine_ls_wR_factor_gt          0.1027
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001

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
C2 C 0.64918(16) 0.1722(3) 0.60449(16) 0.0378(9) Uani 1 1 d . . . . .
C3 C 0.6675(2) 0.0824(3) 0.61145(19) 0.0530(12) Uani 1 1 d . . . . .
H3 H 0.646780 0.039286 0.627911 0.064 Uiso 1 1 calc R U . . .
C4 C 0.7156(2) 0.0584(3) 0.5942(2) 0.0583(14) Uani 1 1 d . . . . .
H4 H 0.727612 -0.002582 0.598121 0.070 Uiso 1 1 calc R U . . .
C5 C 0.74743(18) 0.1193(3) 0.57118(18) 0.0480(11) Uani 1 1 d . . . . .
H5 H 0.781259 0.101176 0.560210 0.058 Uiso 1 1 calc R U . . .
C6 C 0.72894(15) 0.2078(2) 0.56441(14) 0.0330(9) Uani 1 1 d . . . . .
H6 H 0.750039 0.250283 0.547884 0.040 Uiso 1 1 calc R U . . .
C7 C 0.67989(15) 0.2353(2) 0.58144(14) 0.0283(8) Uani 1 1 d . . . . .
C8 C 0.56730(14) 0.4214(3) 0.60115(14) 0.0298(8) Uani 1 1 d . . . . .
C9 C 0.57203(15) 0.5141(3) 0.60897(16) 0.0394(10) Uani 1 1 d . . . . .
H9 H 0.593663 0.548584 0.588143 0.047 Uiso 1 1 calc R U . . .
C10 C 0.54553(17) 0.5571(3) 0.64689(17) 0.0485(11) Uani 1 1 d . . . . .
H10 H 0.548755 0.620643 0.651575 0.058 Uiso 1 1 calc R U . . .
C11 C 0.51471(17) 0.5075(4) 0.67751(17) 0.0517(12) Uani 1 1 d . . . . .
H11 H 0.496800 0.536889 0.703562 0.062 Uiso 1 1 calc R U . . .
C12 C 0.50960(15) 0.4153(3) 0.67066(16) 0.0455(11) Uani 1 1 d . . . . .
H12 H 0.488197 0.381373 0.691982 0.055 Uiso 1 1 calc R U . . .
C13 C 0.53593(14) 0.3715(3) 0.63231(15) 0.0379(9) Uani 1 1 d . . . . .
H13 H 0.532373 0.307986 0.627592 0.046 Uiso 1 1 calc R U . . .
C14 C 0.55840(14) 0.2962(2) 0.51007(13) 0.0251(8) Uani 1 1 d . . . . .
C15 C 0.50143(14) 0.3123(2) 0.50331(14) 0.0278(8) Uani 1 1 d . . . . .
H15 H 0.486509 0.355504 0.524966 0.033 Uiso 1 1 calc R U . . .
C16 C 0.46711(15) 0.2647(2) 0.46483(16) 0.0348(9) Uani 1 1 d . . . . .
H16 H 0.428434 0.275930 0.459836 0.042 Uiso 1 1 calc R U . . .
C17 C 0.48835(15) 0.2008(2) 0.43333(15) 0.0329(9) Uani 1 1 d . . . . .
H17 H 0.464523 0.168374 0.406858 0.039 Uiso 1 1 calc R U . . .
C18 C 0.54450(15) 0.1850(3) 0.44103(14) 0.0328(9) Uani 1 1 d . . . . .
H18 H 0.559205 0.140626 0.419965 0.039 Uiso 1 1 calc R U . . .
C19 C 0.57957(15) 0.2322(2) 0.47861(14) 0.0298(8) Uani 1 1 d . . . . .
H19 H 0.618236 0.221001 0.483067 0.036 Uiso 1 1 calc R U . . .
C20 C 0.62281(14) 0.4594(2) 0.51181(14) 0.0237(8) Uani 1 1 d . . . . .
C21 C 0.58836(14) 0.4905(2) 0.46649(13) 0.0253(8) Uani 1 1 d . . . . .
H21 H 0.552609 0.465164 0.456608 0.030 Uiso 1 1 calc R U . . .
C22 C 0.60682(15) 0.5585(2) 0.43614(14) 0.0306(8) Uani 1 1 d . . . . .
H22 H 0.583853 0.580231 0.405175 0.037 Uiso 1 1 calc R U . . .
C23 C 0.65918(15) 0.5948(2) 0.45128(14) 0.0302(8) Uani 1 1 d . . . . .
H23 H 0.671935 0.641845 0.430696 0.036 Uiso 1 1 calc R U . . .
C24 C 0.69276(14) 0.5630(2) 0.49599(14) 0.0270(8) Uani 1 1 d . . . . .
H24 H 0.728632 0.588229 0.505257 0.032 Uiso 1 1 calc R U . . .
C25 C 0.67579(13) 0.4952(2) 0.52802(13) 0.0234(7) Uani 1 1 d . . . . .
C26 C 0.72819(14) 0.6655(2) 0.61264(15) 0.0299(8) Uani 1 1 d . . . . .
C27 C 0.68782(14) 0.6763(2) 0.64513(15) 0.0297(8) Uani 1 1 d . . . . .
H27 H 0.682748 0.630837 0.670408 0.036 Uiso 1 1 calc R U . . .
C28 C 0.65466(14) 0.7531(2) 0.64113(16) 0.0349(9) Uani 1 1 d . . . . .
H28 H 0.627928 0.761017 0.664356 0.042 Uiso 1 1 calc R U . . .
C29 C 0.66086(15) 0.8177(2) 0.60317(16) 0.0367(9) Uani 1 1 d . . . . .
H29 H 0.638094 0.869995 0.599935 0.044 Uiso 1 1 calc R U . . .
C30 C 0.70031(15) 0.8062(3) 0.56980(17) 0.0389(10) Uani 1 1 d . . . . .
H30 H 0.703761 0.850122 0.543173 0.047 Uiso 1 1 calc R U . . .
C31 C 0.73459(15) 0.7319(2) 0.57467(16) 0.0350(9) Uani 1 1 d . . . . .
H31 H 0.762389 0.725791 0.552435 0.042 Uiso 1 1 calc R U . . .
C32 C 0.82705(15) 0.5755(2) 0.58441(16) 0.0324(9) Uani 1 1 d . . . . .
