# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_ijsf1807a
_database_code_depnum_ccdc_archive 'CCDC 1894927'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2018-03-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H36 O4 P2 Pd'
_chemical_formula_sum            'C40 H36 O4 P2 Pd'
_chemical_formula_weight         749.03
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C86 H73 O2 P5 Pd3'
_chemical_oxdiff_usercomment     'Neil Scott nwjs-3-204-recryst'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.6975(2)
_cell_length_b                   15.0053(3)
_cell_length_c                   19.3767(3)
_cell_angle_alpha                90
_cell_angle_beta                 94.765(2)
_cell_angle_gamma                90
_cell_volume                     3389.33(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5912
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      70.5410
_cell_measurement_theta_min      4.7970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.641
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 -5 1 0.0563
-3 5 2 0.0667
0 1 5 0.0641
0 0 -1 0.0613
-3 4 -5 0.0700
-5 2 -2 0.0436
-4 -5 2 0.0384
5 3 -1 0.0558
5 -2 2 0.0504
-1 -1 5 0.0591
3 2 -5 0.0553
1 0 -1 0.0470

_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.094
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0010 -5.0006 1.0068 -0.0292 0.1608 0.6373
-3.0041 5.0022 1.9905 0.1206 -0.3596 -0.5407
-0.0050 1.0025 4.9950 0.1040 -0.3879 0.0904
0.0011 -0.0005 -0.9991 -0.0305 0.0663 -0.0322
-2.9970 3.9986 -5.0027 -0.0443 0.1609 -0.6955
-5.0031 2.0020 -2.0077 0.3450 0.1123 -0.6253
-4.0083 -4.9952 1.9941 0.7051 0.2245 0.0822
5.0078 2.9954 -0.9922 -0.6784 -0.1962 0.1752
5.0031 -2.0020 2.0077 -0.3450 -0.1123 0.6253
-1.0067 -0.9964 4.9944 0.3013 -0.2563 0.1478
3.0094 1.9948 -4.9915 -0.5508 0.1626 -0.0507
1.0022 -0.0012 -0.9974 -0.1310 0.0477 0.0517

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12675
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.065
_diffrn_reflns_theta_max         67.065
_diffrn_reflns_theta_min         3.731
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  21.00   1.00    1.50    --    0.00 -57.00 -30.00   49
  2  ω     32.00 107.00   1.00    4.50    --   54.00-125.00  60.00   75
  3  ω     49.00  77.00   1.00    4.50    --  108.00-111.00  60.00   28
  4  ω     37.00 114.00   1.00    4.50    --  108.00-111.00 120.00   77
  5  ω     46.00 136.00   1.00    4.50    --  108.00 -77.00 150.00   90
  6  ω    130.00 156.00   1.00    4.50    --  108.00  25.00   0.00   26
  7  ω    108.00 172.00   1.00    4.50    --  108.00  62.00 -61.00   64
  8  ω     99.00 140.00   1.00    4.50    --  108.00 -25.00-150.00   41
  9  ω     48.00  97.00   1.00    4.50    --  108.00 -50.00 -90.00   49
 10  ω     35.00  84.00   1.00    4.50    --  108.00 -25.00-150.00   49
 11  ω     23.00  78.00   1.00    4.50    --   54.00-125.00 -60.00   55
 12  ω      9.00  69.00   1.00    4.50    --   54.00 -57.00 120.00   60
 13  ω     90.00 148.00   1.00    4.50    --  108.00  50.00  60.00   58
 14  ω     68.00  96.00   1.00    4.50    --  108.00 178.00 -30.00   28
 15  ω     31.00 123.00   1.00    4.50    --   54.00  77.00  90.00   92
 16  ω    -26.00  15.00   1.00    1.50    --    0.00  91.00 171.00   41
 17  ω    -61.00 -34.00   1.00    1.50    --    0.00 -57.00 -30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1005092000
_diffrn_orient_matrix_UB_12      -0.0483546000
_diffrn_orient_matrix_UB_13      0.0304178000
_diffrn_orient_matrix_UB_21      -0.0184754000
_diffrn_orient_matrix_UB_22      -0.0565909000
_diffrn_orient_matrix_UB_23      -0.0663276000
_diffrn_orient_matrix_UB_31      0.0836956000
_diffrn_orient_matrix_UB_32      -0.0707040000
_diffrn_orient_matrix_UB_33      0.0323649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5295
_reflns_number_total             6044
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         6044
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0289
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0334P)²+1.5655P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0743
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C14(H14), C9(H9), C16(H16), C12(H12), C17(H17), C15(H15), C32(H32),
 C35(H35), C10(H10), C18(H18), C2(H2), C24(H24), C8(H8), C20(H20), C34(H34),
 C11(H11), C6(H6), C29(H29), C22(H22), C28(H28), C33(H33), C25(H25), C27(H27),
 C23(H23), C21(H21), C5(H5), C3(H3), C4(H4), C26(H26)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.65696(2) 0.73367(2) 0.38059(2) 0.01951(7) Uani 1 1 d . . . . .
P2 P 0.46344(5) 0.76564(4) 0.39172(3) 0.02044(14) Uani 1 1 d . . . . .
P1 P 0.84037(5) 0.71155(4) 0.34632(3) 0.02086(14) Uani 1 1 d . . . . .
O1 O 0.68668(14) 0.86392(12) 0.36144(9) 0.0231(4) Uani 1 1 d . . . . .
O3 O 0.62879(15) 0.60213(12) 0.39606(10) 0.0273(4) Uani 1 1 d . . . . .
O2 O 0.69932(18) 0.88531(14) 0.47610(10) 0.0342(5) Uani 1 1 d . . . . .
O4 O 0.7258(2) 0.61652(15) 0.49886(11) 0.0449(6) Uani 1 1 d . . . . .
C36 C 0.4059(2) 0.94680(19) 0.40518(15) 0.0271(6) Uani 1 1 d . . . . .
H36 H 0.4004 0.9356 0.4520 0.033 Uiso 1 1 calc R . . . .
C31 C 0.4324(2) 0.87812(18) 0.36162(13) 0.0227(5) Uani 1 1 d . . . . .
C14 C 0.8835(2) 0.66103(18) 0.21012(14) 0.0254(6) Uani 1 1 d . . . . .
H14 H 0.9293 0.6156 0.2299 0.030 Uiso 1 1 calc R . . . .
C13 C 0.8291(2) 0.72039(17) 0.25210(13) 0.0218(5) Uani 1 1 d . . . . .
C37 C 0.7017(2) 0.91285(18) 0.41691(14) 0.0252(6) Uani 1 1 d . . . . .
C30 C 0.3597(2) 0.69765(19) 0.33891(14) 0.0262(6) Uani 1 1 d . . . . .
C9 C 1.0335(2) 0.8815(2) 0.47151(15) 0.0330(7) Uani 1 1 d . . . . .
H9 H 1.0444 0.8920 0.5189 0.040 Uiso 1 1 calc R . . . .
C16 C 0.8020(2) 0.73759(19) 0.10870(15) 0.0290(6) Uani 1 1 d . . . . .
H16 H 0.7913 0.7423 0.0607 0.035 Uiso 1 1 calc R . . . .
C12 C 0.9990(2) 0.85082(19) 0.33086(15) 0.0285(6) Uani 1 1 d . . . . .
H12 H 0.9869 0.8415 0.2834 0.034 Uiso 1 1 calc R . . . .
C17 C 0.7512(2) 0.7978(2) 0.15016(15) 0.0304(6) Uani 1 1 d . . . . .
H17 H 0.7086 0.8447 0.1300 0.036 Uiso 1 1 calc R . . . .
C1 C 0.9088(2) 0.6044(2) 0.36517(14) 0.0289(6) Uani 1 1 d . . . . .
C19 C 0.4143(2) 0.75846(17) 0.47816(14) 0.0232(6) Uani 1 1 d . . . . .
C15 C 0.8689(2) 0.6701(2) 0.13887(14) 0.0301(6) Uani 1 1 d . . . . .
H15 H 0.9047 0.6301 0.1109 0.036 Uiso 1 1 calc R . . . .
C32 C 0.4424(2) 0.8963(2) 0.29150(14) 0.0299(6) Uani 1 1 d . . . . .
H32 H 0.4615 0.8508 0.2620 0.036 Uiso 1 1 calc R . . . .
C35 C 0.3874(2) 1.0325(2) 0.37926(16) 0.0340(7) Uani 1 1 d . . . . .
H35 H 0.3690 1.0784 0.4086 0.041 Uiso 1 1 calc R . . . .
C10 C 1.0916(2) 0.93253(19) 0.42669(15) 0.0316(7) Uani 1 1 d . . . . .
H10 H 1.1422 0.9767 0.4436 0.038 Uiso 1 1 calc R . . . .
C18 C 0.7629(2) 0.78946(18) 0.22145(14) 0.0259(6) Uani 1 1 d . . . . .
H18 H 0.7267 0.8297 0.2489 0.031 Uiso 1 1 calc R . . . .
C2 C 0.8516(3) 0.5281(2) 0.33969(17) 0.0364(7) Uani 1 1 d . . . . .
H2 H 0.7814 0.5335 0.3137 0.044 Uiso 1 1 calc R . . . .
C7 C 0.9420(2) 0.79781(18) 0.37630(14) 0.0237(6) Uani 1 1 d . . . . .
C38 C 0.7245(3) 1.00932(19) 0.40177(16) 0.0345(7) Uani 1 1 d . . . . .
H38A H 0.8028 1.0163 0.3914 0.052 Uiso 1 1 calc GR . . . .
H38B H 0.7108 1.0448 0.4415 0.052 Uiso 1 1 calc GR . . . .
H38C H 0.6744 1.0284 0.3628 0.052 Uiso 1 1 calc GR . . . .
C24 C 0.2978(2) 0.75652(18) 0.48855(15) 0.0285(6) Uani 1 1 d . . . . .
H24 H 0.2435 0.7579 0.4507 0.034 Uiso 1 1 calc R . . . .
C8 C 0.9591(2) 0.8149(2) 0.44684(14) 0.0307(6) Uani 1 1 d . . . . .
H8 H 0.9202 0.7814 0.4778 0.037 Uiso 1 1 calc R . . . .
C20 C 0.4946(2) 0.7556(2) 0.53506(15) 0.0315(6) Uani 1 1 d . . . . .
H20 H 0.5726 0.7559 0.5289 0.038 Uiso 1 1 calc R . . . .
C34 C 0.3966(3) 1.0493(2) 0.30973(17) 0.0385(7) Uani 1 1 d . . . . .
H34 H 0.3842 1.1065 0.2923 0.046 Uiso 1 1 calc R . . . .
C11 C 1.0736(2) 0.9172(2) 0.35618(16) 0.0321(6) Uani 1 1 d . . . . .
H11 H 1.1118 0.9517 0.3255 0.038 Uiso 1 1 calc R . . . .
C6 C 1.0126(3) 0.5958(2) 0.40489(16) 0.0406(8) Uani 1 1 d . . . . .
H6 H 1.0517 0.6458 0.4227 0.049 Uiso 1 1 calc R . . . .
C29 C 0.2610(2) 0.7339(2) 0.30570(17) 0.0355(7) Uani 1 1 d . . . . .
H29 H 0.2480 0.7950 0.3082 0.043 Uiso 1 1 calc R . . . .
C22 C 0.3425(3) 0.7510(2) 0.61115(16) 0.0346(7) Uani 1 1 d . . . . .
H22 H 0.3187 0.7491 0.6557 0.042 Uiso 1 1 calc R . . . .
C39 C 0.6703(2) 0.57274(19) 0.45586(15) 0.0309(6) Uani 1 1 d . . . . .
C28 C 0.1815(2) 0.6800(2) 0.26885(16) 0.0401(8) Uani 1 1 d . . . . .
H28 H 0.1157 0.7051 0.2467 0.048 Uiso 1 1 calc R . . . .
C33 C 0.4240(2) 0.9811(2) 0.26614(16) 0.0369(7) Uani 1 1 d . . . . .
H33 H 0.4301 0.9927 0.2194 0.044 Uiso 1 1 calc R . . . .
C25 C 0.3773(3) 0.6063(2) 0.33392(18) 0.0416(8) Uani 1 1 d . . . . .
H25 H 0.4431 0.5807 0.3557 0.050 Uiso 1 1 calc R . . . .
C27 C 0.1991(3) 0.5900(2) 0.26480(17) 0.0418(8) Uani 1 1 d . . . . .
H27 H 0.1449 0.5539 0.2406 0.050 Uiso 1 1 calc R . . . .
C23 C 0.2625(3) 0.75250(19) 0.55488(16) 0.0327(7) Uani 1 1 d . . . . .
H23 H 0.1846 0.7508 0.5615 0.039 Uiso 1 1 calc R . . . .
C21 C 0.4576(3) 0.7524(2) 0.60144(16) 0.0367(7) Uani 1 1 d . . . . .
H21 H 0.5113 0.7512 0.6396 0.044 Uiso 1 1 calc R . . . .
C5 C 1.0575(3) 0.5096(3) 0.4177(2) 0.0574(11) Uani 1 1 d . . . . .
H5 H 1.1271 0.5030 0.4442 0.069 Uiso 1 1 calc R . . . .
C3 C 0.8983(3) 0.4447(2) 0.35266(19) 0.0488(9) Uani 1 1 d . . . . .
H3 H 0.8604 0.3943 0.3347 0.059 Uiso 1 1 calc R . . . .
C40 C 0.6441(3) 0.4753(2) 0.4673(2) 0.0512(9) Uani 1 1 d . . . . .
H40A H 0.5682 0.4620 0.4472 0.077 Uiso 1 1 calc GR . . . .
H40B H 0.6487 0.4630 0.5160 0.077 Uiso 1 1 calc GR . . . .
H40C H 0.6987 0.4391 0.4458 0.077 Uiso 1 1 calc GR . . . .
C4 C 1.0010(3) 0.4363(3) 0.3921(2) 0.0577(11) Uani 1 1 d . . . . .
H4 H 1.0319 0.3800 0.4013 0.069 Uiso 1 1 calc R . . . .
C26 C 0.2969(3) 0.5532(2) 0.2965(2) 0.0523(9) Uani 1 1 d . . . . .
H26 H 0.3097 0.4923 0.2930 0.063 Uiso 1 1 calc R . . . .


_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 P2 2.3414(6) . ?
Pd1 P1 2.3218(6) . ?
Pd1 O1 2.0249(18) . ?
Pd1 O3 2.0274(19) . ?
P2 C31 1.813(3) . ?
P2 C30 1.831(3) . ?
P2 C19 1.819(3) . ?
P1 C13 1.824(3) . ?
P1 C1 1.819(3) . ?
P1 C7 1.820(3) . ?
O1 C37 1.301(3) . ?
O3 C39 1.296(3) . ?
O2 C37 1.222(3) . ?
O4 C39 1.207(4) . ?
C36 H36 0.9300 . ?
C36 C31 1.384(4) . ?
C36 C35 1.391(4) . ?
C31 C32 1.400(4) . ?
C14 H14 0.9300 . ?
C14 C13 1.395(4) . ?
C14 C15 1.384(4) . ?
C13 C18 1.397(4) . ?
C37 C38 1.505(4) . ?
C30 C29 1.386(4) . ?
C30 C25 1.390(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.378(4) . ?
C9 C8 1.384(4) . ?
C16 H16 0.9300 . ?
C16 C17 1.377(4) . ?
C16 C15 1.380(4) . ?
C12 H12 0.9300 . ?
C12 C7 1.396(4) . ?
C12 C11 1.387(4) . ?
C17 H17 0.9300 . ?
C17 C18 1.382(4) . ?
C1 C2 1.395(4) . ?
C1 C6 1.389(4) . ?
C19 C24 1.394(4) . ?
C19 C20 1.388(4) . ?
C15 H15 0.9300 . ?
C32 H32 0.9300 . ?
C32 C33 1.376(4) . ?
C35 H35 0.9300 . ?
C35 C34 1.384(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.384(4) . ?
C18 H18 0.9300 . ?
C2 H2 0.9300 . ?
C2 C3 1.381(4) . ?
C7 C8 1.389(4) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C24 H24 0.9300 . ?
C24 C23 1.384(4) . ?
C8 H8 0.9300 . ?
C20 H20 0.9300 . ?
C20 C21 1.392(4) . ?
C34 H34 0.9300 . ?
C34 C33 1.381(5) . ?
C11 H11 0.9300 . ?
C6 H6 0.9300 . ?
C6 C5 1.410(5) . ?
C29 H29 0.9300 . ?
C29 C28 1.385(4) . ?
C22 H22 0.9300 . ?
C22 C23 1.377(4) . ?
C22 C21 1.374(4) . ?
C39 C40 1.514(4) . ?
C28 H28 0.9300 . ?
C28 C27 1.370(5) . ?
C33 H33 0.9300 . ?
C25 H25 0.9300 . ?
C25 C26 1.389(4) . ?
C27 H27 0.9300 . ?
C27 C26 1.369(5) . ?
C23 H23 0.9300 . ?
C21 H21 0.9300 . ?
C5 H5 0.9300 . ?
C5 C4 1.356(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.375(5) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C4 H4 0.9300 . ?
C26 H26 0.9300 . ?

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
P1 Pd1 P2 168.25(2) . . ?
O1 Pd1 P2 90.06(5) . . ?
O1 Pd1 P1 84.77(5) . . ?
O1 Pd1 O3 177.81(7) . . ?
O3 Pd1 P2 90.89(5) . . ?
O3 Pd1 P1 93.93(6) . . ?
C31 P2 Pd1 109.28(8) . . ?
C31 P2 C30 103.50(12) . . ?
C31 P2 C19 106.34(12) . . ?
C30 P2 Pd1 115.79(9) . . ?
C19 P2 Pd1 117.04(9) . . ?
C19 P2 C30 103.66(12) . . ?
C13 P1 Pd1 106.52(8) . . ?
C1 P1 Pd1 118.07(9) . . ?
C1 P1 C13 105.02(12) . . ?
C1 P1 C7 107.42(13) . . ?
C7 P1 Pd1 113.69(9) . . ?
C7 P1 C13 104.99(12) . . ?
C37 O1 Pd1 113.99(17) . . ?
C39 O3 Pd1 114.21(18) . . ?
C31 C36 H36 119.9 . . ?
C31 C36 C35 120.3(3) . . ?
C35 C36 H36 119.9 . . ?
C36 C31 P2 123.1(2) . . ?
C36 C31 C32 119.2(3) . . ?
C32 C31 P2 117.6(2) . . ?
C13 C14 H14 120.2 . . ?
C15 C14 H14 120.2 . . ?
C15 C14 C13 119.7(3) . . ?
C14 C13 P1 122.6(2) . . ?
C14 C13 C18 119.3(2) . . ?
C18 C13 P1 118.1(2) . . ?
O1 C37 C38 113.3(2) . . ?
O2 C37 O1 124.9(3) . . ?
O2 C37 C38 121.8(3) . . ?
C29 C30 P2 121.9(2) . . ?
C29 C30 C25 118.5(3) . . ?
C25 C30 P2 119.6(2) . . ?
C10 C9 H9 119.6 . . ?
C10 C9 C8 120.8(3) . . ?
C8 C9 H9 119.6 . . ?
C17 C16 H16 120.3 . . ?
C17 C16 C15 119.5(3) . . ?
C15 C16 H16 120.3 . . ?
C7 C12 H12 119.8 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C7 120.4(3) . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.8(3) . . ?
C18 C17 H17 119.6 . . ?
C2 C1 P1 117.6(2) . . ?
C6 C1 P1 123.0(3) . . ?
C6 C1 C2 119.4(3) . . ?
C24 C19 P2 121.5(2) . . ?
C20 C19 P2 119.2(2) . . ?
C20 C19 C24 119.3(3) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 C14 120.9(3) . . ?
C16 C15 H15 119.6 . . ?
C31 C32 H32 119.9 . . ?
C33 C32 C31 120.2(3) . . ?
C33 C32 H32 119.9 . . ?
C36 C35 H35 120.1 . . ?
C34 C35 C36 119.8(3) . . ?
C34 C35 H35 120.1 . . ?
C9 C10 H10 120.4 . . ?
C9 C10 C11 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
C13 C18 H18 120.1 . . ?
C17 C18 C13 119.8(3) . . ?
C17 C18 H18 120.1 . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.6(3) . . ?
C3 C2 H2 119.7 . . ?
C12 C7 P1 122.5(2) . . ?
C8 C7 P1 118.8(2) . . ?
C8 C7 C12 118.6(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C19 C24 H24 119.8 . . ?
C23 C24 C19 120.4(3) . . ?
C23 C24 H24 119.8 . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.6(3) . . ?
C21 C20 H20 120.2 . . ?
C35 C34 H34 120.0 . . ?
C33 C34 C35 120.1(3) . . ?
C33 C34 H34 120.0 . . ?
C12 C11 H11 119.7 . . ?
C10 C11 C12 120.5(3) . . ?
C10 C11 H11 119.7 . . ?
C1 C6 H6 120.7 . . ?
C1 C6 C5 118.7(4) . . ?
C5 C6 H6 120.7 . . ?
C30 C29 H29 119.8 . . ?
C28 C29 C30 120.5(3) . . ?
C28 C29 H29 119.8 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 120.0(3) . . ?
O3 C39 C40 113.2(3) . . ?
O4 C39 O3 124.9(3) . . ?
O4 C39 C40 121.9(3) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 C29 120.5(3) . . ?
C27 C28 H28 119.7 . . ?
C32 C33 C34 120.3(3) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C30 C25 H25 119.9 . . ?
C26 C25 C30 120.3(3) . . ?
C26 C25 H25 119.9 . . ?
C28 C27 H27 120.2 . . ?
C26 C27 C28 119.7(3) . . ?
C26 C27 H27 120.2 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.7(3) . . ?
C22 C21 H21 119.7 . . ?
C6 C5 H5 119.5 . . ?
C4 C5 C6 121.1(3) . . ?
C4 C5 H5 119.5 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.1 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C5 C4 C3 120.4(3) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C25 C26 H26 119.8 . . ?
C27 C26 C25 120.5(3) . . ?
C27 C26 H26 119.8 . . ?

_olex2_date_sample_data_collection 2018-03-16
_olex2_date_sample_submission    2018-03-12
_olex2_exptl_crystal_mounting_method 'oil on micromount '
_olex2_submission_original_sample_id 'Neil Scott -3-204-recrys'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.765
_oxdiff_exptl_absorpt_empirical_full_min 0.814
####################################################################### 
# 
# 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_ijsf1818
_database_code_depnum_ccdc_archive 'CCDC 1894928'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2018-09-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C52 H46 O4 P2 Pd2'
_chemical_formula_sum            'C52 H46 O4 P2 Pd2'
_chemical_formula_weight         1009.63
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C52 H46 O4 P2 Pd2'
_chemical_oxdiff_usercomment     'Neil NWJS-4-273-precipitate2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   11.0527(2)
_cell_length_b                   23.8864(4)
_cell_length_c                   17.0272(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.5561(16)
_cell_angle_gamma                90
_cell_volume                     4432.98(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7467
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.8940
_cell_measurement_theta_min      5.4970
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.587
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2048
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0060
0 -1 0 0.0129
0 0 -1 0.0136
0 0 1 0.0146
-1 0 0 0.1196
1 0 0 0.1266
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.019
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0000 1.0001 0.0000 -0.0619 -0.0180 0.0035
-0.0000 -1.0001 -0.0000 0.0619 0.0180 -0.0035
-0.0001 -0.0000 -0.9999 -0.0016 0.0223 0.0890
0.0001 0.0000 0.9999 0.0016 -0.0223 -0.0890
-1.0000 0.0008 0.0004 -0.0397 0.1352 -0.0105
1.0000 -0.0008 -0.0004 0.0397 -0.1352 0.0105

