# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_dmda150706
_database_code_depnum_ccdc_archive 'CCDC 2163655'
loop_
_audit_author_name
_audit_author_address
'Corinne Bailly'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT990_dmda150706          
;
PROBLEM: Deprecated .res/.hkl Input Style SQUEEZE Job ...          ! Note
RESPONSE: A squeeze procedure has been performed. The residual electronic density is due to a butanone solvent molecule.
;
# Added during the CSD deposition process: Thursday 31 March 2022 10:26 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H100 Cl2 N O28 P Pd, C4 H8 O'
_chemical_formula_sum            'C64 H108 Cl2 N O29 P Pd'
_chemical_formula_weight         1563.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   14.9237(6)
_cell_length_b                   17.5343(7)
_cell_length_c                   15.7250(6)
_cell_angle_alpha                90
_cell_angle_beta                 101.0630(10)
_cell_angle_gamma                90
_cell_volume                     4038.4(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6394
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      23.48

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_F_000             1652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.391
_shelx_estimated_absorpt_T_min   0.909
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7057
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  triumph
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39896
_diffrn_reflns_av_unetI/netI     0.0849
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.723
_diffrn_reflns_theta_max         28.021
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_point_group_measured_fraction_full 0.971
_reflns_number_total             18579
_reflns_number_gt                13244
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_max     0.898
_reflns_Friedel_fraction_full    0.939