C33 C 0.83591(15) 0.5149(3) 0.54489(15) 0.0351(9) Uani 1 1 d . . . . .
H33 H 0.809503 0.469060 0.533839 0.042 Uiso 1 1 calc R U . . .
C34 C 0.88391(16) 0.5216(3) 0.52137(18) 0.0446(11) Uani 1 1 d . . . . .
H34 H 0.889823 0.480663 0.493908 0.054 Uiso 1 1 calc R U . . .
C35 C 0.92221(18) 0.5864(3) 0.5375(2) 0.0553(13) Uani 1 1 d . . . . .
H35 H 0.955065 0.589925 0.521802 0.066 Uiso 1 1 calc R U . . .
C36 C 0.91327(18) 0.6471(3) 0.5768(2) 0.0644(15) Uani 1 1 d . . . . .
H36 H 0.939773 0.692843 0.587852 0.077 Uiso 1 1 calc R U . . .
C37 C 0.86623(16) 0.6413(3) 0.59992(19) 0.0482(11) Uani 1 1 d . . . . .
H37 H 0.860457 0.683053 0.627001 0.058 Uiso 1 1 calc R U . . .
C38 C 0.80554(14) 0.2701(2) 0.67746(14) 0.0259(8) Uani 1 1 d . . . . .
C39 C 0.84911(15) 0.2628(3) 0.64806(16) 0.0388(10) Uani 1 1 d . . . . .
H39 H 0.858361 0.312873 0.627647 0.047 Uiso 1 1 calc R U . . .
C40 C 0.87901(16) 0.1837(3) 0.64826(17) 0.0448(11) Uani 1 1 d . . . . .
H40 H 0.908830 0.179459 0.628289 0.054 Uiso 1 1 calc R U . . .
C41 C 0.86530(16) 0.1103(3) 0.67777(16) 0.0390(10) Uani 1 1 d . . . . .
H41 H 0.885827 0.055761 0.678198 0.047 Uiso 1 1 calc R U . . .
C42 C 0.82176(16) 0.1168(3) 0.70650(15) 0.0363(9) Uani 1 1 d . . . . .
H42 H 0.812112 0.066391 0.726437 0.044 Uiso 1 1 calc R U . . .
C43 C 0.79230(15) 0.1959(2) 0.70634(14) 0.0312(8) Uani 1 1 d . . . . .
H43 H 0.762467 0.199688 0.726324 0.037 Uiso 1 1 calc R U . . .
C44 C 0.72314(13) 0.3667(2) 0.72593(13) 0.0243(7) Uani 1 1 d . . . . .
C45 C 0.74047(17) 0.3856(3) 0.77934(15) 0.0414(10) Uani 1 1 d . . . . .
H45 H 0.777268 0.405542 0.790722 0.050 Uiso 1 1 calc R U . . .
C46 C 0.70458(18) 0.3757(3) 0.81616(16) 0.0488(11) Uani 1 1 d . . . . .
H46 H 0.716873 0.390102 0.852547 0.059 Uiso 1 1 calc R U . . .
C47 C 0.65180(16) 0.3456(2) 0.80125(15) 0.0343(9) Uani 1 1 d . . . . .
H47 H 0.627439 0.339540 0.826933 0.041 Uiso 1 1 calc R U . . .
C48 C 0.63442(16) 0.3244(3) 0.74902(15) 0.0445(11) Uani 1 1 d . . . . .
H48 H 0.598299 0.300872 0.738455 0.053 Uiso 1 1 calc R U . . .
C49 C 0.66930(15) 0.3370(3) 0.71147(16) 0.0434(10) Uani 1 1 d . . . . .
H49 H 0.656043 0.325017 0.674947 0.052 Uiso 1 1 calc R U . . .
C50 C 0.79677(14) 0.5530(2) 0.68929(15) 0.0306(8) Uani 1 1 d . . . . .
H50A H 0.826052 0.599074 0.698167 0.037 Uiso 1 1 calc R U . . .
H50B H 0.767631 0.564018 0.711759 0.037 Uiso 1 1 calc R U . . .
C51 C 0.82056(14) 0.4604(2) 0.69988(16) 0.0321(9) Uani 1 1 d . . . . .
H51A H 0.832393 0.451944 0.738675 0.038 Uiso 1 1 calc R U . . .
H52B H 0.853281 0.452664 0.681549 0.038 Uiso 1 1 calc R U . . .
N1 N 0.66433(11) 0.32722(18) 0.57436(11) 0.0246(6) Uani 1 1 d . . . . .
O1 O 0.60115(11) 0.20065(19) 0.61944(11) 0.0460(7) Uani 1 1 d . . . . .
P1 P 0.60479(4) 0.36881(6) 0.55254(4) 0.0237(2) Uani 1 1 d . . . . .
P2 P 0.76743(4) 0.56115(6) 0.61854(4) 0.0267(2) Uani 1 1 d . . . . .
P3 P 0.76731(4) 0.37610(6) 0.67498(4) 0.0248(2) Uani 1 1 d . . . . .
PD1 Pd 0.71876(2) 0.43579(2) 0.59534(2) 0.02275(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 O1 1.355(4) . ?
C2 C7 1.382(5) . ?
C2 C3 1.405(6) . ?
C3 C4 1.362(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(5) . ?
C6 H6 0.9500 . ?
C7 N1 1.417(4) . ?
C8 C13 1.392(5) . ?
C8 C9 1.389(5) . ?
C8 P1 1.817(3) . ?
C9 C10 1.391(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.372(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.380(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.402(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C19 1.388(5) . ?
C14 C15 1.399(5) . ?
C14 P1 1.798(4) . ?
C15 C16 1.381(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.388(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.374(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.397(5) . ?
C20 C25 1.404(5) . ?
C20 P1 1.786(3) . ?
C21 C22 1.383(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.389(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.378(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.393(4) . ?
C24 H24 0.9500 . ?
C25 PD1 2.061(3) . ?
C26 C27 1.386(5) . ?
C26 C31 1.401(5) . ?
C26 P2 1.812(4) . ?
C27 C28 1.391(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.385(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.377(5) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C33 1.385(5) . ?
C32 C37 1.381(5) . ?
C32 P2 1.816(4) . ?
C33 C34 1.397(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.360(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.369(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C43 1.385(5) . ?
C38 C39 1.393(5) . ?
C38 P3 1.823(3) . ?
C39 C40 1.381(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.388(5) . ?
C40 H40 0.9500 . ?
C41 C42 1.380(5) . ?