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16871
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         3.701
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -67.00  26.00   1.00    5.00    --    0.00 -37.00   0.00   93
  2  ω    -11.00  25.00   1.00    5.00    --    0.00  57.00 -30.00   36
  3  ω    -16.00  28.00   1.00   18.00    --   54.00 -77.00-180.00   44
  4  ω     37.00  85.00   1.00   18.00    --   54.00  57.00 120.00   48
  5  ω     29.00 118.00   1.00   18.00    --   54.00  37.00 -90.00   89
  6  ω     40.00  99.00   1.00   18.00    --   54.00-125.00-150.00   59
  7  ω     28.00  70.00   1.00   18.00    --   54.00-128.00 -21.00   42
  8  ω     51.00 130.00   1.00   18.00    --  108.00 -50.00 -60.00   79
  9  ω     83.00 110.00   1.00   18.00    --  108.00-111.00  60.00   27
 10  ω    101.00 171.00   1.00   18.00    --  108.00  63.00   0.00   70
 11  ω    106.00 140.00   1.00   18.00    --  108.00 -91.00 -60.00   34
 12  ω     82.00 109.00   1.00   18.00    --  108.00-111.00   0.00   27
 13  ω     44.00 100.00   1.00   18.00    --  108.00 -91.00 -60.00   56
 14  ω    105.00 173.00   1.00   18.00    --  108.00  63.00  60.00   68
 15  ω     37.00  63.00   1.00   18.00    --  108.00-111.00   0.00   26
 16  ω    111.00 177.00   1.00   18.00    --  108.00  50.00  30.00   66
 17  ω    105.00 177.00   1.00   18.00    --  108.00 111.00-120.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0396391000
_diffrn_orient_matrix_UB_12      -0.0618537000
_diffrn_orient_matrix_UB_13      0.0015795000
_diffrn_orient_matrix_UB_21      -0.1352585000
_diffrn_orient_matrix_UB_22      -0.0179453000
_diffrn_orient_matrix_UB_23      -0.0223039000
_diffrn_orient_matrix_UB_31      0.0104684000
_diffrn_orient_matrix_UB_32      0.0034703000
_diffrn_orient_matrix_UB_33      -0.0889799000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6909
_reflns_number_total             7909
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0243
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0243P)²+1.5463P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0576
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42),
  C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49), C50(H50),
 C51(H51), C52(H52)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.6398(2) 0.35673(11) 0.47929(14) 0.0174(5) Uani 1 1 d . . . . .
C2 C 0.7032(3) 0.39326(13) 0.54603(16) 0.0267(6) Uani 1 1 d . . . . .
H2A H 0.711001 0.430568 0.526524 0.040 Uiso 1 1 calc GR . . . .
H2B H 0.783176 0.378381 0.565645 0.040 Uiso 1 1 calc GR . . . .
H2C H 0.655651 0.394056 0.588365 0.040 Uiso 1 1 calc GR . . . .
C3 C 0.4863(2) 0.21987(11) 0.46587(14) 0.0172(5) Uani 1 1 d . . . . .
C4 C 0.4536(3) 0.17930(12) 0.52693(16) 0.0271(6) Uani 1 1 d . . . . .
H4A H 0.380546 0.191875 0.545201 0.041 Uiso 1 1 calc GR . . . .
H4B H 0.519744 0.177313 0.571154 0.041 Uiso 1 1 calc GR . . . .
H4C H 0.439516 0.142896 0.503277 0.041 Uiso 1 1 calc GR . . . .
C5 C 0.2939(2) 0.28811(11) 0.27584(14) 0.0154(5) Uani 1 1 d . . . . .
C6 C 0.1910(2) 0.26245(12) 0.29702(16) 0.0213(6) Uani 1 1 d . . . . .
H6 H 0.176757 0.265564 0.349166 0.026 Uiso 1 1 calc R . . . .
C7 C 0.1089(3) 0.23233(13) 0.24235(17) 0.0270(6) Uani 1 1 d . . . . .
H7 H 0.040051 0.216119 0.257754 0.032 Uiso 1 1 calc R . . . .
C8 C 0.1300(3) 0.22643(13) 0.16446(16) 0.0264(6) Uani 1 1 d . . . . .
H8 H 0.076173 0.205807 0.127686 0.032 Uiso 1 1 calc R . . . .
C9 C 0.2319(3) 0.25162(12) 0.14235(15) 0.0240(6) Uani 1 1 d . . . . .
H9 H 0.246410 0.248090 0.090311 0.029 Uiso 1 1 calc R . . . .
C10 C 0.3130(2) 0.28224(11) 0.19750(14) 0.0176(5) Uani 1 1 d . . . . .
H10 H 0.381025 0.299033 0.181711 0.021 Uiso 1 1 calc R . . . .
C11 C 0.5094(2) 0.45385(11) 0.34668(13) 0.0150(5) Uani 1 1 d . . . . .
C12 C 0.6274(2) 0.44054(11) 0.33241(15) 0.0196(6) Uani 1 1 d . . . . .
H12 H 0.640433 0.407231 0.306784 0.023 Uiso 1 1 calc R . . . .
C13 C 0.7246(2) 0.47658(12) 0.35617(15) 0.0235(6) Uani 1 1 d . . . . .
H13 H 0.802057 0.467874 0.345176 0.028 Uiso 1 1 calc R . . . .
C14 C 0.7069(2) 0.52554(12) 0.39623(16) 0.0231(6) Uani 1 1 d . . . . .
H14 H 0.772111 0.549969 0.411445 0.028 Uiso 1 1 calc R . . . .
C15 C 0.5916(3) 0.53808(12) 0.41365(16) 0.0238(6) Uani 1 1 d . . . . .
H15 H 0.579832 0.570395 0.441910 0.029 Uiso 1 1 calc R . . . .
C16 C 0.4940(2) 0.50232(12) 0.38882(15) 0.0205(6) Uani 1 1 d . . . . .
H16 H 0.416937 0.510949 0.400594 0.025 Uiso 1 1 calc R . . . .
C17 C 0.3560(2) 0.41932(11) 0.20145(14) 0.0166(5) Uani 1 1 d . . . . .
C18 C 0.4485(3) 0.43784(12) 0.16171(15) 0.0228(6) Uani 1 1 d . . . . .
H18 H 0.526446 0.444638 0.190211 0.027 Uiso 1 1 calc R . . . .
C19 C 0.4260(3) 0.44629(13) 0.08009(16) 0.0302(7) Uani 1 1 d . . . . .
H19 H 0.488632 0.458987 0.054283 0.036 Uiso 1 1 calc R . . . .
C20 C 0.3121(3) 0.43603(13) 0.03726(16) 0.0323(7) Uani 1 1 d . . . . .
H20 H 0.297591 0.441601 -0.017552 0.039 Uiso 1 1 calc R . . . .
C21 C 0.2185(3) 0.41744(13) 0.07522(17) 0.0312(7) Uani 1 1 d . . . . .
H21 H 0.141049 0.410698 0.046015 0.037 Uiso 1 1 calc R . . . .
C22 C 0.2401(3) 0.40877(12) 0.15717(16) 0.0240(6) Uani 1 1 d . . . . .
H22 H 0.177169 0.395911 0.182551 0.029 Uiso 1 1 calc R . . . .
C23 C 0.2494(2) 0.43855(11) 0.34117(14) 0.0163(5) Uani 1 1 d . . . . .
C24 C 0.2030(2) 0.48959(12) 0.30920(16) 0.0223(6) Uani 1 1 d . . . . .
H24 H 0.237789 0.506740 0.269271 0.027 Uiso 1 1 calc R . . . .
C25 C 0.1048(3) 0.51477(13) 0.33698(17) 0.0279(6) Uani 1 1 d . . . . .
H25 H 0.074105 0.548737 0.315635 0.033 Uiso 1 1 calc R . . . .
C26 C 0.0530(2) 0.48939(13) 0.39624(17) 0.0280(7) Uani 1 1 d . . . . .
H26 H -0.011462 0.506691 0.415613 0.034 Uiso 1 1 calc R . . . .
C27 C 0.0967(3) 0.43837(13) 0.42677(17) 0.0279(6) Uani 1 1 d . . . . .
H27 H 0.060036 0.420774 0.465528 0.034 Uiso 1 1 calc R . . . .
C28 C 0.1955(2) 0.41327(12) 0.39954(15) 0.0213(6) Uani 1 1 d . . . . .
H28 H 0.225505 0.379171 0.420860 0.026 Uiso 1 1 calc R . . . .
C29 C 0.7351(2) 0.30608(11) 0.27970(15) 0.0167(5) Uani 1 1 d . . . . .
C30 C 0.8527(2) 0.32810(12) 0.30384(16) 0.0235(6) Uani 1 1 d . . . . .
H30 H 0.897419 0.317856 0.352913 0.028 Uiso 1 1 calc R . . . .
C31 C 0.9038(3) 0.36514(13) 0.25530(17) 0.0301(7) Uani 1 1 d . . . . .
H31 H 0.982348 0.379132 0.271997 0.036 Uiso 1 1 calc R . . . .
C32 C 0.8390(3) 0.38114(12) 0.18307(17) 0.0295(7) Uani 1 1 d . . . . .
H32 H 0.872692 0.406604 0.151487 0.035 Uiso 1 1 calc R . . . .
C33 C 0.7234(3) 0.35933(12) 0.15730(16) 0.0251(6) Uani 1 1 d . . . . .
H33 H 0.679586 0.369799 0.108059 0.030 Uiso 1 1 calc R . . . .
C34 C 0.6723(2) 0.32150(11) 0.20534(15) 0.0195(5) Uani 1 1 d . . . . .
H34 H 0.595105 0.306445 0.187190 0.023 Uiso 1 1 calc R . . . .
C35 C 0.5543(2) 0.13478(11) 0.31548(14) 0.0164(5) Uani 1 1 d . . . . .
C36 C 0.5879(3) 0.08152(12) 0.34509(15) 0.0214(6) Uani 1 1 d . . . . .
H36 H 0.668824 0.069667 0.348811 0.026 Uiso 1 1 calc R . . . .
C37 C 0.5009(3) 0.04602(12) 0.36912(16) 0.0279(6) Uani 1 1 d . . . . .
H37 H 0.524275 0.010859 0.389729 0.033 Uiso 1 1 calc R . . . .
C38 C 0.3797(3) 0.06295(12) 0.36241(16) 0.0272(6) Uani 1 1 d . . . . .
H38 H 0.321768 0.039207 0.378466 0.033 Uiso 1 1 calc R . . . .
C39 C 0.3452(3) 0.11529(12) 0.33173(16) 0.0236(6) Uani 1 1 d . . . . .
H39 H 0.263586 0.126419 0.326380 0.028 Uiso 1 1 calc R . . . .
C40 C 0.4314(2) 0.15115(11) 0.30897(14) 0.0177(5) Uani 1 1 d . . . . .
H40 H 0.407483 0.186444 0.289166 0.021 Uiso 1 1 calc R . . . .
C41 C 0.6435(2) 0.18659(11) 0.18213(14) 0.0170(5) Uani 1 1 d . . . . .
C42 C 0.5273(2) 0.18122(12) 0.13683(15) 0.0211(6) Uani 1 1 d . . . . .
H42 H 0.460981 0.172492 0.161806 0.025 Uiso 1 1 calc R . . . .
C43 C 0.5088(3) 0.18868(13) 0.05494(16) 0.0276(7) Uani 1 1 d . . . . .
H43 H 0.430345 0.185962 0.025328 0.033 Uiso 1 1 calc R . . . .
C44 C 0.6085(3) 0.20026(13) 0.01754(16) 0.0305(7) Uani 1 1 d . . . . .
H44 H 0.596876 0.205240 -0.037371 0.037 Uiso 1 1 calc R . . . .
C45 C 0.7248(3) 0.20438(13) 0.06157(17) 0.0300(7) Uani 1 1 d . . . . .
H45 H 0.791485 0.211037 0.036002 0.036 Uiso 1 1 calc R . . . .
C46 C 0.7428(3) 0.19868(12) 0.14359(16) 0.0240(6) Uani 1 1 d . . . . .
H46 H 0.820919 0.202886 0.173104 0.029 Uiso 1 1 calc R . . . .
C47 C 0.8145(2) 0.15362(11) 0.32324(16) 0.0191(5) Uani 1 1 d . . . . .
C48 C 0.8563(3) 0.10898(13) 0.28243(19) 0.0308(7) Uani 1 1 d . . . . .
H48 H 0.809590 0.096170 0.235358 0.037 Uiso 1 1 calc R . . . .
C49 C 0.9673(3) 0.08362(14) 0.3119(2) 0.0406(8) Uani 1 1 d . . . . .
H49 H 0.995027 0.053814 0.284591 0.049 Uiso 1 1 calc R . . . .
C50 C 1.0367(3) 0.10251(14) 0.3818(2) 0.0398(9) Uani 1 1 d . . . . .
H50 H 1.110517 0.084981 0.401909 0.048 Uiso 1 1 calc R . . . .
C51 C 0.9974(3) 0.14685(15) 0.42140(19) 0.0355(7) Uani 1 1 d . . . . .
H51 H 1.045375 0.159878 0.467872 0.043 Uiso 1 1 calc R . . . .
C52 C 0.8861(2) 0.17268(12) 0.39271(16) 0.0247(6) Uani 1 1 d . . . . .
H52 H 0.859581 0.202737 0.420152 0.030 Uiso 1 1 calc R . . . .
O1 O 0.52467(16) 0.35623(8) 0.46735(9) 0.0181(4) Uani 1 1 d . . . . .
O2 O 0.70913(16) 0.33074(8) 0.43972(10) 0.0192(4) Uani 1 1 d . . . . .
O3 O 0.39929(16) 0.24912(8) 0.43017(10) 0.0190(4) Uani 1 1 d . . . . .
O4 O 0.59540(16) 0.22034(8) 0.45397(10) 0.0184(4) Uani 1 1 d . . . . .
P1 P 0.38330(6) 0.40666(3) 0.30928(3) 0.01339(13) Uani 1 1 d . . . . .
P2 P 0.66501(6) 0.18582(3) 0.29070(4) 0.01422(13) Uani 1 1 d . . . . .
Pd1 Pd 0.41288(2) 0.32204(2) 0.36353(2) 0.01250(5) Uani 1 1 d . . . . .
Pd2 Pd 0.65905(2) 0.26424(2) 0.35988(2) 0.01322(5) 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 1.510(3) . ?
C1 O1 1.255(3) . ?
C1 O2 1.264(3) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.509(4) . ?
C3 O3 1.261(3) . ?
C3 O4 1.255(3) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 C6 1.392(4) . ?
C5 C10 1.392(3) . ?
C5 Pd1 1.991(2) . ?
C6 H6 0.9300 . ?
C6 C7 1.388(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.391(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.383(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.393(4) . ?
C10 H10 0.9300 . ?
C11 C12 1.402(3) . ?
C11 C16 1.387(4) . ?
C11 P1 1.823(3) . ?
C12 H12 0.9300 . ?
C12 C13 1.384(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.384(4) . ?
C14 H14 0.9300 . ?
C14 C15 1.389(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.385(4) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(4) . ?
C17 C22 1.397(4) . ?
C17 P1 1.836(2) . ?
C18 H18 0.9300 . ?
C18 C19 1.385(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.369(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.380(4) . ?
C21 H21 0.9300 . ?
C21 C22 1.391(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.398(4) . ?
C23 C28 1.380(4) . ?
C23 P1 1.825(3) . ?
C24 H24 0.9300 . ?
C24 C25 1.390(4) . ?
C25 H25 0.9300 . ?
C25 C26 1.381(4) . ?
C26 H26 0.9300 . ?
C26 C27 1.380(4) . ?
C27 H27 0.9300 . ?
C27 C28 1.392(4) . ?
C28 H28 0.9300 . ?
C29 C30 1.400(4) . ?
C29 C34 1.389(4) . ?
C29 Pd2 1.987(3) . ?
C30 H30 0.9300 . ?
C30 C31 1.392(4) . ?
C31 H31 0.9300 . ?
C31 C32 1.371(4) . ?
C32 H32 0.9300 . ?
C32 C33 1.382(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.399(4) . ?
C34 H34 0.9300 . ?
C35 C36 1.396(4) . ?
C35 C40 1.401(3) . ?
C35 P2 1.825(3) . ?
C36 H36 0.9300 . ?
C36 C37 1.394(4) . ?
C37 H37 0.9300 . ?
C37 C38 1.386(4) . ?
C38 H38 0.9300 . ?
C38 C39 1.384(4) . ?
C39 H39 0.9300 . ?
C39 C40 1.384(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.390(4) . ?
C41 C46 1.399(3) . ?
C41 P2 1.824(2) . ?
C42 H42 0.9300 . ?
C42 C43 1.387(4) . ?
C43 H43 0.9300 . ?
C43 C44 1.389(4) . ?
C44 H44 0.9300 . ?
C44 C45 1.380(4) . ?
C45 H45 0.9300 . ?
C45 C46 1.384(4) . ?
C46 H46 0.9300 . ?
C47 C48 1.392(4) . ?
C47 C52 1.386(4) . ?
C47 P2 1.824(3) . ?
C48 H48 0.9300 . ?
C48 C49 1.386(4) . ?
C49 H49 0.9300 . ?
C49 C50 1.380(5) . ?
C50 H50 0.9300 . ?
C50 C51 1.365(5) . ?
C51 H51 0.9300 . ?
C51 C52 1.391(4) . ?
C52 H52 0.9300 . ?
O1 Pd1 2.1432(17) . ?
O2 Pd2 2.1041(17) . ?
O3 Pd1 2.0978(18) . ?
O4 Pd2 2.1298(17) . ?
P1 Pd1 2.2239(7) . ?
P2 Pd2 2.2196(6) . ?
Pd1 Pd2 3.0610(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 117.3(2) . . ?
O1 C1 O2 126.7(2) . . ?
O2 C1 C2 116.0(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 C4 115.9(2) . . ?
O4 C3 C4 117.6(2) . . ?
O4 C3 O3 126.4(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 C10 117.7(2) . . ?
C6 C5 Pd1 116.84(18) . . ?
C10 C5 Pd1 124.99(19) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 C5 121.7(2) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 H7 120.1 . . ?
C6 C7 C8 119.9(3) . . ?
C8 C7 H7 120.1 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.2(3) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 119.8 . . ?
C8 C9 C10 120.5(2) . . ?
C10 C9 H9 119.8 . . ?
C5 C10 C9 121.1(2) . . ?
C5 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C12 C11 P1 118.58(19) . . ?
C16 C11 C12 118.5(2) . . ?
C16 C11 P1 122.96(19) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.5(2) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.3(2) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 120.1 . . ?
C13 C14 C15 119.8(3) . . ?
C15 C14 H14 120.1 . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.8(3) . . ?
C16 C15 H15 120.1 . . ?
C11 C16 H16 119.5 . . ?
C15 C16 C11 121.1(2) . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C22 118.5(2) . . ?
C18 C17 P1 121.8(2) . . ?
C22 C17 P1 119.6(2) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H18 119.6 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.3(3) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.2(3) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.0(3) . . ?
C22 C21 H21 120.0 . . ?
C17 C22 H22 119.9 . . ?
C21 C22 C17 120.2(3) . . ?
C21 C22 H22 119.9 . . ?
C24 C23 P1 120.8(2) . . ?
C28 C23 C24 119.2(2) . . ?
C28 C23 P1 120.0(2) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 C23 120.1(3) . . ?
C25 C24 H24 119.9 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 C24 120.1(3) . . ?
C26 C25 H25 120.0 . . ?
C25 C26 H26 120.0 . . ?
C27 C26 C25 120.1(3) . . ?
C27 C26 H26 120.0 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 C27 120.5(3) . . ?
C23 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 Pd2 117.74(19) . . ?
C34 C29 C30 117.8(2) . . ?
C34 C29 Pd2 123.75(19) . . ?
C29 C30 H30 119.6 . . ?
C31 C30 C29 120.8(3) . . ?
C31 C30 H30 119.6 . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.5(3) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 120.1 . . ?
C31 C32 C33 119.9(3) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.0 . . ?
C32 C33 C34 120.0(3) . . ?
C34 C33 H33 120.0 . . ?
C29 C34 C33 121.0(3) . . ?
C29 C34 H34 119.5 . . ?
C33 C34 H34 119.5 . . ?
C36 C35 C40 118.6(2) . . ?
C36 C35 P2 123.0(2) . . ?
C40 C35 P2 118.3(2) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 C35 120.4(3) . . ?
C37 C36 H36 119.8 . . ?
C36 C37 H37 119.9 . . ?
C38 C37 C36 120.2(3) . . ?
C38 C37 H37 119.9 . . ?
C37 C38 H38 120.1 . . ?
C39 C38 C37 119.8(3) . . ?
C39 C38 H38 120.1 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.3(3) . . ?
C40 C39 H39 119.8 . . ?
C35 C40 H40 119.7 . . ?
C39 C40 C35 120.6(3) . . ?
C39 C40 H40 119.7 . . ?
C42 C41 C46 118.9(2) . . ?
C42 C41 P2 120.97(19) . . ?
C46 C41 P2 119.8(2) . . ?
C41 C42 H42 119.5 . . ?
C43 C42 C41 121.0(2) . . ?
C43 C42 H42 119.5 . . ?
C42 C43 H43 120.3 . . ?
C42 C43 C44 119.4(3) . . ?
C44 C43 H43 120.3 . . ?
C43 C44 H44 119.9 . . ?
C45 C44 C43 120.2(3) . . ?
C45 C44 H44 119.9 . . ?
C44 C45 H45 119.8 . . ?
C44 C45 C46 120.4(3) . . ?
C46 C45 H45 119.8 . . ?
C41 C46 H46 120.0 . . ?
C45 C46 C41 120.1(3) . . ?
C45 C46 H46 120.0 . . ?
C48 C47 P2 122.0(2) . . ?
C52 C47 C48 119.2(3) . . ?
C52 C47 P2 118.7(2) . . ?
C47 C48 H48 120.0 . . ?
C49 C48 C47 120.0(3) . . ?
C49 C48 H48 120.0 . . ?
C48 C49 H49 119.9 . . ?
C50 C49 C48 120.1(3) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 119.9 . . ?
C51 C50 C49 120.2(3) . . ?
C51 C50 H50 119.9 . . ?
C50 C51 H51 119.8 . . ?
C50 C51 C52 120.4(3) . . ?
C52 C51 H51 119.8 . . ?
C47 C52 C51 120.0(3) . . ?
C47 C52 H52 120.0 . . ?
C51 C52 H52 120.0 . . ?
C1 O1 Pd1 124.58(15) . . ?
C1 O2 Pd2 126.68(17) . . ?
C3 O3 Pd1 127.12(17) . . ?
C3 O4 Pd2 124.87(16) . . ?
C11 P1 C17 103.70(11) . . ?
C11 P1 C23 104.40(11) . . ?
C11 P1 Pd1 111.45(8) . . ?
C17 P1 Pd1 123.61(8) . . ?
C23 P1 C17 102.83(11) . . ?
C23 P1 Pd1 109.04(9) . . ?
C35 P2 Pd2 111.16(8) . . ?
C41 P2 C35 105.14(11) . . ?
C41 P2 Pd2 121.26(9) . . ?
C47 P2 C35 104.86(12) . . ?
C47 P2 C41 105.74(12) . . ?
C47 P2 Pd2 107.45(9) . . ?
C5 Pd1 O1 172.89(8) . . ?
C5 Pd1 O3 88.28(9) . . ?
C5 Pd1 P1 91.44(7) . . ?
C5 Pd1 Pd2 106.24(7) . . ?
O1 Pd1 P1 91.21(5) . . ?
O1 Pd1 Pd2 78.22(5) . . ?
O3 Pd1 O1 87.34(7) . . ?
O3 Pd1 P1 163.86(5) . . ?
O3 Pd1 Pd2 77.30(5) . . ?
P1 Pd1 Pd2 118.123(17) . . ?
C29 Pd2 O2 88.19(9) . . ?
C29 Pd2 O4 174.01(9) . . ?
C29 Pd2 P2 90.38(7) . . ?
C29 Pd2 Pd1 105.41(7) . . ?
O2 Pd2 O4 88.28(7) . . ?
O2 Pd2 P2 162.20(5) . . ?
O2 Pd2 Pd1 77.63(5) . . ?
O4 Pd2 P2 91.50(5) . . ?
O4 Pd2 Pd1 78.52(5) . . ?
P2 Pd2 Pd1 119.751(18) . . ?

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
C2 C1 O1 Pd1 166.93(18) . . . . ?
C2 C1 O2 Pd2 166.25(18) . . . . ?
C4 C3 O3 Pd1 163.97(17) . . . . ?
C4 C3 O4 Pd2 170.36(17) . . . . ?
C5 C6 C7 C8 1.1(4) . . . . ?
C6 C5 C10 C9 -0.1(4) . . . . ?
C6 C7 C8 C9 -1.0(4) . . . . ?
C7 C8 C9 C10 0.4(4) . . . . ?
C8 C9 C10 C5 0.2(4) . . . . ?
C10 C5 C6 C7 -0.5(4) . . . . ?
C11 C12 C13 C14 1.7(4) . . . . ?
C12 C11 C16 C15 2.5(4) . . . . ?
C12 C11 P1 C17 -73.2(2) . . . . ?
C12 C11 P1 C23 179.4(2) . . . . ?
C12 C11 P1 Pd1 61.8(2) . . . . ?
C12 C13 C14 C15 1.0(4) . . . . ?
C13 C14 C15 C16 -1.9(4) . . . . ?
C14 C15 C16 C11 0.1(4) . . . . ?
C16 C11 C12 C13 -3.4(4) . . . . ?
C16 C11 P1 C17 106.9(2) . . . . ?
C16 C11 P1 C23 -0.5(2) . . . . ?
C16 C11 P1 Pd1 -118.0(2) . . . . ?
C17 C18 C19 C20 -0.5(5) . . . . ?
C18 C17 C22 C21 -0.8(4) . . . . ?
C18 C17 P1 C11 27.3(2) . . . . ?
C18 C17 P1 C23 135.8(2) . . . . ?
C18 C17 P1 Pd1 -100.6(2) . . . . ?
C18 C19 C20 C21 0.3(5) . . . . ?
C19 C20 C21 C22 -0.4(5) . . . . ?
C20 C21 C22 C17 0.6(5) . . . . ?
C22 C17 C18 C19 0.7(4) . . . . ?
C22 C17 P1 C11 -154.5(2) . . . . ?
C22 C17 P1 C23 -45.9(2) . . . . ?
C22 C17 P1 Pd1 77.7(2) . . . . ?
C23 C24 C25 C26 0.0(4) . . . . ?
C24 C23 C28 C27 -0.5(4) . . . . ?
C24 C23 P1 C11 67.4(2) . . . . ?
C24 C23 P1 C17 -40.6(2) . . . . ?
C24 C23 P1 Pd1 -173.43(19) . . . . ?
C24 C25 C26 C27 -1.4(4) . . . . ?
C25 C26 C27 C28 2.0(4) . . . . ?
C26 C27 C28 C23 -1.0(4) . . . . ?
C28 C23 C24 C25 1.0(4) . . . . ?
C28 C23 P1 C11 -110.3(2) . . . . ?
C28 C23 P1 C17 141.7(2) . . . . ?
C28 C23 P1 Pd1 8.9(2) . . . . ?
C29 C30 C31 C32 0.6(4) . . . . ?
C30 C29 C34 C33 -2.2(4) . . . . ?
C30 C31 C32 C33 -1.6(4) . . . . ?
C31 C32 C33 C34 0.7(4) . . . . ?
C32 C33 C34 C29 1.2(4) . . . . ?
C34 C29 C30 C31 1.3(4) . . . . ?
C35 C36 C37 C38 1.2(4) . . . . ?
C36 C35 C40 C39 0.2(4) . . . . ?
C36 C35 P2 C41 105.4(2) . . . . ?
C36 C35 P2 C47 -5.8(2) . . . . ?
C36 C35 P2 Pd2 -121.65(19) . . . . ?
C36 C37 C38 C39 0.0(4) . . . . ?
C37 C38 C39 C40 -1.1(4) . . . . ?
C38 C39 C40 C35 1.0(4) . . . . ?
C40 C35 C36 C37 -1.3(4) . . . . ?
C40 C35 P2 C41 -78.6(2) . . . . ?
C40 C35 P2 C47 170.17(19) . . . . ?
C40 C35 P2 Pd2 54.4(2) . . . . ?
C41 C42 C43 C44 1.7(5) . . . . ?
C42 C41 C46 C45 -0.8(4) . . . . ?
C42 C41 P2 C35 37.0(3) . . . . ?
C42 C41 P2 C47 147.7(2) . . . . ?
C42 C41 P2 Pd2 -89.9(2) . . . . ?
C42 C43 C44 C45 -0.1(5) . . . . ?
C43 C44 C45 C46 -1.9(5) . . . . ?
C44 C45 C46 C41 2.4(5) . . . . ?
C46 C41 C42 C43 -1.2(4) . . . . ?
C46 C41 P2 C35 -149.9(2) . . . . ?
C46 C41 P2 C47 -39.2(3) . . . . ?
C46 C41 P2 Pd2 83.2(2) . . . . ?
C47 C48 C49 C50 0.0(5) . . . . ?
C48 C47 C52 C51 -0.7(4) . . . . ?
C48 C47 P2 C35 72.8(3) . . . . ?
C48 C47 P2 C41 -38.0(3) . . . . ?
C48 C47 P2 Pd2 -168.8(2) . . . . ?
C48 C49 C50 C51 -1.1(5) . . . . ?
C49 C50 C51 C52 1.3(5) . . . . ?
C50 C51 C52 C47 -0.4(4) . . . . ?
C52 C47 C48 C49 0.9(4) . . . . ?
C52 C47 P2 C35 -104.2(2) . . . . ?
C52 C47 P2 C41 145.0(2) . . . . ?
C52 C47 P2 Pd2 14.1(2) . . . . ?
O1 C1 O2 Pd2 -15.7(4) . . . . ?
O2 C1 O1 Pd1 -11.1(4) . . . . ?
O3 C3 O4 Pd2 -7.6(4) . . . . ?
O4 C3 O3 Pd1 -18.0(4) . . . . ?
P1 C11 C12 C13 176.7(2) . . . . ?
P1 C11 C16 C15 -177.6(2) . . . . ?
P1 C17 C18 C19 179.0(2) . . . . ?
P1 C17 C22 C21 -179.1(2) . . . . ?
P1 C23 C24 C25 -176.7(2) . . . . ?
P1 C23 C28 C27 177.3(2) . . . . ?
P2 C35 C36 C37 174.7(2) . . . . ?
P2 C35 C40 C39 -175.96(19) . . . . ?
P2 C41 C42 C43 172.0(2) . . . . ?
P2 C41 C46 C45 -174.1(2) . . . . ?
P2 C47 C48 C49 -176.1(2) . . . . ?
P2 C47 C52 C51 176.4(2) . . . . ?
Pd1 C5 C6 C7 -173.0(2) . . . . ?
Pd1 C5 C10 C9 171.7(2) . . . . ?
Pd2 C29 C30 C31 -169.7(2) . . . . ?
Pd2 C29 C34 C33 168.3(2) . . . . ?

_olex2_date_sample_data_collection 2018-09-19
_olex2_exptl_crystal_mounting_method 'oil on 200 micrometre micromount'
_olex2_submission_original_sample_id NWJS-4-273-precipitate2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.507
_oxdiff_exptl_absorpt_empirical_full_min 0.796
####################################################################### 
# 
# 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_ijsf1821
_database_code_depnum_ccdc_archive 'CCDC 1894930'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2019-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C54 H45 P3 Pd, 1.61(C3 H7), 0.39(C4 H8 O)'
_chemical_formula_sum            'C60.39 H59.39 O0.39 P3 Pd'
_chemical_formula_weight         990.70
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C76 H66 O4 P4 Pd1'
_chemical_oxdiff_usercomment     'Neil Scott NWJS-4-293-crystals1'
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'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.5043(4)
_cell_length_b                   13.6723(4)
_cell_length_c                   14.3402(4)
_cell_angle_alpha                92.507(2)
_cell_angle_beta                 111.038(2)
_cell_angle_gamma                96.346(2)
_cell_volume                     2446.12(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9032
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      28.6610
_cell_measurement_theta_min      3.4890
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.518
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1031.7
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.1284
5 0 -4 0.0541
-1 0 1 0.0584
-1 0 0 0.0845
-4 0 5 0.0761
0 1 0 0.0451
0 -1 0 0.0332
4 1 -5 0.0709
2 -4 5 0.1183
5 3 -2 0.0733
0 4 5 0.1078
5 2 -5 0.0499
19 2 -7 0.0735

_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.078
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0000 0.0000 1.0000 0.0009 0.0411 0.0338
5.0000 0.0000 -4.0000 0.0324 0.0817 -0.2719
-1.0000 -0.0000 1.0000 -0.0063 -0.0081 0.0611
-1.0000 -0.0000 0.0000 -0.0072 -0.0492 0.0274
-4.0000 -0.0000 5.0000 -0.0242 0.0087 0.2783
-0.0000 1.0000 0.0000 -0.0506 0.0123 -0.0061
0.0000 -1.0000 -0.0000 0.0506 -0.0123 0.0061
4.0000 1.0000 -5.0000 -0.0264 0.0036 -0.2844
2.0000 -4.0000 5.0000 0.2216 0.2551 0.1383
5.0000 3.0000 -2.0000 -0.1175 0.2007 -0.2226
-0.0000 4.0000 5.0000 -0.1976 0.2546 0.1445
5.0000 2.0000 -5.0000 -0.0697 0.0651 -0.3178
19.0000 2.0000 -7.0000 0.0298 0.6722 -0.7685