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0437P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4721 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(11)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         18579
_refine_ls_number_parameters     897
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0478
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0893
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.955
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5086(3) 0.2734(3) 0.2181(3) 0.0254(11) Uani 1 1 d . . . . .
H1 H 0.5197 0.3049 0.1681 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5973(3) 0.2680(3) 0.2846(3) 0.0261(12) Uani 1 1 d . . . . .
H2 H 0.6179 0.3207 0.3032 0.031 Uiso 1 1 calc R U . . .
C3 C 0.5810(3) 0.2244(3) 0.3622(3) 0.0263(11) Uani 1 1 d . . . . .
H3 H 0.5691 0.1697 0.3457 0.032 Uiso 1 1 calc R U . . .
C4 C 0.5006(3) 0.2554(3) 0.3980(3) 0.0268(10) Uani 1 1 d . . . . .
H4 H 0.5191 0.3047 0.4282 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4152(3) 0.2695(3) 0.3274(3) 0.0251(11) Uani 1 1 d . . . . .
H5 H 0.3864 0.2198 0.3061 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3427(3) 0.3232(3) 0.3547(3) 0.0266(11) Uani 1 1 d . . . . .
H6A H 0.3362 0.3673 0.3146 0.032 Uiso 1 1 calc R U . . .
H6B H 0.3698 0.3431 0.4128 0.032 Uiso 1 1 calc R U . . .
C7 C 0.7089(4) 0.2749(3) 0.1948(4) 0.0412(15) Uani 1 1 d . . . . .
H7A H 0.6628 0.2864 0.1431 0.062 Uiso 1 1 calc R U . . .
H7B H 0.7591 0.2461 0.1779 0.062 Uiso 1 1 calc R U . . .
H7C H 0.7326 0.3226 0.2229 0.062 Uiso 1 1 calc R U . . .
C8 C 0.6943(4) 0.1575(4) 0.4637(4) 0.061(2) Uani 1 1 d . . . . .
H8A H 0.6496 0.1335 0.4935 0.091 Uiso 1 1 calc R U . . .
H8B H 0.7518 0.1652 0.5048 0.091 Uiso 1 1 calc R U . . .
H8C H 0.7050 0.1244 0.4164 0.091 Uiso 1 1 calc R U . . .
C11 C 0.4663(3) 0.2297(3) 0.5380(3) 0.0354(14) Uani 1 1 d . . . . .
H11 H 0.5080 0.2735 0.5578 0.042 Uiso 1 1 calc R U . . .
C12 C 0.4805(4) 0.1676(4) 0.6072(3) 0.0410(15) Uani 1 1 d . . . . .
H12 H 0.4736 0.1912 0.6635 0.049 Uiso 1 1 calc R U . . .
C13 C 0.4095(3) 0.1037(3) 0.5860(3) 0.0307(12) Uani 1 1 d . . . . .
H13 H 0.4225 0.0738 0.5356 0.037 Uiso 1 1 calc R U . . .
C14 C 0.3129(3) 0.1359(3) 0.5632(3) 0.0262(11) Uani 1 1 d . . . . .
H14 H 0.2960 0.1605 0.6153 0.031 Uiso 1 1 calc R U . . .
C15 C 0.3110(3) 0.1950(3) 0.4912(3) 0.0255(11) Uani 1 1 d . . . . .
H15 H 0.3324 0.1707 0.4411 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2216(3) 0.2370(3) 0.4585(3) 0.0297(12) Uani 1 1 d . . . . .
H16A H 0.2089 0.2720 0.5043 0.036 Uiso 1 1 calc R U . . .
H16B H 0.1710 0.1997 0.4460 0.036 Uiso 1 1 calc R U . . .
C17 C 0.6196(6) 0.1342(8) 0.6983(7) 0.136(5) Uani 1 1 d . . . . .
H17A H 0.6104 0.1811 0.7295 0.205 Uiso 1 1 calc R U . . .
H17B H 0.6844 0.1292 0.6954 0.205 Uiso 1 1 calc R U . . .
H17C H 0.6005 0.0902 0.7288 0.205 Uiso 1 1 calc R U . . .
C18 C 0.4408(5) -0.0213(4) 0.6420(4) 0.0558(18) Uani 1 1 d . . . . .
H18A H 0.3905 -0.0443 0.6007 0.084 Uiso 1 1 calc R U . . .
H18B H 0.4514 -0.0507 0.6960 0.084 Uiso 1 1 calc R U . . .
H18C H 0.4963 -0.0216 0.6173 0.084 Uiso 1 1 calc R U . . .
C21 C 0.1698(3) 0.0707(3) 0.5661(3) 0.0249(11) Uani 1 1 d . . . . .
H21 H 0.1748 0.1054 0.6173 0.030 Uiso 1 1 calc R U . . .
C22 C 0.1501(3) -0.0102(3) 0.5942(3) 0.0243(11) Uani 1 1 d . . . . .
H22 H 0.0967 -0.0077 0.6240 0.029 Uiso 1 1 calc R U . . .
C23 C 0.1261(3) -0.0645(3) 0.5181(3) 0.0254(11) Uani 1 1 d . . . . .
H23 H 0.1835 -0.0801 0.4988 0.030 Uiso 1 1 calc R U . . .
C24 C 0.0603(3) -0.0310(3) 0.4413(3) 0.0218(10) Uani 1 1 d . . . . .
H24 H -0.0034 -0.0326 0.4527 0.026 Uiso 1 1 calc R U . . .
C25 C 0.0859(3) 0.0515(3) 0.4230(3) 0.0214(10) Uani 1 1 d . . . . .
H25 H 0.1456 0.0510 0.4030 0.026 Uiso 1 1 calc R U . . .
C26 C 0.0163(3) 0.0925(3) 0.3558(3) 0.0273(11) Uani 1 1 d . . . . .
H26A H 0.0354 0.1462 0.3512 0.033 Uiso 1 1 calc R U . . .
H26B H 0.0133 0.0680 0.2986 0.033 Uiso 1 1 calc R U . . .
C27 C 0.2400(4) -0.0096(4) 0.7355(3) 0.0451(15) Uani 1 1 d . . . . .
H27A H 0.2615 0.0428 0.7316 0.068 Uiso 1 1 calc R U . . .
H27B H 0.2863 -0.0391 0.7746 0.068 Uiso 1 1 calc R U . . .
H27C H 0.1831 -0.0092 0.7580 0.068 Uiso 1 1 calc R U . . .
C28 C 0.1434(5) -0.1954(3) 0.5621(4) 0.0555(18) Uani 1 1 d . . . . .
H28A H 0.1660 -0.2088 0.5095 0.083 Uiso 1 1 calc R U . . .
H28B H 0.1098 -0.2386 0.5800 0.083 Uiso 1 1 calc R U . . .
H28C H 0.1952 -0.1829 0.6085 0.083 Uiso 1 1 calc R U . . .
C29 C -0.1373(4) 0.1183(4) 0.3076(4) 0.0509(17) Uani 1 1 d . . . . .
H29A H -0.1163 0.1665 0.2867 0.076 Uiso 1 1 calc R U . . .
H29B H -0.1950 0.1266 0.3272 0.076 Uiso 1 1 calc R U . . .
H29C H -0.1465 0.0808 0.2605 0.076 Uiso 1 1 calc R U . . .
C31 C -0.0141(3) -0.1072(3) 0.3177(3) 0.0253(11) Uani 1 1 d . . . . .
H31 H -0.0622 -0.1101 0.3540 0.030 Uiso 1 1 calc R U . . .
C32 C 0.0041(3) -0.1869(3) 0.2873(3) 0.0269(11) Uani 1 1 d . . . . .
H32 H -0.0545 -0.2079 0.2539 0.032 Uiso 1 1 calc R U . . .
C33 C 0.0733(3) -0.1843(3) 0.2270(3) 0.0243(10) Uani 1 1 d . . . . .
H33 H 0.1345 -0.1711 0.2623 0.029 Uiso 1 1 calc R U . . .
C34 C 0.0489(3) -0.1254(3) 0.1560(3) 0.0219(10) Uani 1 1 d . . . . .
H34 H -0.0014 -0.1453 0.1100 0.026 Uiso 1 1 calc R U . . .
C35 C 0.0202(3) -0.0495(3) 0.1902(3) 0.0231(10) Uani 1 1 d . . . . .
H35 H 0.0756 -0.0252 0.2258 0.028 Uiso 1 1 calc R U . . .
C36 C -0.0212(4) 0.0060(3) 0.1210(3) 0.0291(11) Uani 1 1 d . . . . .
H36A H -0.0420 0.0519 0.1483 0.035 Uiso 1 1 calc R U . . .
H36B H 0.0255 0.0220 0.0877 0.035 Uiso 1 1 calc R U . . .
C37 C -0.0273(4) -0.2593(4) 0.4054(4) 0.0496(16) Uani 1 1 d . . . . .
H37A H -0.0355 -0.2171 0.4440 0.074 Uiso 1 1 calc R U . . .
H37B H -0.0060 -0.3045 0.4400 0.074 Uiso 1 1 calc R U . . .
H37C H -0.0856 -0.2706 0.3670 0.074 Uiso 1 1 calc R U . . .
C38 C 0.1552(5) -0.3012(4) 0.2281(4) 0.0541(18) Uani 1 1 d . . . . .
H38A H 0.2120 -0.2759 0.2214 0.081 Uiso 1 1 calc R U . . .
H38B H 0.1519 -0.3516 0.2007 0.081 Uiso 1 1 calc R U . . .
H38C H 0.1540 -0.3069 0.2898 0.081 Uiso 1 1 calc R U . . .
C39 C -0.1419(5) 0.0290(4) 0.0069(4) 0.0552(19) Uani 1 1 d . . . . .
H39A H -0.1590 0.0720 0.0403 0.083 Uiso 1 1 calc R U . . .
H39B H -0.1969 0.0066 -0.0282 0.083 Uiso 1 1 calc R U . . .
H39C H -0.1015 0.0471 -0.0312 0.083 Uiso 1 1 calc R U . . .
C41 C 0.1227(3) -0.1258(3) 0.0306(3) 0.0271(11) Uani 1 1 d . . . . .
H41 H 0.0733 -0.1638 0.0102 0.033 Uiso 1 1 calc R U . . .
C42 C 0.2138(4) -0.1573(3) 0.0152(3) 0.0327(12) Uani 1 1 d . . . . .
H42 H 0.2061 -0.1720 -0.0473 0.039 Uiso 1 1 calc R U . . .
C43 C 0.2893(3) -0.0990(3) 0.0343(3) 0.0280(11) Uani 1 1 d . . . . .
H43 H 0.3064 -0.0915 0.0984 0.034 Uiso 1 1 calc R U . . .
C44 C 0.2620(3) -0.0226(3) -0.0088(3) 0.0260(11) Uani 1 1 d . . . . .
H44 H 0.2589 -0.0276 -0.0726 0.031 Uiso 1 1 calc R U . . .
C45 C 0.1684(3) 0.0030(3) 0.0078(3) 0.0272(11) Uani 1 1 d . . . . .
H45 H 0.1738 0.0124 0.0713 0.033 Uiso 1 1 calc R U . . .
C46 C 0.1316(4) 0.0742(3) -0.0399(3) 0.0319(12) Uani 1 1 d . . . . .
H46A H 0.0687 0.0840 -0.0309 0.038 Uiso 1 1 calc R U . . .
H46B H 0.1701 0.1184 -0.0172 0.038 Uiso 1 1 calc R U . . .
C47 C 0.2088(5) -0.2897(3) 0.0267(4) 0.0549(10) Uani 1 1 d . . . . .
H47A H 0.1420 -0.2889 0.0168 0.082 Uiso 1 1 calc R U . . .
H47B H 0.2317 -0.3329 0.0640 0.082 Uiso 1 1 calc R U . . .
H47C H 0.2287 -0.2948 -0.0289 0.082 Uiso 1 1 calc R U . . .
C48 C 0.4448(4) -0.1410(4) 0.0666(4) 0.0604(19) Uani 1 1 d . . . . .
H48A H 0.4639 -0.0937 0.0983 0.091 Uiso 1 1 calc R U . . .
H48B H 0.4944 -0.1594 0.0392 0.091 Uiso 1 1 calc R U . . .
H48C H 0.4306 -0.1797 0.1070 0.091 Uiso 1 1 calc R U . . .
C49 C 0.1073(5) 0.1339(4) -0.1753(4) 0.062(2) Uani 1 1 d . . . . .
H49A H 0.0447 0.1481 -0.1712 0.094 Uiso 1 1 calc R U . . .
H49B H 0.1112 0.1270 -0.2363 0.094 Uiso 1 1 calc R U . . .
H49C H 0.1493 0.1744 -0.1500 0.094 Uiso 1 1 calc R U . . .
C51 C 0.3592(4) 0.0837(3) -0.0305(3) 0.0296(12) Uani 1 1 d . . . . .
H51 H 0.3352 0.0678 -0.0917 0.036 Uiso 1 1 calc R U . . .
C52 C 0.4620(3) 0.0883(3) -0.0160(3) 0.0299(12) Uani 1 1 d . . . . .
H52 H 0.4794 0.1256 -0.0582 0.036 Uiso 1 1 calc R U . . .
C53 C 0.5011(3) 0.1157(3) 0.0756(3) 0.0269(11) Uani 1 1 d . . . . .
H53 H 0.4920 0.0752 0.1179 0.032 Uiso 1 1 calc R U . . .
C54 C 0.4554(3) 0.1885(3) 0.0969(3) 0.0244(10) Uani 1 1 d . . . . .
H54 H 0.4778 0.2321 0.0657 0.029 Uiso 1 1 calc R U . . .
C55 C 0.3508(3) 0.1841(3) 0.0711(3) 0.0272(11) Uani 1 1 d . . . . .
H55 H 0.3273 0.1473 0.1103 0.033 Uiso 1 1 calc R U . . .
C56 C 0.3044(3) 0.2587(4) 0.0741(3) 0.0374(13) Uani 1 1 d . . . . .
H56A H 0.2386 0.2533 0.0492 0.045 Uiso 1 1 calc R U . . .
H56B H 0.3104 0.2755 0.1351 0.045 Uiso 1 1 calc R U . . .
C57 C 0.4941(5) -0.0087(5) -0.1111(4) 0.073(2) Uani 1 1 d . . . . .
H57A H 0.4327 -0.0301 -0.1294 0.110 Uiso 1 1 calc R U . . .
H57B H 0.5397 -0.0482 -0.1147 0.110 Uiso 1 1 calc R U . . .
H57C H 0.5024 0.0339 -0.1491 0.110 Uiso 1 1 calc R U . . .
C58 C 0.6527(4) 0.0776(4) 0.1375(4) 0.0526(17) Uani 1 1 d . . . . .
H58A H 0.6435 0.0833 0.1972 0.079 Uiso 1 1 calc R U . . .
H58B H 0.7168 0.0879 0.1353 0.079 Uiso 1 1 calc R U . . .
H58C H 0.6371 0.0255 0.1175 0.079 Uiso 1 1 calc R U . . .
C59 C 0.2974(6) 0.3802(5) 0.0121(7) 0.103(4) Uani 1 1 d . . . . .
H59A H 0.2371 0.3704 -0.0237 0.155 Uiso 1 1 calc R U . . .
H59B H 0.3311 0.4158 -0.0181 0.155 Uiso 1 1 calc R U . . .
H59C H 0.2900 0.4024 0.0675 0.155 Uiso 1 1 calc R U . . .
C60 C 0.1734(4) 0.3828(3) 0.3734(3) 0.0305(12) Uani 1 1 d . . . . .
C61 C 0.1979(4) 0.4289(3) 0.4454(4) 0.0416(14) Uani 1 1 d . . . . .
H61 H 0.2426 0.4118 0.4930 0.050 Uiso 1 1 calc R U . . .
C62 C 0.1579(5) 0.5002(4) 0.4491(5) 0.0547(19) Uani 1 1 d . . . . .
H62 H 0.1732 0.5307 0.4997 0.066 Uiso 1 1 calc R U . . .
C63 C 0.0959(5) 0.5261(4) 0.3789(5) 0.0547(18) Uani 1 1 d . . . . .
H63 H 0.0703 0.5756 0.3804 0.066 Uiso 1 1 calc R U . . .
C64 C 0.0705(4) 0.4815(3) 0.3070(5) 0.0482(16) Uani 1 1 d . . . . .
H64 H 0.0279 0.5003 0.2588 0.058 Uiso 1 1 calc R U . . .
C65 C 0.1073(3) 0.4080(3) 0.3040(4) 0.0322(12) Uani 1 1 d . . . . .
C66 C -0.0236(4) 0.3439(4) 0.2206(4) 0.0463(15) Uani 1 1 d . . . . .
H66A H -0.0358 0.3231 0.2751 0.069 Uiso 1 1 calc R U . . .
H66B H -0.0442 0.3075 0.1736 0.069 Uiso 1 1 calc R U . . .
H66C H -0.0564 0.3922 0.2076 0.069 Uiso 1 1 calc R U . . .
C67 C 0.0938(4) 0.3941(4) 0.1481(4) 0.0464(15) Uani 1 1 d . . . . .
H67A H 0.0583 0.4412 0.1374 0.070 Uiso 1 1 calc R U . . .
H67B H 0.0757 0.3592 0.0992 0.070 Uiso 1 1 calc R U . . .
H67C H 0.1590 0.4059 0.1547 0.070 Uiso 1 1 calc R U . . .
C68 C 0.6343(8) 0.7389(6) 0.1976(5) 0.115(4) Uani 1 1 d . . . . .
H68A H 0.6436 0.7462 0.1381 0.173 Uiso 1 1 calc R U . . .
H68B H 0.5701 0.7483 0.2000 0.173 Uiso 1 1 calc R U . . .
H68C H 0.6506 0.6866 0.2161 0.173 Uiso 1 1 calc R U . . .
C69 C 0.6925(8) 0.7928(7) 0.2556(6) 0.096(3) Uani 1 1 d . . . . .
C70 C 0.6599(8) 0.8717(7) 0.2517(7) 0.123(4) Uani 1 1 d D . . . .
H70A H 0.6013 0.8730 0.2724 0.147 Uiso 1 1 calc R U . . .
H70B H 0.6474 0.8882 0.1904 0.147 Uiso 1 1 calc R U . . .
C71 C 0.7235(7) 0.9285(7) 0.3033(6) 0.126(4) Uani 1 1 d D . . . .
H71A H 0.7571 0.9041 0.3559 0.189 Uiso 1 1 calc R U . . .
H71B H 0.6882 0.9715 0.3192 0.189 Uiso 1 1 calc R U . . .
H71C H 0.7668 0.9470 0.2683 0.189 Uiso 1 1 calc R U . . .
N1 N 0.0764(3) 0.3574(2) 0.2289(3) 0.0301(10) Uani 1 1 d . . . . .
O1 O 0.4819(2) 0.20050(19) 0.1883(2) 0.0239(7) Uani 1 1 d . . . . .
O2 O 0.6686(2) 0.23048(18) 0.2537(2) 0.0309(9) Uani 1 1 d . . . . .
O3 O 0.6602(2) 0.2288(2) 0.4295(2) 0.0387(10) Uani 1 1 d . . . . .
O4 O 0.4859(2) 0.2002(2) 0.4616(2) 0.0277(8) Uani 1 1 d . . . . .
O5 O 0.4421(2) 0.31067(18) 0.2569(2) 0.0253(7) Uani 1 1 d . . . . .
O12 O 0.5694(3) 0.1373(3) 0.6172(3) 0.0604(13) Uani 1 1 d . . . . .
O13 O 0.4180(3) 0.0549(2) 0.6594(2) 0.0399(10) Uani 1 1 d . . . . .
O14 O 0.2539(2) 0.07209(19) 0.5362(2) 0.0246(7) Uani 1 1 d . . . . .
O15 O 0.3738(2) 0.2546(2) 0.52684(19) 0.0309(7) Uani 1 1 d . . . . .
O22 O 0.2240(2) -0.0433(2) 0.6522(2) 0.0332(8) Uani 1 1 d . . . . .
O23 O 0.0838(2) -0.1303(2) 0.5451(2) 0.0337(8) Uani 1 1 d . . . . .
O24 O 0.0666(2) -0.07819(19) 0.3684(2) 0.0231(7) Uani 1 1 d . . . . .
O25 O 0.0963(2) 0.09554(19) 0.5013(2) 0.0254(7) Uani 1 1 d . . . . .
O26 O -0.0703(2) 0.0906(2) 0.3780(2) 0.0384(9) Uani 1 1 d . . . . .
O32 O 0.0383(2) -0.2385(2) 0.3550(2) 0.0360(9) Uani 1 1 d . . . . .
O33 O 0.0796(2) -0.2565(2) 0.1879(2) 0.0336(8) Uani 1 1 d . . . . .
O34 O 0.1295(2) -0.11336(19) 0.1204(2) 0.0241(7) Uani 1 1 d . . . . .
O35 O -0.0460(2) -0.06063(19) 0.2449(2) 0.0241(7) Uani 1 1 d . . . . .
O36 O -0.0957(3) -0.0270(2) 0.0645(2) 0.0439(10) Uani 1 1 d . . . . .
O42 O 0.2426(3) -0.2227(2) 0.0662(3) 0.0549(10) Uani 1 1 d . . . . .
O43 O 0.3671(3) -0.1269(2) 0.0028(2) 0.0385(9) Uani 1 1 d . . . . .
O44 O 0.3328(2) 0.02980(19) 0.0257(2) 0.0270(8) Uani 1 1 d . . . . .
O45 O 0.1029(2) -0.0566(2) -0.0173(2) 0.0289(8) Uani 1 1 d . . . . .
O46 O 0.1311(3) 0.0649(2) -0.1296(2) 0.0473(11) Uani 1 1 d . . . . .
O52 O 0.5046(3) 0.0170(2) -0.0263(2) 0.0406(10) Uani 1 1 d . . . . .
O53 O 0.5962(2) 0.1299(2) 0.0835(2) 0.0364(9) Uani 1 1 d . . . . .
O54 O 0.3254(2) 0.1579(2) -0.0171(2) 0.0299(8) Uani 1 1 d . . . . .
O55 O 0.3439(3) 0.3142(2) 0.0265(3) 0.0514(12) Uani 1 1 d . . . . .
O56 O 0.7601(4) 0.7755(5) 0.3084(5) 0.134(3) Uani 1 1 d . . . . .
P1 P 0.22644(9) 0.29198(7) 0.36012(9) 0.0252(3) Uani 1 1 d . . . . .
Cl1 Cl 0.22092(10) 0.13644(8) 0.26116(9) 0.0387(3) Uani 1 1 d . . . . .
Cl2 Cl 0.05264(11) 0.20702(10) 0.10713(10) 0.0525(4) Uani 1 1 d . . . . .
Pd1 Pd 0.14341(2) 0.24994(2) 0.23869(2) 0.02847(10) 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 O1 1.394(6) . ?
C1 O5 1.420(5) . ?
C1 C2 1.524(7) . ?
C1 H1 1.0000 . ?
C2 O2 1.414(5) . ?
C2 C3 1.500(6) . ?
C2 H2 1.0000 . ?
C3 O3 1.430(5) . ?
C3 C4 1.520(6) . ?
C3 H3 1.0000 . ?
C4 O4 1.438(6) . ?
C4 C5 1.541(6) . ?
C4 H4 1.0000 . ?
C5 O5 1.443(5) . ?
C5 C6 1.556(6) . ?
C5 H5 1.0000 . ?
C6 P1 1.837(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O2 1.428(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O3 1.417(7) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 O4 1.389(6) . ?
C11 O15 1.426(6) . ?
C11 C12 1.526(7) . ?
C11 H11 1.0000 . ?
C12 O12 1.410(7) . ?
C12 C13 1.533(8) . ?
C12 H12 1.0000 . ?
C13 O13 1.423(6) . ?
C13 C14 1.527(7) . ?
C13 H13 1.0000 . ?
C14 O14 1.437(6) . ?
C14 C15 1.531(7) . ?
C14 H14 1.0000 . ?
C15 O15 1.444(6) . ?
C15 C16 1.525(7) . ?
C15 H15 1.0000 . ?
C16 P1 1.836(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 O12 1.351(9) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O13 1.417(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C21 O25 1.415(5) . ?
C21 O14 1.423(5) . ?
C21 C22 1.531(7) . ?
C21 H21 1.0000 . ?
C22 O22 1.414(6) . ?
C22 C23 1.518(7) . ?
C22 H22 1.0000 . ?
C23 O23 1.419(6) . ?
C23 C24 1.521(6) . ?
C23 H23 1.0000 . ?
C24 O24 1.431(5) . ?
C24 C25 1.538(7) . ?
C24 H24 1.0000 . ?
C25 O25 1.436(5) . ?
C25 C26 1.513(6) . ?
C25 H25 1.0000 . ?
C26 O26 1.402(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O22 1.415(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 O23 1.439(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 O26 1.427(6) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 O24 1.406(6) . ?
C31 O35 1.412(6) . ?
C31 C32 1.517(7) . ?
C31 H31 1.0000 . ?
C32 O32 1.416(6) . ?
C32 C33 1.531(6) . ?
C32 H32 1.0000 . ?
C33 O33 1.419(6) . ?
C33 C34 1.513(6) . ?
C33 H33 1.0000 . ?
C34 O34 1.437(5) . ?
C34 C35 1.526(6) . ?
C34 H34 1.0000 . ?
C35 O35 1.443(5) . ?
C35 C36 1.502(7) . ?
C35 H35 1.0000 . ?
C36 O36 1.407(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O32 1.420(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 O33 1.419(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 O36 1.421(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 O34 1.414(5) . ?
C41 O45 1.428(6) . ?
C41 C42 1.529(7) . ?
C41 H41 1.0000 . ?
C42 O42 1.420(7) . ?
C42 C43 1.508(7) . ?
C42 H42 1.0000 . ?
C43 O43 1.432(6) . ?
C43 C44 1.521(7) . ?
C43 H43 1.0000 . ?
C44 O44 1.427(6) . ?
C44 C45 1.536(7) . ?
C44 H44 1.0000 . ?
C45 O45 1.435(6) . ?
C45 C46 1.503(7) . ?
C45 H45 1.0000 . ?
C46 O46 1.419(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O42 1.378(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O43 1.403(7) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 O46 1.418(7) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C51 O44 1.402(6) . ?
C51 O54 1.425(6) . ?
C51 C52 1.510(7) . ?
C51 H51 1.0000 . ?
C52 O52 1.426(6) . ?
C52 C53 1.526(7) . ?
C52 H52 1.0000 . ?
C53 O53 1.422(6) . ?
C53 C54 1.514(7) . ?
C53 H53 1.0000 . ?
C54 O1 1.431(5) . ?
C54 C55 1.537(7) . ?
C54 H54 1.0000 . ?
C55 O54 1.441(6) . ?
C55 C56 1.485(8) . ?
C55 H55 1.0000 . ?
C56 O55 1.423(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O52 1.388(7) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 O53 1.413(7) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 O55 1.345(9) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 C61 1.383(8) . ?
C60 C65 1.395(8) . ?
C60 P1 1.808(5) . ?
C61 C62 1.391(8) . ?
C61 H61 0.9500 . ?
C62 C63 1.374(10) . ?
C62 H62 0.9500 . ?
C63 C64 1.367(9) . ?
C63 H63 0.9500 . ?