C41 H41 0.9500 . ?
C42 C43 1.375(5) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C45 1.385(5) . ?
C44 C49 1.385(5) . ?
C44 P3 1.808(3) . ?
C45 C46 1.381(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.365(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.364(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.382(5) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 C51 1.499(5) . ?
C50 P2 1.832(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 P3 1.845(4) . ?
C51 H51A 0.9900 . ?
C51 H52B 0.9900 . ?
N1 P1 1.601(3) . ?
N1 PD1 2.104(3) . ?
P2 PD1 2.2353(9) . ?
P3 PD1 2.3544(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
O1 C2 C7 117.2(3) . . ?
O1 C2 C3 122.2(4) . . ?
C7 C2 C3 120.6(4) . . ?
C4 C3 C2 118.8(4) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 122.4(4) . . ?
C3 C4 H4 118.8 . . ?
C5 C4 H4 118.8 . . ?
C4 C5 C6 118.4(4) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C7 C6 C5 121.1(4) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C2 C7 C6 118.7(3) . . ?
C2 C7 N1 123.4(3) . . ?
C6 C7 N1 117.9(3) . . ?
C13 C8 C9 119.0(3) . . ?
C13 C8 P1 122.2(3) . . ?
C9 C8 P1 118.7(3) . . ?
C8 C9 C10 120.9(4) . . ?
C8 C9 H9 119.6 . . ?
C10 C9 H9 119.6 . . ?
C11 C10 C9 119.9(4) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C12 120.3(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C13 120.2(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C8 C13 C12 119.8(4) . . ?
C8 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C19 C14 C15 119.8(3) . . ?
C19 C14 P1 119.7(3) . . ?
C15 C14 P1 120.0(3) . . ?
C16 C15 C14 119.3(3) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
C15 C16 C17 120.9(3) . . ?
C15 C16 H16 119.6 . . ?
C17 C16 H16 119.6 . . ?
C18 C17 C16 119.0(3) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C14 119.8(3) . . ?
C18 C19 H19 120.1 . . ?
C14 C19 H19 120.1 . . ?
C21 C20 C25 122.2(3) . . ?
C21 C20 P1 123.5(3) . . ?
C25 C20 P1 114.3(3) . . ?
C22 C21 C20 119.4(3) . . ?
C22 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?
C21 C22 C23 119.5(3) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C22 C23 C24 120.4(3) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C25 122.1(3) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C24 C25 C20 116.4(3) . . ?
C24 C25 PD1 129.0(3) . . ?
C20 C25 PD1 114.5(2) . . ?
C27 C26 C31 119.3(3) . . ?
C27 C26 P2 117.7(3) . . ?
C31 C26 P2 122.9(3) . . ?
C26 C27 C28 120.7(3) . . ?
C26 C27 H27 119.6 . . ?
C28 C27 H27 119.6 . . ?
C29 C28 C27 119.5(3) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 119.9(3) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C31 C30 C29 120.9(4) . . ?
C31 C30 H30 119.5 . . ?
C29 C30 H30 119.5 . . ?
C30 C31 C26 119.5(3) . . ?
C30 C31 H31 120.2 . . ?
C26 C31 H31 120.2 . . ?
C33 C32 C37 119.0(3) . . ?
C33 C32 P2 119.5(3) . . ?
C37 C32 P2 121.3(3) . . ?
C32 C33 C34 119.6(4) . . ?
C32 C33 H33 120.2 . . ?
C34 C33 H33 120.2 . . ?
C35 C34 C33 120.4(4) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 119.9(4) . . ?
C34 C35 H35 120.0 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 120.0(4) . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C32 121.0(4) . . ?
C36 C37 H37 119.5 . . ?
C32 C37 H37 119.5 . . ?
C43 C38 C39 118.6(3) . . ?
C43 C38 P3 122.8(3) . . ?
C39 C38 P3 118.5(3) . . ?
C40 C39 C38 120.7(4) . . ?
C40 C39 H39 119.6 . . ?
C38 C39 H39 119.6 . . ?
C41 C40 C39 119.7(3) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C42 C41 C40 119.8(4) . . ?
C42 C41 H41 120.1 . . ?
C40 C41 H41 120.1 . . ?
C43 C42 C41 120.2(4) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C38 120.9(3) . . ?
C42 C43 H43 119.6 . . ?
C38 C43 H43 119.6 . . ?
C45 C44 C49 117.6(3) . . ?
C45 C44 P3 123.6(3) . . ?
C49 C44 P3 118.8(3) . . ?
C46 C45 C44 120.4(4) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C47 C46 C45 121.2(4) . . ?
C47 C46 H46 119.4 . . ?
C45 C46 H46 119.4 . . ?
C46 C47 C48 119.2(3) . . ?
C46 C47 H47 120.4 . . ?
C48 C47 H47 120.4 . . ?
C47 C48 C49 120.1(4) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 H48 120.0 . . ?
C48 C49 C44 121.4(4) . . ?
C48 C49 H49 119.3 . . ?
C44 C49 H49 119.3 . . ?
C51 C50 P2 108.7(3) . . ?
C51 C50 H50A 110.0 . . ?
P2 C50 H50A 110.0 . . ?
C51 C50 H50B 110.0 . . ?
P2 C50 H50B 110.0 . . ?
H50A C50 H50B 108.3 . . ?
C50 C51 P3 108.8(2) . . ?
C50 C51 H51A 109.9 . . ?
P3 C51 H51A 109.9 . . ?
C50 C51 H52B 109.9 . . ?
P3 C51 H52B 109.9 . . ?
H51A C51 H52B 108.3 . . ?
C7 N1 P1 128.8(2) . . ?
C7 N1 PD1 123.6(2) . . ?
P1 N1 PD1 107.58(14) . . ?
N1 P1 C20 101.40(15) . . ?
N1 P1 C14 115.90(15) . . ?
C20 P1 C14 106.91(16) . . ?
N1 P1 C8 117.12(16) . . ?
C20 P1 C8 105.25(16) . . ?
C14 P1 C8 108.91(16) . . ?
C32 P2 C26 108.31(16) . . ?
C32 P2 C50 104.38(17) . . ?
C26 P2 C50 105.17(17) . . ?
C32 P2 PD1 113.97(13) . . ?
C26 P2 PD1 115.54(11) . . ?
C50 P2 PD1 108.54(11) . . ?
C44 P3 C38 105.49(15) . . ?