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20381
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.267
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      5.00  91.00   1.00   16.00    --   18.24  37.00  60.00   86
  2  ω     -7.00  89.00   1.00   16.00    --   18.24  37.00 150.00   96
  3  ω    -19.00  20.00   1.00   16.00    --   18.24 -99.00 -90.00   39
  4  ω    -17.00  60.00   1.00   16.00    --   18.24 -99.00 -30.00   77
  5  ω    -82.00  11.00   1.00   16.00    --  -18.55 -77.00-180.00   93
  6  ω     -1.00  25.00   1.00   16.00    --  -18.55  57.00  60.00   26
  7  ω    -93.00 -68.00   1.00   16.00    --  -18.55 154.00   6.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0072445000
_diffrn_orient_matrix_UB_12      -0.0505953000
_diffrn_orient_matrix_UB_13      0.0009490000
_diffrn_orient_matrix_UB_21      0.0492362000
_diffrn_orient_matrix_UB_22      0.0122526000
_diffrn_orient_matrix_UB_23      0.0411197000
_diffrn_orient_matrix_UB_31      -0.0273735000
_diffrn_orient_matrix_UB_32      -0.0060736000
_diffrn_orient_matrix_UB_33      0.0337579000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8672
_reflns_number_total             9977
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         9977
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0326
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0159P)²+1.8801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0701
_refine_special_details          
;
disordered solvent- either 1 molecule of hexane (60 %) or 1 molecule of THF (40 %)
THF restraints:
DFIX 1.42 C61 O1 C64 O1
DFIX 1.5 C61 C62 C62 C63 C63 C64
DANG 2.32 C61 C64
DANG 2.36 C61 C63 C62 C64
DANG 2.34 C62 O1 C63 O1
EADP C63 C62
Hexane constraints:
DFIX 1.513 C60 C59
DFIX 1.524 C59 C58
DANG 2.48 C60 C58
DANG 2.49 C59 C58
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C61-O1 = C64-O1
 1.42 with sigma of 0.02
 C61-C62 = C62-C63 = C63-C64
 1.5 with sigma of 0.02
 C60-C59
 1.513 with sigma of 0.02
 C59-C58
 1.524 with sigma of 0.02
 C60-C58
 2.48 with sigma of 0.04
 C59-C58
 2.49 with sigma of 0.04
 C61-C64
 2.32 with sigma of 0.04
 C61-C63 = C62-C64
 2.36 with sigma of 0.04
 C62-O1 = C63-O1
 2.34 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C63) = Uanis(C62)
4. Others
 Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(O1)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C61)=
 Sof(H61A)=Sof(H61B)=Sof(C62)=Sof(H62A)=Sof(H62B)=1-FVAR(1)
 Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(H58C)=Sof(C59)=
 Sof(H59A)=Sof(H59B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C57(H57A,H57B), C56(H56A,H56B), C63(H63A,H63B), C60(H60A,H60B), C64(H64A,
 H64B), C61(H61A,H61B), C59(H59A,H59B), C62(H62A,H62B)
5.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C38(H38), C50(H50), C18(H18), C32(H32), C2(H2), C54(H54), C30(H30),
 C6(H6), C36(H36), C48(H48), C53(H53), C20(H20), C14(H14), C52(H52), C44(H44),
 C5(H5), C12(H12), C9(H9), C3(H3), C51(H51), C35(H35), C29(H29), C27(H27),
 C34(H34), C24(H24), C17(H17), C8(H8), C42(H42), C21(H21), C45(H45), C10(H10),
 C40(H40), C4(H4), C22(H22), C39(H39), C41(H41), C33(H33), C11(H11), C28(H28),
 C47(H47), C15(H15), C23(H23), C46(H46), C16(H16)
5.c Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C58(H58A,H58B,H58C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.32139(2) 0.37183(2) 0.75551(2) 0.01302(5) Uani 1 1 d . . . . .
P3 P 0.30886(4) 0.53910(4) 0.75540(4) 0.01329(12) Uani 1 1 d . . . . .
P2 P 0.47747(5) 0.32832(4) 0.74322(4) 0.01345(12) Uani 1 1 d . . . . .
P1 P 0.18184(5) 0.24640(4) 0.72682(4) 0.01395(12) Uani 1 1 d . . . . .
C25 C 0.46402(18) 0.29665(16) 0.61288(16) 0.0152(5) Uani 1 1 d . . . . .
C37 C 0.26400(17) 0.57649(16) 0.62695(16) 0.0155(5) Uani 1 1 d . . . . .
C49 C 0.21666(17) 0.59474(16) 0.80424(16) 0.0141(4) Uani 1 1 d . . . . .
C26 C 0.36149(18) 0.26835(16) 0.54249(17) 0.0174(5) Uani 1 1 d . . . . .
H26 H 0.303070 0.265874 0.562589 0.021 Uiso 1 1 calc R . . . .
C31 C 0.59901(17) 0.41892(16) 0.78728(16) 0.0142(4) Uani 1 1 d . . . . .
C19 C 0.52957(18) 0.22091(16) 0.80788(16) 0.0157(5) Uani 1 1 d . . . . .
C13 C 0.10811(17) 0.23089(17) 0.59006(16) 0.0154(5) Uani 1 1 d . . . . .
C1 C 0.07185(18) 0.25568(16) 0.77298(16) 0.0162(5) Uani 1 1 d . . . . .
C38 C 0.28120(19) 0.51784(17) 0.55353(17) 0.0202(5) Uani 1 1 d . . . . .
H38 H 0.318869 0.464347 0.571556 0.024 Uiso 1 1 calc R . . . .
C50 C 0.11002(18) 0.55051(17) 0.76935(17) 0.0187(5) Uani 1 1 d . . . . .
H50 H 0.087773 0.496217 0.721837 0.022 Uiso 1 1 calc R . . . .
C18 C 0.09863(18) 0.31695(17) 0.54044(17) 0.0189(5) Uani 1 1 d . . . . .
H18 H 0.126509 0.377909 0.577281 0.023 Uiso 1 1 calc R . . . .
C32 C 0.68249(18) 0.41305(17) 0.87724(17) 0.0191(5) Uani 1 1 d . . . . .
H32 H 0.679698 0.359033 0.913876 0.023 Uiso 1 1 calc R . . . .
C2 C 0.08533(19) 0.32727(17) 0.84960(17) 0.0204(5) Uani 1 1 d . . . . .
H2 H 0.149793 0.369106 0.877479 0.024 Uiso 1 1 calc R . . . .
C54 C 0.24809(18) 0.67479(16) 0.87652(16) 0.0169(5) Uani 1 1 d . . . . .
H54 H 0.319009 0.704426 0.901467 0.020 Uiso 1 1 calc R . . . .
C30 C 0.55034(18) 0.30112(17) 0.58056(17) 0.0184(5) Uani 1 1 d . . . . .
H30 H 0.619505 0.320676 0.626440 0.022 Uiso 1 1 calc R . . . .
C6 C -0.02579(18) 0.19416(18) 0.73222(17) 0.0202(5) Uani 1 1 d . . . . .
H6 H -0.036385 0.146135 0.680358 0.024 Uiso 1 1 calc R . . . .
C36 C 0.60529(19) 0.50165(17) 0.73437(17) 0.0186(5) Uani 1 1 d . . . . .
H36 H 0.549560 0.508057 0.674708 0.022 Uiso 1 1 calc R . . . .
C48 C 0.50655(18) 0.58833(18) 0.90499(17) 0.0195(5) Uani 1 1 d . . . . .
H48 H 0.492195 0.524942 0.922144 0.023 Uiso 1 1 calc R . . . .
C7 C 0.21099(18) 0.11992(16) 0.75398(16) 0.0164(5) Uani 1 1 d . . . . .
C43 C 0.43348(17) 0.62213(16) 0.82102(16) 0.0151(5) Uani 1 1 d . . . . .
C53 C 0.17461(19) 0.71103(17) 0.91193(17) 0.0188(5) Uani 1 1 d . . . . .
H53 H 0.196441 0.764991 0.959805 0.023 Uiso 1 1 calc R . . . .
C20 C 0.50457(19) 0.19951(17) 0.89129(17) 0.0210(5) Uani 1 1 d . . . . .
H20 H 0.461245 0.237779 0.910666 0.025 Uiso 1 1 calc R . . . .
C14 C 0.0652(2) 0.14112(18) 0.53325(18) 0.0247(5) Uani 1 1 d . . . . .
H14 H 0.071024 0.082775 0.564638 0.030 Uiso 1 1 calc R . . . .
C52 C 0.06916(19) 0.66694(18) 0.87604(17) 0.0212(5) Uani 1 1 d . . . . .
H52 H 0.020080 0.691169 0.899730 0.025 Uiso 1 1 calc R . . . .
C44 C 0.45771(19) 0.71634(17) 0.79524(17) 0.0196(5) Uani 1 1 d . . . . .
H44 H 0.410018 0.739917 0.739001 0.023 Uiso 1 1 calc R . . . .
C5 C -0.10684(19) 0.20365(18) 0.76786(18) 0.0241(5) Uani 1 1 d . . . . .
H5 H -0.171283 0.161743 0.740317 0.029 Uiso 1 1 calc R . . . .
C12 C 0.17188(19) 0.06241(18) 0.81417(17) 0.0218(5) Uani 1 1 d . . . . .
H12 H 0.125376 0.086613 0.841268 0.026 Uiso 1 1 calc R . . . .
C9 C 0.3108(2) -0.01143(18) 0.73592(19) 0.0263(6) Uani 1 1 d . . . . .
H9 H 0.357685 -0.035917 0.709423 0.032 Uiso 1 1 calc R . . . .
C3 C 0.0035(2) 0.33720(19) 0.88521(18) 0.0245(5) Uani 1 1 d . . . . .
H3 H 0.013481 0.385606 0.936560 0.029 Uiso 1 1 calc R . . . .
C51 C 0.03696(18) 0.58687(18) 0.80495(17) 0.0211(5) Uani 1 1 d . . . . .
H51 H -0.033918 0.557159 0.780808 0.025 Uiso 1 1 calc R . . . .
C35 C 0.69342(19) 0.57390(17) 0.76985(18) 0.0210(5) Uani 1 1 d . . . . .
H35 H 0.697223 0.627706 0.733206 0.025 Uiso 1 1 calc R . . . .
C29 C 0.5340(2) 0.27675(18) 0.48094(17) 0.0221(5) Uani 1 1 d . . . . .
H29 H 0.591972 0.279953 0.460204 0.027 Uiso 1 1 calc R . . . .
C27 C 0.34495(19) 0.24374(18) 0.44268(17) 0.0222(5) Uani 1 1 d . . . . .
H27 H 0.275875 0.224668 0.396420 0.027 Uiso 1 1 calc R . . . .
C34 C 0.77600(19) 0.56655(18) 0.85963(18) 0.0226(5) Uani 1 1 d . . . . .
H34 H 0.835085 0.615334 0.883465 0.027 Uiso 1 1 calc R . . . .
C24 C 0.5934(2) 0.16211(18) 0.77984(18) 0.0244(6) Uani 1 1 d . . . . .
H24 H 0.611000 0.175470 0.724225 0.029 Uiso 1 1 calc R . . . .
C17 C 0.04851(19) 0.31303(18) 0.43750(17) 0.0229(5) Uani 1 1 d . . . . .
H17 H 0.043873 0.371083 0.405631 0.027 Uiso 1 1 calc R . . . .
C8 C 0.28187(19) 0.08142(17) 0.71607(18) 0.0216(5) Uani 1 1 d . . . . .
H8 H 0.310109 0.119014 0.676699 0.026 Uiso 1 1 calc R . . . .
C42 C 0.20965(18) 0.65793(18) 0.59776(18) 0.0211(5) Uani 1 1 d . . . . .
H42 H 0.198597 0.698772 0.645681 0.025 Uiso 1 1 calc R . . . .
C21 C 0.5436(2) 0.12144(18) 0.94620(18) 0.0243(5) Uani 1 1 d . . . . .
H21 H 0.527130 0.108323 1.002435 0.029 Uiso 1 1 calc R . . . .
C45 C 0.5526(2) 0.77540(18) 0.85292(19) 0.0263(6) Uani 1 1 d . . . . .
H45 H 0.568682 0.837885 0.834661 0.032 Uiso 1 1 calc R . . . .
C10 C 0.2705(2) -0.06813(19) 0.79500(19) 0.0286(6) Uani 1 1 d . . . . .
H10 H 0.289703 -0.130800 0.808190 0.034 Uiso 1 1 calc R . . . .
C40 C 0.18766(19) 0.6184(2) 0.42624(18) 0.0273(6) Uani 1 1 d . . . . .
H40 H 0.161201 0.631613 0.359301 0.033 Uiso 1 1 calc R . . . .
C4 C -0.0926(2) 0.27538(19) 0.84454(18) 0.0243(5) Uani 1 1 d . . . . .
H4 H -0.147316 0.281870 0.868458 0.029 Uiso 1 1 calc R . . . .
C22 C 0.6065(2) 0.06379(18) 0.91731(18) 0.0256(6) Uani 1 1 d . . . . .
H22 H 0.632411 0.011448 0.953792 0.031 Uiso 1 1 calc R . . . .
C39 C 0.2427(2) 0.53852(19) 0.45401(18) 0.0248(6) Uani 1 1 d . . . . .
H39 H 0.254017 0.498425 0.405696 0.030 Uiso 1 1 calc R . . . .
C41 C 0.17207(19) 0.6785(2) 0.49820(18) 0.0260(6) Uani 1 1 d . . . . .
H41 H 0.136202 0.733012 0.479823 0.031 Uiso 1 1 calc R . . . .
C33 C 0.77011(19) 0.48648(18) 0.91345(18) 0.0238(5) Uani 1 1 d . . . . .
H33 H 0.824969 0.481615 0.974204 0.029 Uiso 1 1 calc R . . . .
C11 C 0.2016(2) -0.03064(19) 0.83413(19) 0.0282(6) Uani 1 1 d . . . . .
H11 H 0.174669 -0.068201 0.874400 0.034 Uiso 1 1 calc R . . . .
C28 C 0.4312(2) 0.24758(18) 0.41209(17) 0.0238(5) Uani 1 1 d . . . . .
H28 H 0.420255 0.230601 0.345284 0.029 Uiso 1 1 calc R . . . .
C47 C 0.60052(19) 0.6478(2) 0.96351(18) 0.0263(6) Uani 1 1 d . . . . .
H47 H 0.648090 0.624693 1.020151 0.032 Uiso 1 1 calc R . . . .
C15 C 0.0136(2) 0.1375(2) 0.42998(19) 0.0312(6) Uani 1 1 d . . . . .
H15 H -0.015582 0.076862 0.392887 0.037 Uiso 1 1 calc R . . . .
C23 C 0.6313(2) 0.08370(19) 0.83385(19) 0.0304(6) Uani 1 1 d . . . . .
H23 H 0.673414 0.044376 0.813960 0.036 Uiso 1 1 calc R . . . .
C46 C 0.6233(2) 0.7413(2) 0.93756(19) 0.0298(6) Uani 1 1 d . . . . .
H46 H 0.686159 0.781447 0.976894 0.036 Uiso 1 1 calc R . . . .
C16 C 0.0053(2) 0.22337(19) 0.38174(18) 0.0263(6) Uani 1 1 d . . . . .
H16 H -0.029087 0.220686 0.312499 0.032 Uiso 1 1 calc R . . . .
C57 C 0.4521(2) 1.0017(2) 0.5152(2) 0.0327(6) Uani 1 1 d . . . . .
H57A H 0.456329 0.956700 0.566484 0.039 Uiso 1 1 calc R . . . .
H57B H 0.455164 1.067846 0.544460 0.039 Uiso 1 1 calc R . . . .
C56 C 0.3460(2) 0.9749(2) 0.4297(2) 0.0397(7) Uani 1 1 d . . . . .
H56A H 0.341401 0.907586 0.402613 0.048 Uiso 1 1 calc R . . . .
H56B H 0.343281 1.017766 0.376871 0.048 Uiso 1 1 calc R . . . .
C55 C 0.2493(2) 0.9835(2) 0.4594(2) 0.0464(8) Uani 1 1 d . . . . .
H55A H 0.245162 0.934265 0.504034 0.070 Uiso 1 1 calc GR . . . .
H55B H 0.185192 0.973618 0.400358 0.070 Uiso 1 1 calc GR . . . .
H55C H 0.256665 1.047985 0.492366 0.070 Uiso 1 1 calc GR . . . .
C63 C 0.1665(8) 0.0646(8) 0.0780(7) 0.047(2) Uani 0.391(4) 1 d D . P A 2
H63A H 0.229293 0.082194 0.061200 0.056 Uiso 0.391(4) 1 calc R . P A 2
H63B H 0.143949 -0.006024 0.063735 0.056 Uiso 0.391(4) 1 calc R . P A 2
O1 O 0.0147(4) 0.1281(4) 0.0842(3) 0.0350(15) Uani 0.391(4) 1 d D . P A 2
C60 C 0.0260(4) 0.0238(4) 0.0532(3) 0.0360(12) Uani 0.609(4) 1 d D . P A 1
H60A H -0.026322 0.056699 0.069930 0.043 Uiso 0.609(4) 1 calc R . P A 1
H60B H 0.045896 -0.027628 0.098206 0.043 Uiso 0.609(4) 1 calc R . P A 1
C64 C 0.0767(6) 0.1231(6) 0.0241(6) 0.036(2) Uani 0.391(4) 1 d D . P A 2
H64A H 0.105587 0.188951 0.015912 0.043 Uiso 0.391(4) 1 calc R . P A 2
H64B H 0.033510 0.090325 -0.041708 0.043 Uiso 0.391(4) 1 calc R . P A 2
C61 C 0.0841(6) 0.1291(6) 0.1864(5) 0.041(2) Uani 0.391(4) 1 d D . P A 2
H61A H 0.052190 0.083396 0.220892 0.049 Uiso 0.391(4) 1 calc R . P A 2
H61B H 0.096461 0.194739 0.220265 0.049 Uiso 0.391(4) 1 calc R . P A 2
C58 C 0.1702(5) 0.1465(4) 0.1812(4) 0.0373(14) Uani 0.609(4) 1 d D . P A 1
H58A H 0.237040 0.186659 0.192391 0.056 Uiso 0.609(4) 1 calc GR . P A 1
H58B H 0.181606 0.096104 0.227102 0.056 Uiso 0.609(4) 1 calc GR . P A 1
H58C H 0.120763 0.186988 0.191791 0.056 Uiso 0.609(4) 1 calc GR . P A 1
C59 C 0.1231(5) 0.0972(5) 0.0712(4) 0.0438(16) Uani 0.609(4) 1 d D . P A 1
H59A H 0.104470 0.148020 0.025160 0.053 Uiso 0.609(4) 1 calc R . P A 1
H59B H 0.177278 0.064303 0.057754 0.053 Uiso 0.609(4) 1 calc R . P A 1
C62 C 0.1862(8) 0.0992(8) 0.1868(7) 0.047(2) Uani 0.391(4) 1 d D . P A 2
H62A H 0.206246 0.046032 0.229600 0.056 Uiso 0.391(4) 1 calc R . P A 2
H62B H 0.243100 0.154547 0.211102 0.056 Uiso 0.391(4) 1 calc R . P A 2


_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 P3 2.3119(6) . ?
Pd1 P2 2.3156(6) . ?
Pd1 P1 2.3084(6) . ?
P3 C37 1.836(2) . ?
P3 C49 1.846(2) . ?
P3 C43 1.831(2) . ?
P2 C25 1.839(2) . ?
P2 C31 1.834(2) . ?
P2 C19 1.841(2) . ?
P1 C13 1.843(2) . ?
P1 C1 1.844(2) . ?
P1 C7 1.843(2) . ?
C25 C26 1.389(3) . ?
C25 C30 1.397(3) . ?
C37 C38 1.396(3) . ?
C37 C42 1.398(3) . ?
C49 C50 1.398(3) . ?
C49 C54 1.391(3) . ?
C26 H26 0.9300 . ?
C26 C27 1.387(3) . ?
C31 C32 1.388(3) . ?
C31 C36 1.401(3) . ?
C19 C20 1.389(3) . ?
C19 C24 1.388(3) . ?
C13 C18 1.396(3) . ?
C13 C14 1.387(3) . ?
C1 C2 1.386(3) . ?
C1 C6 1.395(3) . ?
C38 H38 0.9300 . ?
C38 C39 1.386(3) . ?
C50 H50 0.9300 . ?
C50 C51 1.389(3) . ?
C18 H18 0.9300 . ?
C18 C17 1.381(3) . ?
C32 H32 0.9300 . ?
C32 C33 1.389(3) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(3) . ?
C54 H54 0.9300 . ?
C54 C53 1.392(3) . ?
C30 H30 0.9300 . ?
C30 C29 1.384(3) . ?
C6 H6 0.9300 . ?
C6 C5 1.380(3) . ?
C36 H36 0.9300 . ?
C36 C35 1.383(3) . ?
C48 H48 0.9300 . ?
C48 C43 1.391(3) . ?
C48 C47 1.387(3) . ?
C7 C12 1.392(3) . ?
C7 C8 1.396(3) . ?
C43 C44 1.392(3) . ?
C53 H53 0.9300 . ?
C53 C52 1.383(3) . ?
C20 H20 0.9300 . ?
C20 C21 1.392(3) . ?
C14 H14 0.9300 . ?
C14 C15 1.388(3) . ?
C52 H52 0.9300 . ?
C52 C51 1.380(3) . ?
C44 H44 0.9300 . ?
C44 C45 1.390(3) . ?
C5 H5 0.9300 . ?
C5 C4 1.386(3) . ?
C12 H12 0.9300 . ?
C12 C11 1.387(3) . ?
C9 H9 0.9300 . ?
C9 C8 1.381(3) . ?
C9 C10 1.382(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.382(3) . ?
C51 H51 0.9300 . ?
C35 H35 0.9300 . ?
C35 C34 1.384(3) . ?
C29 H29 0.9300 . ?
C29 C28 1.386(3) . ?
C27 H27 0.9300 . ?
C27 C28 1.381(3) . ?
C34 H34 0.9300 . ?
C34 C33 1.378(3) . ?
C24 H24 0.9300 . ?
C24 C23 1.386(3) . ?
C17 H17 0.9300 . ?
C17 C16 1.380(3) . ?
C8 H8 0.9300 . ?
C42 H42 0.9300 . ?
C42 C41 1.386(3) . ?
C21 H21 0.9300 . ?
C21 C22 1.373(3) . ?
C45 H45 0.9300 . ?
C45 C46 1.385(4) . ?
C10 H10 0.9300 . ?
C10 C11 1.378(4) . ?
C40 H40 0.9300 . ?
C40 C39 1.382(4) . ?
C40 C41 1.380(3) . ?
C4 H4 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.383(3) . ?
C39 H39 0.9300 . ?
C41 H41 0.9300 . ?
C33 H33 0.9300 . ?
C11 H11 0.9300 . ?
C28 H28 0.9300 . ?
C47 H47 0.9300 . ?
C47 C46 1.381(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.383(4) . ?
C23 H23 0.9300 . ?
C46 H46 0.9300 . ?
C16 H16 0.9300 . ?
C57 C57 1.510(5) 2_676 ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C57 C56 1.508(4) . ?
C56 H56A 0.9700 . ?
C56 H56B 0.9700 . ?
C56 C55 1.526(4) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C63 H63A 0.9700 . ?
C63 H63B 0.9700 . ?
C63 C64 1.518(10) . ?
C63 C62 1.530(11) . ?
O1 C64 1.404(8) . ?
O1 C61 1.427(8) . ?
C60 C60 1.513(8) 2 ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C60 C59 1.496(7) . ?
C64 H64A 0.9700 . ?
C64 H64B 0.9700 . ?
C61 H61A 0.9700 . ?
C61 H61B 0.9700 . ?
C61 C62 1.479(10) . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
C58 C59 1.562(7) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C62 H62A 0.9700 . ?
C62 H62B 0.9700 . ?

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
P3 Pd1 P2 114.88(2) . . ?
P1 Pd1 P3 126.09(2) . . ?
P1 Pd1 P2 117.11(2) . . ?
C37 P3 Pd1 110.83(7) . . ?
C37 P3 C49 101.07(10) . . ?
C49 P3 Pd1 121.81(7) . . ?
C43 P3 Pd1 116.21(7) . . ?
C43 P3 C37 103.83(10) . . ?
C43 P3 C49 100.68(10) . . ?
C25 P2 Pd1 112.71(7) . . ?
C25 P2 C19 103.50(10) . . ?
C31 P2 Pd1 119.36(7) . . ?
C31 P2 C25 101.22(10) . . ?
C31 P2 C19 100.64(10) . . ?
C19 P2 Pd1 117.02(7) . . ?
C13 P1 Pd1 106.23(7) . . ?
C13 P1 C1 101.18(10) . . ?
C1 P1 Pd1 123.25(8) . . ?
C7 P1 Pd1 119.55(7) . . ?
C7 P1 C13 101.87(10) . . ?
C7 P1 C1 101.43(10) . . ?
C26 C25 P2 117.67(17) . . ?
C26 C25 C30 118.4(2) . . ?
C30 C25 P2 123.91(17) . . ?
C38 C37 P3 118.06(17) . . ?
C38 C37 C42 118.2(2) . . ?
C42 C37 P3 123.69(17) . . ?
C50 C49 P3 117.56(17) . . ?
C54 C49 P3 123.94(17) . . ?
C54 C49 C50 118.4(2) . . ?
C25 C26 H26 119.5 . . ?
C27 C26 C25 121.0(2) . . ?
C27 C26 H26 119.5 . . ?
C32 C31 P2 121.83(17) . . ?
C32 C31 C36 118.0(2) . . ?
C36 C31 P2 119.92(17) . . ?
C20 C19 P2 117.17(17) . . ?
C24 C19 P2 124.26(17) . . ?
C24 C19 C20 118.6(2) . . ?
C18 C13 P1 116.55(17) . . ?
C14 C13 P1 125.23(17) . . ?
C14 C13 C18 118.2(2) . . ?
C2 C1 P1 119.21(17) . . ?
C2 C1 C6 118.5(2) . . ?
C6 C1 P1 122.30(17) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(2) . . ?
C39 C38 H38 119.7 . . ?
C49 C50 H50 119.7 . . ?
C51 C50 C49 120.6(2) . . ?
C51 C50 H50 119.7 . . ?
C13 C18 H18 119.5 . . ?
C17 C18 C13 121.1(2) . . ?
C17 C18 H18 119.5 . . ?
C31 C32 H32 119.4 . . ?
C31 C32 C33 121.1(2) . . ?
C33 C32 H32 119.4 . . ?
C1 C2 H2 119.7 . . ?
C1 C2 C3 120.7(2) . . ?
C3 C2 H2 119.7 . . ?
C49 C54 H54 119.6 . . ?
C49 C54 C53 120.7(2) . . ?
C53 C54 H54 119.6 . . ?
C25 C30 H30 119.7 . . ?
C29 C30 C25 120.7(2) . . ?
C29 C30 H30 119.7 . . ?
C1 C6 H6 119.6 . . ?
C5 C6 C1 120.8(2) . . ?
C5 C6 H6 119.6 . . ?
C31 C36 H36 119.6 . . ?
C35 C36 C31 120.7(2) . . ?
C35 C36 H36 119.6 . . ?
C43 C48 H48 119.5 . . ?
C47 C48 H48 119.5 . . ?
C47 C48 C43 120.9(2) . . ?
C12 C7 P1 124.48(17) . . ?
C12 C7 C8 117.8(2) . . ?
C8 C7 P1 117.59(17) . . ?
C48 C43 P3 116.33(17) . . ?
C48 C43 C44 118.6(2) . . ?
C44 C43 P3 125.01(17) . . ?
C54 C53 H53 119.9 . . ?
C52 C53 C54 120.1(2) . . ?
C52 C53 H53 119.9 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.7(2) . . ?
C21 C20 H20 119.6 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(2) . . ?
C15 C14 H14 119.7 . . ?
C53 C52 H52 120.1 . . ?
C51 C52 C53 119.8(2) . . ?
C51 C52 H52 120.1 . . ?
C43 C44 H44 119.8 . . ?
C45 C44 C43 120.5(2) . . ?
C45 C44 H44 119.8 . . ?
C6 C5 H5 119.9 . . ?
C6 C5 C4 120.3(2) . . ?
C4 C5 H5 119.9 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.6(2) . . ?
C11 C12 H12 119.7 . . ?
C8 C9 H9 119.9 . . ?
C8 C9 C10 120.3(2) . . ?
C10 C9 H9 119.9 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(2) . . ?
C4 C3 H3 119.9 . . ?
C50 C51 H51 119.9 . . ?
C52 C51 C50 120.3(2) . . ?
C52 C51 H51 119.9 . . ?
C36 C35 H35 119.8 . . ?
C36 C35 C34 120.4(2) . . ?
C34 C35 H35 119.8 . . ?
C30 C29 H29 120.0 . . ?
C30 C29 C28 120.0(2) . . ?
C28 C29 H29 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 119.9(2) . . ?
C28 C27 H27 120.0 . . ?
C35 C34 H34 120.2 . . ?
C33 C34 C35 119.6(2) . . ?
C33 C34 H34 120.2 . . ?
C19 C24 H24 119.7 . . ?
C23 C24 C19 120.7(2) . . ?
C23 C24 H24 119.7 . . ?
C18 C17 H17 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C7 C8 H8 119.4 . . ?
C9 C8 C7 121.2(2) . . ?
C9 C8 H8 119.4 . . ?
C37 C42 H42 119.6 . . ?
C41 C42 C37 120.7(2) . . ?
C41 C42 H42 119.6 . . ?
C20 C21 H21 120.0 . . ?
C22 C21 C20 120.0(2) . . ?
C22 C21 H21 120.0 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.1(2) . . ?
C46 C45 H45 120.0 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(2) . . ?
C11 C10 H10 120.4 . . ?
C39 C40 H40 120.1 . . ?
C41 C40 H40 120.1 . . ?
C41 C40 C39 119.8(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.5(2) . . ?
C3 C4 H4 120.3 . . ?
C21 C22 H22 120.0 . . ?
C21 C22 C23 119.9(2) . . ?
C23 C22 H22 120.0 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.3(2) . . ?
C40 C39 H39 119.8 . . ?
C42 C41 H41 119.9 . . ?
C40 C41 C42 120.3(2) . . ?
C40 C41 H41 119.9 . . ?
C32 C33 H33 119.9 . . ?
C34 C33 C32 120.2(2) . . ?
C34 C33 H33 119.9 . . ?
C12 C11 H11 119.6 . . ?
C10 C11 C12 120.8(2) . . ?
C10 C11 H11 119.6 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 C29 120.0(2) . . ?
C27 C28 H28 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 C48 119.9(2) . . ?
C46 C47 H47 120.0 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(2) . . ?
C16 C15 H15 119.7 . . ?
C24 C23 H23 119.9 . . ?
C22 C23 C24 120.1(2) . . ?
C22 C23 H23 119.9 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 119.9(2) . . ?
C47 C46 H46 120.0 . . ?
C17 C16 C15 119.3(2) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C57 C57 H57A 108.8 2_676 . ?
C57 C57 H57B 108.8 2_676 . ?
H57A C57 H57B 107.7 . . ?
C56 C57 C57 113.8(3) . 2_676 ?
C56 C57 H57A 108.8 . . ?
C56 C57 H57B 108.8 . . ?
C57 C56 H56A 108.8 . . ?
C57 C56 H56B 108.8 . . ?
C57 C56 C55 113.8(2) . . ?
H56A C56 H56B 107.7 . . ?
C55 C56 H56A 108.8 . . ?
C55 C56 H56B 108.8 . . ?
C56 C55 H55A 109.5 . . ?
C56 C55 H55B 109.5 . . ?
C56 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C64 C63 H63A 111.8 . . ?
C64 C63 H63B 111.8 . . ?
C64 C63 C62 99.8(6) . . ?
C62 C63 H63A 111.8 . . ?
C62 C63 H63B 111.8 . . ?
C64 O1 C61 108.0(6) . . ?
C60 C60 H60A 108.6 2 . ?
C60 C60 H60B 108.6 2 . ?
H60A C60 H60B 107.6 . . ?
C59 C60 C60 114.5(5) . 2 ?
C59 C60 H60A 108.6 . . ?
C59 C60 H60B 108.6 . . ?
C63 C64 H64A 110.4 . . ?
C63 C64 H64B 110.4 . . ?
O1 C64 C63 106.4(6) . . ?
O1 C64 H64A 110.4 . . ?
O1 C64 H64B 110.4 . . ?
H64A C64 H64B 108.6 . . ?
O1 C61 H61A 110.2 . . ?
O1 C61 H61B 110.2 . . ?
O1 C61 C62 107.5(6) . . ?
H61A C61 H61B 108.5 . . ?
C62 C61 H61A 110.2 . . ?
C62 C61 H61B 110.2 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C59 C58 H58A 109.5 . . ?
C59 C58 H58B 109.5 . . ?
C59 C58 H58C 109.5 . . ?
C60 C59 C58 111.9(4) . . ?
C60 C59 H59A 109.2 . . ?
C60 C59 H59B 109.2 . . ?
C58 C59 H59A 109.2 . . ?
C58 C59 H59B 109.2 . . ?
H59A C59 H59B 107.9 . . ?
C63 C62 H62A 110.5 . . ?
C63 C62 H62B 110.5 . . ?
C61 C62 C63 106.0(7) . . ?
C61 C62 H62A 110.5 . . ?
C61 C62 H62B 110.5 . . ?
H62A C62 H62B 108.7 . . ?