C64 C65 1.405(7) . ?
C64 H64 0.9500 . ?
C65 N1 1.479(7) . ?
C66 N1 1.491(6) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 N1 1.490(7) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C69 1.474(14) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 O56 1.215(10) . ?
C69 C70 1.465(14) . ?
C70 C71 1.501(10) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
N1 Pd1 2.125(4) . ?
P1 Pd1 2.1947(14) . ?
Cl1 Pd1 2.2949(14) . ?
Cl2 Pd1 2.3676(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 O5 112.8(4) . . ?
O1 C1 C2 109.1(4) . . ?
O5 C1 C2 108.7(4) . . ?
O1 C1 H1 108.7 . . ?
O5 C1 H1 108.7 . . ?
C2 C1 H1 108.7 . . ?
O2 C2 C3 107.1(4) . . ?
O2 C2 C1 114.0(4) . . ?
C3 C2 C1 109.5(4) . . ?
O2 C2 H2 108.7 . . ?
C3 C2 H2 108.7 . . ?
C1 C2 H2 108.7 . . ?
O3 C3 C2 109.5(4) . . ?
O3 C3 C4 107.8(4) . . ?
C2 C3 C4 112.5(4) . . ?
O3 C3 H3 109.0 . . ?
C2 C3 H3 109.0 . . ?
C4 C3 H3 109.0 . . ?
O4 C4 C3 104.7(4) . . ?
O4 C4 C5 113.2(4) . . ?
C3 C4 C5 113.1(4) . . ?
O4 C4 H4 108.5 . . ?
C3 C4 H4 108.5 . . ?
C5 C4 H4 108.5 . . ?
O5 C5 C4 108.7(3) . . ?
O5 C5 C6 102.7(3) . . ?
C4 C5 C6 114.9(4) . . ?
O5 C5 H5 110.1 . . ?
C4 C5 H5 110.1 . . ?
C6 C5 H5 110.1 . . ?
C5 C6 P1 123.0(3) . . ?
C5 C6 H6A 106.6 . . ?
P1 C6 H6A 106.6 . . ?
C5 C6 H6B 106.6 . . ?
P1 C6 H6B 106.6 . . ?
H6A C6 H6B 106.5 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O4 C11 O15 111.6(4) . . ?
O4 C11 C12 109.1(5) . . ?
O15 C11 C12 107.8(4) . . ?
O4 C11 H11 109.4 . . ?
O15 C11 H11 109.4 . . ?
C12 C11 H11 109.4 . . ?
O12 C12 C11 110.3(4) . . ?
O12 C12 C13 110.2(5) . . ?
C11 C12 C13 111.7(4) . . ?
O12 C12 H12 108.2 . . ?
C11 C12 H12 108.2 . . ?
C13 C12 H12 108.2 . . ?
O13 C13 C14 110.2(4) . . ?
O13 C13 C12 108.2(4) . . ?
C14 C13 C12 111.3(5) . . ?
O13 C13 H13 109.0 . . ?
C14 C13 H13 109.0 . . ?
C12 C13 H13 109.0 . . ?
O14 C14 C13 106.2(4) . . ?
O14 C14 C15 112.7(4) . . ?
C13 C14 C15 107.8(4) . . ?
O14 C14 H14 110.0 . . ?
C13 C14 H14 110.0 . . ?
C15 C14 H14 110.0 . . ?
O15 C15 C16 104.0(4) . . ?
O15 C15 C14 106.5(4) . . ?
C16 C15 C14 117.8(4) . . ?
O15 C15 H15 109.4 . . ?
C16 C15 H15 109.4 . . ?
C14 C15 H15 109.4 . . ?
C15 C16 P1 111.3(3) . . ?
C15 C16 H16A 109.4 . . ?
P1 C16 H16A 109.4 . . ?
C15 C16 H16B 109.4 . . ?
P1 C16 H16B 109.4 . . ?
H16A C16 H16B 108.0 . . ?
O12 C17 H17A 109.5 . . ?
O12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O13 C18 H18A 109.5 . . ?
O13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O25 C21 O14 111.5(4) . . ?
O25 C21 C22 109.1(4) . . ?
O14 C21 C22 110.0(4) . . ?
O25 C21 H21 108.7 . . ?
O14 C21 H21 108.7 . . ?
C22 C21 H21 108.7 . . ?
O22 C22 C23 106.7(4) . . ?
O22 C22 C21 113.4(4) . . ?
C23 C22 C21 112.5(4) . . ?
O22 C22 H22 108.0 . . ?
C23 C22 H22 108.0 . . ?
C21 C22 H22 108.0 . . ?
O23 C23 C22 109.0(4) . . ?
O23 C23 C24 107.2(4) . . ?
C22 C23 C24 113.7(4) . . ?
O23 C23 H23 108.9 . . ?
C22 C23 H23 108.9 . . ?
C24 C23 H23 108.9 . . ?
O24 C24 C23 106.3(4) . . ?
O24 C24 C25 109.7(3) . . ?
C23 C24 C25 111.5(4) . . ?
O24 C24 H24 109.8 . . ?
C23 C24 H24 109.8 . . ?
C25 C24 H24 109.8 . . ?
O25 C25 C26 106.9(4) . . ?
O25 C25 C24 109.6(3) . . ?
C26 C25 C24 114.5(4) . . ?
O25 C25 H25 108.6 . . ?
C26 C25 H25 108.6 . . ?
C24 C25 H25 108.6 . . ?
O26 C26 C25 110.9(4) . . ?
O26 C26 H26A 109.5 . . ?
C25 C26 H26A 109.5 . . ?
O26 C26 H26B 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 108.0 . . ?
O22 C27 H27A 109.5 . . ?
O22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O23 C28 H28A 109.5 . . ?
O23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O26 C29 H29A 109.5 . . ?
O26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O24 C31 O35 111.6(4) . . ?
O24 C31 C32 109.1(4) . . ?
O35 C31 C32 109.3(4) . . ?
O24 C31 H31 108.9 . . ?
O35 C31 H31 108.9 . . ?
C32 C31 H31 108.9 . . ?
O32 C32 C31 114.3(4) . . ?
O32 C32 C33 107.2(4) . . ?
C31 C32 C33 110.5(4) . . ?
O32 C32 H32 108.2 . . ?
C31 C32 H32 108.2 . . ?
C33 C32 H32 108.2 . . ?
O33 C33 C34 108.4(4) . . ?
O33 C33 C32 110.5(4) . . ?
C34 C33 C32 112.4(4) . . ?
O33 C33 H33 108.5 . . ?
C34 C33 H33 108.5 . . ?
C32 C33 H33 108.5 . . ?
O34 C34 C33 106.6(4) . . ?
O34 C34 C35 108.7(4) . . ?
C33 C34 C35 112.3(4) . . ?
O34 C34 H34 109.7 . . ?
C33 C34 H34 109.7 . . ?
C35 C34 H34 109.7 . . ?
O35 C35 C36 106.6(4) . . ?
O35 C35 C34 111.2(4) . . ?
C36 C35 C34 114.5(4) . . ?
O35 C35 H35 108.1 . . ?
C36 C35 H35 108.1 . . ?
C34 C35 H35 108.1 . . ?
O36 C36 C35 110.9(4) . . ?
O36 C36 H36A 109.5 . . ?
C35 C36 H36A 109.5 . . ?
O36 C36 H36B 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 108.1 . . ?
O32 C37 H37A 109.5 . . ?
O32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O33 C38 H38A 109.5 . . ?
O33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O36 C39 H39A 109.5 . . ?
O36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O34 C41 O45 111.4(4) . . ?
O34 C41 C42 108.6(4) . . ?
O45 C41 C42 108.9(4) . . ?
O34 C41 H41 109.3 . . ?
O45 C41 H41 109.3 . . ?
C42 C41 H41 109.3 . . ?
O42 C42 C43 107.5(4) . . ?
O42 C42 C41 112.6(4) . . ?
C43 C42 C41 112.1(4) . . ?
O42 C42 H42 108.1 . . ?
C43 C42 H42 108.1 . . ?
C41 C42 H42 108.1 . . ?
O43 C43 C42 108.9(4) . . ?
O43 C43 C44 108.2(4) . . ?
C42 C43 C44 112.4(4) . . ?
O43 C43 H43 109.1 . . ?
C42 C43 H43 109.1 . . ?
C44 C43 H43 109.1 . . ?
O44 C44 C43 106.4(4) . . ?
O44 C44 C45 112.2(4) . . ?
C43 C44 C45 110.9(4) . . ?
O44 C44 H44 109.1 . . ?
C43 C44 H44 109.1 . . ?
C45 C44 H44 109.1 . . ?
O45 C45 C46 107.6(4) . . ?
O45 C45 C44 109.5(4) . . ?
C46 C45 C44 114.6(4) . . ?
O45 C45 H45 108.3 . . ?
C46 C45 H45 108.3 . . ?
C44 C45 H45 108.3 . . ?
O46 C46 C45 109.4(4) . . ?
O46 C46 H46A 109.8 . . ?
C45 C46 H46A 109.8 . . ?
O46 C46 H46B 109.8 . . ?
C45 C46 H46B 109.8 . . ?
H46A C46 H46B 108.2 . . ?
O42 C47 H47A 109.5 . . ?
O42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
O42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O43 C48 H48A 109.5 . . ?
O43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O46 C49 H49A 109.5 . . ?
O46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O44 C51 O54 111.8(4) . . ?
O44 C51 C52 109.9(4) . . ?
O54 C51 C52 107.9(4) . . ?
O44 C51 H51 109.1 . . ?
O54 C51 H51 109.1 . . ?
C52 C51 H51 109.1 . . ?
O52 C52 C51 113.5(4) . . ?
O52 C52 C53 106.6(4) . . ?
C51 C52 C53 110.7(4) . . ?
O52 C52 H52 108.7 . . ?
C51 C52 H52 108.7 . . ?
C53 C52 H52 108.7 . . ?
O53 C53 C54 108.6(4) . . ?
O53 C53 C52 109.4(4) . . ?
C54 C53 C52 111.5(4) . . ?
O53 C53 H53 109.1 . . ?
C54 C53 H53 109.1 . . ?
C52 C53 H53 109.1 . . ?
O1 C54 C53 107.2(4) . . ?
O1 C54 C55 110.1(4) . . ?
C53 C54 C55 112.2(4) . . ?
O1 C54 H54 109.1 . . ?
C53 C54 H54 109.1 . . ?
C55 C54 H54 109.1 . . ?
O54 C55 C56 105.8(4) . . ?
O54 C55 C54 109.6(4) . . ?
C56 C55 C54 113.8(4) . . ?
O54 C55 H55 109.1 . . ?
C56 C55 H55 109.1 . . ?
C54 C55 H55 109.1 . . ?
O55 C56 C55 110.1(4) . . ?
O55 C56 H56A 109.6 . . ?
C55 C56 H56A 109.6 . . ?
O55 C56 H56B 109.6 . . ?
C55 C56 H56B 109.6 . . ?
H56A C56 H56B 108.2 . . ?
O52 C57 H57A 109.5 . . ?
O52 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O52 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O53 C58 H58A 109.5 . . ?
O53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O55 C59 H59A 109.5 . . ?
O55 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
O55 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C61 C60 C65 119.5(5) . . ?
C61 C60 P1 123.9(5) . . ?
C65 C60 P1 116.6(4) . . ?
C60 C61 C62 120.7(6) . . ?
C60 C61 H61 119.6 . . ?
C62 C61 H61 119.6 . . ?
C63 C62 C61 119.5(6) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C64 C63 C62 120.8(6) . . ?
C64 C63 H63 119.6 . . ?
C62 C63 H63 119.6 . . ?
C63 C64 C65 120.3(6) . . ?
C63 C64 H64 119.9 . . ?
C65 C64 H64 119.9 . . ?
C60 C65 C64 119.1(5) . . ?
C60 C65 N1 120.1(4) . . ?
C64 C65 N1 120.8(5) . . ?
N1 C66 H66A 109.5 . . ?
N1 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N1 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N1 C67 H67A 109.5 . . ?
N1 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N1 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C69 C68 H68A 109.5 . . ?
C69 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C69 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
O56 C69 C70 119.3(11) . . ?
O56 C69 C68 125.2(10) . . ?
C70 C69 C68 115.3(9) . . ?
C69 C70 C71 115.7(11) . . ?
C69 C70 H70A 108.3 . . ?
C71 C70 H70A 108.3 . . ?
C69 C70 H70B 108.3 . . ?
C71 C70 H70B 108.3 . . ?
H70A C70 H70B 107.4 . . ?
C70 C71 H71A 109.5 . . ?
C70 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C70 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C65 N1 C67 110.1(4) . . ?
C65 N1 C66 108.6(4) . . ?
C67 N1 C66 109.3(4) . . ?
C65 N1 Pd1 113.8(3) . . ?
C67 N1 Pd1 106.7(3) . . ?
C66 N1 Pd1 108.3(3) . . ?
C1 O1 C54 118.6(4) . . ?
C2 O2 C7 114.1(4) . . ?
C8 O3 C3 114.7(4) . . ?
C11 O4 C4 115.9(4) . . ?
C1 O5 C5 114.9(3) . . ?
C17 O12 C12 117.4(7) . . ?
C18 O13 C13 113.5(4) . . ?
C21 O14 C14 116.4(4) . . ?
C11 O15 C15 111.5(4) . . ?
C22 O22 C27 113.4(4) . . ?
C23 O23 C28 113.9(4) . . ?
C31 O24 C24 118.9(3) . . ?
C21 O25 C25 113.2(3) . . ?
C26 O26 C29 109.9(4) . . ?
C32 O32 C37 113.4(4) . . ?
C33 O33 C38 114.4(4) . . ?
C41 O34 C34 117.5(3) . . ?
C31 O35 C35 113.5(3) . . ?
C36 O36 C39 110.2(5) . . ?
C47 O42 C42 112.9(5) . . ?
C48 O43 C43 115.3(4) . . ?
C51 O44 C44 118.1(4) . . ?
C41 O45 C45 114.4(4) . . ?
C49 O46 C46 111.0(5) . . ?
C57 O52 C52 115.0(5) . . ?
C58 O53 C53 114.2(4) . . ?
C51 O54 C55 113.5(4) . . ?
C59 O55 C56 115.1(5) . . ?
C60 P1 C16 106.0(2) . . ?
C60 P1 C6 100.4(2) . . ?
C16 P1 C6 112.7(2) . . ?
C60 P1 Pd1 102.12(19) . . ?
C16 P1 Pd1 116.74(17) . . ?
C6 P1 Pd1 116.12(17) . . ?
N1 Pd1 P1 86.83(12) . . ?
N1 Pd1 Cl1 175.19(13) . . ?
P1 Pd1 Cl1 88.49(5) . . ?
N1 Pd1 Cl2 92.05(12) . . ?
P1 Pd1 Cl2 178.87(6) . . ?
Cl1 Pd1 Cl2 92.63(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C1 C2 O2 55.5(5) . . . . ?
O5 C1 C2 O2 178.9(3) . . . . ?
O1 C1 C2 C3 -64.4(5) . . . . ?
O5 C1 C2 C3 59.0(5) . . . . ?
O2 C2 C3 O3 64.4(5) . . . . ?
C1 C2 C3 O3 -171.5(4) . . . . ?
O2 C2 C3 C4 -175.7(4) . . . . ?
C1 C2 C3 C4 -51.6(5) . . . . ?
O3 C3 C4 O4 -68.2(5) . . . . ?
C2 C3 C4 O4 170.9(4) . . . . ?
O3 C3 C4 C5 168.0(4) . . . . ?
C2 C3 C4 C5 47.2(6) . . . . ?
O4 C4 C5 O5 -166.5(4) . . . . ?
C3 C4 C5 O5 -47.6(6) . . . . ?
O4 C4 C5 C6 79.2(5) . . . . ?
C3 C4 C5 C6 -162.0(4) . . . . ?
O5 C5 C6 P1 125.1(4) . . . . ?
C4 C5 C6 P1 -117.1(4) . . . . ?
O4 C11 C12 O12 55.0(6) . . . . ?
O15 C11 C12 O12 176.3(4) . . . . ?
O4 C11 C12 C13 -67.9(6) . . . . ?
O15 C11 C12 C13 53.4(6) . . . . ?
O12 C12 C13 O13 66.2(5) . . . . ?
C11 C12 C13 O13 -170.8(4) . . . . ?
O12 C12 C13 C14 -172.5(4) . . . . ?
C11 C12 C13 C14 -49.6(6) . . . . ?
O13 C13 C14 O14 -65.6(5) . . . . ?
C12 C13 C14 O14 174.3(4) . . . . ?
O13 C13 C14 C15 173.4(4) . . . . ?
C12 C13 C14 C15 53.3(5) . . . . ?
O14 C14 C15 O15 -179.2(3) . . . . ?
C13 C14 C15 O15 -62.3(5) . . . . ?
O14 C14 C15 C16 64.7(6) . . . . ?
C13 C14 C15 C16 -178.5(4) . . . . ?
O15 C15 C16 P1 72.7(4) . . . . ?
C14 C15 C16 P1 -169.7(3) . . . . ?
O25 C21 C22 O22 173.6(3) . . . . ?
O14 C21 C22 O22 51.0(5) . . . . ?
O25 C21 C22 C23 52.3(5) . . . . ?
O14 C21 C22 C23 -70.3(5) . . . . ?
O22 C22 C23 O23 71.7(5) . . . . ?
C21 C22 C23 O23 -163.3(4) . . . . ?
O22 C22 C23 C24 -168.8(4) . . . . ?
C21 C22 C23 C24 -43.7(5) . . . . ?
O23 C23 C24 O24 -76.6(4) . . . . ?
C22 C23 C24 O24 162.8(4) . . . . ?
O23 C23 C24 C25 163.9(4) . . . . ?
C22 C23 C24 C25 43.3(5) . . . . ?
O24 C24 C25 O25 -169.2(3) . . . . ?
C23 C24 C25 O25 -51.7(5) . . . . ?
O24 C24 C25 C26 70.7(5) . . . . ?
C23 C24 C25 C26 -171.8(4) . . . . ?
O25 C25 C26 O26 -66.9(5) . . . . ?
C24 C25 C26 O26 54.7(5) . . . . ?
O24 C31 C32 O32 56.5(5) . . . . ?
O35 C31 C32 O32 178.8(3) . . . . ?
O24 C31 C32 C33 -64.5(5) . . . . ?
O35 C31 C32 C33 57.7(5) . . . . ?
O32 C32 C33 O33 64.0(5) . . . . ?
C31 C32 C33 O33 -170.8(4) . . . . ?
O32 C32 C33 C34 -174.8(4) . . . . ?
C31 C32 C33 C34 -49.6(5) . . . . ?
O33 C33 C34 O34 -73.5(4) . . . . ?
C32 C33 C34 O34 164.1(4) . . . . ?
O33 C33 C34 C35 167.5(4) . . . . ?
C32 C33 C34 C35 45.1(5) . . . . ?
O34 C34 C35 O35 -166.0(3) . . . . ?
C33 C34 C35 O35 -48.3(5) . . . . ?
O34 C34 C35 C36 73.1(5) . . . . ?
C33 C34 C35 C36 -169.2(4) . . . . ?
O35 C35 C36 O36 -68.5(5) . . . . ?
C34 C35 C36 O36 55.0(5) . . . . ?
O34 C41 C42 O42 53.6(5) . . . . ?
O45 C41 C42 O42 175.0(4) . . . . ?
O34 C41 C42 C43 -67.8(5) . . . . ?
O45 C41 C42 C43 53.6(5) . . . . ?
O42 C42 C43 O43 66.8(5) . . . . ?
C41 C42 C43 O43 -168.9(4) . . . . ?
O42 C42 C43 C44 -173.3(4) . . . . ?
C41 C42 C43 C44 -49.0(5) . . . . ?
O43 C43 C44 O44 -68.9(4) . . . . ?
C42 C43 C44 O44 170.7(4) . . . . ?
O43 C43 C44 C45 168.7(4) . . . . ?
C42 C43 C44 C45 48.4(5) . . . . ?
O44 C44 C45 O45 -172.0(4) . . . . ?
C43 C44 C45 O45 -53.1(5) . . . . ?
O44 C44 C45 C46 67.0(5) . . . . ?
C43 C44 C45 C46 -174.1(4) . . . . ?
O45 C45 C46 O46 -68.4(5) . . . . ?
C44 C45 C46 O46 53.6(6) . . . . ?
O44 C51 C52 O52 56.9(5) . . . . ?
O54 C51 C52 O52 179.1(4) . . . . ?
O44 C51 C52 C53 -62.8(5) . . . . ?
O54 C51 C52 C53 59.3(5) . . . . ?
O52 C52 C53 O53 64.4(5) . . . . ?
C51 C52 C53 O53 -171.8(4) . . . . ?
O52 C52 C53 C54 -175.5(4) . . . . ?
C51 C52 C53 C54 -51.7(5) . . . . ?
O53 C53 C54 O1 -71.6(5) . . . . ?
C52 C53 C54 O1 167.8(4) . . . . ?
O53 C53 C54 C55 167.5(4) . . . . ?
C52 C53 C54 C55 46.9(5) . . . . ?
O1 C54 C55 O54 -169.2(4) . . . . ?
C53 C54 C55 O54 -49.9(5) . . . . ?
O1 C54 C55 C56 72.4(5) . . . . ?
C53 C54 C55 C56 -168.3(4) . . . . ?
O54 C55 C56 O55 -69.0(5) . . . . ?
C54 C55 C56 O55 51.4(6) . . . . ?
C65 C60 C61 C62 -0.4(8) . . . . ?
P1 C60 C61 C62 176.2(4) . . . . ?
C60 C61 C62 C63 -2.6(9) . . . . ?
C61 C62 C63 C64 2.5(10) . . . . ?
C62 C63 C64 C65 0.4(9) . . . . ?
C61 C60 C65 C64 3.2(7) . . . . ?
P1 C60 C65 C64 -173.5(4) . . . . ?
C61 C60 C65 N1 -176.3(4) . . . . ?
P1 C60 C65 N1 6.9(6) . . . . ?
C63 C64 C65 C60 -3.3(8) . . . . ?
C63 C64 C65 N1 176.2(5) . . . . ?
O56 C69 C70 C71 10.8(15) . . . . ?
C68 C69 C70 C71 -173.7(9) . . . . ?
C60 C65 N1 C67 -121.0(5) . . . . ?
C64 C65 N1 C67 59.5(6) . . . . ?
C60 C65 N1 C66 119.4(5) . . . . ?
C64 C65 N1 C66 -60.1(6) . . . . ?
C60 C65 N1 Pd1 -1.3(6) . . . . ?
C64 C65 N1 Pd1 179.2(4) . . . . ?
O5 C1 O1 C54 106.7(4) . . . . ?
C2 C1 O1 C54 -132.3(4) . . . . ?
C53 C54 O1 C1 135.0(4) . . . . ?
C55 C54 O1 C1 -102.7(5) . . . . ?
C3 C2 O2 C7 -164.4(4) . . . . ?
C1 C2 O2 C7 74.3(5) . . . . ?
C2 C3 O3 C8 -127.1(5) . . . . ?
C4 C3 O3 C8 110.2(5) . . . . ?
O15 C11 O4 C4 77.6(5) . . . . ?
C12 C11 O4 C4 -163.4(4) . . . . ?
C3 C4 O4 C11 138.8(4) . . . . ?
C5 C4 O4 C11 -97.5(5) . . . . ?
O1 C1 O5 C5 56.0(5) . . . . ?
C2 C1 O5 C5 -65.2(5) . . . . ?
C4 C5 O5 C1 58.6(5) . . . . ?
C6 C5 O5 C1 -179.3(4) . . . . ?
C11 C12 O12 C17 128.5(8) . . . . ?
C13 C12 O12 C17 -107.7(8) . . . . ?
C14 C13 O13 C18 118.9(5) . . . . ?
C12 C13 O13 C18 -119.1(5) . . . . ?
O25 C21 O14 C14 100.8(4) . . . . ?
C22 C21 O14 C14 -138.0(4) . . . . ?
C13 C14 O14 C21 138.7(4) . . . . ?
C15 C14 O14 C21 -103.5(4) . . . . ?
O4 C11 O15 C15 53.8(5) . . . . ?
C12 C11 O15 C15 -66.0(5) . . . . ?
C16 C15 O15 C11 -163.3(4) . . . . ?
C14 C15 O15 C11 71.6(4) . . . . ?
C23 C22 O22 C27 -165.3(4) . . . . ?
C21 C22 O22 C27 70.2(5) . . . . ?
C22 C23 O23 C28 -101.6(5) . . . . ?
C24 C23 O23 C28 134.9(4) . . . . ?
O35 C31 O24 C24 95.1(4) . . . . ?
C32 C31 O24 C24 -144.0(4) . . . . ?
C23 C24 O24 C31 128.8(4) . . . . ?
C25 C24 O24 C31 -110.5(4) . . . . ?
O14 C21 O25 C25 57.3(5) . . . . ?
C22 C21 O25 C25 -64.4(4) . . . . ?
C26 C25 O25 C21 -170.7(4) . . . . ?
C24 C25 O25 C21 64.7(5) . . . . ?
C25 C26 O26 C29 -170.6(4) . . . . ?
C31 C32 O32 C37 69.9(6) . . . . ?
C33 C32 O32 C37 -167.2(4) . . . . ?
C34 C33 O33 C38 137.2(4) . . . . ?
C32 C33 O33 C38 -99.3(5) . . . . ?
O45 C41 O34 C34 94.0(5) . . . . ?
C42 C41 O34 C34 -146.1(4) . . . . ?
C33 C34 O34 C41 122.9(4) . . . . ?
C35 C34 O34 C41 -115.9(4) . . . . ?
O24 C31 O35 C35 56.7(5) . . . . ?
C32 C31 O35 C35 -64.0(5) . . . . ?
C36 C35 O35 C31 -175.3(4) . . . . ?
C34 C35 O35 C31 59.2(5) . . . . ?
C35 C36 O36 C39 172.0(5) . . . . ?
C43 C42 O42 C47 -148.0(5) . . . . ?
C41 C42 O42 C47 88.0(6) . . . . ?
C42 C43 O43 C48 -115.5(5) . . . . ?
C44 C43 O43 C48 122.0(5) . . . . ?
O54 C51 O44 C44 105.0(5) . . . . ?
C52 C51 O44 C44 -135.2(4) . . . . ?
C43 C44 O44 C51 141.1(4) . . . . ?
C45 C44 O44 C51 -97.4(5) . . . . ?
O34 C41 O45 C45 57.8(5) . . . . ?
C42 C41 O45 C45 -61.9(5) . . . . ?
C46 C45 O45 C41 -172.7(4) . . . . ?
C44 C45 O45 C41 62.2(5) . . . . ?
C45 C46 O46 C49 -173.0(5) . . . . ?
C51 C52 O52 C57 72.1(6) . . . . ?
C53 C52 O52 C57 -165.8(5) . . . . ?
C54 C53 O53 C58 127.4(5) . . . . ?
C52 C53 O53 C58 -110.7(5) . . . . ?
O44 C51 O54 C55 55.1(5) . . . . ?
C52 C51 O54 C55 -65.9(5) . . . . ?
C56 C55 O54 C51 -175.9(4) . . . . ?
C54 C55 O54 C51 61.0(5) . . . . ?
C55 C56 O55 C59 169.0(7) . . . . ?
C61 C60 P1 C16 52.2(5) . . . . ?
C65 C60 P1 C16 -131.2(4) . . . . ?
C61 C60 P1 C6 -65.3(5) . . . . ?
C65 C60 P1 C6 111.3(4) . . . . ?
C61 C60 P1 Pd1 174.9(4) . . . . ?
C65 C60 P1 Pd1 -8.5(4) . . . . ?
C15 C16 P1 C60 -137.6(4) . . . . ?
C15 C16 P1 C6 -28.7(4) . . . . ?
C15 C16 P1 Pd1 109.5(3) . . . . ?
C5 C6 P1 C60 -169.1(4) . . . . ?
C5 C6 P1 C16 78.5(4) . . . . ?
C5 C6 P1 Pd1 -59.9(4) . . . . ?