C44 P3 C51 105.96(17) . . ?
C38 P3 C51 103.76(16) . . ?
C44 P3 PD1 111.22(11) . . ?
C38 P3 PD1 122.88(12) . . ?
C51 P3 PD1 106.20(12) . . ?
C25 PD1 N1 83.78(12) . . ?
C25 PD1 P2 92.81(10) . . ?
N1 PD1 P2 173.01(8) . . ?
C25 PD1 P3 176.57(9) . . ?
N1 PD1 P3 98.55(8) . . ?
P2 PD1 P3 84.60(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
O1 C2 C3 C4 178.4(4) . . . . ?
C7 C2 C3 C4 -1.2(6) . . . . ?
C2 C3 C4 C5 1.4(7) . . . . ?
C3 C4 C5 C6 -1.5(7) . . . . ?
C4 C5 C6 C7 1.4(6) . . . . ?
O1 C2 C7 C6 -178.5(3) . . . . ?
C3 C2 C7 C6 1.1(6) . . . . ?
O1 C2 C7 N1 1.8(5) . . . . ?
C3 C2 C7 N1 -178.6(4) . . . . ?
C5 C6 C7 C2 -1.2(5) . . . . ?
C5 C6 C7 N1 178.5(3) . . . . ?
C13 C8 C9 C10 -0.6(6) . . . . ?
P1 C8 C9 C10 -178.0(3) . . . . ?
C8 C9 C10 C11 0.7(6) . . . . ?
C9 C10 C11 C12 -0.4(7) . . . . ?
C10 C11 C12 C13 0.0(6) . . . . ?
C9 C8 C13 C12 0.3(6) . . . . ?
P1 C8 C13 C12 177.5(3) . . . . ?
C11 C12 C13 C8 0.0(6) . . . . ?
C19 C14 C15 C16 -0.8(5) . . . . ?
P1 C14 C15 C16 170.6(3) . . . . ?
C14 C15 C16 C17 0.7(5) . . . . ?
C15 C16 C17 C18 0.2(6) . . . . ?
C16 C17 C18 C19 -0.9(5) . . . . ?
C17 C18 C19 C14 0.8(5) . . . . ?
C15 C14 C19 C18 0.0(5) . . . . ?
P1 C14 C19 C18 -171.4(3) . . . . ?
C25 C20 C21 C22 0.4(5) . . . . ?
P1 C20 C21 C22 -177.3(3) . . . . ?
C20 C21 C22 C23 -0.1(5) . . . . ?
C21 C22 C23 C24 0.4(5) . . . . ?
C22 C23 C24 C25 -1.0(5) . . . . ?
C23 C24 C25 C20 1.2(5) . . . . ?
C23 C24 C25 PD1 178.8(3) . . . . ?
C21 C20 C25 C24 -0.8(5) . . . . ?
P1 C20 C25 C24 177.0(2) . . . . ?
C21 C20 C25 PD1 -178.9(2) . . . . ?
P1 C20 C25 PD1 -1.0(3) . . . . ?
C31 C26 C27 C28 -1.4(5) . . . . ?
P2 C26 C27 C28 -177.4(3) . . . . ?
C26 C27 C28 C29 2.1(5) . . . . ?
C27 C28 C29 C30 -0.7(6) . . . . ?
C28 C29 C30 C31 -1.5(6) . . . . ?
C29 C30 C31 C26 2.3(6) . . . . ?
C27 C26 C31 C30 -0.8(5) . . . . ?
P2 C26 C31 C30 174.9(3) . . . . ?
C37 C32 C33 C34 -0.3(6) . . . . ?
P2 C32 C33 C34 -175.2(3) . . . . ?
C32 C33 C34 C35 0.9(6) . . . . ?
C33 C34 C35 C36 -1.1(7) . . . . ?
C34 C35 C36 C37 0.8(7) . . . . ?
C35 C36 C37 C32 -0.2(7) . . . . ?
C33 C32 C37 C36 0.0(6) . . . . ?
P2 C32 C37 C36 174.7(4) . . . . ?
C43 C38 C39 C40 -0.9(6) . . . . ?
P3 C38 C39 C40 -179.4(3) . . . . ?
C38 C39 C40 C41 0.4(6) . . . . ?
C39 C40 C41 C42 0.3(6) . . . . ?
C40 C41 C42 C43 -0.6(6) . . . . ?
C41 C42 C43 C38 0.2(6) . . . . ?
C39 C38 C43 C42 0.6(6) . . . . ?
P3 C38 C43 C42 179.1(3) . . . . ?
C49 C44 C45 C46 -0.6(6) . . . . ?
P3 C44 C45 C46 -179.1(3) . . . . ?
C44 C45 C46 C47 1.2(7) . . . . ?
C45 C46 C47 C48 0.5(7) . . . . ?
C46 C47 C48 C49 -2.7(7) . . . . ?
C47 C48 C49 C44 3.4(7) . . . . ?
C45 C44 C49 C48 -1.6(6) . . . . ?
P3 C44 C49 C48 176.9(3) . . . . ?
P2 C50 C51 P3 -52.5(3) . . . . ?
C2 C7 N1 P1 -44.8(5) . . . . ?
C6 C7 N1 P1 135.6(3) . . . . ?
C2 C7 N1 PD1 132.4(3) . . . . ?
C6 C7 N1 PD1 -47.3(4) . . . . ?
C7 N1 P1 C20 -139.9(3) . . . . ?
PD1 N1 P1 C20 42.55(17) . . . . ?
C7 N1 P1 C14 -24.6(3) . . . . ?
PD1 N1 P1 C14 157.87(13) . . . . ?
C7 N1 P1 C8 106.2(3) . . . . ?
PD1 N1 P1 C8 -71.32(19) . . . . ?
C21 C20 P1 N1 149.9(3) . . . . ?
C25 C20 P1 N1 -28.0(3) . . . . ?
C21 C20 P1 C14 28.1(3) . . . . ?
C25 C20 P1 C14 -149.8(2) . . . . ?
C21 C20 P1 C8 -87.7(3) . . . . ?
C25 C20 P1 C8 94.5(3) . . . . ?
C19 C14 P1 N1 -29.7(3) . . . . ?
C15 C14 P1 N1 159.0(3) . . . . ?
C19 C14 P1 C20 82.5(3) . . . . ?
C15 C14 P1 C20 -88.9(3) . . . . ?
C19 C14 P1 C8 -164.2(3) . . . . ?