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
Pd1 P3 C37 C38 -23.4(2) . . . . ?
Pd1 P3 C37 C42 153.85(18) . . . . ?
Pd1 P3 C49 C50 -50.29(19) . . . . ?
Pd1 P3 C49 C54 126.74(16) . . . . ?
Pd1 P3 C43 C48 -33.29(18) . . . . ?
Pd1 P3 C43 C44 149.20(16) . . . . ?
Pd1 P2 C25 C26 -21.8(2) . . . . ?
Pd1 P2 C25 C30 157.04(17) . . . . ?
Pd1 P2 C31 C32 104.27(17) . . . . ?
Pd1 P2 C31 C36 -69.88(18) . . . . ?
Pd1 P2 C19 C20 -27.2(2) . . . . ?
Pd1 P2 C19 C24 154.25(19) . . . . ?
Pd1 P1 C13 C18 -37.42(18) . . . . ?
Pd1 P1 C13 C14 140.28(19) . . . . ?
Pd1 P1 C1 C2 -18.0(2) . . . . ?
Pd1 P1 C1 C6 160.81(15) . . . . ?
Pd1 P1 C7 C12 126.93(18) . . . . ?
Pd1 P1 C7 C8 -49.4(2) . . . . ?
P3 C37 C38 C39 175.63(18) . . . . ?
P3 C37 C42 C41 -175.92(18) . . . . ?
P3 C49 C50 C51 178.25(17) . . . . ?
P3 C49 C54 C53 -178.11(16) . . . . ?
P3 C43 C44 C45 176.93(17) . . . . ?
P2 C25 C26 C27 179.76(18) . . . . ?
P2 C25 C30 C29 -179.56(18) . . . . ?
P2 C31 C32 C33 -174.78(17) . . . . ?
P2 C31 C36 C35 175.90(17) . . . . ?
P2 C19 C20 C21 -177.99(19) . . . . ?
P2 C19 C24 C23 178.6(2) . . . . ?
P1 C13 C18 C17 177.47(17) . . . . ?
P1 C13 C14 C15 -178.13(19) . . . . ?
P1 C1 C2 C3 179.09(18) . . . . ?
P1 C1 C6 C5 -179.38(18) . . . . ?
P1 C7 C12 C11 -177.23(19) . . . . ?
P1 C7 C8 C9 177.73(19) . . . . ?
C25 P2 C31 C32 -131.46(18) . . . . ?
C25 P2 C31 C36 54.39(19) . . . . ?
C25 P2 C19 C20 -151.80(19) . . . . ?
C25 P2 C19 C24 29.6(2) . . . . ?
C25 C26 C27 C28 -0.3(4) . . . . ?
C25 C30 C29 C28 0.0(4) . . . . ?
C37 P3 C49 C50 72.93(18) . . . . ?
C37 P3 C49 C54 -110.05(19) . . . . ?
C37 P3 C43 C48 -155.26(16) . . . . ?
C37 P3 C43 C44 27.2(2) . . . . ?
C37 C38 C39 C40 0.7(4) . . . . ?
C37 C42 C41 C40 0.2(4) . . . . ?
C49 P3 C37 C38 -153.84(18) . . . . ?
C49 P3 C37 C42 23.4(2) . . . . ?
C49 P3 C43 C48 100.40(17) . . . . ?
C49 P3 C43 C44 -77.1(2) . . . . ?
C49 C50 C51 C52 -0.5(3) . . . . ?
C49 C54 C53 C52 0.6(3) . . . . ?
C26 C25 C30 C29 -0.8(3) . . . . ?
C26 C27 C28 C29 -0.5(4) . . . . ?
C31 P2 C25 C26 -150.43(18) . . . . ?
C31 P2 C25 C30 28.4(2) . . . . ?
C31 P2 C19 C20 103.80(19) . . . . ?
C31 P2 C19 C24 -74.8(2) . . . . ?
C31 C32 C33 C34 -0.6(3) . . . . ?
C31 C36 C35 C34 -1.4(3) . . . . ?
C19 P2 C25 C26 105.61(18) . . . . ?
C19 P2 C25 C30 -75.6(2) . . . . ?
C19 P2 C31 C32 -25.2(2) . . . . ?
C19 P2 C31 C36 160.62(17) . . . . ?
C19 C20 C21 C22 -0.8(4) . . . . ?
C19 C24 C23 C22 -0.7(4) . . . . ?
C13 P1 C1 C2 -136.04(18) . . . . ?
C13 P1 C1 C6 42.8(2) . . . . ?
C13 P1 C7 C12 -116.5(2) . . . . ?
C13 P1 C7 C8 67.23(19) . . . . ?
C13 C18 C17 C16 0.9(4) . . . . ?
C13 C14 C15 C16 0.8(4) . . . . ?
C1 P1 C13 C18 92.35(18) . . . . ?
C1 P1 C13 C14 -90.0(2) . . . . ?
C1 P1 C7 C12 -12.3(2) . . . . ?
C1 P1 C7 C8 171.39(18) . . . . ?
C1 C2 C3 C4 0.1(4) . . . . ?
C1 C6 C5 C4 0.5(4) . . . . ?
C38 C37 C42 C41 1.3(3) . . . . ?
C50 C49 C54 C53 -1.1(3) . . . . ?
C18 C13 C14 C15 -0.5(4) . . . . ?
C18 C17 C16 C15 -0.6(4) . . . . ?
C32 C31 C36 C35 1.5(3) . . . . ?
C2 C1 C6 C5 -0.6(3) . . . . ?
C2 C3 C4 C5 -0.2(4) . . . . ?
C54 C49 C50 C51 1.1(3) . . . . ?
C54 C53 C52 C51 0.0(3) . . . . ?
C30 C25 C26 C27 0.9(3) . . . . ?
C30 C29 C28 C27 0.6(4) . . . . ?
C6 C1 C2 C3 0.3(3) . . . . ?
C6 C5 C4 C3 -0.1(4) . . . . ?
C36 C31 C32 C33 -0.5(3) . . . . ?
C36 C35 C34 C33 0.2(3) . . . . ?
C48 C43 C44 C45 -0.5(3) . . . . ?
C48 C47 C46 C45 -0.3(3) . . . . ?
C7 P1 C13 C18 -163.29(17) . . . . ?
C7 P1 C13 C14 14.4(2) . . . . ?
C7 P1 C1 C2 119.25(18) . . . . ?
C7 P1 C1 C6 -61.9(2) . . . . ?
C7 C12 C11 C10 0.1(4) . . . . ?
C43 P3 C37 C38 102.12(19) . . . . ?
C43 P3 C37 C42 -80.7(2) . . . . ?
C43 P3 C49 C50 179.48(17) . . . . ?
C43 P3 C49 C54 -3.5(2) . . . . ?
C43 C48 C47 C46 -1.1(3) . . . . ?
C43 C44 C45 C46 -0.9(3) . . . . ?
C53 C52 C51 C50 0.0(3) . . . . ?
C20 C19 C24 C23 0.1(4) . . . . ?
C20 C21 C22 C23 0.3(4) . . . . ?
C14 C13 C18 C17 -0.4(3) . . . . ?
C14 C15 C16 C17 -0.3(4) . . . . ?
C44 C45 C46 C47 1.3(3) . . . . ?
C12 C7 C8 C9 1.2(4) . . . . ?
C9 C10 C11 C12 0.5(4) . . . . ?
C35 C34 C33 C32 0.8(3) . . . . ?
C24 C19 C20 C21 0.7(4) . . . . ?
C8 C7 C12 C11 -1.0(4) . . . . ?
C8 C9 C10 C11 -0.3(4) . . . . ?
C42 C37 C38 C39 -1.7(3) . . . . ?
C21 C22 C23 C24 0.5(4) . . . . ?
C10 C9 C8 C7 -0.6(4) . . . . ?
C39 C40 C41 C42 -1.2(4) . . . . ?
C41 C40 C39 C38 0.8(4) . . . . ?
C47 C48 C43 P3 -176.12(17) . . . . ?
C47 C48 C43 C44 1.6(3) . . . . ?
C57 C57 C56 C55 -177.1(3) 2_676 . . . ?
O1 C61 C62 C63 -8.7(11) . . . . ?
C60 C60 C59 C58 177.8(6) 2 . . . ?
C64 C63 C62 C61 25.8(11) . . . . ?
C64 O1 C61 C62 -14.1(9) . . . . ?
C61 O1 C64 C63 31.7(9) . . . . ?
C62 C63 C64 O1 -35.0(10) . . . . ?

_olex2_date_sample_data_collection 2018-10-19
_olex2_date_sample_submission    2018-10-19
_olex2_exptl_crystal_mounting_method 'oil on micrount 200 micrometres'
_olex2_submission_original_sample_id 'Neil Scott NWJS-4-293-crystals1'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.153
_oxdiff_exptl_absorpt_empirical_full_min 0.904
####################################################################### 
# 
# 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_ijsf1905
_database_code_depnum_ccdc_archive 'CCDC 1901195'
loop_
_audit_author_name
_audit_author_address
'Rachel R Parker'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-03-05 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2019-03-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C78 H65 Br2 P5 Pd3, C4 H8 O'
_chemical_formula_sum            'C82 H73 Br2 O P5 Pd3'
_chemical_formula_weight         1708.27
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C78 H65 Br2 P5 Pd3'
_chemical_oxdiff_usercomment     'Neil Scott NWJS-4-325-crystals2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.3726(5)
_cell_length_b                   23.1564(6)
_cell_length_c                   18.9888(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.645(2)
_cell_angle_gamma                90
_cell_volume                     7164.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7691
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      71.0000
_cell_measurement_theta_min      4.2030
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    8.728
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.292
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3424
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 -1 0.0864
5 -1 4 0.0570
1 0 0 0.0227
3 -5 0 0.0370
5 3 1 0.0323
-1 0 0 0.0131
0 0 1 0.1160
-1 5 3 0.0881
-1 5 0 0.0534
5 4 -4 0.0571
5 -2 -1 0.0318

_exptl_crystal_size_max          0.277
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.036
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.0002 1.0011 -0.9999 -0.0393 -0.0924 0.0313
5.0053 -1.0005 4.0005 -0.3228 0.5101 -0.0092
1.0010 0.0005 0.0002 -0.0848 0.0396 -0.0134
3.0008 -5.0009 0.0009 -0.1612 0.2150 -0.3445
5.0064 3.0032 1.0007 -0.4594 0.2136 0.1455
-1.0010 -0.0005 -0.0002 0.0848 -0.0396 0.0134
0.0002 -0.0006 0.9999 0.0207 0.0732 0.0296
-0.9983 4.9999 2.9991 0.0536 0.0838 0.4067
-0.9989 5.0018 -0.0005 -0.0084 -0.1358 0.3178
5.0058 4.0067 -3.9986 -0.5813 -0.1716 0.0583
5.0039 -1.9979 -0.9987 -0.4074 0.1634 -0.2182

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24240
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.902
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     19.00  66.00   1.00    8.00    --    0.00  57.00   0.00   47
  2  ω     31.00  59.00   1.00    8.00    --    0.00  57.00 -60.00   28
  3  ω    -21.00  30.00   1.00    8.00    --    0.00  57.00 -60.00   51
  4  ω    -12.00  74.00   1.00   31.50    --   54.00 -57.00 -30.00   86
  5  ω    -14.00  67.00   1.00   31.50    --   54.00 -57.00  60.00   81
  6  ω    -17.00  59.00   1.00   31.50    --   54.00 -37.00 120.00   76
  7  ω     50.00 106.00   1.00   31.50    --   54.00-125.00-180.00   56
  8  ω     96.00 121.00   1.00   31.50    --   54.00  37.00 -60.00   25
  9  ω    136.00 163.00   1.00   31.50    --  108.00  63.00  60.00   27
 10  ω     87.00 169.00   1.00   31.50    --  108.00  50.00 150.00   82
 11  ω     39.00 177.00   1.00   31.50    --  108.00  12.00 120.00  138
 12  ω     67.00 112.00   1.00   31.50    --  108.00-111.00 -30.00   45
 13  ω     62.00 146.00   1.00   31.50    --  108.00 -91.00  30.00   84
 14  ω     47.00 101.00   1.00   31.50    --  108.00-111.00 -90.00   54
 15  ω     40.00 100.00   1.00   31.50    --  108.00 -77.00 -60.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0847294000
_diffrn_orient_matrix_UB_12      -0.0186032000
_diffrn_orient_matrix_UB_13      0.0206698000
_diffrn_orient_matrix_UB_21      0.0395791000
_diffrn_orient_matrix_UB_22      -0.0192332000
_diffrn_orient_matrix_UB_23      0.0731888000
_diffrn_orient_matrix_UB_31      -0.0133876000
_diffrn_orient_matrix_UB_32      0.0608685000
_diffrn_orient_matrix_UB_33      0.0296648000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10201
_reflns_number_total             12724
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.882
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         12724
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0704
_refine_ls_restrained_S_all      1.201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+148.0454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1630
_refine_ls_wR_factor_ref         0.1714
_refine_special_details          
;
Disordered thf modelled in 2 positions; rotated upon itself. Bond lengths and angles restrained. disordered C and O constrained to have same ADPs.
DFIX 1.5 C82A C79
DFIX 1.42 O1A C82A
DFIX 1.42 O1A C81
DFIX 1.5 C82B C81
DFIX 1.5 C81 C80
DFIX 1.5 C80 C79
DFIX 1.42 C82B O1B
DFIX 1.42 O1B C79
SADI 0.01 O1B C79 O1B C82B O1A C82A O1A C81
DANG 2.36 C82A C80
DANG 2.34 C79 O1A
DANG 2.34 O1A C80
DANG 2.32 C82A C81
DANG 2.36 C81 C79
DANG 2.36 C82B C80
DANG 2.34 C81 O1B
DANG 2.34 O1B C80
DANG 2.32 C82B C79
EADP O1A C82B
EADP O1B C82A

Poor R value due to poos quality/grubby diffraction data.

Large Q-peaks around PD centres parallel to face- due to positional slippage in the crystal- reflected in poor quality diffraction spots.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C82A-C79
 1.5 with sigma of 0.02
 O1A-C82A
 1.42 with sigma of 0.02
 O1A-C81
 1.42 with sigma of 0.02
 C82B-C81
 1.5 with sigma of 0.02
 C81-C80
 1.5 with sigma of 0.02
 C80-C79
 1.5 with sigma of 0.02
 C82B-O1B
 1.42 with sigma of 0.02
 O1B-C79
 1.42 with sigma of 0.02
 C82A-C80
 2.36 with sigma of 0.04
 C79-O1A
 2.34 with sigma of 0.04
 O1A-C80
 2.34 with sigma of 0.04
 C82A-C81
 2.32 with sigma of 0.04
 C81-C79
 2.36 with sigma of 0.04
 C82B-C80
 2.36 with sigma of 0.04
 C81-O1B
 2.34 with sigma of 0.04
 O1B-C80
 2.34 with sigma of 0.04
 C82B-C79
 2.32 with sigma of 0.04
 O1B-C79 \\sim O1B-C82B \\sim O1A-C82A \\sim O1A-C81
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1A) = Uanis(C82B)
Uanis(O1B) = Uanis(C82A)
4. Others
 Sof(H79C)=Sof(H79D)=Sof(H81C)=Sof(H81D)=Sof(O1A)=Sof(C82A)=Sof(H82C)=
 Sof(H82D)=1-FVAR(1)
 Sof(C82B)=Sof(H82A)=Sof(H82B)=Sof(H79A)=Sof(H79B)=Sof(O1B)=Sof(H81A)=
 Sof(H81B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C82B(H82A,H82B), C79(H79A,H79B), C79(H79C,H79D), C80(H80A,H80B), C81(H81A,
 H81B), C81(H81C,H81D), C82A(H82C,H82D)
5.b Aromatic/amide H refined with riding coordinates:
 C74(H74), C56(H56), C58(H58), C6(H6), C78(H78), C8(H8), C75(H75), C57(H57),
 C24(H24), C26(H26), C12(H12), C60(H60), C76(H76), C59(H59), C68(H68), C42(H42),
  C2(H2), C14(H14), C38(H38), C20(H20), C54(H54), C5(H5), C62(H62), C66(H66),
 C21(H21), C30(H30), C11(H11), C9(H9), C3(H3), C77(H77), C27(H27), C44(H44),
 C4(H4), C23(H23), C71(H71), C40(H40), C36(H36), C22(H22), C33(H33), C17(H17),
 C41(H41), C10(H10), C15(H15), C28(H28), C18(H18), C65(H65), C72(H72), C63(H63),
  C48(H48), C32(H32), C70(H70), C29(H29), C39(H39), C64(H64), C45(H45),
 C53(H53), C46(H46), C51(H51), C69(H69), C34(H34), C50(H50), C16(H16), C35(H35),
  C52(H52), C47(H47)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.80046(5) 0.54791(3) 0.31536(3) 0.02028(17) Uani 1 1 d . . . . .
Pd2 Pd 0.76698(5) 0.42873(3) 0.29378(4) 0.02169(17) Uani 1 1 d . . . . .
Pd3 Pd 0.75810(5) 0.50281(3) 0.17513(4) 0.02196(17) Uani 1 1 d . . . . .
Br1 Br 0.64512(7) 0.42672(5) 0.16912(5) 0.0302(3) Uani 1 1 d . . . . .
Br2 Br 0.89055(7) 0.39732(5) 0.22939(6) 0.0307(3) Uani 1 1 d . . . . .
P2 P 0.72745(15) 0.48617(10) 0.37698(12) 0.0205(5) Uani 1 1 d . . . . .
P5 P 0.84125(16) 0.57484(11) 0.20899(12) 0.0208(5) Uani 1 1 d . . . . .
P3 P 0.73177(16) 0.33877(11) 0.33218(13) 0.0223(5) Uani 1 1 d . . . . .
P1 P 0.82231(16) 0.62828(10) 0.38574(12) 0.0207(5) Uani 1 1 d . . . . .
P4 P 0.73943(16) 0.51970(11) 0.05641(13) 0.0227(5) Uani 1 1 d . . . . .
C74 C 0.9966(6) 0.5299(4) 0.2391(5) 0.023(2) Uani 1 1 d . . . . .
H74 H 0.9730 0.5105 0.2750 0.027 Uiso 1 1 calc R . . . .
C55 C 0.8149(6) 0.5609(4) 0.0119(5) 0.023(2) Uani 1 1 d . . . . .
C56 C 0.8802(6) 0.5316(4) -0.0144(5) 0.024(2) Uani 1 1 d . . . . .
H56 H 0.8835 0.4917 -0.0103 0.028 Uiso 1 1 calc R . . . .
C19 C 0.7667(6) 0.4652(4) 0.4663(5) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.7292(6) 0.6715(4) 0.3868(5) 0.025(2) Uani 1 1 d . . . . .
C73 C 0.9486(6) 0.5668(4) 0.1939(5) 0.026(2) Uani 1 1 d . . . . .
C58 C 0.9364(7) 0.6211(5) -0.0508(5) 0.031(2) Uani 1 1 d . . . . .
H58 H 0.9770 0.6414 -0.0711 0.037 Uiso 1 1 calc R . . . .
C6 C 0.7977(7) 0.6034(4) 0.5261(5) 0.027(2) Uani 1 1 d . . . . .
H6 H 0.7428 0.5993 0.5089 0.032 Uiso 1 1 calc R . . . .
C78 C 0.9843(7) 0.5923(4) 0.1372(5) 0.027(2) Uani 1 1 d . . . . .
H78 H 0.9525 0.6149 0.1046 0.032 Uiso 1 1 calc R . . . .
C8 C 0.9720(7) 0.6551(4) 0.3380(5) 0.027(2) Uani 1 1 d . . . . .
H8 H 0.9821 0.6158 0.3432 0.032 Uiso 1 1 calc R . . . .
C61 C 0.6416(7) 0.5555(4) 0.0289(5) 0.026(2) Uani 1 1 d . . . . .
C75 C 1.0780(7) 0.5220(5) 0.2311(5) 0.029(2) Uani 1 1 d . . . . .
H75 H 1.1094 0.4982 0.2626 0.035 Uiso 1 1 calc R . . . .
C7 C 0.8979(6) 0.6781(4) 0.3558(5) 0.022(2) Uani 1 1 d . . . . .
C57 C 0.9404(6) 0.5616(5) -0.0466(5) 0.028(2) Uani 1 1 d . . . . .
H57 H 0.9828 0.5418 -0.0650 0.034 Uiso 1 1 calc R . . . .
C24 C 0.7204(7) 0.4414(5) 0.5167(5) 0.030(2) Uani 1 1 d . . . . .
H24 H 0.6643 0.4359 0.5063 0.036 Uiso 1 1 calc R . . . .
C26 C 0.5892(7) 0.5321(4) 0.4393(6) 0.031(2) Uani 1 1 d . . . . .
H26 H 0.6197 0.5312 0.4832 0.037 Uiso 1 1 calc R . . . .
C1 C 0.8547(6) 0.6186(4) 0.4804(5) 0.023(2) Uani 1 1 d . . . . .
C12 C 0.8837(7) 0.7370(4) 0.3458(5) 0.027(2) Uani 1 1 d . . . . .
H12 H 0.8344 0.7529 0.3569 0.032 Uiso 1 1 calc R . . . .
C60 C 0.8115(7) 0.6206(4) 0.0059(5) 0.024(2) Uani 1 1 d . . . . .
H60 H 0.7683 0.6408 0.0227 0.029 Uiso 1 1 calc R . . . .
C76 C 1.1145(7) 0.5488(5) 0.1769(5) 0.030(2) Uani 1 1 d . . . . .
H76 H 1.1700 0.5436 0.1721 0.037 Uiso 1 1 calc R . . . .
C59 C 0.8725(7) 0.6504(4) -0.0250(5) 0.027(2) Uani 1 1 d . . . . .
H59 H 0.8702 0.6905 -0.0283 0.032 Uiso 1 1 calc R . . . .
C68 C 0.8597(7) 0.6928(4) 0.1708(5) 0.025(2) Uani 1 1 d . . . . .
H68 H 0.9158 0.6882 0.1828 0.030 Uiso 1 1 calc R . . . .
C31 C 0.8135(7) 0.3029(4) 0.3872(5) 0.026(2) Uani 1 1 d . . . . .
C42 C 0.5743(6) 0.3690(4) 0.3604(5) 0.028(2) Uani 1 1 d . . . . .
H42 H 0.5781 0.3950 0.3235 0.033 Uiso 1 1 calc R . . . .
C2 C 0.9373(7) 0.6232(4) 0.5066(5) 0.029(2) Uani 1 1 d . . . . .
H2 H 0.9765 0.6327 0.4763 0.035 Uiso 1 1 calc R . . . .
C14 C 0.7196(7) 0.7138(4) 0.4378(5) 0.028(2) Uani 1 1 d . . . . .
H14 H 0.7612 0.7200 0.4740 0.034 Uiso 1 1 calc R . . . .
C38 C 0.6336(7) 0.2954(4) 0.4376(5) 0.028(2) Uani 1 1 d . . . . .
H38 H 0.6776 0.2718 0.4534 0.033 Uiso 1 1 calc R . . . .
C20 C 0.8513(7) 0.4708(4) 0.4834(5) 0.029(2) Uani 1 1 d . . . . .
H20 H 0.8832 0.4854 0.4496 0.035 Uiso 1 1 calc R . . . .
C54 C 0.7023(7) 0.4456(5) -0.0605(6) 0.036(3) Uani 1 1 d . . . . .
H54 H 0.6739 0.4766 -0.0822 0.043 Uiso 1 1 calc R . . . .
C5 C 0.8214(8) 0.5942(5) 0.5976(5) 0.033(3) Uani 1 1 d . . . . .
H5 H 0.7823 0.5849 0.6280 0.040 Uiso 1 1 calc R . . . .
C62 C 0.5814(7) 0.5572(5) 0.0758(5) 0.031(2) Uani 1 1 d . . . . .
H62 H 0.5926 0.5411 0.1206 0.037 Uiso 1 1 calc R . . . .
C66 C 0.6236(7) 0.5806(5) -0.0373(5) 0.034(3) Uani 1 1 d . . . . .
H66 H 0.6633 0.5813 -0.0691 0.041 Uiso 1 1 calc R . . . .
C21 C 0.8887(7) 0.4554(5) 0.5484(6) 0.034(3) Uani 1 1 d . . . . .
H21 H 0.9449 0.4605 0.5588 0.040 Uiso 1 1 calc R . . . .
C30 C 0.5752(7) 0.5148(5) 0.3134(6) 0.033(3) Uani 1 1 d . . . . .
H30 H 0.5974 0.5024 0.2728 0.040 Uiso 1 1 calc R . . . .
C11 C 0.9421(8) 0.7722(4) 0.3196(5) 0.033(3) Uani 1 1 d . . . . .
H11 H 0.9315 0.8114 0.3126 0.039 Uiso 1 1 calc R . . . .
C9 C 1.0313(7) 0.6911(5) 0.3124(5) 0.029(2) Uani 1 1 d . . . . .
H9 H 1.0809 0.6756 0.3013 0.035 Uiso 1 1 calc R . . . .
C3 C 0.9609(7) 0.6135(5) 0.5781(5) 0.032(2) Uani 1 1 d . . . . .
H3 H 1.0158 0.6167 0.5955 0.038 Uiso 1 1 calc R . . . .
C67 C 0.8068(7) 0.6463(4) 0.1763(5) 0.029(2) Uani 1 1 d . . . . .
C77 C 1.0664(6) 0.5839(4) 0.1296(5) 0.027(2) Uani 1 1 d . . . . .
H77 H 1.0899 0.6017 0.0927 0.033 Uiso 1 1 calc R . . . .
C27 C 0.5107(8) 0.5549(5) 0.4323(7) 0.040(3) Uani 1 1 d . . . . .
H27 H 0.4885 0.5689 0.4722 0.048 Uiso 1 1 calc R . . . .
C44 C 0.6544(7) 0.2380(4) 0.2752(6) 0.031(2) Uani 1 1 d . . . . .
H44 H 0.6360 0.2332 0.3196 0.038 Uiso 1 1 calc R . . . .
C4 C 0.9028(8) 0.5990(4) 0.6234(5) 0.033(3) Uani 1 1 d . . . . .
H4 H 0.9187 0.5924 0.6711 0.040 Uiso 1 1 calc R . . . .
C23 C 0.7586(8) 0.4258(5) 0.5832(5) 0.034(3) Uani 1 1 d . . . . .
H23 H 0.7272 0.4109 0.6172 0.041 Uiso 1 1 calc R . . . .
C49 C 0.7386(7) 0.4507(4) 0.0081(5) 0.029(2) Uani 1 1 d . . . . .
C71 C 0.6916(8) 0.7071(5) 0.1379(6) 0.037(3) Uani 1 1 d . . . . .
H71 H 0.6353 0.7119 0.1279 0.044 Uiso 1 1 calc R . . . .
C40 C 0.4968(7) 0.3266(5) 0.4470(6) 0.036(3) Uani 1 1 d . . . . .
H40 H 0.4486 0.3241 0.4690 0.043 Uiso 1 1 calc R . . . .
C36 C 0.8681(6) 0.2658(5) 0.3567(6) 0.032(2) Uani 1 1 d . . . . .
H36 H 0.8606 0.2580 0.3085 0.038 Uiso 1 1 calc R . . . .
C25 C 0.6220(7) 0.5104(4) 0.3795(5) 0.030(2) Uani 1 1 d . . . . .
C22 C 0.8420(8) 0.4322(5) 0.5988(5) 0.034(3) Uani 1 1 d . . . . .
H22 H 0.8670 0.4210 0.6428 0.041 Uiso 1 1 calc R . . . .
C43 C 0.7031(6) 0.2851(4) 0.2620(5) 0.027(2) Uani 1 1 d . . . . .
C33 C 0.8931(7) 0.2897(5) 0.4993(6) 0.037(3) Uani 1 1 d . . . . .
H33 H 0.9011 0.2972 0.5477 0.044 Uiso 1 1 calc R . . . .
C17 C 0.5945(7) 0.6954(5) 0.3305(6) 0.038(3) Uani 1 1 d . . . . .
H17 H 0.5525 0.6891 0.2947 0.046 Uiso 1 1 calc R . . . .
C41 C 0.5024(7) 0.3659(5) 0.3919(6) 0.037(3) Uani 1 1 d . . . . .
H41 H 0.4582 0.3896 0.3768 0.044 Uiso 1 1 calc R . . . .
C10 C 1.0163(7) 0.7492(5) 0.3038(5) 0.033(3) Uani 1 1 d . . . . .
H10 H 1.0560 0.7731 0.2872 0.039 Uiso 1 1 calc R . . . .
C15 C 0.6490(8) 0.7465(5) 0.4349(6) 0.035(3) Uani 1 1 d . . . . .
H15 H 0.6433 0.7746 0.4691 0.042 Uiso 1 1 calc R . . . .
C28 C 0.4650(8) 0.5571(5) 0.3680(7) 0.043(3) Uani 1 1 d . . . . .
H28 H 0.4120 0.5720 0.3646 0.051 Uiso 1 1 calc R . . . .
C18 C 0.6660(7) 0.6625(5) 0.3337(5) 0.032(2) Uani 1 1 d . . . . .
H18 H 0.6714 0.6342 0.2998 0.039 Uiso 1 1 calc R . . . .
C37 C 0.6411(6) 0.3345(4) 0.3820(5) 0.025(2) Uani 1 1 d . . . . .
C65 C 0.5478(7) 0.6045(5) -0.0563(6) 0.037(3) Uani 1 1 d . . . . .
H65 H 0.5362 0.6200 -0.1014 0.044 Uiso 1 1 calc R . . . .
C72 C 0.7242(7) 0.6538(4) 0.1605(5) 0.028(2) Uani 1 1 d . . . . .
H72 H 0.6890 0.6228 0.1650 0.034 Uiso 1 1 calc R . . . .
C63 C 0.5061(7) 0.5820(6) 0.0578(6) 0.042(3) Uani 1 1 d . . . . .
H63 H 0.4671 0.5828 0.0902 0.050 Uiso 1 1 calc R . . . .
C48 C 0.7303(8) 0.2915(5) 0.1949(5) 0.040(3) Uani 1 1 d . . . . .
H48 H 0.7631 0.3229 0.1856 0.048 Uiso 1 1 calc R . . . .
C32 C 0.8288(7) 0.3157(5) 0.4592(5) 0.031(2) Uani 1 1 d . . . . .
H32 H 0.7954 0.3418 0.4801 0.038 Uiso 1 1 calc R . . . .
C70 C 0.7457(8) 0.7532(5) 0.1306(5) 0.037(3) Uani 1 1 d . . . . .
H70 H 0.7253 0.7888 0.1143 0.044 Uiso 1 1 calc R . . . .
C29 C 0.4976(7) 0.5372(6) 0.3083(6) 0.042(3) Uani 1 1 d . . . . .
H29 H 0.4668 0.5391 0.2646 0.051 Uiso 1 1 calc R . . . .
C39 C 0.5616(7) 0.2918(5) 0.4687(5) 0.033(3) Uani 1 1 d . . . . .
H39 H 0.5569 0.2654 0.5049 0.040 Uiso 1 1 calc R . . . .
C64 C 0.4887(8) 0.6059(5) -0.0091(6) 0.041(3) Uani 1 1 d . . . . .
H64 H 0.4378 0.6226 -0.0220 0.049 Uiso 1 1 calc R . . . .
C45 C 0.6332(8) 0.1981(5) 0.2221(6) 0.036(3) Uani 1 1 d . . . . .
H45 H 0.6014 0.1663 0.2313 0.044 Uiso 1 1 calc R . . . .
C53 C 0.7085(8) 0.3939(6) -0.0969(7) 0.044(3) Uani 1 1 d . . . . .
H53 H 0.6832 0.3901 -0.1427 0.052 Uiso 1 1 calc R . . . .
C46 C 0.6593(8) 0.2056(5) 0.1552(6) 0.038(3) Uani 1 1 d . . . . .
H46 H 0.6434 0.1795 0.1193 0.046 Uiso 1 1 calc R . . . .
C51 C 0.7883(8) 0.3538(5) 0.0028(7) 0.046(3) Uani 1 1 d . . . . .
H51 H 0.8175 0.3230 0.0241 0.055 Uiso 1 1 calc R . . . .
C69 C 0.8288(8) 0.7460(5) 0.1475(6) 0.038(3) Uani 1 1 d . . . . .
H69 H 0.8643 0.7769 0.1433 0.046 Uiso 1 1 calc R . . . .
C34 C 0.9454(8) 0.2533(5) 0.4695(8) 0.046(3) Uani 1 1 d . . . . .
H34 H 0.9893 0.2368 0.4971 0.055 Uiso 1 1 calc R . . . .
C82B C 0.368(2) 0.4266(10) 0.239(3) 0.054(4) Uani 0.244(15) 1 d D . P A 2
H82A H 0.3769 0.4437 0.2861 0.065 Uiso 0.244(15) 1 calc R . P A 2
H82B H 0.4162 0.4341 0.2146 0.065 Uiso 0.244(15) 1 calc R . P A 2
C50 C 0.7817(8) 0.4050(5) 0.0396(6) 0.038(3) Uani 1 1 d . . . . .
H50 H 0.8063 0.4084 0.0857 0.045 Uiso 1 1 calc R . . . .
C79 C 0.2310(8) 0.4101(5) 0.1993(6) 0.052(4) Uani 1 1 d D . . . .
H79A H 0.2211 0.4237 0.1509 0.063 Uiso 0.244(15) 1 calc R . P A 1
H79B H 0.1790 0.4076 0.2196 0.063 Uiso 0.244(15) 1 calc R . P A 1
H79C H 0.1947 0.4142 0.1561 0.063 Uiso 0.756(15) 1 calc R . P A 2
H79D H 0.1996 0.4152 0.2396 0.063 Uiso 0.756(15) 1 calc R . P A 2
C16 C 0.5865(8) 0.7378(5) 0.3815(6) 0.038(3) Uani 1 1 d . . . . .
H16 H 0.5391 0.7601 0.3796 0.046 Uiso 1 1 calc R . . . .
C35 C 0.9329(7) 0.2411(5) 0.3980(7) 0.044(3) Uani 1 1 d . . . . .
H35 H 0.9683 0.2161 0.3776 0.053 Uiso 1 1 calc R . . . .
C52 C 0.7517(9) 0.3485(5) -0.0656(8) 0.054(4) Uani 1 1 d . . . . .
H52 H 0.7563 0.3141 -0.0903 0.064 Uiso 1 1 calc R . . . .
C80 C 0.2739(7) 0.3521(5) 0.2021(6) 0.048(3) Uani 1 1 d D . . . .
H80A H 0.2421 0.3234 0.2247 0.057 Uiso 1 1 calc R . . . .
H80B H 0.2824 0.3389 0.1549 0.057 Uiso 1 1 calc R . . . .
C47 C 0.7085(10) 0.2514(5) 0.1422(6) 0.053(4) Uani 1 1 d . . . . .
H47 H 0.7273 0.2557 0.0978 0.063 Uiso 1 1 calc R . . . .
O1B O 0.2970(13) 0.4501(9) 0.2013(19) 0.053(5) Uani 0.244(15) 1 d D . P A 2
C81 C 0.3545(7) 0.3629(5) 0.2450(7) 0.049(3) Uani 1 1 d D . . . .
H81A H 0.3697 0.3301 0.2753 0.059 Uiso 0.244(15) 1 calc R . P A 1
H81B H 0.3975 0.3696 0.2143 0.059 Uiso 0.244(15) 1 calc R . P A 1
H81C H 0.3518 0.3516 0.2939 0.059 Uiso 0.756(15) 1 calc R . P A 2
H81D H 0.3982 0.3415 0.2259 0.059 Uiso 0.756(15) 1 calc R . P A 2
O1A O 0.3415(7) 0.4129(5) 0.2861(6) 0.054(4) Uani 0.756(15) 1 d D . P A 1
C82A C 0.2889(11) 0.4495(6) 0.2421(9) 0.053(5) Uani 0.756(15) 1 d D . P A 1
H82C H 0.3202 0.4724 0.2115 0.063 Uiso 0.756(15) 1 calc R . P A 1
H82D H 0.2590 0.4754 0.2705 0.063 Uiso 0.756(15) 1 calc R . P A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Pd2 2.8355(10) . ?
Pd1 Pd3 2.8808(10) . ?
Pd1 P2 2.262(2) . ?
Pd1 P5 2.276(2) . ?
Pd1 P1 2.299(2) . ?
Pd2 Pd3 2.8240(10) . ?
Pd2 Br1 2.9423(13) . ?
Pd2 Br2 2.5698(13) . ?
Pd2 P2 2.210(2) . ?
Pd2 P3 2.299(3) . ?
Pd3 Br1 2.5490(13) . ?
Pd3 P5 2.208(3) . ?
Pd3 P4 2.279(3) . ?
P2 C19 1.819(9) . ?
P2 C25 1.820(11) . ?
P5 C73 1.817(11) . ?
P5 C67 1.836(10) . ?
P3 C31 1.816(11) . ?
P3 C43 1.848(10) . ?
P3 C37 1.839(10) . ?
P1 C13 1.826(10) . ?
P1 C7 1.823(10) . ?
P1 C1 1.836(10) . ?
P4 C55 1.832(10) . ?
P4 C61 1.833(11) . ?
P4 C49 1.841(10) . ?
C74 H74 0.9300 . ?
C74 C73 1.398(14) . ?
C74 C75 1.368(14) . ?
C55 C56 1.398(14) . ?
C55 C60 1.389(14) . ?
C56 H56 0.9300 . ?
C56 C57 1.395(14) . ?
C19 C24 1.392(13) . ?
C19 C20 1.397(15) . ?
C13 C14 1.397(14) . ?
C13 C18 1.388(15) . ?
C73 C78 1.405(13) . ?
C58 H58 0.9300 . ?
C58 C57 1.379(15) . ?
C58 C59 1.377(15) . ?
C6 H6 0.9300 . ?
C6 C1 1.381(13) . ?
C6 C5 1.391(14) . ?
C78 H78 0.9300 . ?
C78 C77 1.378(15) . ?
C8 H8 0.9300 . ?
C8 C7 1.397(14) . ?
C8 C9 1.401(14) . ?
C61 C62 1.392(14) . ?
C61 C66 1.390(14) . ?
C75 H75 0.9300 . ?
C75 C76 1.389(14) . ?
C7 C12 1.392(14) . ?
C57 H57 0.9300 . ?
C24 H24 0.9300 . ?
C24 C23 1.400(14) . ?
C26 H26 0.9300 . ?
C26 C27 1.384(16) . ?
C26 C25 1.396(14) . ?
C1 C2 1.400(15) . ?
C12 H12 0.9300 . ?
C12 C11 1.386(14) . ?
C60 H60 0.9300 . ?
C60 C59 1.391(14) . ?
C76 H76 0.9300 . ?
C76 C77 1.394(15) . ?
C59 H59 0.9300 . ?
C68 H68 0.9300 . ?
C68 C67 1.392(14) . ?
C68 C69 1.389(15) . ?
C31 C36 1.404(14) . ?
C31 C32 1.397(14) . ?
C42 H42 0.9300 . ?
C42 C41 1.373(15) . ?
C42 C37 1.385(15) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(14) . ?
C14 H14 0.9300 . ?
C14 C15 1.379(15) . ?
C38 H38 0.9300 . ?
C38 C37 1.405(14) . ?
C38 C39 1.372(15) . ?
C20 H20 0.9300 . ?
C20 C21 1.372(15) . ?
C54 H54 0.9300 . ?
C54 C49 1.382(15) . ?
C54 C53 1.391(16) . ?
C5 H5 0.9300 . ?
C5 C4 1.378(16) . ?
C62 H62 0.9300 . ?
C62 C63 1.373(16) . ?
C66 H66 0.9300 . ?
C66 C65 1.374(16) . ?
C21 H21 0.9300 . ?
C21 C22 1.389(15) . ?
C30 H30 0.9300 . ?
C30 C25 1.408(15) . ?
C30 C29 1.367(16) . ?
C11 H11 0.9300 . ?
C11 C10 1.388(16) . ?
C9 H9 0.9300 . ?
C9 C10 1.375(15) . ?
C3 H3 0.9300 . ?
C3 C4 1.384(15) . ?
C67 C72 1.367(16) . ?
C77 H77 0.9300 . ?
C27 H27 0.9300 . ?
C27 C28 1.369(17) . ?
C44 H44 0.9300 . ?
C44 C43 1.390(14) . ?
C44 C45 1.384(15) . ?
C4 H4 0.9300 . ?
C23 H23 0.9300 . ?
C23 C22 1.377(16) . ?
C49 C50 1.377(16) . ?
C71 H71 0.9300 . ?
C71 C72 1.395(15) . ?
C71 C70 1.404(17) . ?
C40 H40 0.9300 . ?
C40 C41 1.398(16) . ?
C40 C39 1.362(16) . ?
C36 H36 0.9300 . ?
C36 C35 1.380(17) . ?
C22 H22 0.9300 . ?
C43 C48 1.398(14) . ?
C33 H33 0.9300 . ?
C33 C32 1.375(15) . ?
C33 C34 1.364(17) . ?
C17 H17 0.9300 . ?
C17 C18 1.391(16) . ?
C17 C16 1.395(16) . ?
C41 H41 0.9300 . ?
C10 H10 0.9300 . ?
C15 H15 0.9300 . ?
C15 C16 1.383(17) . ?
C28 H28 0.9300 . ?
C28 C29 1.379(16) . ?
C18 H18 0.9300 . ?
C65 H65 0.9300 . ?
C65 C64 1.383(17) . ?
C72 H72 0.9300 . ?
C63 H63 0.9300 . ?
C63 C64 1.390(17) . ?
C48 H48 0.9300 . ?
C48 C47 1.386(16) . ?
C32 H32 0.9300 . ?
C70 H70 0.9300 . ?
C70 C69 1.377(17) . ?
C29 H29 0.9300 . ?
C39 H39 0.9300 . ?
C64 H64 0.9300 . ?
C45 H45 0.9300 . ?
C45 C46 1.391(15) . ?
C53 H53 0.9300 . ?
C53 C52 1.37(2) . ?
C46 H46 0.9300 . ?
C46 C47 1.369(17) . ?
C51 H51 0.9300 . ?
C51 C50 1.385(16) . ?
C51 C52 1.38(2) . ?
C69 H69 0.9300 . ?
C34 H34 0.9300 . ?
C34 C35 1.382(19) . ?
C82B H82A 0.9700 . ?
C82B H82B 0.9700 . ?
C82B O1B 1.419(10) . ?
C82B C81 1.497(18) . ?
C50 H50 0.9300 . ?
C79 H79A 0.9700 . ?
C79 H79B 0.9700 . ?
C79 H79C 0.9700 . ?
C79 H79D 0.9700 . ?
C79 C80 1.514(13) . ?
C79 O1B 1.421(10) . ?
C79 C82A 1.496(15) . ?
C16 H16 0.9300 . ?
C35 H35 0.9300 . ?
C52 H52 0.9300 . ?
C80 H80A 0.9700 . ?
C80 H80B 0.9700 . ?
C80 C81 1.500(13) . ?
C47 H47 0.9300 . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C81 H81C 0.9700 . ?
C81 H81D 0.9700 . ?
C81 O1A 1.424(9) . ?
O1A C82A 1.420(9) . ?
C82A H82C 0.9700 . ?
C82A H82D 0.9700 . ?