_refine_diff_density_max         0.529
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.062

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.287 0.501 0.207 28.5 2.3
2 0.409 0.940 0.353 188.8 24.5
3 0.591 0.440 0.647 188.7 25.1
4 0.395 0.673 0.124 10.6 1.1
5 0.605 0.173 0.876 10.6 1.1
6 0.713 1.001 0.793 28.5 2.7
_platon_squeeze_details          
;
The residual electron density was assigned to one molecule of
the butanone solvent [57/2= 29 e per asymmetric unit; one molecule of C4H8O1 would give 40 e]. 
;

_shelxl_version_number           2013-4

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

data_dagc210928_02
_database_code_depnum_ccdc_archive 'CCDC 2163657'
loop_
_audit_author_name
_audit_author_address
'Lydia Karmazin'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_dagc210928_02       
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The compound crystalized as a chiral dimer.
;
# Added during the CSD deposition process: Thursday 31 March 2022 01:04 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 Br2 N Ni P'
_chemical_formula_sum            'C12 H20 Br2 N Ni P'
_chemical_formula_weight         427.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_H-M_alt        'P 1'
_space_group_name_Hall           'P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'

_cell_length_a                   7.2760(3)
_cell_length_b                   8.6431(3)
_cell_length_c                   13.5955(5)
_cell_angle_alpha                83.1970(10)
_cell_angle_beta                 84.0140(10)
_cell_angle_gamma                71.1770(10)
_cell_volume                     801.57(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9979
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.87

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_F_000             424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    6.275
_shelx_estimated_absorpt_T_min   0.398
_shelx_estimated_absorpt_T_max   0.520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54711
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.500
_diffrn_reflns_theta_max         27.920
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             7331
_reflns_number_gt                7056
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_max     0.903
_reflns_Friedel_fraction_full    0.922