C15 C14 P1 C8 24.4(3) . . . . ?
C13 C8 P1 N1 -82.9(3) . . . . ?
C9 C8 P1 N1 94.4(3) . . . . ?
C13 C8 P1 C20 165.4(3) . . . . ?
C9 C8 P1 C20 -17.3(3) . . . . ?
C13 C8 P1 C14 51.1(4) . . . . ?
C9 C8 P1 C14 -131.7(3) . . . . ?
C33 C32 P2 C26 -125.1(3) . . . . ?
C37 C32 P2 C26 60.1(4) . . . . ?
C33 C32 P2 C50 123.2(3) . . . . ?
C37 C32 P2 C50 -51.5(4) . . . . ?
C33 C32 P2 PD1 4.9(3) . . . . ?
C37 C32 P2 PD1 -169.8(3) . . . . ?
C27 C26 P2 C32 -166.5(3) . . . . ?
C31 C26 P2 C32 17.7(4) . . . . ?
C27 C26 P2 C50 -55.4(3) . . . . ?
C31 C26 P2 C50 128.8(3) . . . . ?
C27 C26 P2 PD1 64.3(3) . . . . ?
C31 C26 P2 PD1 -111.5(3) . . . . ?
C51 C50 P2 C32 -77.1(3) . . . . ?
C51 C50 P2 C26 169.0(2) . . . . ?
C51 C50 P2 PD1 44.8(3) . . . . ?
C45 C44 P3 C38 83.7(3) . . . . ?
C49 C44 P3 C38 -94.8(3) . . . . ?
C45 C44 P3 C51 -25.9(4) . . . . ?
C49 C44 P3 C51 155.6(3) . . . . ?
C45 C44 P3 PD1 -140.9(3) . . . . ?
C49 C44 P3 PD1 40.6(3) . . . . ?
C43 C38 P3 C44 11.1(3) . . . . ?
C39 C38 P3 C44 -170.4(3) . . . . ?
C43 C38 P3 C51 122.2(3) . . . . ?
C39 C38 P3 C51 -59.3(3) . . . . ?
C43 C38 P3 PD1 -117.7(3) . . . . ?
C39 C38 P3 PD1 60.8(3) . . . . ?
C50 C51 P3 C44 -80.7(3) . . . . ?
C50 C51 P3 C38 168.5(3) . . . . ?
C50 C51 P3 PD1 37.7(3) . . . . ?

_refine_diff_density_max         0.504
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.083

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.023 0.250 399 110 ' '
2 0.500 -0.023 0.750 399 110 ' '
3 0.000 0.477 0.750 399 110 ' '
4 0.000 0.523 0.250 399 110 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1855710'
_audit_update_record             
;
2018-07-13 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C77 H64 Cl6 N2 O2 P4 Pd2'
_chemical_formula_weight         1598.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   23.8548(12)
_cell_length_b                   9.0603(5)
_cell_length_c                   35.985(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.589(3)
_cell_angle_gamma                90
_cell_volume                     7453.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1919
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      25.45

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_F_000             3240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.830
_shelx_estimated_absorpt_T_min   0.852
_shelx_estimated_absorpt_T_max   0.907
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.7945
_exptl_absorpt_correction_T_max  0.8879
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56722
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_theta_min         1.181
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             10462
_reflns_number_gt                8154
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0756P)²+3.3958P] 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         10462
_refine_ls_number_parameters     428
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1396
_refine_ls_wR_factor_gt          0.1327
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_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
C2 C 0.64365(13) 0.2266(3) 0.37891(9) 0.0127(6) Uani 1 1 d . . . . .
C3 C 0.59012(14) 0.2857(3) 0.38017(9) 0.0151(6) Uani 1 1 d . . . . .
H3 H 0.588511 0.343276 0.401905 0.018 Uiso 1 1 calc R U . . .
C4 C 0.53948(14) 0.2622(4) 0.35048(10) 0.0168(6) Uani 1 1 d . . . . .
H4 H 0.503574 0.302899 0.352134 0.020 Uiso 1 1 calc R U . . .
C5 C 0.54072(15) 0.1787(4) 0.31798(10) 0.0180(7) Uani 1 1 d . . . . .
H5 H 0.506088 0.164324 0.297292 0.022 Uiso 1 1 calc R U . . .
C6 C 0.59333(15) 0.1174(4) 0.31645(10) 0.0182(7) Uani 1 1 d . . . . .
H6 H 0.594345 0.058823 0.294754 0.022 Uiso 1 1 calc R U . . .
C7 C 0.64431(14) 0.1402(3) 0.34598(9) 0.0127(6) Uani 1 1 d . . . . .
C8 C 0.70364(13) 0.0509(3) 0.26847(9) 0.0136(6) Uani 1 1 d . . . . .
C9 C 0.68270(14) 0.1945(3) 0.26128(10) 0.0163(6) Uani 1 1 d . . . . .
H9 H 0.677288 0.253449 0.281825 0.020 Uiso 1 1 calc R U . . .
C10 C 0.66979(15) 0.2512(4) 0.22410(11) 0.0225(7) Uani 1 1 d . . . . .
H10 H 0.654975 0.348712 0.219066 0.027 Uiso 1 1 calc R U . . .
C11 C 0.67832(16) 0.1667(4) 0.19432(11) 0.0240(8) Uani 1 1 d . . . . .
H11 H 0.669317 0.206513 0.168868 0.029 Uiso 1 1 calc R U . . .
C12 C 0.69977(16) 0.0252(4) 0.20114(10) 0.0219(7) Uani 1 1 d . . . . .
H12 H 0.705670 -0.032247 0.180486 0.026 Uiso 1 1 calc R U . . .
C13 C 0.71273(15) -0.0333(4) 0.23815(10) 0.0183(7) Uani 1 1 d . . . . .
H13 H 0.727814 -0.130682 0.242950 0.022 Uiso 1 1 calc R U . . .
C14 C 0.68704(13) -0.2043(3) 0.31232(9) 0.0124(6) Uani 1 1 d . . . . .
C15 C 0.64275(15) -0.2491(4) 0.27975(10) 0.0179(7) Uani 1 1 d . . . . .
H15 H 0.629670 -0.184488 0.258220 0.021 Uiso 1 1 calc R U . . .
C16 C 0.61767(16) -0.3886(4) 0.27874(10) 0.0203(7) Uani 1 1 d . . . . .