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
Pd2 Pd1 Pd3 59.21(2) . . ?
P2 Pd1 Pd2 49.85(6) . . ?
P2 Pd1 Pd3 99.07(7) . . ?
P2 Pd1 P5 148.03(9) . . ?
P2 Pd1 P1 105.72(9) . . ?
P5 Pd1 Pd2 101.99(7) . . ?
P5 Pd1 Pd3 49.00(7) . . ?
P5 Pd1 P1 104.58(9) . . ?
P1 Pd1 Pd2 152.73(7) . . ?
P1 Pd1 Pd3 147.19(7) . . ?
Pd1 Pd2 Br1 103.76(3) . . ?
Pd3 Pd2 Pd1 61.20(2) . . ?
Pd3 Pd2 Br1 52.42(3) . . ?
Br2 Pd2 Pd1 101.20(4) . . ?
Br2 Pd2 Pd3 76.91(3) . . ?
Br2 Pd2 Br1 96.67(4) . . ?
P2 Pd2 Pd1 51.47(6) . . ?
P2 Pd2 Pd3 102.07(7) . . ?
P2 Pd2 Br1 111.19(8) . . ?
P2 Pd2 Br2 144.10(8) . . ?
P2 Pd2 P3 102.61(9) . . ?
P3 Pd2 Pd1 152.49(7) . . ?
P3 Pd2 Pd3 143.95(7) . . ?
P3 Pd2 Br1 93.98(7) . . ?
P3 Pd2 Br2 97.36(7) . . ?
Pd2 Pd3 Pd1 59.60(2) . . ?
Br1 Pd3 Pd1 113.55(4) . . ?
Br1 Pd3 Pd2 66.17(3) . . ?
P5 Pd3 Pd1 51.07(6) . . ?
P5 Pd3 Pd2 104.16(7) . . ?
P5 Pd3 Br1 163.53(7) . . ?
P5 Pd3 P4 100.22(9) . . ?
P4 Pd3 Pd1 148.09(7) . . ?
P4 Pd3 Pd2 152.23(7) . . ?
P4 Pd3 Br1 92.76(7) . . ?
Pd3 Br1 Pd2 61.40(3) . . ?
Pd2 P2 Pd1 78.68(8) . . ?
C19 P2 Pd1 119.6(3) . . ?
C19 P2 Pd2 113.8(3) . . ?
C19 P2 C25 107.9(5) . . ?
C25 P2 Pd1 111.7(3) . . ?
C25 P2 Pd2 123.3(4) . . ?
Pd3 P5 Pd1 79.93(8) . . ?
C73 P5 Pd1 119.0(3) . . ?
C73 P5 Pd3 117.0(3) . . ?
C73 P5 C67 107.9(5) . . ?
C67 P5 Pd1 116.1(3) . . ?
C67 P5 Pd3 115.0(4) . . ?
C31 P3 Pd2 113.8(3) . . ?
C31 P3 C43 103.2(5) . . ?
C31 P3 C37 105.4(5) . . ?
C43 P3 Pd2 115.7(3) . . ?
C37 P3 Pd2 116.9(3) . . ?
C37 P3 C43 100.0(5) . . ?
C13 P1 Pd1 111.6(3) . . ?
C13 P1 C1 102.5(5) . . ?
C7 P1 Pd1 113.8(3) . . ?
C7 P1 C13 104.4(5) . . ?
C7 P1 C1 104.1(4) . . ?
C1 P1 Pd1 118.9(3) . . ?
C55 P4 Pd3 121.0(3) . . ?
C55 P4 C61 104.1(5) . . ?
C55 P4 C49 101.2(5) . . ?
C61 P4 Pd3 112.8(3) . . ?
C61 P4 C49 106.7(5) . . ?
C49 P4 Pd3 109.7(3) . . ?
C73 C74 H74 119.7 . . ?
C75 C74 H74 119.7 . . ?
C75 C74 C73 120.6(9) . . ?
C56 C55 P4 119.1(7) . . ?
C60 C55 P4 122.2(8) . . ?
C60 C55 C56 118.6(9) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 C55 120.8(9) . . ?
C57 C56 H56 119.6 . . ?
C24 C19 P2 125.5(8) . . ?
C24 C19 C20 118.1(9) . . ?
C20 C19 P2 116.3(7) . . ?
C14 C13 P1 122.9(8) . . ?
C18 C13 P1 118.3(8) . . ?
C18 C13 C14 118.9(10) . . ?
C74 C73 P5 117.4(7) . . ?
C74 C73 C78 118.4(10) . . ?
C78 C73 P5 124.1(8) . . ?
C57 C58 H58 119.8 . . ?
C59 C58 H58 119.8 . . ?
C59 C58 C57 120.4(10) . . ?
C1 C6 H6 119.6 . . ?
C1 C6 C5 120.8(10) . . ?
C5 C6 H6 119.6 . . ?
C73 C78 H78 119.9 . . ?
C77 C78 C73 120.3(10) . . ?
C77 C78 H78 119.9 . . ?
C7 C8 H8 119.8 . . ?
C7 C8 C9 120.4(10) . . ?
C9 C8 H8 119.8 . . ?
C62 C61 P4 119.0(8) . . ?
C66 C61 P4 123.3(8) . . ?
C66 C61 C62 117.7(10) . . ?
C74 C75 H75 119.4 . . ?
C74 C75 C76 121.2(10) . . ?
C76 C75 H75 119.4 . . ?
C8 C7 P1 117.8(7) . . ?
C12 C7 P1 123.6(8) . . ?
C12 C7 C8 118.5(9) . . ?
C56 C57 H57 120.3 . . ?
C58 C57 C56 119.4(10) . . ?
C58 C57 H57 120.3 . . ?
C19 C24 H24 120.1 . . ?
C19 C24 C23 119.9(10) . . ?
C23 C24 H24 120.1 . . ?
C27 C26 H26 120.4 . . ?
C27 C26 C25 119.2(11) . . ?
C25 C26 H26 120.4 . . ?
C6 C1 P1 119.9(8) . . ?
C6 C1 C2 118.9(9) . . ?
C2 C1 P1 121.0(7) . . ?
C7 C12 H12 119.5 . . ?
C11 C12 C7 120.9(10) . . ?
C11 C12 H12 119.5 . . ?
C55 C60 H60 119.9 . . ?
C55 C60 C59 120.3(10) . . ?
C59 C60 H60 119.9 . . ?
C75 C76 H76 120.7 . . ?
C75 C76 C77 118.7(10) . . ?
C77 C76 H76 120.7 . . ?
C58 C59 C60 120.5(10) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C67 C68 H68 120.0 . . ?
C69 C68 H68 120.0 . . ?
C69 C68 C67 120.0(11) . . ?
C36 C31 P3 120.3(8) . . ?
C32 C31 P3 121.2(8) . . ?
C32 C31 C36 118.2(10) . . ?
C41 C42 H42 119.1 . . ?
C41 C42 C37 121.9(10) . . ?
C37 C42 H42 119.1 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.1(10) . . ?
C3 C2 H2 120.0 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.6(10) . . ?
C15 C14 H14 119.7 . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C39 C38 C37 120.3(10) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 C19 122.0(10) . . ?
C21 C20 H20 119.0 . . ?
C49 C54 H54 120.1 . . ?
C49 C54 C53 119.8(12) . . ?
C53 C54 H54 120.1 . . ?
C6 C5 H5 119.9 . . ?
C4 C5 C6 120.1(10) . . ?
C4 C5 H5 119.9 . . ?
C61 C62 H62 119.1 . . ?
C63 C62 C61 121.9(10) . . ?
C63 C62 H62 119.1 . . ?
C61 C66 H66 119.6 . . ?
C65 C66 C61 120.9(11) . . ?
C65 C66 H66 119.6 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.6(11) . . ?
C22 C21 H21 120.2 . . ?
C25 C30 H30 119.6 . . ?
C29 C30 H30 119.6 . . ?
C29 C30 C25 120.7(11) . . ?
C12 C11 H11 120.0 . . ?
C12 C11 C10 120.1(10) . . ?
C10 C11 H11 120.0 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(10) . . ?
C10 C9 H9 120.0 . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(11) . . ?
C4 C3 H3 119.9 . . ?
C68 C67 P5 123.3(9) . . ?
C72 C67 P5 116.9(8) . . ?
C72 C67 C68 119.6(10) . . ?
C78 C77 C76 120.7(9) . . ?
C78 C77 H77 119.7 . . ?
C76 C77 H77 119.7 . . ?
C26 C27 H27 119.3 . . ?
C28 C27 C26 121.4(11) . . ?
C28 C27 H27 119.3 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C45 C44 C43 120.0(10) . . ?
C5 C4 C3 119.9(10) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C24 C23 H23 119.6 . . ?
C22 C23 C24 120.8(10) . . ?
C22 C23 H23 119.6 . . ?
C54 C49 P4 121.7(9) . . ?
C50 C49 P4 118.2(8) . . ?
C50 C49 C54 119.8(10) . . ?
C72 C71 H71 120.7 . . ?
C72 C71 C70 118.5(11) . . ?
C70 C71 H71 120.7 . . ?
C41 C40 H40 119.8 . . ?
C39 C40 H40 119.8 . . ?
C39 C40 C41 120.3(10) . . ?
C31 C36 H36 119.8 . . ?
C35 C36 C31 120.4(11) . . ?
C35 C36 H36 119.8 . . ?
C26 C25 P2 125.0(9) . . ?
C26 C25 C30 118.6(10) . . ?
C30 C25 P2 115.7(8) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(10) . . ?
C23 C22 H22 120.2 . . ?
C44 C43 P3 120.5(8) . . ?
C44 C43 C48 119.1(10) . . ?
C48 C43 P3 120.3(8) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C34 C33 C32 121.1(12) . . ?
C18 C17 H17 120.3 . . ?
C18 C17 C16 119.4(11) . . ?
C16 C17 H17 120.3 . . ?
C42 C41 C40 118.8(11) . . ?
C42 C41 H41 120.6 . . ?
C40 C41 H41 120.6 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 C11 120.0(10) . . ?
C9 C10 H10 120.0 . . ?
C14 C15 H15 119.8 . . ?
C14 C15 C16 120.4(10) . . ?
C16 C15 H15 119.8 . . ?
C27 C28 H28 120.1 . . ?
C27 C28 C29 119.9(11) . . ?
C29 C28 H28 120.1 . . ?
C13 C18 C17 120.9(11) . . ?
C13 C18 H18 119.6 . . ?
C17 C18 H18 119.6 . . ?
C42 C37 P3 118.1(8) . . ?
C42 C37 C38 118.0(9) . . ?
C38 C37 P3 123.8(8) . . ?
C66 C65 H65 119.7 . . ?
C66 C65 C64 120.7(11) . . ?
C64 C65 H65 119.7 . . ?
C67 C72 C71 121.4(10) . . ?
C67 C72 H72 119.3 . . ?
C71 C72 H72 119.3 . . ?
C62 C63 H63 120.2 . . ?
C62 C63 C64 119.5(11) . . ?
C64 C63 H63 120.2 . . ?
C43 C48 H48 119.8 . . ?
C47 C48 C43 120.3(11) . . ?
C47 C48 H48 119.8 . . ?
C31 C32 H32 119.9 . . ?
C33 C32 C31 120.3(11) . . ?
C33 C32 H32 119.9 . . ?
C71 C70 H70 119.9 . . ?
C69 C70 C71 120.2(10) . . ?
C69 C70 H70 119.9 . . ?
C30 C29 C28 120.1(11) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C38 C39 H39 119.6 . . ?
C40 C39 C38 120.7(10) . . ?
C40 C39 H39 119.6 . . ?
C65 C64 C63 119.3(11) . . ?
C65 C64 H64 120.3 . . ?
C63 C64 H64 120.3 . . ?
C44 C45 H45 119.9 . . ?
C44 C45 C46 120.3(10) . . ?
C46 C45 H45 119.9 . . ?
C54 C53 H53 119.8 . . ?
C52 C53 C54 120.3(12) . . ?
C52 C53 H53 119.8 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 C45 120.0(10) . . ?
C47 C46 H46 120.0 . . ?
C50 C51 H51 119.9 . . ?
C52 C51 H51 119.9 . . ?
C52 C51 C50 120.2(12) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 C68 120.1(11) . . ?
C70 C69 H69 119.9 . . ?
C33 C34 H34 120.1 . . ?
C33 C34 C35 119.8(12) . . ?
C35 C34 H34 120.1 . . ?
H82A C82B H82B 108.6 . . ?
O1B C82B H82A 110.3 . . ?
O1B C82B H82B 110.3 . . ?
O1B C82B C81 107.0(15) . . ?
C81 C82B H82A 110.3 . . ?
C81 C82B H82B 110.3 . . ?
C49 C50 C51 120.1(12) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
H79A C79 H79B 108.9 . . ?
H79C C79 H79D 109.1 . . ?
C80 C79 H79A 110.8 . . ?
C80 C79 H79B 110.8 . . ?
C80 C79 H79C 111.1 . . ?
C80 C79 H79D 111.1 . . ?
O1B C79 H79C 111.1 . . ?
O1B C79 H79D 111.1 . . ?
O1B C79 C80 103.2(13) . . ?
C82A C79 H79A 110.8 . . ?
C82A C79 H79B 110.8 . . ?
C82A C79 C80 104.7(9) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 C17 119.9(11) . . ?
C15 C16 H16 120.0 . . ?
C36 C35 C34 120.2(11) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
C53 C52 C51 119.8(11) . . ?
C53 C52 H52 120.1 . . ?
C51 C52 H52 120.1 . . ?
C79 C80 H80A 110.8 . . ?
C79 C80 H80B 110.8 . . ?
H80A C80 H80B 108.9 . . ?
C81 C80 C79 104.6(8) . . ?
C81 C80 H80A 110.8 . . ?
C81 C80 H80B 110.8 . . ?
C48 C47 H47 119.9 . . ?
C46 C47 C48 120.2(11) . . ?
C46 C47 H47 119.9 . . ?
C82B O1B C79 110.3(17) . . ?
C82B C81 C80 104.8(11) . . ?
C82B C81 H81C 110.8 . . ?
C82B C81 H81D 110.8 . . ?
C80 C81 H81A 110.7 . . ?
C80 C81 H81B 110.7 . . ?
C80 C81 H81C 110.8 . . ?
C80 C81 H81D 110.8 . . ?
H81A C81 H81B 108.8 . . ?
H81C C81 H81D 108.9 . . ?
O1A C81 C80 105.2(9) . . ?
O1A C81 H81A 110.7 . . ?
O1A C81 H81B 110.7 . . ?
C82A O1A C81 106.1(10) . . ?
C79 C82A H82C 110.6 . . ?
C79 C82A H82D 110.6 . . ?
O1A C82A C79 105.7(10) . . ?
O1A C82A H82C 110.6 . . ?
O1A C82A H82D 110.6 . . ?
H82C C82A H82D 108.7 . . ?