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0059P)²+0.2114P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3189 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(3)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7331
_refine_ls_number_parameters     315
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0376
_refine_ls_wR_factor_gt          0.0362
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4057(5) 0.3720(4) 0.7390(3) 0.0214(7) Uani 1 1 d . . . . .
C2 C 0.2479(6) 0.5085(5) 0.7618(3) 0.0309(9) Uani 1 1 d . . . . .
H2 H 0.1889 0.5879 0.7104 0.037 Uiso 1 1 calc R U . . .
C3 C 0.1773(6) 0.5281(5) 0.8598(3) 0.0313(9) Uani 1 1 d . . . . .
H3 H 0.0699 0.6211 0.8754 0.038 Uiso 1 1 calc R U . . .
C4 C 0.2621(6) 0.4132(5) 0.9348(3) 0.0300(9) Uani 1 1 d . . . . .
H4 H 0.2143 0.4284 1.0018 0.036 Uiso 1 1 calc R U . . .
C5 C 0.4169(5) 0.2759(5) 0.9127(3) 0.0251(8) Uani 1 1 d . . . . .
H5 H 0.4741 0.1960 0.9642 0.030 Uiso 1 1 calc R U . . .
C6 C 0.4886(5) 0.2556(4) 0.8134(3) 0.0193(7) Uani 1 1 d . . . . .
C7 C 0.5418(9) 0.5000(5) 0.5962(4) 0.0659(19) Uani 1 1 d . . . . .
H7A H 0.4262 0.5966 0.6027 0.099 Uiso 1 1 calc R U . . .
H7B H 0.5882 0.4930 0.5261 0.099 Uiso 1 1 calc R U . . .
H7C H 0.6443 0.5095 0.6342 0.099 Uiso 1 1 calc R U . . .
C8 C 0.3332(7) 0.3327(7) 0.5759(3) 0.0543(15) Uani 1 1 d . . . . .
H8A H 0.2187 0.4307 0.5794 0.081 Uiso 1 1 calc R U . . .
H8B H 0.2972 0.2358 0.6040 0.081 Uiso 1 1 calc R U . . .
H8C H 0.3822 0.3199 0.5064 0.081 Uiso 1 1 calc R U . . .
C9 C 0.8867(5) 0.0795(5) 0.8480(3) 0.0273(8) Uani 1 1 d . . . . .
H9A H 0.8435 0.0694 0.9193 0.033 Uiso 1 1 calc R U . . .
H9B H 0.9994 -0.0186 0.8348 0.033 Uiso 1 1 calc R U . . .
C10 C 0.9499(7) 0.2325(6) 0.8252(4) 0.0415(11) Uani 1 1 d . . . . .
H10A H 0.9912 0.2437 0.7545 0.062 Uiso 1 1 calc R U . . .
H10B H 1.0586 0.2228 0.8649 0.062 Uiso 1 1 calc R U . . .
H10C H 0.8406 0.3294 0.8414 0.062 Uiso 1 1 calc R U . . .
C11 C 0.6275(6) -0.0990(5) 0.8160(3) 0.0296(8) Uani 1 1 d . . . . .
H11A H 0.7425 -0.1958 0.8037 0.035 Uiso 1 1 calc R U . . .
H11B H 0.5941 -0.1013 0.8886 0.035 Uiso 1 1 calc R U . . .
C12 C 0.4575(7) -0.1121(6) 0.7648(4) 0.0441(12) Uani 1 1 d . . . . .
H12A H 0.3416 -0.0188 0.7787 0.066 Uiso 1 1 calc R U . . .
H12B H 0.4314 -0.2147 0.7898 0.066 Uiso 1 1 calc R U . . .
H12C H 0.4899 -0.1113 0.6930 0.066 Uiso 1 1 calc R U . . .
C13 C 0.3426(5) 0.6307(4) 0.2541(2) 0.0150(6) Uani 1 1 d . . . . .
C14 C 0.2897(5) 0.4894(4) 0.2765(3) 0.0193(7) Uani 1 1 d . . . . .
H14 H 0.3639 0.3907 0.2483 0.023 Uiso 1 1 calc R U . . .
C15 C 0.1263(5) 0.4938(4) 0.3410(3) 0.0211(7) Uani 1 1 d . . . . .
H15 H 0.0898 0.3973 0.3573 0.025 Uiso 1 1 calc R U . . .
C16 C 0.0165(5) 0.6384(4) 0.3814(3) 0.0217(7) Uani 1 1 d . . . . .
H16 H -0.0942 0.6401 0.4256 0.026 Uiso 1 1 calc R U . . .
C17 C 0.0675(5) 0.7795(4) 0.3576(3) 0.0205(7) Uani 1 1 d . . . . .
H17 H -0.0091 0.8786 0.3846 0.025 Uiso 1 1 calc R U . . .
C18 C 0.2325(5) 0.7767(4) 0.2936(3) 0.0171(7) Uani 1 1 d . . . . .
C19 C 0.6894(5) 0.5002(4) 0.2307(3) 0.0198(7) Uani 1 1 d . . . . .
H19A H 0.7088 0.5279 0.2958 0.030 Uiso 1 1 calc R U . . .
H19B H 0.8065 0.4930 0.1863 0.030 Uiso 1 1 calc R U . . .
H19C H 0.6645 0.3944 0.2380 0.030 Uiso 1 1 calc R U . . .
C20 C 0.4892(5) 0.5877(4) 0.0880(3) 0.0227(7) Uani 1 1 d . . . . .
H20A H 0.4785 0.4767 0.0944 0.034 Uiso 1 1 calc R U . . .
H20B H 0.6001 0.5922 0.0415 0.034 Uiso 1 1 calc R U . . .
H20C H 0.3694 0.6663 0.0631 0.034 Uiso 1 1 calc R U . . .
C21 C 0.3439(5) 1.0212(4) 0.3770(2) 0.0180(7) Uani 1 1 d . . . . .
H21A H 0.3804 1.1230 0.3630 0.022 Uiso 1 1 calc R U . . .
H21B H 0.2157 1.0486 0.4152 0.022 Uiso 1 1 calc R U . . .
C22 C 0.4947(6) 0.8954(5) 0.4397(3) 0.0294(9) Uani 1 1 d . . . . .
H22A H 0.4581 0.7951 0.4547 0.044 Uiso 1 1 calc R U . . .
H22B H 0.5005 0.9402 0.5018 0.044 Uiso 1 1 calc R U . . .
H22C H 0.6225 0.8699 0.4029 0.044 Uiso 1 1 calc R U . . .
C23 C 0.1318(5) 1.1100(4) 0.1983(3) 0.0185(7) Uani 1 1 d . . . . .
H23A H 0.0062 1.1217 0.2374 0.022 Uiso 1 1 calc R U . . .
H23B H 0.1601 1.2149 0.1964 0.022 Uiso 1 1 calc R U . . .
C24 C 0.1130(5) 1.0772(5) 0.0931(3) 0.0239(8) Uani 1 1 d . . . . .
H24A H 0.2378 1.0631 0.0544 0.036 Uiso 1 1 calc R U . . .
H24B H 0.0126 1.1701 0.0623 0.036 Uiso 1 1 calc R U . . .
H24C H 0.0766 0.9771 0.0948 0.036 Uiso 1 1 calc R U . . .
N1 N 0.4914(5) 0.3508(4) 0.6348(2) 0.0259(7) Uani 1 1 d . . . . .
N2 N 0.5189(4) 0.6306(3) 0.1876(2) 0.0144(5) Uani 1 1 d . . . . .
P1 P 0.69111(13) 0.08597(11) 0.77428(7) 0.01909(18) Uani 1 1 d . . . . .
P2 P 0.32309(12) 0.94716(9) 0.26008(7) 0.01403(16) Uani 1 1 d . . . . .
Ni1 Ni 0.72400(6) 0.14997(5) 0.61916(3) 0.01859(9) Uani 1 1 d . . . . .
Ni2 Ni 0.58108(6) 0.84141(5) 0.17017(3) 0.01341(8) Uani 1 1 d . . . . .
Br1 Br 0.77894(5) 0.21075(4) 0.44670(3) 0.02971(9) Uani 1 1 d . . . . .
Br2 Br 0.98754(6) -0.08737(5) 0.61937(3) 0.04204(12) Uani 1 1 d . . . . .
Br3 Br 0.86890(5) 0.74262(4) 0.06433(3) 0.02261(8) Uani 1 1 d . . . . .
Br4 Br 0.61912(4) 1.09810(4) 0.16141(3) 0.01951(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.376(5) . ?
C1 C2 1.395(5) . ?
C1 N1 1.495(4) . ?
C2 C3 1.386(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.405(5) . ?
C5 H5 0.9500 . ?
C6 P1 1.798(4) . ?
C7 N1 1.476(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N1 1.525(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.523(6) . ?
C9 P1 1.808(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.523(6) . ?
C11 P1 1.817(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.387(5) . ?
C13 C18 1.394(5) . ?
C13 N2 1.489(4) . ?
C14 C15 1.394(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.389(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.403(5) . ?
C17 H17 0.9500 . ?
C18 P2 1.794(3) . ?
C19 N2 1.498(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N2 1.500(4) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.522(5) . ?
C21 P2 1.821(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.518(5) . ?
C23 P2 1.823(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N1 Ni1 2.010(3) . ?
N2 Ni2 1.997(3) . ?
P1 Ni1 2.1248(10) . ?
P2 Ni2 2.1290(9) . ?
Ni1 Br2 2.3122(6) . ?
Ni1 Br1 2.3626(5) . ?
Ni2 Br4 2.3107(5) . ?
Ni2 Br3 2.3862(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
C6 C1 C2 120.1(3) . . ?
C6 C1 N1 118.7(3) . . ?
C2 C1 N1 121.2(3) . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 119.5(4) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C1 C6 C5 120.0(4) . . ?
C1 C6 P1 115.7(3) . . ?
C5 C6 P1 124.3(3) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 111.9(3) . . ?
C10 C9 H9A 109.2 . . ?
P1 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
P1 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 113.4(3) . . ?
C12 C11 H11A 108.9 . . ?
P1 C11 H11A 108.9 . . ?
C12 C11 H11B 108.9 . . ?
P1 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C18 120.8(3) . . ?
C14 C13 N2 121.1(3) . . ?
C18 C13 N2 118.2(3) . . ?
C13 C14 C15 119.2(3) . . ?
C13 C14 H14 120.4 . . ?
C15 C14 H14 120.4 . . ?
C16 C15 C14 120.5(3) . . ?
C16 C15 H15 119.8 . . ?
C14 C15 H15 119.8 . . ?
C17 C16 C15 120.2(3) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.0(3) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 H17 120.0 . . ?
C13 C18 C17 119.3(3) . . ?
C13 C18 P2 115.4(2) . . ?
C17 C18 P2 125.2(3) . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P2 112.3(3) . . ?
C22 C21 H21A 109.1 . . ?
P2 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
P2 C21 H21B 109.1 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 112.7(2) . . ?
C24 C23 H23A 109.1 . . ?
P2 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
P2 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 N1 C1 107.9(3) . . ?
C7 N1 C8 110.3(4) . . ?
C1 N1 C8 106.4(3) . . ?
C7 N1 Ni1 110.4(3) . . ?
C1 N1 Ni1 114.7(2) . . ?
C8 N1 Ni1 107.0(3) . . ?
C13 N2 C19 107.7(2) . . ?
C13 N2 C20 107.5(2) . . ?
C19 N2 C20 109.4(3) . . ?
C13 N2 Ni2 115.4(2) . . ?
C19 N2 Ni2 107.8(2) . . ?
C20 N2 Ni2 109.0(2) . . ?
C6 P1 C9 105.16(17) . . ?
C6 P1 C11 106.64(18) . . ?
C9 P1 C11 105.62(18) . . ?
C6 P1 Ni1 102.20(12) . . ?
C9 P1 Ni1 117.33(13) . . ?
C11 P1 Ni1 118.57(14) . . ?
C18 P2 C21 105.47(16) . . ?
C18 P2 C23 107.13(16) . . ?
C21 P2 C23 105.87(16) . . ?
C18 P2 Ni2 102.23(11) . . ?
C21 P2 Ni2 118.92(12) . . ?
C23 P2 Ni2 116.11(12) . . ?
N1 Ni1 P1 88.63(9) . . ?
N1 Ni1 Br2 173.87(9) . . ?
P1 Ni1 Br2 85.25(3) . . ?
N1 Ni1 Br1 94.48(8) . . ?
P1 Ni1 Br1 176.73(3) . . ?
Br2 Ni1 Br1 91.64(2) . . ?
N2 Ni2 P2 88.63(8) . . ?
N2 Ni2 Br4 173.17(8) . . ?
P2 Ni2 Br4 84.55(3) . . ?
N2 Ni2 Br3 95.22(8) . . ?
P2 Ni2 Br3 175.83(3) . . ?
Br4 Ni2 Br3 91.604(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
C6 C1 C2 C3 1.2(6) . . . . ?
N1 C1 C2 C3 -177.2(4) . . . . ?
C1 C2 C3 C4 -0.1(6) . . . . ?
C2 C3 C4 C5 -1.0(6) . . . . ?
C3 C4 C5 C6 0.9(6) . . . . ?
C2 C1 C6 C5 -1.3(5) . . . . ?
N1 C1 C6 C5 177.2(3) . . . . ?
C2 C1 C6 P1 -179.9(3) . . . . ?
N1 C1 C6 P1 -1.5(4) . . . . ?
C4 C5 C6 C1 0.2(5) . . . . ?
C4 C5 C6 P1 178.7(3) . . . . ?
C18 C13 C14 C15 -1.2(5) . . . . ?
N2 C13 C14 C15 178.4(3) . . . . ?
C13 C14 C15 C16 0.7(5) . . . . ?
C14 C15 C16 C17 0.4(5) . . . . ?
C15 C16 C17 C18 -1.0(6) . . . . ?
C14 C13 C18 C17 0.6(5) . . . . ?
N2 C13 C18 C17 -179.0(3) . . . . ?
C14 C13 C18 P2 178.5(3) . . . . ?
N2 C13 C18 P2 -1.1(4) . . . . ?
C16 C17 C18 C13 0.5(5) . . . . ?
C16 C17 C18 P2 -177.2(3) . . . . ?
C6 C1 N1 C7 -124.2(4) . . . . ?
C2 C1 N1 C7 54.3(5) . . . . ?
C6 C1 N1 C8 117.4(4) . . . . ?
C2 C1 N1 C8 -64.1(5) . . . . ?
C6 C1 N1 Ni1 -0.7(4) . . . . ?
C2 C1 N1 Ni1 177.8(3) . . . . ?
C14 C13 N2 C19 -56.1(4) . . . . ?
C18 C13 N2 C19 123.5(3) . . . . ?
C14 C13 N2 C20 61.7(4) . . . . ?
C18 C13 N2 C20 -118.7(3) . . . . ?
C14 C13 N2 Ni2 -176.5(2) . . . . ?
C18 C13 N2 Ni2 3.1(4) . . . . ?
C1 C6 P1 C9 125.7(3) . . . . ?
C5 C6 P1 C9 -52.9(3) . . . . ?
C1 C6 P1 C11 -122.5(3) . . . . ?
C5 C6 P1 C11 58.9(3) . . . . ?
C1 C6 P1 Ni1 2.6(3) . . . . ?
C5 C6 P1 Ni1 -175.9(3) . . . . ?
C10 C9 P1 C6 -64.5(3) . . . . ?
C10 C9 P1 C11 -177.1(3) . . . . ?
C10 C9 P1 Ni1 48.2(4) . . . . ?
C12 C11 P1 C6 66.1(4) . . . . ?
C12 C11 P1 C9 177.6(3) . . . . ?
C12 C11 P1 Ni1 -48.4(4) . . . . ?
C13 C18 P2 C21 -126.1(3) . . . . ?
C17 C18 P2 C21 51.6(3) . . . . ?
C13 C18 P2 C23 121.4(3) . . . . ?
C17 C18 P2 C23 -60.8(3) . . . . ?
C13 C18 P2 Ni2 -1.1(3) . . . . ?
C17 C18 P2 Ni2 176.6(3) . . . . ?
C22 C21 P2 C18 64.7(3) . . . . ?
C22 C21 P2 C23 178.0(3) . . . . ?
C22 C21 P2 Ni2 -49.1(3) . . . . ?
C24 C23 P2 C18 -75.1(3) . . . . ?
C24 C23 P2 C21 172.7(2) . . . . ?
C24 C23 P2 Ni2 38.3(3) . . . . ?

_refine_diff_density_max         0.539
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.060

####################################################################### 
# 
# 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_dagc211007
_database_code_depnum_ccdc_archive 'CCDC 2163658'
loop_
_audit_author_name
_audit_author_address
'Corinne Bailly'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H40 Cl N2 P2 Pd, Cl, 2(H2 O)'
_chemical_formula_sum            'C24 H44 Cl2 N2 O2 P2 Pd'
_chemical_formula_weight         631.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

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

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

_cell_length_a                   13.1872(4)
_cell_length_b                   11.4097(3)
_cell_length_c                   38.4881(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5791.0(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      28.00

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             2624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.959
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6896
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            94671
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         2.117
_diffrn_reflns_theta_max         28.016
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13931
_reflns_number_gt                12131
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.999