H16 H 0.588218 -0.419777 0.256276 0.024 Uiso 1 1 calc R U . . .
C17 C 0.63560(15) -0.4819(3) 0.31044(10) 0.0173(7) Uani 1 1 d . . . . .
H17 H 0.617932 -0.576210 0.309817 0.021 Uiso 1 1 calc R U . . .
C18 C 0.67951(15) -0.4378(4) 0.34324(10) 0.0188(7) Uani 1 1 d . . . . .
H18 H 0.691846 -0.502007 0.364919 0.023 Uiso 1 1 calc R U . . .
C19 C 0.70514(14) -0.2998(4) 0.34415(10) 0.0172(6) Uani 1 1 d . . . . .
H19 H 0.735129 -0.269915 0.366476 0.021 Uiso 1 1 calc R U . . .
C20 C 0.79651(13) -0.0361(3) 0.33865(9) 0.0119(6) Uani 1 1 d . . . . .
C21 C 0.83062(15) -0.1136(3) 0.31969(9) 0.0154(6) Uani 1 1 d . . . . .
H21 H 0.812322 -0.169976 0.297251 0.018 Uiso 1 1 calc R U . . .
C22 C 0.89136(14) -0.1089(4) 0.33339(9) 0.0165(6) Uani 1 1 d . . . . .
H22 H 0.914804 -0.162952 0.320803 0.020 Uiso 1 1 calc R U . . .
C23 C 0.91694(14) -0.0238(4) 0.36580(10) 0.0169(6) Uani 1 1 d . . . . .
H23 H 0.958327 -0.015399 0.374683 0.020 Uiso 1 1 calc R U . . .
C24 C 0.88257(13) 0.0501(3) 0.38564(9) 0.0140(6) Uani 1 1 d . . . . .
H24 H 0.901363 0.105036 0.408258 0.017 Uiso 1 1 calc R U . . .
C25 C 0.82120(13) 0.0455(3) 0.37309(9) 0.0121(6) Uani 1 1 d . . . . .
C26 C 0.87491(14) 0.1054(3) 0.48416(9) 0.0142(6) Uani 1 1 d . . . . .
C27 C 0.88362(15) -0.0376(4) 0.47384(9) 0.0180(7) Uani 1 1 d . . . . .
H27 H 0.862794 -0.073692 0.448938 0.022 Uiso 1 1 calc R U . . .
C28 C 0.92301(18) -0.1293(4) 0.49994(11) 0.0254(8) Uani 1 1 d . . . . .
H28 H 0.929270 -0.227263 0.492569 0.030 Uiso 1 1 calc R U . . .
C29 C 0.95288(16) -0.0785(4) 0.53636(10) 0.0244(8) Uani 1 1 d . . . . .
H29 H 0.979585 -0.141419 0.554000 0.029 Uiso 1 1 calc R U . . .
C30 C 0.94402(16) 0.0624(4) 0.54705(10) 0.0244(8) Uani 1 1 d . . . . .
H30 H 0.964610 0.097161 0.572143 0.029 Uiso 1 1 calc R U . . .
C31 C 0.90519(16) 0.1549(4) 0.52149(10) 0.0214(7) Uani 1 1 d . . . . .
H31 H 0.899008 0.252294 0.529262 0.026 Uiso 1 1 calc R U . . .
C32 C 0.87048(14) 0.3794(3) 0.44115(9) 0.0143(6) Uani 1 1 d . . . . .
C33 C 0.93123(15) 0.3867(4) 0.45698(10) 0.0198(7) Uani 1 1 d . . . . .
H33 H 0.951439 0.310747 0.473720 0.024 Uiso 1 1 calc R U . . .
C34 C 0.96195(16) 0.5061(4) 0.44802(11) 0.0248(8) Uani 1 1 d . . . . .
H34 H 1.003256 0.510715 0.458461 0.030 Uiso 1 1 calc R U . . .
C35 C 0.93272(17) 0.6178(4) 0.42408(11) 0.0234(8) Uani 1 1 d . . . . .
H35 H 0.953968 0.699190 0.418369 0.028 Uiso 1 1 calc R U . . .
C36 C 0.87254(17) 0.6116(4) 0.40838(11) 0.0229(7) Uani 1 1 d . . . . .
H36 H 0.852445 0.688574 0.391984 0.028 Uiso 1 1 calc R U . . .
C37 C 0.84198(15) 0.4927(4) 0.41674(10) 0.0208(7) Uani 1 1 d . . . . .
H37 H 0.800793 0.487999 0.405669 0.025 Uiso 1 1 calc R U . . .
C38 C 0.78509(14) 0.3235(3) 0.48031(9) 0.0142(6) Uani 1 1 d . . . . .
H38A H 0.813588 0.380446 0.500657 0.017 Uiso 1 1 calc R U . . .
H38B H 0.757874 0.395238 0.463670 0.017 Uiso 1 1 calc R U . . .
C39 C 0.750000 0.2246(5) 0.500000 0.0152(9) Uani 1 2 d S T P . .
C40 C 0.5075(2) -0.3611(5) 0.32880(14) 0.0365(10) Uani 1 1 d . . . . .
N1 N 0.70030(11) 0.0876(3) 0.34645(8) 0.0128(5) Uani 1 1 d . . . . .
O1 O 0.69303(10) 0.2503(2) 0.40705(6) 0.0155(5) Uani 1 1 d . . . . .
P1 P 0.71909(3) -0.02196(8) 0.31715(2) 0.01086(16) Uani 1 1 d . . . . .
P2 P 0.82494(3) 0.22923(9) 0.45061(2) 0.01138(16) Uani 1 1 d . . . . .
PD1 Pd 0.76325(2) 0.14656(2) 0.39535(2) 0.01035(8) Uani 1 1 d . . . . .
CL1 Cl 0.46581(6) -0.45647(16) 0.28632(3) 0.0509(3) Uani 1 1 d . . . . .
CL2 Cl 0.47350(5) -0.37942(12) 0.36550(3) 0.0363(2) Uani 1 1 d . . . . .
CL3 Cl 0.51459(11) -0.17686(15) 0.31763(7) 0.1086(9) Uani 1 1 d . . . . .
H39 H 0.7707(17) 0.172(4) 0.5188(11) 0.021(10) Uiso 1 1 d . . . . .
H40 H 0.547(3) -0.429(7) 0.3349(18) 0.08(2) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 O1 1.333(4) . ?
C2 C3 1.397(4) . ?