_olex2_date_sample_data_collection 2019-02-15
_olex2_date_sample_submission    2019-02-13
_olex2_exptl_crystal_mounting_method 'oil on micromount 200 micrometre'
_olex2_submission_original_sample_id 'Neil Scott NWJS-4-325-crystals2'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.349
_oxdiff_exptl_absorpt_empirical_full_min 0.711
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
####################################################################### 
# 
# 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_ijsf1804
_database_code_depnum_ccdc_archive 'CCDC 1894931'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2018-02-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C78 H65 Cl P5 Pd3, 5(C H Cl3), Cl'
_chemical_formula_sum            'C83 H70 Cl17 P5 Pd3'
_chemical_formula_weight         2144.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C84 H71 Cl20 P5 Pd3'
_chemical_oxdiff_usercomment     'Neil Scott nwjs-3-175'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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                   17.6962(2)
_cell_length_b                   18.85329(16)
_cell_length_c                   29.4453(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.7594(12)
_cell_angle_gamma                90
_cell_volume                     9406.62(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23798
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      70.9170
_cell_measurement_theta_min      3.9130
_shelx_estimated_absorpt_T_max   0.731
_shelx_estimated_absorpt_T_min   0.250
_exptl_absorpt_coefficient_mu    10.146
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.265
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orangish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             4280
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 -1 0.0286
-1 0 1 0.0046
0 1 -1 0.0778
0 -1 1 0.0778
0 1 1 0.0732
0 -1 -1 0.0852
0 0 1 0.0743
0 0 -1 0.0710
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.033
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0017 -0.0002 -1.0011 -0.0099 0.0872 0.0265
-1.0017 0.0002 1.0011 0.0099 -0.0872 -0.0265
0.0017 0.9998 -1.0008 0.0785 0.0090 0.0585
-0.0017 -0.9998 1.0008 -0.0785 -0.0090 -0.0585
0.0008 0.9995 0.9986 0.0840 0.0072 -0.0506
-0.0008 -0.9995 -0.9986 -0.0840 -0.0072 0.0506
-0.0005 -0.0001 0.9997 0.0027 -0.0009 -0.0545
0.0005 0.0001 -0.9997 -0.0027 0.0009 0.0545

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51053
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.077
_diffrn_reflns_theta_max         67.077
_diffrn_reflns_theta_min         3.507
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00  21.00   1.00    2.50    --    0.00 -57.00-150.00   90
  2  ω    -69.00  21.00   1.00    2.50    --    0.00 -57.00 120.00   90
  3  ω    -18.00  80.00   1.00   10.00    --   54.00 -37.00 -90.00   98
  4  ω     23.00 111.00   1.00   10.00    --   54.00-125.00 -60.00   88
  5  ω     28.00 126.00   1.00   10.00    --   54.00  37.00  90.00   98
  6  ω      1.00  96.00   1.00   10.00    --   54.00 -99.00 150.00   95
  7  ω     38.00 138.00   1.00   20.00    --  108.00 -77.00 150.00  100
  8  ω     36.00 116.00   1.00   20.00    --  108.00-111.00 150.00   80
  9  ω     38.00 130.00   1.00   20.00    --  108.00 -50.00-120.00   92
 10  ω     86.00 178.00   1.00   20.00    --  108.00  50.00 -30.00   92
 11  ω    100.00 178.00   1.00   20.00    --  108.00 111.00-120.00   78
 12  ω     36.00 116.00   1.00   20.00    --  108.00-111.00-150.00   80
 13  ω     74.00 178.00   1.00   20.00    --  108.00  25.00  60.00  104
 14  ω    100.00 178.00   1.00   20.00    --  108.00 111.00 -90.00   78
 15  ω    -30.00  70.00   1.00    2.50    --    0.00  77.00  60.00  100
 16  ω    -59.00  -4.00   1.00    2.50    --    0.00 128.00-137.00   55
 17  ω     28.00  69.00   1.00   10.00    --   54.00  37.00 -90.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0070680000
_diffrn_orient_matrix_UB_12      0.0812522000
_diffrn_orient_matrix_UB_13      0.0027549000
_diffrn_orient_matrix_UB_21      0.0862199000
_diffrn_orient_matrix_UB_22      0.0079650000
_diffrn_orient_matrix_UB_23      -0.0008676000
_diffrn_orient_matrix_UB_31      -0.0280286000
_diffrn_orient_matrix_UB_32      0.0039262000
_diffrn_orient_matrix_UB_33      -0.0545453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14442
_reflns_number_total             16773
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         16773
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0358
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0527P)²+8.9004P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0978
_refine_special_details          
;
The crystal contained a number of chloroforms which were disordered.
Within  the asymmetric unit, there were 6 chloroforms modelled as follows:
2 ordered chloroforms modelled in a single site
3 disordered chloroforms modelled over two sites with refined occupancies
of 0.52:0.48(2), 0.535:0.465 and 0.706:0.294.  The C-Cl bond lengths 
in these chloroforms were restrained to be equal
1 highly disordered chloroform for which a suitable discrete atom model 
could not be obtained so this was modelled using a solvent mask.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl13-C82 \\sim Cl22-C82A \\sim Cl23-C82A \\sim Cl14-C82 \\sim Cl21-C82A \\sim
Cl12-C82
 with sigma of 0.02
 Cl18-C81A \\sim Cl9-C81 \\sim Cl10-C81 \\sim Cl19-C81A \\sim Cl11-C81 \\sim
Cl20-C81A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C82A) = Uanis(C82)
Uanis(C81) = Uanis(C81A)
4. Others
 Sof(H83A)=Sof(Cl24)=Sof(Cl25)=Sof(Cl26)=1-FVAR(1)
 Sof(H83)=Sof(Cl15)=Sof(Cl16)=Sof(Cl17)=FVAR(1)
 Sof(C82A)=Sof(H82A)=Sof(Cl21)=Sof(Cl22)=Sof(Cl23)=1-FVAR(2)
 Sof(C82)=Sof(H82)=Sof(Cl12)=Sof(Cl13)=Sof(Cl14)=FVAR(2)
 Sof(C81)=Sof(H81)=Sof(Cl9)=Sof(Cl10)=Sof(Cl11)=1-FVAR(3)
 Sof(C81A)=Sof(H81A)=Sof(Cl18)=Sof(Cl19)=Sof(Cl20)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C81(H81), C81A(H81A), C82(H82), C82A(H82A), C83(H83), C83(H83A), C79(H79),
 C80(H80)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75),
  C76(H76), C77(H77), C78(H78)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.6980(2) 0.73413(18) 0.54412(11) 0.0285(7) Uani 1 1 d . . . . .
C2 C 0.7436(2) 0.7927(2) 0.53999(13) 0.0372(9) Uani 1 1 d . . . . .
H2 H 0.7678 0.7944 0.5151 0.045 Uiso 1 1 calc R . . . .
C3 C 0.7540(3) 0.8486(2) 0.57193(14) 0.0457(10) Uani 1 1 d . . . . .
H3 H 0.7848 0.8885 0.5687 0.055 Uiso 1 1 calc R . . . .
C4 C 0.7195(3) 0.8461(2) 0.60847(14) 0.0449(10) Uani 1 1 d . . . . .
H4 H 0.7270 0.8841 0.6305 0.054 Uiso 1 1 calc R . . . .
C5 C 0.6746(3) 0.7891(2) 0.61298(13) 0.0418(9) Uani 1 1 d . . . . .
H5 H 0.6511 0.7877 0.6382 0.050 Uiso 1 1 calc R . . . .
C6 C 0.6630(2) 0.7331(2) 0.58086(12) 0.0347(8) Uani 1 1 d . . . . .
H6 H 0.6311 0.6940 0.5840 0.042 Uiso 1 1 calc R . . . .
C7 C 0.7841(2) 0.64517(18) 0.49942(12) 0.0290(7) Uani 1 1 d . . . . .
C8 C 0.8479(2) 0.6459(2) 0.54095(13) 0.0349(8) Uani 1 1 d . . . . .
H8 H 0.8390 0.6549 0.5707 0.042 Uiso 1 1 calc R . . . .
C9 C 0.9235(2) 0.6337(2) 0.53851(15) 0.0446(10) Uani 1 1 d . . . . .
H9 H 0.9665 0.6347 0.5667 0.054 Uiso 1 1 calc R . . . .
C10 C 0.9374(3) 0.6202(3) 0.49572(17) 0.0538(12) Uani 1 1 d . . . . .
H10 H 0.9896 0.6117 0.4943 0.065 Uiso 1 1 calc R . . . .
C11 C 0.8740(3) 0.6191(3) 0.45432(16) 0.0532(11) Uani 1 1 d . . . . .
H11 H 0.8830 0.6093 0.4246 0.064 Uiso 1 1 calc R . . . .
C12 C 0.7989(2) 0.6320(2) 0.45654(13) 0.0376(9) Uani 1 1 d . . . . .
H12 H 0.7563 0.6320 0.4282 0.045 Uiso 1 1 calc R . . . .
C13 C 0.6532(2) 0.58783(18) 0.53140(11) 0.0274(7) Uani 1 1 d . . . . .
C14 C 0.7041(2) 0.5360(2) 0.55608(13) 0.0368(8) Uani 1 1 d . . . . .
H14 H 0.7585 0.5376 0.5578 0.044 Uiso 1 1 calc R . . . .
C15 C 0.6749(3) 0.4812(2) 0.57848(15) 0.0471(10) Uani 1 1 d . . . . .
H15 H 0.7096 0.4453 0.5951 0.057 Uiso 1 1 calc R . . . .
C16 C 0.5963(3) 0.4789(2) 0.57661(13) 0.0397(9) Uani 1 1 d . . . . .
H16 H 0.5771 0.4417 0.5920 0.048 Uiso 1 1 calc R . . . .
C17 C 0.5454(2) 0.5310(2) 0.55217(12) 0.0361(8) Uani 1 1 d . . . . .
H17 H 0.4912 0.5298 0.5511 0.043 Uiso 1 1 calc R . . . .
C18 C 0.5734(2) 0.5846(2) 0.52945(12) 0.0338(8) Uani 1 1 d . . . . .
H18 H 0.5380 0.6197 0.5123 0.041 Uiso 1 1 calc R . . . .
C19 C 0.6118(2) 0.85042(19) 0.43701(11) 0.0285(7) Uani 1 1 d . . . . .
C20 C 0.6841(2) 0.8417(2) 0.42798(13) 0.0357(8) Uani 1 1 d . . . . .
H20 H 0.7010 0.7956 0.4222 0.043 Uiso 1 1 calc R . . . .
C21 C 0.7321(3) 0.9002(2) 0.42738(15) 0.0482(10) Uani 1 1 d . . . . .
H21 H 0.7819 0.8938 0.4218 0.058 Uiso 1 1 calc R . . . .
C22 C 0.7072(3) 0.9677(2) 0.43494(16) 0.0550(12) Uani 1 1 d . . . . .
H22 H 0.7392 1.0077 0.4338 0.066 Uiso 1 1 calc R . . . .
C23 C 0.6356(3) 0.9765(2) 0.44420(14) 0.0485(11) Uani 1 1 d . . . . .
H23 H 0.6189 1.0228 0.4497 0.058 Uiso 1 1 calc R . . . .
C24 C 0.5878(2) 0.9189(2) 0.44567(12) 0.0366(9) Uani 1 1 d . . . . .
H24 H 0.5390 0.9256 0.4525 0.044 Uiso 1 1 calc R . . . .
C25 C 0.4908(2) 0.77945(18) 0.47188(12) 0.0296(7) Uani 1 1 d . . . . .
C26 C 0.5098(3) 0.8215(2) 0.51256(12) 0.0365(9) Uani 1 1 d . . . . .
H26 H 0.5540 0.8524 0.5189 0.044 Uiso 1 1 calc R . . . .
C27 C 0.4643(3) 0.8183(2) 0.54378(14) 0.0462(11) Uani 1 1 d . . . . .
H27 H 0.4772 0.8476 0.5712 0.055 Uiso 1 1 calc R . . . .
C28 C 0.4006(3) 0.7732(2) 0.53554(15) 0.0490(11) Uani 1 1 d . . . . .
H28 H 0.3699 0.7716 0.5572 0.059 Uiso 1 1 calc R . . . .
C29 C 0.3811(3) 0.7302(2) 0.49566(14) 0.0456(10) Uani 1 1 d . . . . .
H29 H 0.3376 0.6986 0.4900 0.055 Uiso 1 1 calc R . . . .
C30 C 0.4257(2) 0.7337(2) 0.46427(13) 0.0353(8) Uani 1 1 d . . . . .
H30 H 0.4121 0.7044 0.4368 0.042 Uiso 1 1 calc R . . . .
C31 C 0.4931(2) 0.91266(19) 0.31530(12) 0.0306(7) Uani 1 1 d . . . . .
C32 C 0.5703(2) 0.88946(19) 0.32049(12) 0.0314(8) Uani 1 1 d . . . . .
H32 H 0.5859 0.8431 0.3322 0.038 Uiso 1 1 calc R . . . .
C33 C 0.6240(2) 0.9338(2) 0.30867(14) 0.0369(8) Uani 1 1 d . . . . .
H33 H 0.6765 0.9182 0.3125 0.044 Uiso 1 1 calc R . . . .
C34 C 0.6012(2) 1.0004(2) 0.29134(15) 0.0439(10) Uani 1 1 d . . . . .
H34 H 0.6383 1.0306 0.2832 0.053 Uiso 1 1 calc R . . . .
C35 C 0.5256(3) 1.0242(2) 0.28554(16) 0.0485(11) Uani 1 1 d . . . . .
H35 H 0.5109 1.0705 0.2736 0.058 Uiso 1 1 calc R . . . .
C36 C 0.4705(2) 0.9803(2) 0.29729(15) 0.0426(10) Uani 1 1 d . . . . .
H36 H 0.4180 0.9963 0.2930 0.051 Uiso 1 1 calc R . . . .
C37 C 0.3807(2) 0.89451(19) 0.37119(12) 0.0314(8) Uani 1 1 d . . . . .
C38 C 0.3989(3) 0.9629(2) 0.38856(15) 0.0461(11) Uani 1 1 d . . . . .
H38 H 0.4332 0.9920 0.3771 0.055 Uiso 1 1 calc R . . . .
C39 C 0.3655(3) 0.9884(3) 0.42348(17) 0.0645(17) Uani 1 1 d . . . . .
H39 H 0.3786 1.0347 0.4361 0.077 Uiso 1 1 calc R . . . .
C40 C 0.3146(3) 0.9478(3) 0.43949(15) 0.0620(15) Uani 1 1 d . . . . .
H40 H 0.2913 0.9664 0.4623 0.074 Uiso 1 1 calc R . . . .
C41 C 0.2972(3) 0.8804(3) 0.42263(14) 0.0529(12) Uani 1 1 d . . . . .
H41 H 0.2622 0.8519 0.4340 0.063 Uiso 1 1 calc R . . . .
C42 C 0.3305(2) 0.8538(2) 0.38899(12) 0.0377(9) Uani 1 1 d . . . . .
H42 H 0.3187 0.8067 0.3779 0.045 Uiso 1 1 calc R . . . .
C43 C 0.3405(2) 0.86012(17) 0.27237(11) 0.0248(7) Uani 1 1 d . . . . .
C44 C 0.3597(2) 0.85913(17) 0.22939(12) 0.0275(7) Uani 1 1 d . . . . .
H44 H 0.4132 0.8551 0.2294 0.033 Uiso 1 1 calc R . . . .
C45 C 0.3001(2) 0.86414(18) 0.18670(12) 0.0315(8) Uani 1 1 d . . . . .
H45 H 0.3130 0.8631 0.1575 0.038 Uiso 1 1 calc R . . . .
C46 C 0.2221(2) 0.87055(18) 0.18649(12) 0.0307(8) Uani 1 1 d . . . . .
H46 H 0.1818 0.8747 0.1572 0.037 Uiso 1 1 calc R . . . .
C47 C 0.2027(2) 0.87091(19) 0.22870(12) 0.0324(8) Uani 1 1 d . . . . .
H47 H 0.1490 0.8746 0.2284 0.039 Uiso 1 1 calc R . . . .
C48 C 0.2616(2) 0.86589(18) 0.27161(12) 0.0278(7) Uani 1 1 d . . . . .
H48 H 0.2480 0.8664 0.3006 0.033 Uiso 1 1 calc R . . . .
C49 C 0.4664(2) 0.69903(17) 0.23647(11) 0.0258(7) Uani 1 1 d . . . . .
C50 C 0.5402(2) 0.73062(19) 0.24309(12) 0.0311(7) Uani 1 1 d . . . . .
H50 H 0.5737 0.7373 0.2744 0.037 Uiso 1 1 calc R . . . .
C51 C 0.5653(2) 0.7523(2) 0.20523(14) 0.0381(9) Uani 1 1 d . . . . .
H51 H 0.6160 0.7732 0.2104 0.046 Uiso 1 1 calc R . . . .
C52 C 0.5160(3) 0.7434(2) 0.15932(14) 0.0413(9) Uani 1 1 d . . . . .
H52 H 0.5328 0.7585 0.1330 0.050 Uiso 1 1 calc R . . . .
C53 C 0.4426(3) 0.7127(2) 0.15203(13) 0.0396(9) Uani 1 1 d . . . . .
H53 H 0.4089 0.7071 0.1207 0.047 Uiso 1 1 calc R . . . .
C54 C 0.4177(2) 0.68984(19) 0.19009(12) 0.0325(8) Uani 1 1 d . . . . .
H54 H 0.3675 0.6679 0.1847 0.039 Uiso 1 1 calc R . . . .
C55 C 0.3399(2) 0.64322(17) 0.27185(11) 0.0242(7) Uani 1 1 d . . . . .
C56 C 0.2790(2) 0.68796(18) 0.24584(11) 0.0295(7) Uani 1 1 d . . . . .
H56 H 0.2917 0.7309 0.2328 0.035 Uiso 1 1 calc R . . . .
C57 C 0.2010(2) 0.6699(2) 0.23920(13) 0.0355(8) Uani 1 1 d . . . . .
H57 H 0.1604 0.7009 0.2222 0.043 Uiso 1 1 calc R . . . .
C58 C 0.1817(2) 0.6073(2) 0.25701(15) 0.0390(9) Uani 1 1 d . . . . .
H58 H 0.1278 0.5957 0.2527 0.047 Uiso 1 1 calc R . . . .
C59 C 0.2407(2) 0.5609(2) 0.28143(15) 0.0410(9) Uani 1 1 d . . . . .
H59 H 0.2271 0.5168 0.2926 0.049 Uiso 1 1 calc R . . . .
C60 C 0.3190(2) 0.57927(19) 0.28930(13) 0.0332(8) Uani 1 1 d . . . . .
H60 H 0.3592 0.5482 0.3068 0.040 Uiso 1 1 calc R . . . .
C61 C 0.64235(19) 0.51083(19) 0.29220(11) 0.0267(7) Uani 1 1 d . . . . .
C62 C 0.6832(2) 0.5750(2) 0.30101(16) 0.0431(9) Uani 1 1 d . . . . .
H62 H 0.6562 0.6172 0.3048 0.052 Uiso 1 1 calc R . . . .
C63 C 0.7620(2) 0.5778(2) 0.30425(16) 0.0456(10) Uani 1 1 d . . . . .
H63 H 0.7889 0.6220 0.3097 0.055 Uiso 1 1 calc R . . . .
C64 C 0.8024(2) 0.5174(2) 0.29970(15) 0.0442(10) Uani 1 1 d . . . . .
H64 H 0.8569 0.5197 0.3016 0.053 Uiso 1 1 calc R . . . .
C65 C 0.7635(3) 0.4537(2) 0.29231(18) 0.0519(11) Uani 1 1 d . . . . .
H65 H 0.7914 0.4116 0.2896 0.062 Uiso 1 1 calc R . . . .
C66 C 0.6836(2) 0.4502(2) 0.28879(15) 0.0403(9) Uani 1 1 d . . . . .
H66 H 0.6574 0.4057 0.2840 0.048 Uiso 1 1 calc R . . . .
C67 C 0.4890(2) 0.51516(17) 0.22377(11) 0.0282(7) Uani 1 1 d . . . . .
C68 C 0.5299(3) 0.5322(2) 0.19154(13) 0.0402(9) Uani 1 1 d . . . . .
H68 H 0.5842 0.5445 0.2025 0.048 Uiso 1 1 calc R . . . .
C69 C 0.4910(3) 0.5313(3) 0.14298(14) 0.0549(13) Uani 1 1 d . . . . .
H69 H 0.5192 0.5425 0.1209 0.066 Uiso 1 1 calc R . . . .
C70 C 0.4127(3) 0.5146(2) 0.12705(14) 0.0525(13) Uani 1 1 d . . . . .
H70 H 0.3869 0.5134 0.0939 0.063 Uiso 1 1 calc R . . . .
C71 C 0.3710(3) 0.4993(2) 0.15879(15) 0.0475(11) Uani 1 1 d . . . . .
H71 H 0.3163 0.4885 0.1475 0.057 Uiso 1 1 calc R . . . .
C72 C 0.4086(2) 0.49960(19) 0.20745(13) 0.0350(8) Uani 1 1 d . . . . .
H72 H 0.3796 0.4893 0.2293 0.042 Uiso 1 1 calc R . . . .
C73 C 0.51515(19) 0.42102(17) 0.30182(12) 0.0252(7) Uani 1 1 d . . . . .
C74 C 0.5055(2) 0.40676(18) 0.34630(12) 0.0293(7) Uani 1 1 d . . . . .
H74 H 0.5058 0.4448 0.3675 0.035 Uiso 1 1 calc R . . . .
C75 C 0.4955(2) 0.3379(2) 0.35995(13) 0.0341(8) Uani 1 1 d . . . . .
H75 H 0.4895 0.3287 0.3904 0.041 Uiso 1 1 calc R . . . .
C76 C 0.4944(2) 0.28278(19) 0.32887(14) 0.0357(8) Uani 1 1 d . . . . .
H76 H 0.4880 0.2354 0.3382 0.043 Uiso 1 1 calc R . . . .
C77 C 0.5026(2) 0.29604(19) 0.28417(13) 0.0341(8) Uani 1 1 d . . . . .
H77 H 0.5016 0.2579 0.2629 0.041 Uiso 1 1 calc R . . . .
C78 C 0.5121(2) 0.36503(18) 0.27065(12) 0.0290(7) Uani 1 1 d . . . . .
H78 H 0.5166 0.3742 0.2398 0.035 Uiso 1 1 calc R . . . .
Cl1 Cl 0.61626(5) 0.54968(4) 0.40655(3) 0.02849(17) Uani 1 1 d . . . . .
P1 P 0.68408(5) 0.66189(4) 0.50122(3) 0.02393(17) Uani 1 1 d . . . . .
P2 P 0.54613(5) 0.77484(4) 0.42900(3) 0.02407(17) Uani 1 1 d . . . . .
P3 P 0.42133(5) 0.85232(4) 0.32744(3) 0.02387(17) Uani 1 1 d . . . . .
P4 P 0.44128(5) 0.67203(4) 0.28923(3) 0.02243(16) Uani 1 1 d . . . . .
P5 P 0.53753(5) 0.51120(4) 0.28742(3) 0.02283(16) Uani 1 1 d . . . . .
Pd1 Pd 0.59571(2) 0.66870(2) 0.42750(2) 0.02252(6) Uani 1 1 d . . . . .
Pd2 Pd 0.47854(2) 0.74434(2) 0.35334(2) 0.02106(6) Uani 1 1 d . . . . .
Pd3 Pd 0.52431(2) 0.60006(2) 0.33766(2) 0.02229(6) Uani 1 1 d . . . . .
C81 C 0.7909(9) 0.4241(12) 0.4352(5) 0.065(3) Uani 0.52(2) 1 d D . P A 1
H81 H 0.7770 0.4708 0.4188 0.077 Uiso 0.52(2) 1 calc R . P A 1
C81A C 0.7733(9) 0.4307(13) 0.4373(5) 0.065(3) Uani 0.48(2) 1 d D . P A 2
H81A H 0.7509 0.4791 0.4284 0.077 Uiso 0.48(2) 1 calc R . P A 2
Cl9 Cl 0.8576(3) 0.3823(12) 0.4112(2) 0.133(4) Uani 0.52(2) 1 d D . P A 1
Cl10 Cl 0.8329(6) 0.4410(5) 0.4952(3) 0.102(3) Uani 0.52(2) 1 d D . P A 1
Cl11 Cl 0.7046(7) 0.3753(7) 0.4253(5) 0.083(3) Uani 0.52(2) 1 d D . P A 1
Cl18 Cl 0.8505(4) 0.4169(4) 0.4127(3) 0.0842(19) Uani 0.48(2) 1 d D . P A 2
Cl19 Cl 0.8123(8) 0.4257(6) 0.4985(3) 0.124(4) Uani 0.48(2) 1 d D . P A 2
Cl20 Cl 0.6993(7) 0.3681(7) 0.4175(4) 0.065(2) Uani 0.48(2) 1 d D . P A 2
C82 C 1.0984(8) 0.7375(6) 0.3709(4) 0.048(3) Uani 0.535(5) 1 d D . P B 1
H82 H 1.0498 0.7096 0.3552 0.058 Uiso 0.535(5) 1 calc R . P B 1
C82A C 1.1150(9) 0.7262(7) 0.3630(5) 0.048(3) Uani 0.465(5) 1 d D . P B 2
H82A H 1.0790 0.6978 0.3369 0.058 Uiso 0.465(5) 1 calc R . P B 2
Cl12 Cl 1.1328(3) 0.7092(2) 0.42869(14) 0.0741(11) Uani 0.535(5) 1 d D . P B 1
Cl13 Cl 1.1667(2) 0.72340(17) 0.33845(14) 0.0830(14) Uani 0.535(5) 1 d D . P B
1
Cl14 Cl 1.0723(2) 0.82687(14) 0.36789(10) 0.0585(7) Uani 0.535(5) 1 d D . P B 1
Cl21 Cl 1.0901(7) 0.7127(3) 0.4147(3) 0.150(4) Uani 0.465(5) 1 d D . P B 2
Cl22 Cl 1.2117(2) 0.69843(16) 0.37128(19) 0.0955(16) Uani 0.465(5) 1 d D . P B
2
Cl23 Cl 1.1063(2) 0.81591(17) 0.34755(18) 0.0794(16) Uani 0.465(5) 1 d D . P B
2
C83 C 0.8486(3) 0.7902(2) 0.33539(17) 0.0543(11) Uani 1 1 d . . . . .
H83 H 0.8806 0.7615 0.3191 0.065 Uiso 0.706(9) 1 calc R . P C 1
H83A H 0.8783 0.7572 0.3202 0.065 Uiso 0.294(9) 1 calc R . P C 2
Cl15 Cl 0.8750(3) 0.8799(3) 0.33248(16) 0.0882(15) Uani 0.706(9) 1 d . . P C 1
Cl16 Cl 0.74916(19) 0.77877(18) 0.3037(2) 0.111(2) Uani 0.706(9) 1 d . . P C 1
Cl17 Cl 0.8683(3) 0.75998(16) 0.39143(12) 0.0783(11) Uani 0.706(9) 1 d . . P C
1
Cl24 Cl 0.8514(6) 0.8736(6) 0.3187(6) 0.108(5) Uani 0.294(9) 1 d . . P C 2
Cl25 Cl 0.7522(4) 0.7583(3) 0.3336(3) 0.061(2) Uani 0.294(9) 1 d . . P C 2
Cl26 Cl 0.8921(5) 0.7968(9) 0.4021(3) 0.118(4) Uani 0.294(9) 1 d . . P C 2
C79 C 1.0225(2) 0.5128(2) 0.34944(13) 0.0354(8) Uani 1 1 d . . . . .
H79 H 0.9894 0.5454 0.3249 0.043 Uiso 1 1 calc R . . . .
Cl3 Cl 1.00464(10) 0.53107(7) 0.40341(4) 0.0680(4) Uani 1 1 d . . . . .
Cl4 Cl 0.99582(6) 0.42452(5) 0.33189(3) 0.0409(2) Uani 1 1 d . . . . .
Cl5 Cl 1.12172(7) 0.52709(7) 0.35297(5) 0.0645(3) Uani 1 1 d . . . . .
C80 C 0.7962(3) 0.6758(3) 0.18108(16) 0.0510(11) Uani 1 1 d . . . . .
H80 H 0.8356 0.6672 0.2126 0.061 Uiso 1 1 calc R . . . .
Cl6 Cl 0.83927(9) 0.65332(8) 0.13642(5) 0.0671(3) Uani 1 1 d . . . . .
Cl7 Cl 0.77016(10) 0.76556(8) 0.17703(8) 0.0955(5) Uani 1 1 d . . . . .
Cl8 Cl 0.71305(8) 0.62310(8) 0.17695(5) 0.0722(4) Uani 1 1 d . . . . .
Cl2 Cl 0.94098(6) 0.66214(4) 0.28982(3) 0.0383(2) 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 1.394(5) . ?
C1 C6 1.392(5) . ?
C1 P1 1.826(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.365(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(5) . ?
C6 H6 0.9500 . ?
C7 C8 1.405(5) . ?
C7 C12 1.384(5) . ?
C7 P1 1.813(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.375(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.399(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.371(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(5) . ?
C13 C18 1.400(5) . ?
C13 P1 1.821(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.403(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.376(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.387(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.380(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.390(6) . ?
C19 C24 1.405(5) . ?
C19 P2 1.811(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.396(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.386(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.386(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.395(5) . ?
C25 C30 1.405(5) . ?
C25 P2 1.809(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.388(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.376(7) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(6) . ?
C29 H29 0.9500 . ?
C29 C30 1.379(5) . ?
C30 H30 0.9500 . ?
C31 C32 1.402(5) . ?
C31 C36 1.394(5) . ?
C31 P3 1.815(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.383(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.371(6) . ?
C34 H34 0.9500 . ?
C34 C35 1.373(6) . ?
C35 H35 0.9500 . ?
C35 C36 1.397(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.391(5) . ?
C37 C42 1.386(6) . ?
C37 P3 1.828(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.410(7) . ?
C39 H39 0.9500 . ?
C39 C40 1.365(8) . ?
C40 H40 0.9500 . ?
C40 C41 1.366(8) . ?
C41 H41 0.9500 . ?
C41 C42 1.385(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.402(5) . ?
C43 C48 1.395(5) . ?
C43 P3 1.833(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.392(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.382(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.390(5) . ?
C48 H48 0.9500 . ?
C49 C50 1.396(5) . ?
C49 C54 1.400(5) . ?
C49 P4 1.808(3) . ?
C50 H50 0.9500 . ?
C50 C51 1.376(5) . ?
C51 H51 0.9500 . ?
C51 C52 1.391(6) . ?
C52 H52 0.9500 . ?
C52 C53 1.382(6) . ?
C53 H53 0.9500 . ?
C53 C54 1.386(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.408(5) . ?
C55 C60 1.401(5) . ?
C55 P4 1.802(3) . ?
C56 H56 0.9500 . ?
C56 C57 1.379(5) . ?
C57 H57 0.9500 . ?
C57 C58 1.373(5) . ?
C58 H58 0.9500 . ?
C58 C59 1.393(6) . ?
C59 H59 0.9500 . ?
C59 C60 1.382(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.395(5) . ?
C61 C66 1.376(5) . ?
C61 P5 1.819(3) . ?
C62 H62 0.9500 . ?
C62 C63 1.371(6) . ?
C63 H63 0.9500 . ?
C63 C64 1.371(6) . ?
C64 H64 0.9500 . ?
C64 C65 1.370(6) . ?
C65 H65 0.9500 . ?
C65 C66 1.389(6) . ?
C66 H66 0.9500 . ?
C67 C68 1.386(5) . ?
C67 C72 1.397(5) . ?
C67 P5 1.824(3) . ?
C68 H68 0.9500 . ?
C68 C69 1.397(6) . ?
C69 H69 0.9500 . ?
C69 C70 1.366(7) . ?
C70 H70 0.9500 . ?
C70 C71 1.378(7) . ?
C71 H71 0.9500 . ?
C71 C72 1.395(5) . ?
C72 H72 0.9500 . ?
C73 C74 1.395(5) . ?
C73 C78 1.390(5) . ?
C73 P5 1.823(3) . ?
C74 H74 0.9500 . ?
C74 C75 1.385(5) . ?
C75 H75 0.9500 . ?
C75 C76 1.381(5) . ?
C76 H76 0.9500 . ?
C76 C77 1.388(5) . ?
C77 H77 0.9500 . ?
C77 C78 1.385(5) . ?
C78 H78 0.9500 . ?
Cl1 Pd1 2.3828(8) . ?
Cl1 Pd3 2.4002(8) . ?
P1 Pd1 2.2837(8) . ?
P2 Pd1 2.1905(8) . ?
P2 Pd2 2.2775(8) . ?
P3 Pd2 2.3034(8) . ?
P4 Pd2 2.2670(8) . ?
P4 Pd3 2.1967(8) . ?
P5 Pd3 2.2913(8) . ?
Pd1 Pd2 2.9138(3) . ?
Pd1 Pd3 2.8882(3) . ?
Pd2 Pd3 2.9127(3) . ?
C81 H81 1.0000 . ?
C81 Cl9 1.731(12) . ?
C81 Cl10 1.737(11) . ?
C81 Cl11 1.734(11) . ?
C81A H81A 1.0000 . ?
C81A Cl18 1.740(12) . ?
C81A Cl19 1.736(12) . ?
C81A Cl20 1.734(12) . ?
C82 H82 1.0000 . ?
C82 Cl12 1.719(10) . ?
C82 Cl13 1.764(10) . ?
C82 Cl14 1.742(10) . ?
C82A H82A 1.0000 . ?
C82A Cl21 1.723(11) . ?
C82A Cl22 1.738(12) . ?
C82A Cl23 1.746(11) . ?
C83 H83 1.0000 . ?
C83 H83A 1.0000 . ?
C83 Cl15 1.764(7) . ?
C83 Cl16 1.751(6) . ?
C83 Cl17 1.684(5) . ?
C83 Cl24 1.652(12) . ?
C83 Cl25 1.796(7) . ?
C83 Cl26 1.896(9) . ?
C79 H79 1.0000 . ?
C79 Cl3 1.741(4) . ?
C79 Cl4 1.767(4) . ?
C79 Cl5 1.750(4) . ?
C80 H80 1.0000 . ?
C80 Cl6 1.751(5) . ?
C80 Cl7 1.749(5) . ?
C80 Cl8 1.751(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 119.8(3) . . ?
C6 C1 C2 118.4(3) . . ?
C6 C1 P1 121.8(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.6(4) . . ?
C3 C2 H2 119.7 . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.9(4) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.8 . . ?
C4 C5 C6 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 120.4(4) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 P1 121.3(3) . . ?
C12 C7 C8 118.7(3) . . ?
C12 C7 P1 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.1(4) . . ?
C9 C8 H8 120.0 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.7(4) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 120.3 . . ?
C9 C10 C11 119.4(4) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0(4) . . ?
C12 C11 H11 120.0 . . ?
C7 C12 H12 119.5 . . ?
C11 C12 C7 121.1(4) . . ?
C11 C12 H12 119.5 . . ?
C14 C13 C18 119.1(3) . . ?
C14 C13 P1 123.8(3) . . ?
C18 C13 P1 117.1(3) . . ?
C13 C14 H14 120.2 . . ?
C13 C14 C15 119.7(4) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(4) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.8(4) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.0(4) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 119.6 . . ?
C17 C18 C13 120.8(4) . . ?
C17 C18 H18 119.6 . . ?
C20 C19 C24 119.2(4) . . ?
C20 C19 P2 118.3(3) . . ?
C24 C19 P2 122.0(3) . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.4(4) . . ?
C21 C20 H20 119.8 . . ?
C20 C21 H21 119.9 . . ?
C22 C21 C20 120.1(4) . . ?
C22 C21 H21 119.9 . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(4) . . ?
C23 C22 H22 120.2 . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 121.1(4) . . ?
C24 C23 H23 119.5 . . ?
C19 C24 H24 120.2 . . ?
C23 C24 C19 119.6(4) . . ?
C23 C24 H24 120.2 . . ?
C26 C25 C30 118.1(4) . . ?
C26 C25 P2 125.6(3) . . ?
C30 C25 P2 116.3(3) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 119.6 . . ?
C28 C27 C26 120.8(4) . . ?
C28 C27 H27 119.6 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.1(4) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 H29 120.4 . . ?
C30 C29 C28 119.3(4) . . ?
C30 C29 H29 120.4 . . ?
C25 C30 H30 119.2 . . ?
C29 C30 C25 121.6(4) . . ?
C29 C30 H30 119.2 . . ?
C32 C31 P3 119.9(3) . . ?
C36 C31 C32 119.3(3) . . ?
C36 C31 P3 120.6(3) . . ?
C31 C32 H32 119.9 . . ?
C33 C32 C31 120.2(3) . . ?
C33 C32 H32 119.9 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.8(4) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.4 . . ?
C33 C34 C35 121.1(4) . . ?
C35 C34 H34 119.4 . . ?
C34 C35 H35 120.0 . . ?
C34 C35 C36 120.0(4) . . ?
C36 C35 H35 120.0 . . ?
C31 C36 C35 119.5(4) . . ?
C31 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C38 C37 P3 124.5(3) . . ?
C42 C37 C38 118.6(4) . . ?
C42 C37 P3 116.8(3) . . ?
C37 C38 H38 120.5 . . ?
C37 C38 C39 118.9(5) . . ?
C39 C38 H38 120.5 . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.2(4) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 120.1 . . ?
C39 C40 C41 119.9(4) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 120.1 . . ?
C40 C41 C42 119.9(5) . . ?
C42 C41 H41 120.1 . . ?
C37 C42 H42 119.3 . . ?
C41 C42 C37 121.5(4) . . ?
C41 C42 H42 119.3 . . ?
C44 C43 P3 117.8(3) . . ?
C48 C43 C44 119.3(3) . . ?
C48 C43 P3 122.9(3) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 C43 119.8(3) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 119.8 . . ?
C46 C45 C44 120.3(3) . . ?
C46 C45 H45 119.8 . . ?
C45 C46 H46 119.9 . . ?
C47 C46 C45 120.2(3) . . ?
C47 C46 H46 119.9 . . ?
C46 C47 H47 119.9 . . ?
C46 C47 C48 120.1(3) . . ?
C48 C47 H47 119.9 . . ?
C43 C48 H48 119.8 . . ?
C47 C48 C43 120.3(3) . . ?
C47 C48 H48 119.8 . . ?
C50 C49 C54 118.5(3) . . ?
C50 C49 P4 116.9(2) . . ?
C54 C49 P4 124.7(3) . . ?
C49 C50 H50 119.3 . . ?
C51 C50 C49 121.4(3) . . ?
C51 C50 H50 119.3 . . ?
C50 C51 H51 120.2 . . ?
C50 C51 C52 119.5(4) . . ?
C52 C51 H51 120.2 . . ?
C51 C52 H52 120.0 . . ?
C53 C52 C51 119.9(4) . . ?
C53 C52 H52 120.0 . . ?
C52 C53 H53 119.7 . . ?
C52 C53 C54 120.6(4) . . ?
C54 C53 H53 119.7 . . ?
C49 C54 H54 120.0 . . ?
C53 C54 C49 120.0(4) . . ?
C53 C54 H54 120.0 . . ?
C56 C55 P4 121.1(3) . . ?
C60 C55 C56 118.3(3) . . ?
C60 C55 P4 120.1(3) . . ?
C55 C56 H56 119.8 . . ?
C57 C56 C55 120.4(3) . . ?
C57 C56 H56 119.8 . . ?
C56 C57 H57 119.8 . . ?
C58 C57 C56 120.5(3) . . ?
C58 C57 H57 119.8 . . ?
C57 C58 H58 119.8 . . ?
C57 C58 C59 120.3(4) . . ?
C59 C58 H58 119.8 . . ?
C58 C59 H59 120.2 . . ?
C60 C59 C58 119.7(4) . . ?
C60 C59 H59 120.2 . . ?
C55 C60 H60 119.6 . . ?
C59 C60 C55 120.8(3) . . ?
C59 C60 H60 119.6 . . ?
C62 C61 P5 118.2(3) . . ?
C66 C61 C62 118.5(3) . . ?
C66 C61 P5 123.3(3) . . ?
C61 C62 H62 119.7 . . ?
C63 C62 C61 120.5(4) . . ?
C63 C62 H62 119.7 . . ?
C62 C63 H63 119.7 . . ?
C62 C63 C64 120.7(4) . . ?
C64 C63 H63 119.7 . . ?
C63 C64 H64 120.3 . . ?
C65 C64 C63 119.4(4) . . ?
C65 C64 H64 120.3 . . ?
C64 C65 H65 119.8 . . ?
C64 C65 C66 120.5(4) . . ?
C66 C65 H65 119.8 . . ?
C61 C66 C65 120.3(4) . . ?
C61 C66 H66 119.8 . . ?
C65 C66 H66 119.8 . . ?
C68 C67 C72 119.6(3) . . ?
C68 C67 P5 122.0(3) . . ?
C72 C67 P5 118.4(3) . . ?
C67 C68 H68 120.1 . . ?
C67 C68 C69 119.9(4) . . ?
C69 C68 H68 120.1 . . ?
C68 C69 H69 119.8 . . ?
C70 C69 C68 120.4(4) . . ?
C70 C69 H69 119.8 . . ?
C69 C70 H70 119.9 . . ?
C69 C70 C71 120.3(4) . . ?
C71 C70 H70 119.9 . . ?
C70 C71 H71 119.8 . . ?
C70 C71 C72 120.4(4) . . ?
C72 C71 H71 119.8 . . ?
C67 C72 H72 120.3 . . ?
C71 C72 C67 119.4(4) . . ?
C71 C72 H72 120.3 . . ?
C74 C73 P5 119.4(3) . . ?
C78 C73 C74 118.8(3) . . ?
C78 C73 P5 121.6(3) . . ?
C73 C74 H74 119.6 . . ?
C75 C74 C73 120.9(3) . . ?
C75 C74 H74 119.6 . . ?
C74 C75 H75 120.3 . . ?
C76 C75 C74 119.5(3) . . ?
C76 C75 H75 120.3 . . ?
C75 C76 H76 119.8 . . ?
C75 C76 C77 120.5(3) . . ?
C77 C76 H76 119.8 . . ?
C76 C77 H77 120.1 . . ?
C78 C77 C76 119.8(3) . . ?
C78 C77 H77 120.1 . . ?
C73 C78 H78 119.7 . . ?
C77 C78 C73 120.6(3) . . ?
C77 C78 H78 119.7 . . ?
Pd1 Cl1 Pd3 74.29(2) . . ?
C1 P1 Pd1 122.30(11) . . ?
C7 P1 C1 102.25(17) . . ?
C7 P1 C13 108.26(16) . . ?
C7 P1 Pd1 112.88(11) . . ?
C13 P1 C1 103.52(15) . . ?
C13 P1 Pd1 106.71(11) . . ?
C19 P2 Pd1 118.40(12) . . ?
C19 P2 Pd2 117.54(11) . . ?
C25 P2 C19 109.11(17) . . ?
C25 P2 Pd1 111.00(12) . . ?
C25 P2 Pd2 117.23(12) . . ?
Pd1 P2 Pd2 81.38(3) . . ?
C31 P3 C37 107.77(18) . . ?
C31 P3 C43 100.80(16) . . ?
C31 P3 Pd2 110.71(12) . . ?
C37 P3 C43 102.90(15) . . ?
C37 P3 Pd2 112.07(12) . . ?
C43 P3 Pd2 121.35(11) . . ?
C49 P4 Pd2 117.50(11) . . ?
C49 P4 Pd3 116.59(11) . . ?
C55 P4 C49 108.19(15) . . ?
C55 P4 Pd2 116.39(11) . . ?
C55 P4 Pd3 115.02(11) . . ?
Pd3 P4 Pd2 81.45(3) . . ?
C61 P5 C67 104.28(16) . . ?
C61 P5 C73 105.27(16) . . ?
C61 P5 Pd3 104.15(11) . . ?
C67 P5 Pd3 121.88(11) . . ?
C73 P5 C67 101.99(15) . . ?
C73 P5 Pd3 117.53(11) . . ?
Cl1 Pd1 Pd2 113.303(19) . . ?
Cl1 Pd1 Pd3 53.130(18) . . ?
P1 Pd1 Cl1 94.55(3) . . ?
P1 Pd1 Pd2 152.14(2) . . ?
P1 Pd1 Pd3 147.58(2) . . ?
P2 Pd1 Cl1 163.22(3) . . ?
P2 Pd1 P1 101.58(3) . . ?
P2 Pd1 Pd2 50.61(2) . . ?
P2 Pd1 Pd3 110.84(2) . . ?
Pd3 Pd1 Pd2 60.265(8) . . ?
P2 Pd2 P3 99.06(3) . . ?
P2 Pd2 Pd1 48.01(2) . . ?
P2 Pd2 Pd3 107.41(2) . . ?
P3 Pd2 Pd1 146.15(2) . . ?
P3 Pd2 Pd3 152.70(2) . . ?
P4 Pd2 P2 155.64(3) . . ?
P4 Pd2 P3 105.14(3) . . ?
P4 Pd2 Pd1 107.64(2) . . ?
P4 Pd2 Pd3 48.23(2) . . ?
Pd3 Pd2 Pd1 59.432(8) . . ?
Cl1 Pd3 Pd1 52.578(19) . . ?
Cl1 Pd3 Pd2 112.79(2) . . ?
P4 Pd3 Cl1 163.07(3) . . ?
P4 Pd3 P5 101.90(3) . . ?
P4 Pd3 Pd1 110.61(2) . . ?
P4 Pd3 Pd2 50.32(2) . . ?
P5 Pd3 Cl1 94.92(3) . . ?
P5 Pd3 Pd1 145.07(2) . . ?
P5 Pd3 Pd2 150.46(2) . . ?
Pd1 Pd3 Pd2 60.303(7) . . ?
Cl9 C81 H81 107.8 . . ?
Cl9 C81 Cl10 110.8(9) . . ?
Cl9 C81 Cl11 111.2(10) . . ?
Cl10 C81 H81 107.8 . . ?
Cl11 C81 H81 107.8 . . ?
Cl11 C81 Cl10 111.4(11) . . ?
Cl18 C81A H81A 109.2 . . ?
Cl19 C81A H81A 109.2 . . ?
Cl19 C81A Cl18 107.4(9) . . ?
Cl20 C81A H81A 109.2 . . ?
Cl20 C81A Cl18 111.5(10) . . ?
Cl20 C81A Cl19 110.3(12) . . ?
Cl12 C82 H82 107.7 . . ?
Cl12 C82 Cl13 112.8(7) . . ?
Cl12 C82 Cl14 111.3(6) . . ?
Cl13 C82 H82 107.7 . . ?
Cl14 C82 H82 107.7 . . ?
Cl14 C82 Cl13 109.4(6) . . ?
Cl21 C82A H82A 109.3 . . ?
Cl21 C82A Cl22 108.9(8) . . ?
Cl21 C82A Cl23 110.3(7) . . ?
Cl22 C82A H82A 109.3 . . ?
Cl22 C82A Cl23 109.8(8) . . ?
Cl23 C82A H82A 109.3 . . ?
Cl15 C83 H83 107.5 . . ?
Cl16 C83 H83 107.5 . . ?
Cl16 C83 Cl15 109.4(3) . . ?
Cl17 C83 H83 107.5 . . ?
Cl17 C83 Cl15 112.9(3) . . ?
Cl17 C83 Cl16 111.9(4) . . ?
Cl24 C83 H83A 113.3 . . ?
Cl24 C83 Cl25 114.8(5) . . ?
Cl24 C83 Cl26 102.0(6) . . ?
Cl25 C83 H83A 113.3 . . ?
Cl25 C83 Cl26 98.7(4) . . ?
Cl26 C83 H83A 113.3 . . ?
Cl3 C79 H79 108.4 . . ?
Cl3 C79 Cl4 110.5(2) . . ?
Cl3 C79 Cl5 111.0(2) . . ?
Cl4 C79 H79 108.4 . . ?
Cl5 C79 H79 108.4 . . ?
Cl5 C79 Cl4 109.9(2) . . ?
Cl6 C80 H80 108.6 . . ?
Cl7 C80 H80 108.6 . . ?
Cl7 C80 Cl6 110.3(3) . . ?
Cl7 C80 Cl8 110.2(3) . . ?
Cl8 C80 H80 108.6 . . ?
Cl8 C80 Cl6 110.4(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C74 H74 Cl1 0.95 2.79 3.499(4) 132.6 .
C81A H81A Cl1 1.00 2.64 3.48(2) 141.8 .
C82 H82 Cl2 1.00 2.47 3.412(15) 157.6 .
C82A H82A Cl2 1.00 2.53 3.430(17) 149.9 .
C83 H83A Cl2 1.00 2.41 3.401(5) 170.5 .
C79 H79 Cl2 1.00 2.48 3.410(4) 155.2 .
C80 H80 Cl2 1.00 2.49 3.485(5) 172.2 .