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0323P)²+4.6496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5095 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.341(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13931
_refine_ls_number_parameters     611
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0719
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0431(5) 0.7487(4) 0.2753(2) 0.0137(16) Uani 1 1 d . . . . .
C2 C 0.0124(5) 0.8521(6) 0.25931(19) 0.0171(13) Uani 1 1 d . . . . .
H2 H 0.0394 0.9253 0.2666 0.021 Uiso 1 1 calc R U . . .
C3 C -0.0576(5) 0.8471(6) 0.23269(18) 0.0198(14) Uani 1 1 d . . . . .
H3 H -0.0790 0.9173 0.2216 0.024 Uiso 1 1 calc R U . . .
C4 C -0.0968(5) 0.7409(5) 0.2221(3) 0.0197(17) Uani 1 1 d . . . . .
H4 H -0.1447 0.7389 0.2036 0.024 Uiso 1 1 calc R U . . .
C5 C -0.0677(4) 0.6376(6) 0.23777(18) 0.0179(13) Uani 1 1 d . . . . .
H5 H -0.0944 0.5647 0.2301 0.022 Uiso 1 1 calc R U . . .
C6 C 0.0022(4) 0.6423(5) 0.26521(17) 0.0126(12) Uani 1 1 d . . . . .
C7 C 0.0892(4) 0.8359(5) 0.33063(17) 0.0202(12) Uani 1 1 d . . . . .
H7A H 0.1146 0.9143 0.3250 0.030 Uiso 1 1 calc R U . . .
H7B H 0.1175 0.8107 0.3529 0.030 Uiso 1 1 calc R U . . .
H7C H 0.0151 0.8379 0.3322 0.030 Uiso 1 1 calc R U . . .
C8 C 0.2177(4) 0.7903(5) 0.28707(16) 0.0200(12) Uani 1 1 d . . . . .
H8A H 0.2329 0.7415 0.2668 0.030 Uiso 1 1 calc R U . . .
H8B H 0.2723 0.7824 0.3042 0.030 Uiso 1 1 calc R U . . .
H8C H 0.2120 0.8724 0.2799 0.030 Uiso 1 1 calc R U . . .
C9 C 0.0962(5) 0.4171(5) 0.25506(18) 0.0221(14) Uani 1 1 d . . . . .
H9A H 0.1110 0.3398 0.2655 0.027 Uiso 1 1 calc R U . . .
H9B H 0.0446 0.4051 0.2367 0.027 Uiso 1 1 calc R U . . .
C10 C 0.1924(5) 0.4641(6) 0.23842(17) 0.0281(14) Uani 1 1 d . . . . .
H10A H 0.1791 0.5418 0.2286 0.042 Uiso 1 1 calc R U . . .
H10B H 0.2142 0.4108 0.2199 0.042 Uiso 1 1 calc R U . . .
H10C H 0.2458 0.4700 0.2560 0.042 Uiso 1 1 calc R U . . .
C11 C -0.0747(4) 0.4458(5) 0.30253(17) 0.0234(13) Uani 1 1 d . . . . .
H11A H -0.1256 0.4517 0.2837 0.028 Uiso 1 1 calc R U . . .
H11B H -0.0634 0.3616 0.3074 0.028 Uiso 1 1 calc R U . . .
C12 C -0.1163(4) 0.5051(6) 0.33507(19) 0.0296(15) Uani 1 1 d . . . . .
H12A H -0.0728 0.4863 0.3549 0.044 Uiso 1 1 calc R U . . .
H12B H -0.1852 0.4770 0.3396 0.044 Uiso 1 1 calc R U . . .
H12C H -0.1175 0.5902 0.3316 0.044 Uiso 1 1 calc R U . . .
C13 C 0.2263(4) 0.4089(4) 0.39735(14) 0.0133(10) Uani 1 1 d . . . . .
C14 C 0.3216(4) 0.3701(4) 0.40851(15) 0.0153(11) Uani 1 1 d . . . . .
H14 H 0.3714 0.3483 0.3919 0.018 Uiso 1 1 calc R U . . .
C15 C 0.3435(4) 0.3632(5) 0.44369(15) 0.0191(12) Uani 1 1 d . . . . .
H15 H 0.4085 0.3374 0.4510 0.023 Uiso 1 1 calc R U . . .
C16 C 0.2711(5) 0.3939(5) 0.46824(16) 0.0200(12) Uani 1 1 d . . . . .
H16 H 0.2862 0.3885 0.4923 0.024 Uiso 1 1 calc R U . . .
C17 C 0.1761(5) 0.4326(5) 0.45726(16) 0.0189(12) Uani 1 1 d . . . . .
H17 H 0.1264 0.4536 0.4740 0.023 Uiso 1 1 calc R U . . .
C18 C 0.1535(4) 0.4407(5) 0.42191(17) 0.0157(12) Uani 1 1 d . . . . .
C19 C -0.0259(4) 0.4050(5) 0.42454(17) 0.0230(13) Uani 1 1 d . . . . .
H19A H -0.0101 0.3219 0.4211 0.034 Uiso 1 1 calc R U . . .
H19B H -0.0902 0.4237 0.4130 0.034 Uiso 1 1 calc R U . . .
H19C H -0.0318 0.4213 0.4495 0.034 Uiso 1 1 calc R U . . .
C20 C 0.0368(5) 0.6024(5) 0.41647(19) 0.0236(14) Uani 1 1 d . . . . .
H20A H 0.0310 0.6153 0.4416 0.035 Uiso 1 1 calc R U . . .
H20B H -0.0262 0.6265 0.4051 0.035 Uiso 1 1 calc R U . . .
H20C H 0.0934 0.6486 0.4073 0.035 Uiso 1 1 calc R U . . .
C21 C 0.2963(4) 0.3449(4) 0.32788(15) 0.0161(10) Uani 1 1 d . . . . .
H21A H 0.3234 0.2778 0.3413 0.019 Uiso 1 1 calc R U . . .
H21B H 0.2712 0.3138 0.3055 0.019 Uiso 1 1 calc R U . . .
C22 C 0.3831(4) 0.4292(5) 0.32049(17) 0.0234(13) Uani 1 1 d . . . . .
H22A H 0.3583 0.4942 0.3062 0.035 Uiso 1 1 calc R U . . .
H22B H 0.4371 0.3878 0.3081 0.035 Uiso 1 1 calc R U . . .
H22C H 0.4096 0.4599 0.3425 0.035 Uiso 1 1 calc R U . . .
C23 C 0.0956(4) 0.2881(5) 0.34999(17) 0.0154(12) Uani 1 1 d . . . . .
H23A H 0.0301 0.3183 0.3588 0.018 Uiso 1 1 calc R U . . .
H23B H 0.0856 0.2652 0.3254 0.018 Uiso 1 1 calc R U . . .
C24 C 0.1237(5) 0.1791(5) 0.37074(17) 0.0197(12) Uani 1 1 d . . . . .
H24A H 0.1861 0.1451 0.3613 0.030 Uiso 1 1 calc R U . . .
H24B H 0.0687 0.1216 0.3692 0.030 Uiso 1 1 calc R U . . .
H24C H 0.1345 0.2006 0.3951 0.030 Uiso 1 1 calc R U . . .
C25 C 0.7139(5) 0.2545(4) 0.6148(2) 0.0125(15) Uani 1 1 d . . . . .
C26 C 0.7424(4) 0.1515(5) 0.63253(18) 0.0166(13) Uani 1 1 d . . . . .
H26 H 0.7146 0.0779 0.6260 0.020 Uiso 1 1 calc R U . . .
C27 C 0.8114(4) 0.1591(6) 0.65949(17) 0.0170(13) Uani 1 1 d . . . . .
H27 H 0.8311 0.0898 0.6714 0.020 Uiso 1 1 calc R U . . .
C28 C 0.8526(4) 0.2659(6) 0.6696(2) 0.0168(15) Uani 1 1 d . . . . .
H28 H 0.8996 0.2697 0.6883 0.020 Uiso 1 1 calc R U . . .
C29 C 0.8239(4) 0.3669(6) 0.65200(17) 0.0179(13) Uani 1 1 d . . . . .
H29 H 0.8518 0.4404 0.6586 0.022 Uiso 1 1 calc R U . . .
C30 C 0.7538(5) 0.3613(5) 0.62440(19) 0.0162(13) Uani 1 1 d . . . . .
C31 C 0.5386(4) 0.2105(5) 0.60261(16) 0.0188(12) Uani 1 1 d . . . . .
H31A H 0.5464 0.1315 0.6123 0.028 Uiso 1 1 calc R U . . .
H31B H 0.4860 0.2096 0.5846 0.028 Uiso 1 1 calc R U . . .
H31C H 0.5189 0.2648 0.6211 0.028 Uiso 1 1 calc R U . . .
C32 C 0.6712(4) 0.1645(5) 0.55977(16) 0.0209(12) Uani 1 1 d . . . . .
H32A H 0.7386 0.1863 0.5513 0.031 Uiso 1 1 calc R U . . .
H32B H 0.6229 0.1655 0.5404 0.031 Uiso 1 1 calc R U . . .
H32C H 0.6738 0.0856 0.5698 0.031 Uiso 1 1 calc R U . . .
C33 C 0.8300(5) 0.5601(5) 0.58701(18) 0.0256(14) Uani 1 1 d . . . . .
H33A H 0.8168 0.6435 0.5815 0.031 Uiso 1 1 calc R U . . .
H33B H 0.8802 0.5572 0.6061 0.031 Uiso 1 1 calc R U . . .
C34 C 0.8734(4) 0.4999(6) 0.55527(19) 0.0318(16) Uani 1 1 d . . . . .
H34A H 0.8768 0.4152 0.5594 0.048 Uiso 1 1 calc R U . . .
H34B H 0.9417 0.5300 0.5507 0.048 Uiso 1 1 calc R U . . .
H34C H 0.8298 0.5153 0.5352 0.048 Uiso 1 1 calc R U . . .
C35 C 0.6545(5) 0.5822(5) 0.63469(18) 0.0250(15) Uani 1 1 d . . . . .
H35A H 0.7035 0.5948 0.6538 0.030 Uiso 1 1 calc R U . . .
H35B H 0.6368 0.6595 0.6248 0.030 Uiso 1 1 calc R U . . .
C36 C 0.5597(6) 0.5239(6) 0.64884(17) 0.0328(16) Uani 1 1 d . . . . .
H36A H 0.5078 0.5209 0.6306 0.049 Uiso 1 1 calc R U . . .
H36B H 0.5340 0.5690 0.6686 0.049 Uiso 1 1 calc R U . . .
H36C H 0.5760 0.4440 0.6564 0.049 Uiso 1 1 calc R U . . .
C37 C 0.5293(4) 0.5911(4) 0.49212(14) 0.0135(11) Uani 1 1 d . . . . .
C38 C 0.4341(4) 0.6278(5) 0.48069(15) 0.0161(11) Uani 1 1 d . . . . .
H38 H 0.3836 0.6486 0.4972 0.019 Uiso 1 1 calc R U . . .
C39 C 0.4124(4) 0.6340(5) 0.44523(15) 0.0190(12) Uani 1 1 d . . . . .
H39 H 0.3476 0.6596 0.4375 0.023 Uiso 1 1 calc R U . . .
C40 C 0.4862(5) 0.6025(5) 0.42139(17) 0.0198(13) Uani 1 1 d . . . . .
H40 H 0.4715 0.6055 0.3972 0.024 Uiso 1 1 calc R U . . .
C41 C 0.5806(5) 0.5671(5) 0.43233(16) 0.0203(12) Uani 1 1 d . . . . .
H41 H 0.6309 0.5471 0.4157 0.024 Uiso 1 1 calc R U . . .
C42 C 0.6029(4) 0.5602(5) 0.46767(16) 0.0140(12) Uani 1 1 d . . . . .
C43 C 0.7820(4) 0.5985(5) 0.46558(17) 0.0245(13) Uani 1 1 d . . . . .
H43A H 0.7866 0.5853 0.4405 0.037 Uiso 1 1 calc R U . . .
H43B H 0.8468 0.5785 0.4765 0.037 Uiso 1 1 calc R U . . .
H43C H 0.7663 0.6811 0.4700 0.037 Uiso 1 1 calc R U . . .
C44 C 0.7219(5) 0.4006(5) 0.47366(19) 0.0229(14) Uani 1 1 d . . . . .
H44A H 0.6656 0.3538 0.4828 0.034 Uiso 1 1 calc R U . . .
H44B H 0.7849 0.3778 0.4853 0.034 Uiso 1 1 calc R U . . .
H44C H 0.7285 0.3871 0.4486 0.034 Uiso 1 1 calc R U . . .
C45 C 0.6567(4) 0.7140(5) 0.53989(17) 0.0156(12) Uani 1 1 d . . . . .
H45A H 0.6648 0.7377 0.5645 0.019 Uiso 1 1 calc R U . . .
H45B H 0.7232 0.6851 0.5316 0.019 Uiso 1 1 calc R U . . .
C46 C 0.6277(5) 0.8226(5) 0.51858(17) 0.0202(12) Uani 1 1 d . . . . .
H46A H 0.6293 0.8032 0.4938 0.030 Uiso 1 1 calc R U . . .
H46B H 0.6761 0.8858 0.5233 0.030 Uiso 1 1 calc R U . . .
H46C H 0.5593 0.8481 0.5250 0.030 Uiso 1 1 calc R U . . .
C47 C 0.4563(4) 0.6522(4) 0.56135(16) 0.0169(10) Uani 1 1 d . . . . .
H47A H 0.4802 0.6827 0.5840 0.020 Uiso 1 1 calc R U . . .
H47B H 0.4291 0.7194 0.5480 0.020 Uiso 1 1 calc R U . . .
C48 C 0.3686(4) 0.5654(5) 0.56822(17) 0.0219(12) Uani 1 1 d . . . . .
H48A H 0.3432 0.5351 0.5461 0.033 Uiso 1 1 calc R U . . .
H48B H 0.3137 0.6059 0.5805 0.033 Uiso 1 1 calc R U . . .
H48C H 0.3934 0.5002 0.5825 0.033 Uiso 1 1 calc R U . . .
N1 N 0.1204(5) 0.7516(4) 0.30283(19) 0.0132(14) Uani 1 1 d . . . . .
N2 N 0.0552(3) 0.4770(4) 0.40969(13) 0.0167(10) Uani 1 1 d . . . . .
N3 N 0.6380(4) 0.2498(3) 0.5869(2) 0.0115(14) Uani 1 1 d . . . . .
N4 N 0.7020(3) 0.5252(4) 0.48003(13) 0.0178(10) Uani 1 1 d . . . . .
P1 P 0.04342(10) 0.51149(12) 0.28809(4) 0.0143(3) Uani 1 1 d . . . . .
P2 P 0.18899(10) 0.40649(11) 0.35168(4) 0.0122(3) Uani 1 1 d . . . . .
P3 P 0.71245(11) 0.49100(12) 0.60122(4) 0.0151(3) Uani 1 1 d . . . . .
P4 P 0.56542(10) 0.59303(11) 0.53783(4) 0.0123(3) Uani 1 1 d . . . . .
Cl1 Cl 0.27227(10) 0.66933(12) 0.36520(4) 0.0208(3) Uani 1 1 d . . . . .
Cl2 Cl 0.48625(10) 0.32876(12) 0.52403(4) 0.0200(3) Uani 1 1 d . . . . .
Cl3 Cl 0.58876(11) 0.88678(13) 0.61145(4) 0.0226(3) Uani 1 1 d . . . . .
Cl4 Cl 0.84918(11) 0.88541(13) 0.77907(4) 0.0224(3) Uani 1 1 d . . . . .
Pd1 Pd 0.15073(3) 0.58294(3) 0.32764(2) 0.01156(9) Uani 1 1 d . . . . .
Pd2 Pd 0.60600(3) 0.41727(3) 0.56183(2) 0.01157(9) Uani 1 1 d . . . . .
O1 O 0.5202(4) 0.6733(4) 0.72089(13) 0.0426(13) Uani 1 1 d . . . . .
O2 O 0.6693(4) 0.8435(5) 0.72712(14) 0.0440(13) Uani 1 1 d . . . . .
O3 O 0.7695(4) 0.8688(4) 0.66383(14) 0.0400(12) Uani 1 1 d . . . . .
O4 O 0.9213(4) 0.6913(4) 0.66667(13) 0.0358(11) Uani 1 1 d . . . . .
H1W H 0.5652 0.7428 0.7299 0.050 Uiso 1 1 d . . . . .
H2W H 0.4731 0.6509 0.7408 0.050 Uiso 1 1 d . . . . .
H3W H 0.7229 0.8446 0.7421 0.050 Uiso 1 1 d . . . . .
H4W H 0.6952 0.8442 0.7011 0.050 Uiso 1 1 d . . . . .
H5W H 0.8241 0.8307 0.6750 0.050 Uiso 1 1 d . . . . .
H6W H 0.7161 0.8590 0.6451 0.050 Uiso 1 1 d . . . . .
H7W H 0.9644 0.7169 0.6857 0.050 Uiso 1 1 d . . . . .
H8W H 0.9660 0.6737 0.6501 0.050 Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.384(8) . ?
C1 C2 1.390(9) . ?
C1 N1 1.471(10) . ?
C2 C3 1.381(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.379(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.379(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.403(9) . ?
C5 H5 0.9500 . ?
C6 P1 1.816(6) . ?
C7 N1 1.496(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N1 1.486(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.519(9) . ?
C9 P1 1.805(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.525(9) . ?
C11 P1 1.816(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.395(8) . ?
C13 C14 1.400(7) . ?
C13 P2 1.825(6) . ?
C14 C15 1.387(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.388(8) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.396(9) . ?
C17 H17 0.9500 . ?
C18 N2 1.440(7) . ?
C19 N2 1.465(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N2 1.474(7) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.522(7) . ?
C21 P2 1.827(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.524(8) . ?
C23 P2 1.829(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C30 1.378(8) . ?
C25 C26 1.409(8) . ?
C25 N3 1.469(10) . ?
C26 C27 1.383(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.390(9) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.410(9) . ?
C29 H29 0.9500 . ?
C30 P3 1.811(6) . ?
C31 N3 1.513(8) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N3 1.493(8) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.514(10) . ?
C33 P3 1.823(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C36 1.517(10) . ?
C35 P3 1.824(7) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.395(8) . ?
C37 C42 1.397(8) . ?
C37 P4 1.822(6) . ?
C38 C39 1.396(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.385(9) . ?
C39 H39 0.9500 . ?
C40 C41 1.375(9) . ?
C40 H40 0.9500 . ?
C41 C42 1.394(9) . ?
C41 H41 0.9500 . ?
C42 N4 1.447(7) . ?
C43 N4 1.457(7) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N4 1.466(7) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.534(8) . ?
C45 P4 1.833(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.545(7) . ?
C47 P4 1.829(5) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N1 Pd1 2.185(5) . ?
N3 Pd2 2.181(5) . ?
P1 Pd1 2.2326(15) . ?
P2 Pd1 2.2724(14) . ?
P3 Pd2 2.2308(14) . ?
P4 Pd2 2.2719(14) . ?
Cl1 Pd1 2.3728(14) . ?
Cl2 Pd2 2.3729(14) . ?
O1 H1W 1.0495 . ?
O1 H2W 1.0192 . ?
O2 H3W 0.9120 . ?
O2 H4W 1.0578 . ?
O3 H5W 0.9446 . ?
O3 H6W 1.0139 . ?
O4 H7W 0.9720 . ?
O4 H8W 0.8913 . ?