C2 C7 1.424(4) . ?
C3 C4 1.382(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.400(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.383(5) . ?
C6 H6 0.9500 . ?
C7 N1 1.414(4) . ?
C8 C9 1.392(4) . ?
C8 C13 1.398(4) . ?
C8 P1 1.809(3) . ?
C9 C10 1.383(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(5) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C15 1.396(5) . ?
C14 C19 1.402(4) . ?
C14 P1 1.808(3) . ?
C15 C16 1.394(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.385(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.395(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.388(5) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 C21 1.392(4) . ?
C20 C25 1.419(4) . ?
C20 P1 1.792(3) . ?
C21 C22 1.392(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.386(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.402(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.404(4) . ?
C24 H24 0.9500 . ?
C25 PD1 2.006(3) . ?
C26 C27 1.380(4) . ?
C26 C31 1.405(5) . ?
C26 P2 1.821(3) . ?
C27 C28 1.397(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.368(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.385(5) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 C37 1.395(5) . ?
C32 C33 1.399(5) . ?
C32 P2 1.832(3) . ?
C33 C34 1.396(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.382(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.386(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.381(5) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
C38 C39 1.531(4) . ?
C38 P2 1.832(3) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 C38 1.531(4) 2_656 ?
C39 H39 0.86(4) . ?
C40 CL3 1.736(4) . ?
C40 CL2 1.744(4) . ?
C40 CL1 1.790(5) . ?
C40 H40 1.10(6) . ?
N1 P1 1.602(3) . ?
N1 PD1 2.032(3) . ?
O1 PD1 2.066(2) . ?
P2 PD1 2.2384(8) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C2 C3 122.1(3) . . ?
O1 C2 C7 120.2(3) . . ?
C3 C2 C7 117.7(3) . . ?
C4 C3 C2 121.4(3) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C6 C5 C4 119.0(3) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C7 C6 C5 121.1(3) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 N1 125.4(3) . . ?
C6 C7 C2 120.4(3) . . ?
N1 C7 C2 114.2(3) . . ?
C9 C8 C13 119.5(3) . . ?
C9 C8 P1 119.0(2) . . ?
C13 C8 P1 121.5(2) . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C11 C10 C9 120.3(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.9(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C8 120.0(3) . . ?
C12 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
C15 C14 C19 119.3(3) . . ?
C15 C14 P1 123.0(2) . . ?
C19 C14 P1 117.5(2) . . ?
C16 C15 C14 120.1(3) . . ?
C16 C15 H15 119.9 . . ?
C14 C15 H15 119.9 . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.2(3) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C19 C18 C17 119.8(3) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.1 . . ?
C18 C19 C14 120.4(3) . . ?
C18 C19 H19 119.8 . . ?
C14 C19 H19 119.8 . . ?
C21 C20 C25 122.4(3) . . ?
C21 C20 P1 119.9(2) . . ?
C25 C20 P1 117.4(2) . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 118.6(3) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 120.9(3) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 H23 119.6 . . ?
C23 C24 C25 122.0(3) . . ?
C23 C24 H24 119.0 . . ?
C25 C24 H24 119.0 . . ?
C24 C25 C20 115.5(3) . . ?
C24 C25 PD1 129.2(2) . . ?
C20 C25 PD1 115.2(2) . . ?
C27 C26 C31 118.8(3) . . ?
C27 C26 P2 121.4(2) . . ?
C31 C26 P2 119.9(2) . . ?
C26 C27 C28 120.1(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 120.4(3) . . ?
C29 C28 H28 119.8 . . ?
C27 C28 H28 119.8 . . ?
C30 C29 C28 120.0(3) . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.4(3) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C30 C31 C26 120.4(3) . . ?
C30 C31 H31 119.8 . . ?
C26 C31 H31 119.8 . . ?
C37 C32 C33 118.9(3) . . ?
C37 C32 P2 117.1(2) . . ?
C33 C32 P2 124.0(3) . . ?
C34 C33 C32 119.6(3) . . ?
C34 C33 H33 120.2 . . ?
C32 C33 H33 120.2 . . ?
C35 C34 C33 120.5(3) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.3(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C37 C36 C35 119.5(3) . . ?
C37 C36 H36 120.3 . . ?
C35 C36 H36 120.3 . . ?
C36 C37 C32 121.2(3) . . ?
C36 C37 H37 119.4 . . ?
C32 C37 H37 119.4 . . ?
C39 C38 P2 116.1(2) . . ?
C39 C38 H38A 108.3 . . ?
P2 C38 H38A 108.3 . . ?
C39 C38 H38B 108.3 . . ?
P2 C38 H38B 108.3 . . ?
H38A C38 H38B 107.4 . . ?
C38 C39 C38 108.4(4) 2_656 . ?
C38 C39 H39 103(3) 2_656 . ?
C38 C39 H39 115(3) . . ?
CL3 C40 CL2 111.3(2) . . ?
CL3 C40 CL1 109.5(3) . . ?
CL2 C40 CL1 109.6(2) . . ?
CL3 C40 H40 116(3) . . ?
CL2 C40 H40 111(3) . . ?
CL1 C40 H40 98(3) . . ?
C7 N1 P1 129.9(2) . . ?
C7 N1 PD1 112.6(2) . . ?
P1 N1 PD1 117.15(14) . . ?
C2 O1 PD1 111.33(18) . . ?
N1 P1 C20 101.98(14) . . ?
N1 P1 C14 116.06(14) . . ?
C20 P1 C14 109.39(14) . . ?
N1 P1 C8 113.16(14) . . ?
C20 P1 C8 110.13(14) . . ?
C14 P1 C8 106.06(14) . . ?
C26 P2 C38 104.55(15) . . ?
C26 P2 C32 105.66(15) . . ?
C38 P2 C32 101.31(14) . . ?
C26 P2 PD1 121.52(11) . . ?
C38 P2 PD1 110.81(11) . . ?
C32 P2 PD1 110.94(11) . . ?
C25 PD1 N1 87.55(11) . . ?
C25 PD1 O1 168.60(11) . . ?
N1 PD1 O1 81.63(9) . . ?
C25 PD1 P2 98.88(9) . . ?
N1 PD1 P2 173.38(7) . . ?
O1 PD1 P2 91.85(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
O1 C2 C3 C4 178.9(3) . . . . ?
C7 C2 C3 C4 -0.4(5) . . . . ?
C2 C3 C4 C5 -0.5(5) . . . . ?