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.6(6) . . . . ?
C2 C1 C6 C5 -0.9(5) . . . . ?
C2 C1 P1 C7 48.2(3) . . . . ?
C2 C1 P1 C13 160.7(3) . . . . ?
C2 C1 P1 Pd1 -79.2(3) . . . . ?
C2 C3 C4 C5 -0.6(6) . . . . ?
C3 C4 C5 C6 -0.1(6) . . . . ?
C4 C5 C6 C1 0.8(6) . . . . ?
C6 C1 C2 C3 0.2(5) . . . . ?
C6 C1 P1 C7 -132.8(3) . . . . ?
C6 C1 P1 C13 -20.3(3) . . . . ?
C6 C1 P1 Pd1 99.8(3) . . . . ?
C7 C8 C9 C10 -0.5(7) . . . . ?
C8 C7 C12 C11 0.8(6) . . . . ?
C8 C7 P1 C1 40.6(3) . . . . ?
C8 C7 P1 C13 -68.3(3) . . . . ?
C8 C7 P1 Pd1 173.8(3) . . . . ?
C8 C9 C10 C11 0.2(8) . . . . ?
C9 C10 C11 C12 0.6(8) . . . . ?
C10 C11 C12 C7 -1.1(7) . . . . ?
C12 C7 C8 C9 0.0(6) . . . . ?
C12 C7 P1 C1 -138.7(3) . . . . ?
C12 C7 P1 C13 112.4(3) . . . . ?
C12 C7 P1 Pd1 -5.5(3) . . . . ?
C13 C14 C15 C16 -0.8(6) . . . . ?
C14 C13 C18 C17 0.7(5) . . . . ?
C14 C13 P1 C1 -96.8(3) . . . . ?
C14 C13 P1 C7 11.2(3) . . . . ?
C14 C13 P1 Pd1 132.9(3) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C15 C16 C17 C18 0.6(6) . . . . ?
C16 C17 C18 C13 -1.1(5) . . . . ?
C18 C13 C14 C15 0.3(5) . . . . ?
C18 C13 P1 C1 82.5(3) . . . . ?
C18 C13 P1 C7 -169.5(3) . . . . ?
C18 C13 P1 Pd1 -47.7(3) . . . . ?
C19 C20 C21 C22 -1.2(6) . . . . ?
C20 C19 C24 C23 1.2(5) . . . . ?
C20 C19 P2 C25 146.9(3) . . . . ?
C20 C19 P2 Pd1 18.7(3) . . . . ?
C20 C19 P2 Pd2 -76.4(3) . . . . ?
C20 C21 C22 C23 1.6(6) . . . . ?
C21 C22 C23 C24 -0.6(6) . . . . ?
C22 C23 C24 C19 -0.8(6) . . . . ?
C24 C19 C20 C21 -0.2(5) . . . . ?
C24 C19 P2 C25 -41.8(3) . . . . ?
C24 C19 P2 Pd1 -170.0(2) . . . . ?
C24 C19 P2 Pd2 94.8(3) . . . . ?
C25 C26 C27 C28 0.8(6) . . . . ?
C26 C25 C30 C29 0.4(6) . . . . ?
C26 C25 P2 C19 -16.5(4) . . . . ?
C26 C25 P2 Pd1 115.7(3) . . . . ?
C26 C25 P2 Pd2 -153.3(3) . . . . ?
C26 C27 C28 C29 0.0(7) . . . . ?
C27 C28 C29 C30 -0.7(7) . . . . ?
C28 C29 C30 C25 0.5(6) . . . . ?
C30 C25 C26 C27 -1.0(5) . . . . ?
C30 C25 P2 C19 167.0(3) . . . . ?
C30 C25 P2 Pd1 -60.8(3) . . . . ?
C30 C25 P2 Pd2 30.2(3) . . . . ?
C31 C32 C33 C34 -0.7(6) . . . . ?
C32 C31 C36 C35 -1.2(6) . . . . ?
C32 C31 P3 C37 125.2(3) . . . . ?
C32 C31 P3 C43 -127.3(3) . . . . ?
C32 C31 P3 Pd2 2.3(3) . . . . ?
C32 C33 C34 C35 0.2(6) . . . . ?
C33 C34 C35 C36 -0.1(7) . . . . ?
C34 C35 C36 C31 0.6(7) . . . . ?
C36 C31 C32 C33 1.2(5) . . . . ?
C36 C31 P3 C37 -59.8(3) . . . . ?
C36 C31 P3 C43 47.6(3) . . . . ?
C36 C31 P3 Pd2 177.3(3) . . . . ?
C37 C38 C39 C40 -1.6(6) . . . . ?
C38 C37 C42 C41 1.4(5) . . . . ?
C38 C37 P3 C31 4.3(3) . . . . ?
C38 C37 P3 C43 -101.7(3) . . . . ?
C38 C37 P3 Pd2 126.3(3) . . . . ?
C38 C39 C40 C41 2.0(7) . . . . ?
C39 C40 C41 C42 -0.7(6) . . . . ?
C40 C41 C42 C37 -1.0(6) . . . . ?
C42 C37 C38 C39 -0.1(5) . . . . ?
C42 C37 P3 C31 -173.5(3) . . . . ?
C42 C37 P3 C43 80.5(3) . . . . ?
C42 C37 P3 Pd2 -51.5(3) . . . . ?
C43 C44 C45 C46 0.4(5) . . . . ?
C44 C43 C48 C47 -0.3(5) . . . . ?
C44 C43 P3 C31 44.3(3) . . . . ?
C44 C43 P3 C37 155.5(3) . . . . ?
C44 C43 P3 Pd2 -78.3(3) . . . . ?
C44 C45 C46 C47 -1.0(5) . . . . ?
C45 C46 C47 C48 1.0(5) . . . . ?
C46 C47 C48 C43 -0.3(5) . . . . ?
C48 C43 C44 C45 0.2(5) . . . . ?
C48 C43 P3 C31 -136.7(3) . . . . ?
C48 C43 P3 C37 -25.4(3) . . . . ?
C48 C43 P3 Pd2 100.8(3) . . . . ?
C49 C50 C51 C52 0.8(6) . . . . ?
C50 C49 C54 C53 -0.8(5) . . . . ?
C50 C49 P4 C55 173.1(3) . . . . ?
C50 C49 P4 Pd2 38.8(3) . . . . ?
C50 C49 P4 Pd3 -55.4(3) . . . . ?
C50 C51 C52 C53 -0.4(6) . . . . ?
C51 C52 C53 C54 -0.6(6) . . . . ?
C52 C53 C54 C49 1.2(6) . . . . ?
C54 C49 C50 C51 -0.2(5) . . . . ?
C54 C49 P4 C55 -7.5(3) . . . . ?
C54 C49 P4 Pd2 -141.9(3) . . . . ?
C54 C49 P4 Pd3 124.0(3) . . . . ?
C55 C56 C57 C58 -1.4(6) . . . . ?
C56 C55 C60 C59 -0.4(5) . . . . ?
C56 C55 P4 C49 -55.7(3) . . . . ?
C56 C55 P4 Pd2 79.2(3) . . . . ?
C56 C55 P4 Pd3 172.0(2) . . . . ?
C56 C57 C58 C59 -0.9(6) . . . . ?
C57 C58 C59 C60 2.5(6) . . . . ?
C58 C59 C60 C55 -1.8(6) . . . . ?
C60 C55 C56 C57 2.0(5) . . . . ?
C60 C55 P4 C49 132.6(3) . . . . ?
C60 C55 P4 Pd2 -92.5(3) . . . . ?
C60 C55 P4 Pd3 0.3(3) . . . . ?
C61 C62 C63 C64 -1.1(7) . . . . ?
C62 C61 C66 C65 -2.4(6) . . . . ?
C62 C61 P5 C67 97.0(3) . . . . ?
C62 C61 P5 C73 -156.1(3) . . . . ?
C62 C61 P5 Pd3 -31.8(3) . . . . ?
C62 C63 C64 C65 -0.7(7) . . . . ?
C63 C64 C65 C66 0.9(7) . . . . ?
C64 C65 C66 C61 0.7(7) . . . . ?
C66 C61 C62 C63 2.6(6) . . . . ?
C66 C61 P5 C67 -84.8(3) . . . . ?
C66 C61 P5 C73 22.2(4) . . . . ?
C66 C61 P5 Pd3 146.5(3) . . . . ?
C67 C68 C69 C70 0.8(6) . . . . ?
C68 C67 C72 C71 2.0(5) . . . . ?
C68 C67 P5 C61 -14.0(3) . . . . ?
C68 C67 P5 C73 -123.4(3) . . . . ?
C68 C67 P5 Pd3 103.1(3) . . . . ?
C68 C69 C70 C71 0.9(7) . . . . ?
C69 C70 C71 C72 -1.1(6) . . . . ?
C70 C71 C72 C67 -0.3(6) . . . . ?
C72 C67 C68 C69 -2.2(6) . . . . ?
C72 C67 P5 C61 165.2(3) . . . . ?
C72 C67 P5 C73 55.8(3) . . . . ?
C72 C67 P5 Pd3 -77.7(3) . . . . ?
C73 C74 C75 C76 -0.6(5) . . . . ?
C74 C73 C78 C77 -2.4(5) . . . . ?
C74 C73 P5 C61 103.4(3) . . . . ?
C74 C73 P5 C67 -147.9(3) . . . . ?
C74 C73 P5 Pd3 -11.9(3) . . . . ?
C74 C75 C76 C77 -0.5(6) . . . . ?
C75 C76 C77 C78 0.1(6) . . . . ?
C76 C77 C78 C73 1.3(5) . . . . ?
C78 C73 C74 C75 2.0(5) . . . . ?
C78 C73 P5 C61 -72.6(3) . . . . ?
C78 C73 P5 C67 36.0(3) . . . . ?
C78 C73 P5 Pd3 172.0(2) . . . . ?
P1 C1 C2 C3 179.2(3) . . . . ?
P1 C1 C6 C5 -179.9(3) . . . . ?
P1 C7 C8 C9 -179.4(3) . . . . ?
P1 C7 C12 C11 -179.8(4) . . . . ?
P1 C13 C14 C15 179.6(3) . . . . ?
P1 C13 C18 C17 -178.7(3) . . . . ?
P2 C19 C20 C21 171.3(3) . . . . ?
P2 C19 C24 C23 -170.0(3) . . . . ?
P2 C25 C26 C27 -177.5(3) . . . . ?
P2 C25 C30 C29 177.2(3) . . . . ?
P3 C31 C32 C33 176.2(3) . . . . ?
P3 C31 C36 C35 -176.2(3) . . . . ?
P3 C37 C38 C39 -177.9(3) . . . . ?
P3 C37 C42 C41 179.4(3) . . . . ?
P3 C43 C44 C45 179.3(3) . . . . ?
P3 C43 C48 C47 -179.3(3) . . . . ?
P4 C49 C50 C51 179.2(3) . . . . ?
P4 C49 C54 C53 179.8(3) . . . . ?
P4 C55 C56 C57 -169.8(3) . . . . ?
P4 C55 C60 C59 171.5(3) . . . . ?
P5 C61 C62 C63 -179.1(3) . . . . ?
P5 C61 C66 C65 179.4(3) . . . . ?
P5 C67 C68 C69 177.0(3) . . . . ?
P5 C67 C72 C71 -177.2(3) . . . . ?
P5 C73 C74 C75 -174.2(3) . . . . ?
P5 C73 C78 C77 173.7(3) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.500 416.8 105.9 '2 highly-disordered chloroforms'
2 -0.062 0.385 0.847 12.5 0.0 ?
3 0.062 0.615 0.153 12.5 0.0 ?
4 0.500 0.500 0.000 416.8 105.9 '2 highly-disordered chloroforms'
5 0.438 0.115 0.347 12.5 0.0 ?
6 0.562 0.885 0.653 12.5 0.5 ?