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
C6 C1 C2 120.4(7) . . ?
C6 C1 N1 119.5(5) . . ?
C2 C1 N1 120.1(5) . . ?
C3 C2 C1 119.2(6) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 120.4(7) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C5 C4 C3 121.2(8) . . ?
C5 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
C4 C5 C6 118.7(7) . . ?
C4 C5 H5 120.7 . . ?
C6 C5 H5 120.7 . . ?
C1 C6 C5 120.1(6) . . ?
C1 C6 P1 117.9(5) . . ?
C5 C6 P1 122.0(5) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 114.1(4) . . ?
C10 C9 H9A 108.7 . . ?
P1 C9 H9A 108.7 . . ?
C10 C9 H9B 108.7 . . ?
P1 C9 H9B 108.7 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 112.1(4) . . ?
C12 C11 H11A 109.2 . . ?
P1 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
P1 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 119.5(5) . . ?
C18 C13 P2 118.1(4) . . ?
C14 C13 P2 122.2(4) . . ?
C15 C14 C13 120.3(5) . . ?
C15 C14 H14 119.8 . . ?
C13 C14 H14 119.8 . . ?
C14 C15 C16 120.4(5) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C17 119.5(6) . . ?
C15 C16 H16 120.3 . . ?
C17 C16 H16 120.3 . . ?
C16 C17 C18 120.6(6) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C13 C18 C17 119.7(5) . . ?
C13 C18 N2 118.2(5) . . ?
C17 C18 N2 122.0(5) . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P2 115.6(4) . . ?
C22 C21 H21A 108.4 . . ?
P2 C21 H21A 108.4 . . ?
C22 C21 H21B 108.4 . . ?
P2 C21 H21B 108.4 . . ?
H21A C21 H21B 107.4 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 114.8(4) . . ?
C24 C23 H23A 108.6 . . ?
P2 C23 H23A 108.6 . . ?
C24 C23 H23B 108.6 . . ?
P2 C23 H23B 108.6 . . ?
H23A C23 H23B 107.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C30 C25 C26 120.4(7) . . ?
C30 C25 N3 119.2(5) . . ?
C26 C25 N3 120.4(5) . . ?
C27 C26 C25 119.1(6) . . ?
C27 C26 H26 120.5 . . ?
C25 C26 H26 120.5 . . ?
C26 C27 C28 121.5(6) . . ?
C26 C27 H27 119.2 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 C29 119.0(7) . . ?
C27 C28 H28 120.5 . . ?
C29 C28 H28 120.5 . . ?
C28 C29 C30 120.5(6) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C25 C30 C29 119.5(6) . . ?
C25 C30 P3 118.4(5) . . ?
C29 C30 P3 122.1(5) . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 P3 111.5(4) . . ?
C34 C33 H33A 109.3 . . ?
P3 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
P3 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 C35 P3 110.4(4) . . ?
C36 C35 H35A 109.6 . . ?
P3 C35 H35A 109.6 . . ?
C36 C35 H35B 109.6 . . ?
P3 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C42 119.2(5) . . ?
C38 C37 P4 122.4(4) . . ?
C42 C37 P4 118.2(4) . . ?
C37 C38 C39 120.6(5) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 H38 119.7 . . ?
C40 C39 C38 119.3(5) . . ?
C40 C39 H39 120.3 . . ?
C38 C39 H39 120.3 . . ?
C41 C40 C39 120.6(6) . . ?
C41 C40 H40 119.7 . . ?
C39 C40 H40 119.7 . . ?
C40 C41 C42 120.4(6) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C41 C42 C37 119.8(5) . . ?
C41 C42 N4 121.8(5) . . ?
C37 C42 N4 118.4(5) . . ?
N4 C43 H43A 109.5 . . ?
N4 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
N4 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N4 C44 H44A 109.5 . . ?
N4 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
N4 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C46 C45 P4 115.0(4) . . ?
C46 C45 H45A 108.5 . . ?
P4 C45 H45A 108.5 . . ?
C46 C45 H45B 108.5 . . ?
P4 C45 H45B 108.5 . . ?
H45A C45 H45B 107.5 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 P4 115.9(4) . . ?
C48 C47 H47A 108.3 . . ?
P4 C47 H47A 108.3 . . ?
C48 C47 H47B 108.3 . . ?
P4 C47 H47B 108.3 . . ?
H47A C47 H47B 107.4 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C1 N1 C8 108.1(6) . . ?
C1 N1 C7 109.8(5) . . ?
C8 N1 C7 109.8(5) . . ?
C1 N1 Pd1 114.9(3) . . ?
C8 N1 Pd1 106.4(4) . . ?
C7 N1 Pd1 107.7(4) . . ?
C18 N2 C19 111.6(5) . . ?
C18 N2 C20 111.7(5) . . ?
C19 N2 C20 110.8(5) . . ?
C25 N3 C32 109.6(5) . . ?
C25 N3 C31 108.0(6) . . ?
C32 N3 C31 109.9(4) . . ?
C25 N3 Pd2 115.1(3) . . ?
C32 N3 Pd2 108.6(5) . . ?
C31 N3 Pd2 105.6(3) . . ?
C42 N4 C43 111.7(5) . . ?
C42 N4 C44 112.0(5) . . ?
C43 N4 C44 111.3(5) . . ?
C9 P1 C6 105.3(3) . . ?
C9 P1 C11 107.5(3) . . ?
C6 P1 C11 103.3(3) . . ?
C9 P1 Pd1 117.0(2) . . ?
C6 P1 Pd1 102.7(2) . . ?
C11 P1 Pd1 119.1(2) . . ?
C13 P2 C21 106.3(3) . . ?
C13 P2 C23 103.1(3) . . ?
C21 P2 C23 102.7(3) . . ?
C13 P2 Pd1 116.00(17) . . ?
C21 P2 Pd1 107.99(19) . . ?
C23 P2 Pd1 119.36(19) . . ?
C30 P3 C33 104.2(3) . . ?
C30 P3 C35 104.1(3) . . ?
C33 P3 C35 108.7(3) . . ?
C30 P3 Pd2 102.5(2) . . ?
C33 P3 Pd2 119.6(2) . . ?
C35 P3 Pd2 115.6(2) . . ?
C37 P4 C47 106.1(3) . . ?
C37 P4 C45 102.8(3) . . ?
C47 P4 C45 102.5(3) . . ?
C37 P4 Pd2 116.34(17) . . ?
C47 P4 Pd2 108.04(18) . . ?
C45 P4 Pd2 119.5(2) . . ?
N1 Pd1 P1 84.71(17) . . ?
N1 Pd1 P2 177.17(18) . . ?
P1 Pd1 P2 95.45(5) . . ?
N1 Pd1 Cl1 91.36(17) . . ?
P1 Pd1 Cl1 174.40(6) . . ?
P2 Pd1 Cl1 88.28(5) . . ?
N3 Pd2 P3 84.72(17) . . ?
N3 Pd2 P4 176.83(18) . . ?
P3 Pd2 P4 95.26(5) . . ?
N3 Pd2 Cl2 91.56(16) . . ?
P3 Pd2 Cl2 174.85(6) . . ?
P4 Pd2 Cl2 88.25(5) . . ?
H1W O1 H2W 106.6 . . ?
H3W O2 H4W 110.4 . . ?
H5W O3 H6W 143.3 . . ?
H7W O4 H8W 102.7 . . ?

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
C6 C1 C2 C3 -1.5(11) . . . . ?
N1 C1 C2 C3 177.8(6) . . . . ?
C1 C2 C3 C4 0.1(10) . . . . ?
C2 C3 C4 C5 0.3(12) . . . . ?
C3 C4 C5 C6 0.7(11) . . . . ?
C2 C1 C6 C5 2.6(11) . . . . ?
N1 C1 C6 C5 -176.7(6) . . . . ?
C2 C1 C6 P1 -178.3(5) . . . . ?
N1 C1 C6 P1 2.4(9) . . . . ?
C4 C5 C6 C1 -2.2(10) . . . . ?
C4 C5 C6 P1 178.8(6) . . . . ?
C18 C13 C14 C15 0.0(8) . . . . ?
P2 C13 C14 C15 -174.0(4) . . . . ?
C13 C14 C15 C16 0.5(8) . . . . ?
C14 C15 C16 C17 -0.5(8) . . . . ?
C15 C16 C17 C18 0.0(9) . . . . ?
C14 C13 C18 C17 -0.5(8) . . . . ?
P2 C13 C18 C17 173.8(4) . . . . ?
C14 C13 C18 N2 -178.2(5) . . . . ?
P2 C13 C18 N2 -4.0(7) . . . . ?
C16 C17 C18 C13 0.5(9) . . . . ?
C16 C17 C18 N2 178.2(5) . . . . ?
C30 C25 C26 C27 -0.4(10) . . . . ?
N3 C25 C26 C27 -177.8(6) . . . . ?
C25 C26 C27 C28 0.4(10) . . . . ?
C26 C27 C28 C29 -0.4(10) . . . . ?
C27 C28 C29 C30 0.3(10) . . . . ?
C26 C25 C30 C29 0.3(10) . . . . ?
N3 C25 C30 C29 177.8(6) . . . . ?
C26 C25 C30 P3 -178.8(5) . . . . ?
N3 C25 C30 P3 -1.4(9) . . . . ?
C28 C29 C30 C25 -0.3(10) . . . . ?
C28 C29 C30 P3 178.9(5) . . . . ?
C42 C37 C38 C39 -0.3(8) . . . . ?
P4 C37 C38 C39 174.7(4) . . . . ?
C37 C38 C39 C40 0.5(8) . . . . ?
C38 C39 C40 C41 -1.0(8) . . . . ?
C39 C40 C41 C42 1.2(9) . . . . ?
C40 C41 C42 C37 -0.9(9) . . . . ?
C40 C41 C42 N4 -178.9(5) . . . . ?
C38 C37 C42 C41 0.4(8) . . . . ?
P4 C37 C42 C41 -174.8(4) . . . . ?
C38 C37 C42 N4 178.5(5) . . . . ?
P4 C37 C42 N4 3.3(7) . . . . ?
C6 C1 N1 C8 113.5(7) . . . . ?
C2 C1 N1 C8 -65.8(8) . . . . ?
C6 C1 N1 C7 -126.8(6) . . . . ?
C2 C1 N1 C7 54.0(9) . . . . ?
C6 C1 N1 Pd1 -5.2(9) . . . . ?
C2 C1 N1 Pd1 175.6(5) . . . . ?
C13 C18 N2 C19 123.1(6) . . . . ?
C17 C18 N2 C19 -54.6(7) . . . . ?
C13 C18 N2 C20 -112.3(6) . . . . ?
C17 C18 N2 C20 70.0(7) . . . . ?
C30 C25 N3 C32 126.5(6) . . . . ?
C26 C25 N3 C32 -56.1(8) . . . . ?
C30 C25 N3 C31 -113.9(6) . . . . ?
C26 C25 N3 C31 63.6(7) . . . . ?
C30 C25 N3 Pd2 3.8(8) . . . . ?
C26 C25 N3 Pd2 -178.8(5) . . . . ?
C41 C42 N4 C43 55.5(7) . . . . ?
C37 C42 N4 C43 -122.5(6) . . . . ?
C41 C42 N4 C44 -70.1(7) . . . . ?
C37 C42 N4 C44 111.9(6) . . . . ?
C10 C9 P1 C6 66.4(5) . . . . ?
C10 C9 P1 C11 176.1(5) . . . . ?
C10 C9 P1 Pd1 -46.9(5) . . . . ?
C1 C6 P1 C9 -121.6(6) . . . . ?
C5 C6 P1 C9 57.5(6) . . . . ?
C1 C6 P1 C11 125.8(6) . . . . ?
C5 C6 P1 C11 -55.2(6) . . . . ?
C1 C6 P1 Pd1 1.4(6) . . . . ?
C5 C6 P1 Pd1 -179.6(5) . . . . ?
C12 C11 P1 C9 169.2(4) . . . . ?
C12 C11 P1 C6 -79.7(5) . . . . ?
C12 C11 P1 Pd1 33.3(5) . . . . ?
C18 C13 P2 C21 -173.3(4) . . . . ?
C14 C13 P2 C21 0.8(5) . . . . ?
C18 C13 P2 C23 -65.6(5) . . . . ?
C14 C13 P2 C23 108.4(5) . . . . ?
C18 C13 P2 Pd1 66.7(5) . . . . ?
C14 C13 P2 Pd1 -119.2(4) . . . . ?
C22 C21 P2 C13 -79.8(5) . . . . ?
C22 C21 P2 C23 172.3(4) . . . . ?
C22 C21 P2 Pd1 45.3(5) . . . . ?
C24 C23 P2 C13 -42.4(5) . . . . ?
C24 C23 P2 C21 68.0(5) . . . . ?
C24 C23 P2 Pd1 -172.7(4) . . . . ?
C25 C30 P3 C33 -126.8(6) . . . . ?
C29 C30 P3 C33 54.1(6) . . . . ?
C25 C30 P3 C35 119.3(6) . . . . ?
C29 C30 P3 C35 -59.8(6) . . . . ?
C25 C30 P3 Pd2 -1.4(6) . . . . ?
C29 C30 P3 Pd2 179.4(5) . . . . ?
C34 C33 P3 C30 78.7(5) . . . . ?
C34 C33 P3 C35 -170.8(4) . . . . ?
C34 C33 P3 Pd2 -34.9(5) . . . . ?
C36 C35 P3 C30 -65.8(5) . . . . ?
C36 C35 P3 C33 -176.5(5) . . . . ?
C36 C35 P3 Pd2 45.7(5) . . . . ?
C38 C37 P4 C47 -1.1(5) . . . . ?
C42 C37 P4 C47 173.9(4) . . . . ?
C38 C37 P4 C45 -108.4(5) . . . . ?
C42 C37 P4 C45 66.6(5) . . . . ?
C38 C37 P4 Pd2 119.0(4) . . . . ?
C42 C37 P4 Pd2 -66.0(4) . . . . ?
C48 C47 P4 C37 79.4(5) . . . . ?
C48 C47 P4 C45 -173.1(4) . . . . ?
C48 C47 P4 Pd2 -46.0(5) . . . . ?
C46 C45 P4 C37 41.2(5) . . . . ?
C46 C45 P4 C47 -68.8(5) . . . . ?
C46 C45 P4 Pd2 171.9(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H2W Cl4 1.02 2.24 3.248(5) 170.5 3_465
O2 H3W Cl4 0.91 2.24 3.139(5) 168.7 .
O2 H4W O3 1.06 1.76 2.786(7) 162.3 .
O3 H5W O4 0.94 2.07 2.850(7) 139.1 .
O3 H6W Cl3 1.01 2.14 3.129(5) 163.1 .
O4 H7W O1 0.97 1.99 2.906(7) 156.9 3_565
O4 H8W Cl3 0.89 2.30 3.192(5) 173.7 3_565

_refine_diff_density_max         2.453
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.088

####################################################################### 
# 
# 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_dagc211001
_database_code_depnum_ccdc_archive 'CCDC 2163751'
loop_
_audit_author_name
_audit_author_address
'Corinne Bailly'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H20 Cl2 N P Pd, 2(C H Cl3)'
_chemical_formula_sum            'C14 H22 Cl8 N P Pd'
_chemical_formula_weight         625.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   17.0385(7)
_cell_length_b                   8.8900(3)
_cell_length_c                   32.4365(14)
_cell_angle_alpha                90
_cell_angle_beta                 92.933(2)
_cell_angle_gamma                90
_cell_volume                     4906.8(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9540
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.98