C3 C4 C5 C6 1.4(5) . . . . ?
C4 C5 C6 C7 -1.4(5) . . . . ?
C5 C6 C7 N1 -177.4(3) . . . . ?
C5 C6 C7 C2 0.5(5) . . . . ?
O1 C2 C7 C6 -178.9(3) . . . . ?
C3 C2 C7 C6 0.3(4) . . . . ?
O1 C2 C7 N1 -0.8(4) . . . . ?
C3 C2 C7 N1 178.5(3) . . . . ?
C13 C8 C9 C10 1.5(5) . . . . ?
P1 C8 C9 C10 -179.0(3) . . . . ?
C8 C9 C10 C11 -0.9(5) . . . . ?
C9 C10 C11 C12 0.0(5) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C11 C12 C13 C8 0.5(5) . . . . ?
C9 C8 C13 C12 -1.4(5) . . . . ?
P1 C8 C13 C12 179.2(3) . . . . ?
C19 C14 C15 C16 -1.2(5) . . . . ?
P1 C14 C15 C16 -176.5(3) . . . . ?
C14 C15 C16 C17 1.6(5) . . . . ?
C15 C16 C17 C18 -1.1(5) . . . . ?
C16 C17 C18 C19 0.2(5) . . . . ?
C17 C18 C19 C14 0.2(5) . . . . ?
C15 C14 C19 C18 0.3(5) . . . . ?
P1 C14 C19 C18 175.9(3) . . . . ?
C25 C20 C21 C22 -2.5(5) . . . . ?
P1 C20 C21 C22 171.4(2) . . . . ?
C20 C21 C22 C23 -1.1(5) . . . . ?
C21 C22 C23 C24 3.3(5) . . . . ?
C22 C23 C24 C25 -2.1(5) . . . . ?
C23 C24 C25 C20 -1.3(4) . . . . ?
C23 C24 C25 PD1 -177.7(2) . . . . ?
C21 C20 C25 C24 3.6(4) . . . . ?
P1 C20 C25 C24 -170.4(2) . . . . ?
C21 C20 C25 PD1 -179.5(2) . . . . ?
P1 C20 C25 PD1 6.5(3) . . . . ?
C31 C26 C27 C28 -1.5(5) . . . . ?
P2 C26 C27 C28 178.9(3) . . . . ?
C26 C27 C28 C29 0.9(6) . . . . ?
C27 C28 C29 C30 -0.1(6) . . . . ?
C28 C29 C30 C31 0.0(6) . . . . ?
C29 C30 C31 C26 -0.6(6) . . . . ?
C27 C26 C31 C30 1.4(5) . . . . ?
P2 C26 C31 C30 -179.0(3) . . . . ?
C37 C32 C33 C34 -0.2(5) . . . . ?
P2 C32 C33 C34 -179.8(3) . . . . ?
C32 C33 C34 C35 0.8(5) . . . . ?
C33 C34 C35 C36 -0.6(6) . . . . ?
C34 C35 C36 C37 -0.2(6) . . . . ?
C35 C36 C37 C32 0.8(5) . . . . ?
C33 C32 C37 C36 -0.6(5) . . . . ?
P2 C32 C37 C36 179.0(3) . . . . ?
P2 C38 C39 C38 -174.1(3) . . . 2_656 ?
C6 C7 N1 P1 -7.3(5) . . . . ?
C2 C7 N1 P1 174.7(2) . . . . ?
C6 C7 N1 PD1 179.8(3) . . . . ?
C2 C7 N1 PD1 1.8(3) . . . . ?
C3 C2 O1 PD1 -179.9(2) . . . . ?
C7 C2 O1 PD1 -0.6(3) . . . . ?
C7 N1 P1 C20 -178.5(3) . . . . ?
PD1 N1 P1 C20 -5.90(19) . . . . ?
C7 N1 P1 C14 -59.7(3) . . . . ?
PD1 N1 P1 C14 112.89(17) . . . . ?
C7 N1 P1 C8 63.2(3) . . . . ?
PD1 N1 P1 C8 -124.15(16) . . . . ?
C21 C20 P1 N1 -174.6(2) . . . . ?
C25 C20 P1 N1 -0.4(3) . . . . ?
C21 C20 P1 C14 62.0(3) . . . . ?
C25 C20 P1 C14 -123.8(2) . . . . ?
C21 C20 P1 C8 -54.2(3) . . . . ?
C25 C20 P1 C8 120.0(2) . . . . ?
C15 C14 P1 N1 105.9(3) . . . . ?
C19 C14 P1 N1 -69.5(3) . . . . ?
C15 C14 P1 C20 -139.4(3) . . . . ?
C19 C14 P1 C20 45.2(3) . . . . ?
C15 C14 P1 C8 -20.7(3) . . . . ?
C19 C14 P1 C8 163.9(2) . . . . ?
C9 C8 P1 N1 5.6(3) . . . . ?
C13 C8 P1 N1 -175.0(3) . . . . ?
C9 C8 P1 C20 -107.8(3) . . . . ?
C13 C8 P1 C20 71.6(3) . . . . ?
C9 C8 P1 C14 133.9(2) . . . . ?
C13 C8 P1 C14 -46.6(3) . . . . ?
C27 C26 P2 C38 137.3(3) . . . . ?
C31 C26 P2 C38 -42.3(3) . . . . ?
C27 C26 P2 C32 -116.2(3) . . . . ?
C31 C26 P2 C32 64.2(3) . . . . ?
C27 C26 P2 PD1 11.2(3) . . . . ?
C31 C26 P2 PD1 -168.4(2) . . . . ?
C39 C38 P2 C26 -59.8(2) . . . . ?
C39 C38 P2 C32 -169.5(2) . . . . ?
C39 C38 P2 PD1 72.8(2) . . . . ?
C37 C32 P2 C26 -178.3(3) . . . . ?
C33 C32 P2 C26 1.4(3) . . . . ?
C37 C32 P2 C38 -69.5(3) . . . . ?
C33 C32 P2 C38 110.2(3) . . . . ?
C37 C32 P2 PD1 48.2(3) . . . . ?
C33 C32 P2 PD1 -132.1(3) . . . . ?

_refine_diff_density_max         1.754
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.133

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.250 0.235 0.000 230 103 ' '
2 0.250 0.264 0.500 230 103 ' '
3 0.750 0.764 0.000 230 103 ' '
4 0.750 0.735 0.500 230 103 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?