_olex2_date_sample_data_collection 2018-02-01
_olex2_date_sample_submission    2018-01-30
_olex2_exptl_crystal_mounting_method 
'hydrocarbon oil on 200 micrometre micromount'
_olex2_submission_original_sample_id NWJS-3-175
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.861

###end
####################################################################### 
# 
# 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_ijsf1817
_database_code_depnum_ccdc_archive 'CCDC 1894929'
loop_
_audit_author_name
_audit_author_address
'Adrian C Whitwood'
;University of York
United Kingdom
;
_audit_update_record             
;
2019-01-31 deposited with the CCDC.	2019-07-05 downloaded from the CCDC.
;
_audit_creation_date             2019-01-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C50 H43 O2 P3 Pd2, C4 H8 O'
_chemical_formula_sum            'C54 H51 O3 P3 Pd2'
_chemical_formula_weight         1053.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C54 H51 O3 P3 Pd2'
_chemical_oxdiff_usercomment     'Neil Scott NWJS-3-246-crystal1'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.8269(2)
_cell_length_b                   29.4867(5)
_cell_length_c                   14.1794(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.7289(19)
_cell_angle_gamma                90
_cell_volume                     4683.01(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7773
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      71.0530
_cell_measurement_theta_min      3.5840
_shelx_estimated_absorpt_T_max   0.877
_shelx_estimated_absorpt_T_min   0.248
_exptl_absorpt_coefficient_mu    7.503
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.0112
-1 0 0 0.0072
0 0 -1 0.1194
0 0 1 0.1194
0 1 0 0.0467
0 -1 0 0.0467
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.018
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0018 -0.0155 0.0018 0.1253 0.0327 -0.0472
-1.0018 0.0155 -0.0018 -0.1253 -0.0327 0.0472
0.0014 0.0040 -1.0010 -0.0617 0.0962 0.0104
-0.0014 -0.0040 1.0010 0.0617 -0.0962 -0.0104
0.0017 0.9996 0.0001 0.0170 0.0056 0.0491
-0.0017 -0.9996 -0.0001 -0.0170 -0.0056 -0.0491

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17077
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.078
_diffrn_reflns_theta_max         67.078
_diffrn_reflns_theta_min         3.617
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  18.00   1.00    1.00    --    0.00  57.00-180.00   38
  2  ω     24.00  51.00   1.00    1.00    --    0.00  57.00-180.00   27
  3  ω    -16.00  55.00   1.00    1.00    --    0.00  57.00  90.00   71
  4  ω    -15.00  50.00   1.00    3.00    --   54.00 -57.00-150.00   65
  5  ω    -12.00  69.00   1.00    3.00    --   54.00 -57.00 120.00   81
  6  ω     71.00 123.00   1.00    3.00    --   54.00  57.00 -90.00   52
  7  ω     48.00  83.00   1.00    3.00    --   54.00 -99.00-180.00   35
  8  ω     21.00  81.00   1.00    3.00    --   54.00 -77.00 -90.00   60
  9  ω    118.00 172.00   1.00    3.00    --  108.00 111.00-120.00   54
 10  ω    109.00 134.00   1.00    3.00    --  108.00 -37.00 120.00   25
 11  ω     49.00  78.00   1.00    3.00    --  108.00 -37.00 120.00   29
 12  ω     38.00 122.00   1.00    3.00    --  108.00 -50.00 120.00   84
 13  ω     40.00 126.00   1.00    3.00    --  108.00 -37.00 -60.00   86
 14  ω     44.00  79.00   1.00    3.00    --  108.00-111.00 -30.00   35
 15  ω     89.00 176.00   1.00    3.00    --  108.00  63.00 -90.00   87
 16  ω     65.00 132.00   1.00    3.00    --  108.00 -77.00 -60.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1252616000
_diffrn_orient_matrix_UB_12      0.0167507000
_diffrn_orient_matrix_UB_13      0.0619243000
_diffrn_orient_matrix_UB_21      0.0328977000
_diffrn_orient_matrix_UB_22      0.0055497000
_diffrn_orient_matrix_UB_23      -0.0960565000
_diffrn_orient_matrix_UB_31      -0.0463042000
_diffrn_orient_matrix_UB_32      0.0491710000
_diffrn_orient_matrix_UB_33      -0.0102082000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7242
_reflns_number_total             8345
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.000044(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8345
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0301P)²+2.0234P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0684
_refine_special_details          
;
The THF exhibited some disorder but attempts to model it in more
than one position were unsuccessful i producing a reasonable structure. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3A-C54A \\sim O3A-C51A
 with sigma of 0.02
 C53A-C54A \\sim C51A-C52A
 with sigma of 0.02
 O3A-C52A \\sim O3A-C53A
 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C51A(H51A,H51B), C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A,H54B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
  C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.7332(2) 0.41603(10) 0.8043(2) 0.0177(6) Uani 1 1 d . . . . .
C2 C 0.8584(3) 0.39613(11) 0.8385(3) 0.0300(7) Uani 1 1 d . . . . .
H2A H 0.887842 0.393648 0.781549 0.045 Uiso 1 1 calc GR . . . .
H2B H 0.856496 0.365971 0.867028 0.045 Uiso 1 1 calc GR . . . .
H2C H 0.911486 0.415940 0.889076 0.045 Uiso 1 1 calc GR . . . .
C3 C 0.2743(2) 0.48356(9) 0.8007(2) 0.0160(6) Uani 1 1 d . . . . .
C4 C 0.3408(2) 0.49374(9) 0.8990(2) 0.0175(6) Uani 1 1 d . . . . .
H4 H 0.425238 0.495974 0.917392 0.021 Uiso 1 1 calc R . . . .
C5 C 0.2851(3) 0.50060(10) 0.9700(2) 0.0213(6) Uani 1 1 d . . . . .
H5 H 0.331282 0.507735 1.036592 0.026 Uiso 1 1 calc R . . . .
C6 C 0.1625(3) 0.49711(10) 0.9443(2) 0.0239(7) Uani 1 1 d . . . . .
H6 H 0.124450 0.502051 0.993097 0.029 Uiso 1 1 calc R . . . .
C7 C 0.0947(3) 0.48639(11) 0.8472(2) 0.0264(7) Uani 1 1 d . . . . .
H7 H 0.010404 0.483758 0.829698 0.032 Uiso 1 1 calc R . . . .
C8 C 0.1503(3) 0.47953(10) 0.7758(2) 0.0223(7) Uani 1 1 d . . . . .
H8 H 0.103830 0.472049 0.709484 0.027 Uiso 1 1 calc R . . . .
C9 C 0.2620(2) 0.49115(10) 0.5933(2) 0.0159(6) Uani 1 1 d . . . . .
C10 C 0.1768(3) 0.52518(11) 0.5761(2) 0.0241(7) Uani 1 1 d . . . . .
H10 H 0.156445 0.537801 0.630174 0.029 Uiso 1 1 calc R . . . .
C11 C 0.1214(3) 0.54082(12) 0.4799(2) 0.0312(8) Uani 1 1 d . . . . .
H11 H 0.062532 0.563944 0.468120 0.037 Uiso 1 1 calc R . . . .
C12 C 0.1516(3) 0.52281(13) 0.4014(2) 0.0329(8) Uani 1 1 d . . . . .
H12 H 0.114669 0.534130 0.336019 0.039 Uiso 1 1 calc R . . . .
C13 C 0.2348(3) 0.48861(12) 0.4170(2) 0.0297(8) Uani 1 1 d . . . . .
H13 H 0.254603 0.476127 0.362530 0.036 Uiso 1 1 calc R . . . .
C14 C 0.2894(3) 0.47256(11) 0.5125(2) 0.0227(7) Uani 1 1 d . . . . .
H14 H 0.346112 0.448680 0.523293 0.027 Uiso 1 1 calc R . . . .
C15 C 0.4742(2) 0.59233(9) 0.8459(2) 0.0153(6) Uani 1 1 d . . . . .
C16 C 0.5266(3) 0.59881(9) 0.9489(2) 0.0185(6) Uani 1 1 d . . . . .
H16 H 0.610319 0.595029 0.978827 0.022 Uiso 1 1 calc R . . . .
C17 C 0.4565(3) 0.61075(10) 1.0073(2) 0.0225(7) Uani 1 1 d . . . . .
H17 H 0.492634 0.615159 1.076876 0.027 Uiso 1 1 calc R . . . .
C18 C 0.3351(3) 0.61619(10) 0.9647(2) 0.0230(7) Uani 1 1 d . . . . .
H18 H 0.287597 0.624070 1.005012 0.028 Uiso 1 1 calc R . . . .
C19 C 0.2819(3) 0.61019(10) 0.8630(2) 0.0229(7) Uani 1 1 d . . . . .
H19 H 0.198219 0.614332 0.833664 0.028 Uiso 1 1 calc R . . . .
C20 C 0.3507(3) 0.59814(9) 0.8040(2) 0.0181(6) Uani 1 1 d . . . . .
H20 H 0.313648 0.593794 0.734464 0.022 Uiso 1 1 calc R . . . .
C21 C 0.4969(2) 0.59630(10) 0.6506(2) 0.0171(6) Uani 1 1 d . . . . .
C22 C 0.4735(3) 0.64285(10) 0.6395(2) 0.0230(7) Uani 1 1 d . . . . .
H22 H 0.490116 0.661678 0.696710 0.028 Uiso 1 1 calc R . . . .
C23 C 0.4262(3) 0.66166(11) 0.5452(2) 0.0266(7) Uani 1 1 d . . . . .
H23 H 0.411615 0.693365 0.538186 0.032 Uiso 1 1 calc R . . . .
C24 C 0.4003(3) 0.63450(11) 0.4613(2) 0.0250(7) Uani 1 1 d . . . . .
H24 H 0.367880 0.647555 0.396947 0.030 Uiso 1 1 calc R . . . .
C25 C 0.4215(3) 0.58840(11) 0.4711(2) 0.0224(7) Uani 1 1 d . . . . .
H25 H 0.402832 0.569667 0.413650 0.027 Uiso 1 1 calc R . . . .
C26 C 0.4704(2) 0.56934(10) 0.5659(2) 0.0182(6) Uani 1 1 d . . . . .
H26 H 0.485764 0.537679 0.572384 0.022 Uiso 1 1 calc R . . . .
C27 C 0.7067(2) 0.59608(10) 0.82399(19) 0.0166(6) Uani 1 1 d . . . . .
C28 C 0.7209(3) 0.64246(10) 0.8448(2) 0.0209(6) Uani 1 1 d . . . . .
H28 H 0.652737 0.661028 0.836493 0.025 Uiso 1 1 calc R . . . .
C29 C 0.8341(3) 0.66149(11) 0.8776(2) 0.0243(7) Uani 1 1 d . . . . .
H29 H 0.843062 0.693110 0.890714 0.029 Uiso 1 1 calc R . . . .
C30 C 0.9340(3) 0.63471(11) 0.8912(2) 0.0253(7) Uani 1 1 d . . . . .
H30 H 1.011265 0.648010 0.913372 0.030 Uiso 1 1 calc R . . . .
C31 C 0.9219(3) 0.58861(11) 0.8728(2) 0.0255(7) Uani 1 1 d . . . . .
H31 H 0.990658 0.570162 0.883016 0.031 Uiso 1 1 calc R . . . .
C32 C 0.8083(3) 0.56932(10) 0.8391(2) 0.0197(6) Uani 1 1 d . . . . .
H32 H 0.800023 0.537665 0.826250 0.024 Uiso 1 1 calc R . . . .
C33 C 0.2699(2) 0.32450(10) 0.7609(2) 0.0187(6) Uani 1 1 d . . . . .
C34 C 0.2468(3) 0.27878(11) 0.7713(2) 0.0269(7) Uani 1 1 d . . . . .
H34 H 0.276845 0.256594 0.736954 0.032 Uiso 1 1 calc R . . . .
C35 C 0.1801(3) 0.26520(12) 0.8314(2) 0.0353(8) Uani 1 1 d . . . . .
H35 H 0.165324 0.233918 0.838441 0.042 Uiso 1 1 calc R . . . .
C36 C 0.1356(3) 0.29754(12) 0.8807(2) 0.0334(8) Uani 1 1 d . . . . .
H36 H 0.088009 0.288461 0.920164 0.040 Uiso 1 1 calc R . . . .
C37 C 0.1599(3) 0.34304(12) 0.8730(2) 0.0297(7) Uani 1 1 d . . . . .
H37 H 0.130769 0.365088 0.908305 0.036 Uiso 1 1 calc R . . . .
C38 C 0.2269(3) 0.35630(11) 0.8139(2) 0.0221(6) Uani 1 1 d . . . . .
H38 H 0.243859 0.387546 0.809171 0.026 Uiso 1 1 calc R . . . .
C39 C 0.2316(2) 0.35183(10) 0.5590(2) 0.0176(6) Uani 1 1 d . . . . .
C40 C 0.1115(3) 0.35183(12) 0.5496(2) 0.0321(8) Uani 1 1 d . . . . .
H40 H 0.087216 0.346729 0.606458 0.038 Uiso 1 1 calc R . . . .
C41 C 0.0262(3) 0.35928(14) 0.4574(3) 0.0406(9) Uani 1 1 d . . . . .
H41 H -0.056065 0.359522 0.451637 0.049 Uiso 1 1 calc R . . . .
C42 C 0.0601(3) 0.36634(12) 0.3737(2) 0.0316(8) Uani 1 1 d . . . . .
H42 H 0.001287 0.371101 0.310723 0.038 Uiso 1 1 calc R . . . .
C43 C 0.1794(3) 0.36644(11) 0.3823(2) 0.0266(7) Uani 1 1 d . . . . .
H43 H 0.203110 0.371363 0.325200 0.032 Uiso 1 1 calc R . . . .
C44 C 0.2650(3) 0.35935(10) 0.4745(2) 0.0215(6) Uani 1 1 d . . . . .
H44 H 0.347169 0.359613 0.480108 0.026 Uiso 1 1 calc R . . . .
C45 C 0.4289(3) 0.29408(10) 0.6589(2) 0.0205(6) Uani 1 1 d . . . . .
C46 C 0.3835(3) 0.26458(10) 0.5785(2) 0.0261(7) Uani 1 1 d . . . . .
H46 H 0.307131 0.269990 0.531170 0.031 Uiso 1 1 calc R . . . .
C47 C 0.4502(3) 0.22741(11) 0.5681(3) 0.0322(8) Uani 1 1 d . . . . .
H47 H 0.419610 0.207646 0.512826 0.039 Uiso 1 1 calc R . . . .
C48 C 0.5599(3) 0.21882(12) 0.6368(3) 0.0355(8) Uani 1 1 d . . . . .
H48 H 0.604943 0.193220 0.629127 0.043 Uiso 1 1 calc R . . . .
C49 C 0.6047(3) 0.24754(12) 0.7172(3) 0.0406(9) Uani 1 1 d . . . . .
H49 H 0.679789 0.241277 0.765605 0.049 Uiso 1 1 calc R . . . .
C50 C 0.5399(3) 0.28572(11) 0.7275(3) 0.0303(7) Uani 1 1 d . . . . .
H50 H 0.572045 0.305955 0.781648 0.036 Uiso 1 1 calc R . . . .
O1 O 0.72530(16) 0.45883(7) 0.80188(14) 0.0182(4) Uani 1 1 d . . . . .
O2 O 0.64833(16) 0.38775(7) 0.78011(14) 0.0178(4) Uani 1 1 d . . . . .
P1 P 0.35699(6) 0.47217(2) 0.71521(5) 0.01441(15) Uani 1 1 d . . . . .
P2 P 0.56076(6) 0.56884(2) 0.77192(5) 0.01437(15) Uani 1 1 d . . . . .
P3 P 0.35016(6) 0.34483(2) 0.67856(5) 0.01598(15) Uani 1 1 d . . . . .
Pd1 Pd 0.54772(2) 0.49104(2) 0.76213(2) 0.01304(6) Uani 1 1 d . . . . .
Pd2 Pd 0.46246(2) 0.40930(2) 0.73031(2) 0.01367(6) Uani 1 1 d . . . . .
C51A C 0.8978(4) 0.26785(16) 1.1599(5) 0.0820(18) Uani 1 1 d D . . A 1
H51A H 0.869885 0.271638 1.218167 0.098 Uiso 1 1 calc R . . A 1
H51B H 0.984947 0.273395 1.181120 0.098 Uiso 1 1 calc R . . A 1
C52A C 0.8692(5) 0.22102(16) 1.1167(5) 0.0848(18) Uani 1 1 d D . . A 1
H52A H 0.795419 0.209073 1.126278 0.102 Uiso 1 1 calc R . . A 1
H52B H 0.935730 0.199712 1.146687 0.102 Uiso 1 1 calc R . . A 1
C53A C 0.8523(5) 0.22906(17) 1.0073(5) 0.094(2) Uani 1 1 d D . . A 1
H53A H 0.929751 0.231089 0.994613 0.113 Uiso 1 1 calc R . . A 1
H53B H 0.802740 0.205119 0.964716 0.113 Uiso 1 1 calc R . . A 1
C54A C 0.7893(4) 0.27361(16) 0.9924(4) 0.0773(17) Uani 1 1 d D . . A 1
H54A H 0.802996 0.290276 0.936376 0.093 Uiso 1 1 calc R . . A 1
H54B H 0.702350 0.269060 0.977194 0.093 Uiso 1 1 calc R . . A 1
O3A O 0.8368(3) 0.29822(11) 1.0824(3) 0.0915(14) Uani 1 1 d D . . A 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.520(4) . ?
C1 O1 1.265(3) . ?
C1 O2 1.264(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.396(4) . ?
C3 C8 1.399(4) . ?
C3 P1 1.816(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.384(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.381(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.387(4) . ?
C9 C14 1.399(4) . ?
C9 P1 1.821(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.389(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.380(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.376(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.404(4) . ?
C15 C20 1.399(4) . ?
C15 P2 1.821(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.392(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.388(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(4) . ?
C21 C26 1.390(4) . ?
C21 P2 1.830(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.389(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.385(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.381(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.399(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.398(4) . ?
C27 C32 1.396(4) . ?
C27 P2 1.831(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.382(4) . ?
C30 H30 0.9500 . ?
C30 C31 1.383(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.394(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.393(4) . ?
C33 C38 1.395(4) . ?
C33 P3 1.827(3) . ?
C34 H34 0.9500 . ?
C34 C35 1.393(4) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(5) . ?
C36 H36 0.9500 . ?
C36 C37 1.384(5) . ?
C37 H37 0.9500 . ?
C37 C38 1.382(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.384(4) . ?
C39 C44 1.394(4) . ?
C39 P3 1.832(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.389(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.384(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.377(4) . ?
C43 H43 0.9500 . ?
C43 C44 1.388(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.397(4) . ?
C45 C50 1.382(4) . ?
C45 P3 1.831(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.386(4) . ?
C47 H47 0.9500 . ?
C47 C48 1.374(5) . ?
C48 H48 0.9500 . ?
C48 C49 1.381(5) . ?
C49 H49 0.9500 . ?
C49 C50 1.396(5) . ?
C50 H50 0.9500 . ?
O1 Pd1 2.2070(19) . ?
O2 Pd2 2.1766(18) . ?
P1 Pd1 2.2083(7) . ?
P1 Pd2 2.2062(7) . ?
P2 Pd1 2.3003(7) . ?
P3 Pd2 2.2999(7) . ?
Pd1 Pd2 2.5958(3) . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C51A C52A 1.504(6) . ?
C51A O3A 1.421(6) . ?
C52A H52A 0.9900 . ?
C52A H52B 0.9900 . ?
C52A C53A 1.517(8) . ?
C53A H53A 0.9900 . ?
C53A H53B 0.9900 . ?
C53A C54A 1.492(6) . ?
C54A H54A 0.9900 . ?
C54A H54B 0.9900 . ?
C54A O3A 1.419(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 116.7(3) . . ?
O2 C1 C2 116.0(3) . . ?
O2 C1 O1 127.3(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 C8 118.6(3) . . ?
C4 C3 P1 117.1(2) . . ?
C8 C3 P1 124.1(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.1(3) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.1(3) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 120.1 . . ?
C8 C7 C6 119.9(3) . . ?
C8 C7 H7 120.1 . . ?
C3 C8 H8 119.8 . . ?
C7 C8 C3 120.5(3) . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C14 119.1(3) . . ?
C10 C9 P1 125.5(2) . . ?
C14 C9 P1 115.0(2) . . ?
C9 C10 H10 120.0 . . ?
C9 C10 C11 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11 120.0 . . ?
C11 C12 H12 119.7 . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12 119.7 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.5(3) . . ?
C14 C13 H13 120.2 . . ?
C9 C14 H14 119.7 . . ?
C13 C14 C9 120.6(3) . . ?
C13 C14 H14 119.7 . . ?
C16 C15 P2 120.6(2) . . ?
C20 C15 C16 118.5(3) . . ?
C20 C15 P2 120.3(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.3(3) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.8 . . ?
C18 C17 C16 120.3(3) . . ?
C18 C17 H17 119.8 . . ?
C17 C18 H18 119.9 . . ?
C17 C18 C19 120.1(3) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.1(3) . . ?
C20 C19 H19 120.0 . . ?
C15 C20 H20 119.7 . . ?
C19 C20 C15 120.6(3) . . ?
C19 C20 H20 119.7 . . ?
C22 C21 P2 123.2(2) . . ?
C26 C21 C22 118.8(3) . . ?
C26 C21 P2 118.0(2) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.4(3) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0(3) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.1 . . ?
C24 C25 C26 119.9(3) . . ?
C26 C25 H25 120.1 . . ?
C21 C26 C25 120.6(3) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
C28 C27 P2 123.3(2) . . ?
C32 C27 C28 118.8(3) . . ?
C32 C27 P2 117.9(2) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 C27 120.3(3) . . ?
C29 C28 H28 119.9 . . ?
C28 C29 H29 119.8 . . ?
C30 C29 C28 120.4(3) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 119.9 . . ?
C29 C30 C31 120.2(3) . . ?
C31 C30 H30 119.9 . . ?
C30 C31 H31 120.1 . . ?
C30 C31 C32 119.7(3) . . ?
C32 C31 H31 120.1 . . ?
C27 C32 H32 119.7 . . ?
C31 C32 C27 120.6(3) . . ?
C31 C32 H32 119.7 . . ?
C34 C33 C38 118.4(3) . . ?
C34 C33 P3 123.0(2) . . ?
C38 C33 P3 118.5(2) . . ?
C33 C34 H34 119.6 . . ?
C35 C34 C33 120.8(3) . . ?
C35 C34 H34 119.6 . . ?
C34 C35 H35 120.2 . . ?
C36 C35 C34 119.6(3) . . ?
C36 C35 H35 120.2 . . ?
C35 C36 H36 119.8 . . ?
C35 C36 C37 120.4(3) . . ?
C37 C36 H36 119.8 . . ?
C36 C37 H37 120.1 . . ?
C38 C37 C36 119.8(3) . . ?
C38 C37 H37 120.1 . . ?
C33 C38 H38 119.5 . . ?
C37 C38 C33 121.0(3) . . ?
C37 C38 H38 119.5 . . ?
C40 C39 C44 118.8(3) . . ?
C40 C39 P3 123.1(2) . . ?
C44 C39 P3 118.0(2) . . ?
C39 C40 H40 119.9 . . ?
C39 C40 C41 120.2(3) . . ?
C41 C40 H40 119.9 . . ?
C40 C41 H41 119.7 . . ?
C42 C41 C40 120.6(3) . . ?
C42 C41 H41 119.7 . . ?
C41 C42 H42 120.2 . . ?
C43 C42 C41 119.7(3) . . ?
C43 C42 H42 120.2 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0(3) . . ?
C44 C43 H43 120.0 . . ?
C39 C44 H44 119.6 . . ?
C43 C44 C39 120.7(3) . . ?
C43 C44 H44 119.6 . . ?
C46 C45 P3 123.5(2) . . ?
C50 C45 C46 119.5(3) . . ?
C50 C45 P3 117.0(2) . . ?
C45 C46 H46 120.1 . . ?
C47 C46 C45 119.8(3) . . ?
C47 C46 H46 120.1 . . ?
C46 C47 H47 119.6 . . ?
C48 C47 C46 120.7(3) . . ?
C48 C47 H47 119.6 . . ?
C47 C48 H48 120.1 . . ?
C47 C48 C49 119.8(3) . . ?
C49 C48 H48 120.1 . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.2(3) . . ?
C50 C49 H49 119.9 . . ?
C45 C50 C49 120.0(3) . . ?
C45 C50 H50 120.0 . . ?
C49 C50 H50 120.0 . . ?
C1 O1 Pd1 119.47(18) . . ?
C1 O2 Pd2 121.76(18) . . ?
C3 P1 C9 106.04(13) . . ?
C3 P1 Pd1 117.98(9) . . ?
C3 P1 Pd2 119.96(9) . . ?
C9 P1 Pd1 117.89(9) . . ?
C9 P1 Pd2 120.50(9) . . ?
Pd2 P1 Pd1 72.03(2) . . ?
C15 P2 C21 103.53(13) . . ?
C15 P2 C27 103.43(13) . . ?
C15 P2 Pd1 112.02(9) . . ?
C21 P2 C27 103.66(13) . . ?
C21 P2 Pd1 112.64(10) . . ?
C27 P2 Pd1 119.88(10) . . ?
C33 P3 C39 103.16(13) . . ?
C33 P3 C45 102.89(13) . . ?
C33 P3 Pd2 115.65(10) . . ?
C39 P3 Pd2 113.22(10) . . ?
C45 P3 C39 103.13(13) . . ?
C45 P3 Pd2 117.02(10) . . ?
O1 Pd1 P1 139.88(6) . . ?
O1 Pd1 P2 111.96(5) . . ?
O1 Pd1 Pd2 85.95(5) . . ?
P1 Pd1 P2 108.16(3) . . ?
P1 Pd1 Pd2 53.945(19) . . ?
P2 Pd1 Pd2 162.04(2) . . ?
O2 Pd2 P1 139.23(6) . . ?
O2 Pd2 P3 106.37(5) . . ?
O2 Pd2 Pd1 85.36(5) . . ?
P1 Pd2 P3 114.39(3) . . ?
P1 Pd2 Pd1 54.023(19) . . ?
P3 Pd2 Pd1 167.21(2) . . ?
H51A C51A H51B 108.7 . . ?
C52A C51A H51A 110.6 . . ?
C52A C51A H51B 110.6 . . ?
O3A C51A H51A 110.6 . . ?
O3A C51A H51B 110.6 . . ?
O3A C51A C52A 105.8(5) . . ?
C51A C52A H52A 111.3 . . ?
C51A C52A H52B 111.3 . . ?
C51A C52A C53A 102.2(5) . . ?
H52A C52A H52B 109.2 . . ?
C53A C52A H52A 111.3 . . ?
C53A C52A H52B 111.3 . . ?
C52A C53A H53A 111.7 . . ?
C52A C53A H53B 111.7 . . ?
H53A C53A H53B 109.5 . . ?
C54A C53A C52A 100.3(5) . . ?
C54A C53A H53A 111.7 . . ?
C54A C53A H53B 111.7 . . ?
C53A C54A H54A 110.4 . . ?
C53A C54A H54B 110.4 . . ?
H54A C54A H54B 108.6 . . ?
O3A C54A C53A 106.7(5) . . ?
O3A C54A H54A 110.4 . . ?
O3A C54A H54B 110.4 . . ?
C54A O3A C51A 109.2(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 C1 O1 Pd1 -176.26(19) . . . . ?
C2 C1 O2 Pd2 179.47(18) . . . . ?
C3 C4 C5 C6 0.5(4) . . . . ?
C4 C3 C8 C7 1.2(5) . . . . ?
C4 C3 P1 C9 -149.1(2) . . . . ?
C4 C3 P1 Pd1 -14.4(3) . . . . ?
C4 C3 P1 Pd2 70.1(2) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C8 -0.5(5) . . . . ?
C6 C7 C8 C3 -0.3(5) . . . . ?
C8 C3 C4 C5 -1.3(4) . . . . ?
C8 C3 P1 C9 35.7(3) . . . . ?
C8 C3 P1 Pd1 170.4(2) . . . . ?
C8 C3 P1 Pd2 -105.1(2) . . . . ?
C9 C10 C11 C12 -0.6(5) . . . . ?
C10 C9 C14 C13 1.6(5) . . . . ?
C10 C9 P1 C3 27.6(3) . . . . ?
C10 C9 P1 Pd1 -107.2(3) . . . . ?
C10 C9 P1 Pd2 168.2(2) . . . . ?
C10 C11 C12 C13 1.4(5) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C12 C13 C14 C9 -0.8(5) . . . . ?
C14 C9 C10 C11 -0.9(5) . . . . ?
C14 C9 P1 C3 -160.0(2) . . . . ?
C14 C9 P1 Pd1 65.3(2) . . . . ?
C14 C9 P1 Pd2 -19.4(3) . . . . ?
C15 C16 C17 C18 0.2(4) . . . . ?
C16 C15 C20 C19 0.2(4) . . . . ?
C16 C15 P2 C21 -147.9(2) . . . . ?
C16 C15 P2 C27 -40.0(3) . . . . ?
C16 C15 P2 Pd1 90.5(2) . . . . ?
C16 C17 C18 C19 -0.6(5) . . . . ?
C17 C18 C19 C20 0.8(5) . . . . ?
C18 C19 C20 C15 -0.6(4) . . . . ?
C20 C15 C16 C17 0.0(4) . . . . ?
C20 C15 P2 C21 41.2(3) . . . . ?
C20 C15 P2 C27 149.1(2) . . . . ?
C20 C15 P2 Pd1 -80.4(2) . . . . ?
C21 C22 C23 C24 0.8(5) . . . . ?
C22 C21 C26 C25 0.0(4) . . . . ?
C22 C21 P2 C15 46.2(3) . . . . ?
C22 C21 P2 C27 -61.5(3) . . . . ?
C22 C21 P2 Pd1 167.4(2) . . . . ?
C22 C23 C24 C25 0.0(5) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C24 C25 C26 C21 0.7(4) . . . . ?
C26 C21 C22 C23 -0.8(4) . . . . ?
C26 C21 P2 C15 -133.7(2) . . . . ?
C26 C21 P2 C27 118.5(2) . . . . ?
C26 C21 P2 Pd1 -12.5(2) . . . . ?
C27 C28 C29 C30 -0.9(4) . . . . ?
C28 C27 C32 C31 -1.0(4) . . . . ?
C28 C27 P2 C15 -45.6(3) . . . . ?
C28 C27 P2 C21 62.2(3) . . . . ?
C28 C27 P2 Pd1 -171.14(19) . . . . ?
C28 C29 C30 C31 -0.3(4) . . . . ?
C29 C30 C31 C32 0.8(4) . . . . ?
C30 C31 C32 C27 -0.2(4) . . . . ?
C32 C27 C28 C29 1.5(4) . . . . ?
C32 C27 P2 C15 137.5(2) . . . . ?
C32 C27 P2 C21 -114.7(2) . . . . ?
C32 C27 P2 Pd1 11.9(2) . . . . ?
C33 C34 C35 C36 0.5(5) . . . . ?
C34 C33 C38 C37 -1.9(4) . . . . ?
C34 C33 P3 C39 87.5(3) . . . . ?
C34 C33 P3 C45 -19.5(3) . . . . ?
C34 C33 P3 Pd2 -148.3(2) . . . . ?
C34 C35 C36 C37 -1.9(5) . . . . ?
C35 C36 C37 C38 1.5(5) . . . . ?
C36 C37 C38 C33 0.5(5) . . . . ?
C38 C33 C34 C35 1.4(4) . . . . ?
C38 C33 P3 C39 -90.7(2) . . . . ?
C38 C33 P3 C45 162.3(2) . . . . ?
C38 C33 P3 Pd2 33.4(3) . . . . ?
C39 C40 C41 C42 0.6(6) . . . . ?
C40 C39 C44 C43 -0.4(5) . . . . ?
C40 C39 P3 C33 14.0(3) . . . . ?
C40 C39 P3 C45 120.8(3) . . . . ?
C40 C39 P3 Pd2 -111.7(3) . . . . ?
C40 C41 C42 C43 -0.7(6) . . . . ?
C41 C42 C43 C44 0.2(5) . . . . ?
C42 C43 C44 C39 0.3(5) . . . . ?
C44 C39 C40 C41 -0.1(5) . . . . ?
C44 C39 P3 C33 -168.7(2) . . . . ?
C44 C39 P3 C45 -61.9(3) . . . . ?
C44 C39 P3 Pd2 65.6(2) . . . . ?
C45 C46 C47 C48 0.9(5) . . . . ?
C46 C45 C50 C49 -1.3(5) . . . . ?
C46 C45 P3 C33 93.6(3) . . . . ?
C46 C45 P3 C39 -13.4(3) . . . . ?
C46 C45 P3 Pd2 -138.4(2) . . . . ?
C46 C47 C48 C49 -0.1(5) . . . . ?
C47 C48 C49 C50 -1.4(5) . . . . ?
C48 C49 C50 C45 2.1(5) . . . . ?
C50 C45 C46 C47 -0.2(5) . . . . ?
C50 C45 P3 C33 -87.5(3) . . . . ?
C50 C45 P3 C39 165.5(2) . . . . ?
C50 C45 P3 Pd2 40.5(3) . . . . ?
O1 C1 O2 Pd2 -1.5(4) . . . . ?
O2 C1 O1 Pd1 4.7(4) . . . . ?
P1 C3 C4 C5 -176.7(2) . . . . ?
P1 C3 C8 C7 176.3(2) . . . . ?
P1 C9 C10 C11 171.2(2) . . . . ?
P1 C9 C14 C13 -171.3(2) . . . . ?
P2 C15 C16 C17 -171.0(2) . . . . ?
P2 C15 C20 C19 171.3(2) . . . . ?
P2 C21 C22 C23 179.2(2) . . . . ?
P2 C21 C26 C25 -180.0(2) . . . . ?
P2 C27 C28 C29 -175.4(2) . . . . ?
P2 C27 C32 C31 176.1(2) . . . . ?
P3 C33 C34 C35 -176.9(2) . . . . ?
P3 C33 C38 C37 176.5(2) . . . . ?
P3 C39 C40 C41 177.2(3) . . . . ?
P3 C39 C44 C43 -177.8(2) . . . . ?
P3 C45 C46 C47 178.6(2) . . . . ?
P3 C45 C50 C49 179.8(3) . . . . ?
C51A C52A C53A C54A -38.6(5) . . . . ?
C52A C51A O3A C54A -8.9(6) . . . . ?
C52A C53A C54A O3A 34.6(5) . . . . ?
C53A C54A O3A C51A -16.8(6) . . . . ?
O3A C51A C52A C53A 30.2(5) . . . . ?

_olex2_date_sample_data_collection 2018-07-18
_olex2_date_sample_submission    2018-07-16
_olex2_exptl_crystal_mounting_method 'oil on 100 micrometre micromount'
_olex2_submission_original_sample_id NWJS-3-246-crystal1
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.281
_oxdiff_exptl_absorpt_empirical_full_min 0.811