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_F_000             2480
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    1.694
_shelx_estimated_absorpt_T_min   0.785
_shelx_estimated_absorpt_T_max   0.876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6858
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            145578
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_theta_min         2.376
_diffrn_reflns_theta_max         29.051
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13078
_reflns_number_gt                9676
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0228P)²+12.6917P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13078
_refine_ls_number_parameters     459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0784
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2846(2) 0.1545(4) 0.92843(11) 0.0182(7) Uani 1 1 d . . . . .
C2 C 0.3037(2) 0.1391(4) 0.97058(11) 0.0200(7) Uani 1 1 d . . . . .
H2 H 0.3130 0.2257 0.9873 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3088(2) -0.0027(4) 0.98786(11) 0.0236(8) Uani 1 1 d . . . . .
H3 H 0.3217 -0.0128 1.0166 0.028 Uiso 1 1 calc R U . . .
C4 C 0.2956(2) -0.1306(4) 0.96398(11) 0.0226(8) Uani 1 1 d . . . . .
H4 H 0.2993 -0.2275 0.9762 0.027 Uiso 1 1 calc R U . . .
C5 C 0.2772(2) -0.1158(4) 0.92246(11) 0.0216(8) Uani 1 1 d . . . . .
H5 H 0.2682 -0.2031 0.9060 0.026 Uiso 1 1 calc R U . . .
C6 C 0.2714(2) 0.0268(4) 0.90427(10) 0.0174(7) Uani 1 1 d . . . . .
C7 C 0.3537(2) 0.3884(4) 0.91594(12) 0.0266(8) Uani 1 1 d . . . . .
H7A H 0.3657 0.4017 0.9456 0.040 Uiso 1 1 calc R U . . .
H7B H 0.3495 0.4871 0.9026 0.040 Uiso 1 1 calc R U . . .
H7C H 0.3959 0.3305 0.9039 0.040 Uiso 1 1 calc R U . . .
C8 C 0.2139(2) 0.3903(4) 0.92943(11) 0.0237(8) Uani 1 1 d . . . . .
H8A H 0.1645 0.3341 0.9262 0.036 Uiso 1 1 calc R U . . .
H8B H 0.2074 0.4893 0.9164 0.036 Uiso 1 1 calc R U . . .
H8C H 0.2281 0.4032 0.9589 0.036 Uiso 1 1 calc R U . . .
C9 C 0.1548(2) -0.0389(4) 0.83813(11) 0.0224(8) Uani 1 1 d . . . . .
H9A H 0.1379 -0.0181 0.8090 0.027 Uiso 1 1 calc R U . . .
H9B H 0.1633 -0.1486 0.8409 0.027 Uiso 1 1 calc R U . . .
C10 C 0.0896(2) 0.0080(6) 0.86571(14) 0.0374(11) Uani 1 1 d . . . . .
H10A H 0.1029 -0.0240 0.8941 0.056 Uiso 1 1 calc R U . . .
H10B H 0.0401 -0.0394 0.8559 0.056 Uiso 1 1 calc R U . . .
H10C H 0.0837 0.1176 0.8649 0.056 Uiso 1 1 calc R U . . .
C11 C 0.3211(2) -0.0356(4) 0.82181(11) 0.0200(7) Uani 1 1 d . . . . .
H11A H 0.3245 -0.1424 0.8304 0.024 Uiso 1 1 calc R U . . .
H11B H 0.3055 -0.0330 0.7920 0.024 Uiso 1 1 calc R U . . .
C12 C 0.4019(2) 0.0377(5) 0.82871(13) 0.0305(9) Uani 1 1 d . . . . .
H12A H 0.3998 0.1412 0.8183 0.046 Uiso 1 1 calc R U . . .
H12B H 0.4408 -0.0195 0.8139 0.046 Uiso 1 1 calc R U . . .
H12C H 0.4169 0.0384 0.8583 0.046 Uiso 1 1 calc R U . . .
C13 C 0.2296(2) -0.0980(4) 0.67730(10) 0.0163(7) Uani 1 1 d . . . . .
C14 C 0.2088(2) -0.1090(4) 0.71816(11) 0.0206(7) Uani 1 1 d . . . . .
H14 H 0.2028 -0.0212 0.7344 0.025 Uiso 1 1 calc R U . . .
C15 C 0.1970(2) -0.2505(5) 0.73480(12) 0.0253(8) Uani 1 1 d . . . . .
H15 H 0.1835 -0.2590 0.7628 0.030 Uiso 1 1 calc R U . . .
C16 C 0.2047(2) -0.3798(4) 0.71148(12) 0.0259(8) Uani 1 1 d . . . . .
H16 H 0.1960 -0.4758 0.7233 0.031 Uiso 1 1 calc R U . . .
C17 C 0.2249(2) -0.3683(4) 0.67091(11) 0.0227(8) Uani 1 1 d . . . . .
H17 H 0.2302 -0.4564 0.6547 0.027 Uiso 1 1 calc R U . . .
C18 C 0.2378(2) -0.2262(4) 0.65371(10) 0.0170(7) Uani 1 1 d . . . . .
C19 C 0.1730(2) 0.1483(4) 0.66217(12) 0.0255(8) Uani 1 1 d . . . . .
H19A H 0.1278 0.1001 0.6477 0.038 Uiso 1 1 calc R U . . .
H19B H 0.1825 0.2465 0.6496 0.038 Uiso 1 1 calc R U . . .
H19C H 0.1620 0.1621 0.6913 0.038 Uiso 1 1 calc R U . . .
C20 C 0.3126(2) 0.1236(5) 0.68223(11) 0.0258(8) Uani 1 1 d . . . . .
H20A H 0.2991 0.1427 0.7108 0.039 Uiso 1 1 calc R U . . .
H20B H 0.3252 0.2190 0.6689 0.039 Uiso 1 1 calc R U . . .
H20C H 0.3582 0.0565 0.6821 0.039 Uiso 1 1 calc R U . . .
C21 C 0.3572(2) -0.2971(4) 0.59583(11) 0.0209(7) Uani 1 1 d . . . . .
H21A H 0.3504 -0.4046 0.6027 0.025 Uiso 1 1 calc R U . . .
H21B H 0.3717 -0.2908 0.5667 0.025 Uiso 1 1 calc R U . . .
C22 C 0.4237(2) -0.2311(5) 0.62371(13) 0.0275(9) Uani 1 1 d . . . . .
H22A H 0.4321 -0.1258 0.6162 0.041 Uiso 1 1 calc R U . . .
H22B H 0.4720 -0.2884 0.6202 0.041 Uiso 1 1 calc R U . . .
H22C H 0.4095 -0.2368 0.6526 0.041 Uiso 1 1 calc R U . . .
C23 C 0.1911(2) -0.2926(4) 0.56832(11) 0.0223(8) Uani 1 1 d . . . . .
H23A H 0.2032 -0.2764 0.5391 0.027 Uiso 1 1 calc R U . . .
H23B H 0.1931 -0.4021 0.5738 0.027 Uiso 1 1 calc R U . . .
C24 C 0.1086(2) -0.2355(5) 0.57499(14) 0.0333(10) Uani 1 1 d . . . . .
H24A H 0.0942 -0.2603 0.6031 0.050 Uiso 1 1 calc R U . . .
H24B H 0.0714 -0.2831 0.5550 0.050 Uiso 1 1 calc R U . . .
H24C H 0.1070 -0.1261 0.5712 0.050 Uiso 1 1 calc R U . . .
C25 C 0.0480(3) 0.5047(6) 0.81808(16) 0.0458(12) Uani 1 1 d . . . . .
H25 H 0.1043 0.4829 0.8131 0.055 Uiso 1 1 calc R U . . .
C26 C 0.5243(2) 0.7748(5) 0.94048(13) 0.0299(9) Uani 1 1 d . . . . .
H26 H 0.5827 0.7625 0.9432 0.036 Uiso 1 1 calc R U . . .
C27 C 0.3921(2) 0.5445(5) 0.76474(12) 0.0282(9) Uani 1 1 d . . . . .
H27 H 0.3369 0.5417 0.7738 0.034 Uiso 1 1 calc R U . . .
C28 C 0.1098(2) 0.2955(5) 0.52729(13) 0.0320(9) Uani 1 1 d . . . . .
H28 H 0.1669 0.2850 0.5354 0.038 Uiso 1 1 calc R U . . .
N1 N 0.27751(17) 0.3054(3) 0.90942(8) 0.0166(6) Uani 1 1 d . . . . .
N2 N 0.24411(17) 0.0511(3) 0.65903(8) 0.0162(6) Uani 1 1 d . . . . .
P1 P 0.24683(5) 0.05765(10) 0.85030(3) 0.01633(18) Uani 1 1 d . . . . .
P2 P 0.26536(5) -0.19952(10) 0.60140(3) 0.01527(17) Uani 1 1 d . . . . .
Cl1 Cl 0.24854(5) 0.57268(10) 0.83875(3) 0.02119(18) Uani 1 1 d . . . . .
Cl2 Cl 0.21064(6) 0.27271(10) 0.77680(3) 0.0268(2) Uani 1 1 d . . . . .
Cl3 Cl 0.28277(5) 0.31434(9) 0.59028(3) 0.02110(18) Uani 1 1 d . . . . .
Cl4 Cl 0.31142(6) 0.00621(10) 0.53066(3) 0.0268(2) Uani 1 1 d . . . . .
Cl5 Cl -0.00656(9) 0.34026(19) 0.81054(6) 0.0689(4) Uani 1 1 d . . . . .
Cl6 Cl 0.01594(9) 0.6495(2) 0.78605(6) 0.0882(7) Uani 1 1 d . . . . .
Cl7 Cl 0.04057(8) 0.5617(2) 0.87036(5) 0.0660(4) Uani 1 1 d . . . . .
Cl8 Cl 0.48970(8) 0.70147(14) 0.89237(4) 0.0454(3) Uani 1 1 d . . . . .
Cl9 Cl 0.50151(6) 0.96783(11) 0.94348(3) 0.0314(2) Uani 1 1 d . . . . .
Cl10 Cl 0.48216(7) 0.67676(13) 0.98103(4) 0.0442(3) Uani 1 1 d . . . . .
Cl11 Cl 0.39879(7) 0.42889(14) 0.72124(4) 0.0428(3) Uani 1 1 d . . . . .
Cl12 Cl 0.41514(8) 0.72960(13) 0.75143(4) 0.0483(3) Uani 1 1 d . . . . .
Cl13 Cl 0.45517(8) 0.47910(17) 0.80534(4) 0.0519(3) Uani 1 1 d . . . . .
Cl14 Cl 0.07417(8) 0.12095(15) 0.50945(5) 0.0537(3) Uani 1 1 d . . . . .
Cl15 Cl 0.09903(7) 0.43092(13) 0.48816(3) 0.0381(3) Uani 1 1 d . . . . .
Cl16 Cl 0.05955(7) 0.35288(15) 0.57099(4) 0.0446(3) Uani 1 1 d . . . . .
Pd1 Pd 0.24685(2) 0.30290(3) 0.84553(2) 0.01600(6) Uani 1 1 d . . . . .
Pd2 Pd 0.27354(2) 0.04471(3) 0.59670(2) 0.01471(6) 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 C6 1.391(5) . ?
C1 C2 1.395(5) . ?
C1 N1 1.479(4) . ?
C2 C3 1.381(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.373(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.400(5) . ?
C5 H5 0.9500 . ?
C6 P1 1.800(4) . ?
C7 N1 1.499(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 N1 1.496(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.520(5) . ?
C9 P1 1.813(4) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.529(5) . ?
C11 P1 1.806(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C18 1.384(5) . ?
C13 C14 1.393(5) . ?
C13 N2 1.478(4) . ?
C14 C15 1.388(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.386(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.381(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.403(5) . ?
C17 H17 0.9500 . ?
C18 P2 1.799(3) . ?
C19 N2 1.496(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 N2 1.501(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.530(5) . ?
C21 P2 1.806(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.521(5) . ?
C23 P2 1.816(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 Cl6 1.726(5) . ?
C25 Cl5 1.743(5) . ?
C25 Cl7 1.781(5) . ?
C25 H25 1.0000 . ?
C26 Cl10 1.762(4) . ?
C26 Cl9 1.763(4) . ?
C26 Cl8 1.765(4) . ?
C26 H26 1.0000 . ?
C27 Cl12 1.751(4) . ?
C27 Cl11 1.754(4) . ?
C27 Cl13 1.755(4) . ?
C27 H27 1.0000 . ?
C28 Cl15 1.752(4) . ?
C28 Cl14 1.754(5) . ?
C28 Cl16 1.768(4) . ?
C28 H28 1.0000 . ?
N1 Pd1 2.111(3) . ?
N2 Pd2 2.108(3) . ?
P1 Pd1 2.1857(9) . ?
P2 Pd2 2.1815(9) . ?
Cl1 Pd1 2.4087(9) . ?
Cl2 Pd1 2.2982(9) . ?
Cl3 Pd2 2.4119(9) . ?
Cl4 Pd2 2.2941(9) . ?

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
C6 C1 C2 119.6(3) . . ?
C6 C1 N1 119.9(3) . . ?
C2 C1 N1 120.5(3) . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 121.1(3) . . ?
C2 C3 H3 119.5 . . ?
C4 C3 H3 119.5 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 119.7(3) . . ?
C1 C6 P1 116.5(3) . . ?
C5 C6 P1 123.7(3) . . ?
N1 C7 H7A 109.5 . . ?
N1 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
N1 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 P1 113.1(3) . . ?
C10 C9 H9A 109.0 . . ?
P1 C9 H9A 109.0 . . ?
C10 C9 H9B 109.0 . . ?
P1 C9 H9B 109.0 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P1 112.2(3) . . ?
C12 C11 H11A 109.2 . . ?
P1 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
P1 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C18 C13 C14 120.4(3) . . ?
C18 C13 N2 119.6(3) . . ?
C14 C13 N2 120.1(3) . . ?
C15 C14 C13 118.9(3) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
C16 C15 C14 121.3(3) . . ?
C16 C15 H15 119.3 . . ?
C14 C15 H15 119.3 . . ?
C17 C16 C15 119.6(4) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C13 C18 C17 120.0(3) . . ?
C13 C18 P2 116.8(3) . . ?
C17 C18 P2 123.2(3) . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 H20A 109.5 . . ?
N2 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N2 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C22 C21 P2 112.1(3) . . ?
C22 C21 H21A 109.2 . . ?
P2 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
P2 C21 H21B 109.2 . . ?
H21A C21 H21B 107.9 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 P2 112.7(3) . . ?
C24 C23 H23A 109.1 . . ?
P2 C23 H23A 109.1 . . ?
C24 C23 H23B 109.1 . . ?
P2 C23 H23B 109.1 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Cl6 C25 Cl5 113.0(3) . . ?
Cl6 C25 Cl7 109.0(3) . . ?
Cl5 C25 Cl7 108.0(3) . . ?
Cl6 C25 H25 108.9 . . ?
Cl5 C25 H25 108.9 . . ?
Cl7 C25 H25 108.9 . . ?
Cl10 C26 Cl9 109.9(2) . . ?
Cl10 C26 Cl8 110.3(2) . . ?
Cl9 C26 Cl8 110.1(2) . . ?
Cl10 C26 H26 108.8 . . ?
Cl9 C26 H26 108.8 . . ?
Cl8 C26 H26 108.8 . . ?
Cl12 C27 Cl11 109.1(2) . . ?
Cl12 C27 Cl13 111.1(2) . . ?
Cl11 C27 Cl13 110.3(2) . . ?
Cl12 C27 H27 108.7 . . ?
Cl11 C27 H27 108.7 . . ?
Cl13 C27 H27 108.7 . . ?
Cl15 C28 Cl14 110.3(2) . . ?
Cl15 C28 Cl16 110.2(2) . . ?
Cl14 C28 Cl16 110.3(2) . . ?
Cl15 C28 H28 108.7 . . ?
Cl14 C28 H28 108.7 . . ?
Cl16 C28 H28 108.7 . . ?
C1 N1 C8 108.8(3) . . ?
C1 N1 C7 109.6(3) . . ?
C8 N1 C7 109.4(3) . . ?
C1 N1 Pd1 114.2(2) . . ?
C8 N1 Pd1 106.4(2) . . ?
C7 N1 Pd1 108.2(2) . . ?
C13 N2 C19 109.7(3) . . ?
C13 N2 C20 109.0(3) . . ?
C19 N2 C20 109.2(3) . . ?
C13 N2 Pd2 114.4(2) . . ?
C19 N2 Pd2 108.3(2) . . ?
C20 N2 Pd2 106.0(2) . . ?
C6 P1 C11 107.08(17) . . ?
C6 P1 C9 107.16(17) . . ?
C11 P1 C9 106.99(17) . . ?
C6 P1 Pd1 102.70(12) . . ?
C11 P1 Pd1 114.77(12) . . ?
C9 P1 Pd1 117.38(13) . . ?
C18 P2 C21 107.49(17) . . ?
C18 P2 C23 106.83(17) . . ?
C21 P2 C23 107.65(17) . . ?
C18 P2 Pd2 102.58(12) . . ?
C21 P2 Pd2 114.34(13) . . ?
C23 P2 Pd2 117.20(13) . . ?
N1 Pd1 P1 86.68(8) . . ?
N1 Pd1 Cl2 173.76(8) . . ?
P1 Pd1 Cl2 87.20(3) . . ?
N1 Pd1 Cl1 94.33(8) . . ?
P1 Pd1 Cl1 178.61(3) . . ?
Cl2 Pd1 Cl1 91.81(3) . . ?
N2 Pd2 P2 86.60(8) . . ?
N2 Pd2 Cl4 172.45(8) . . ?
P2 Pd2 Cl4 86.50(3) . . ?
N2 Pd2 Cl3 94.34(8) . . ?
P2 Pd2 Cl3 179.05(3) . . ?
Cl4 Pd2 Cl3 92.58(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 C3 -0.3(5) . . . . ?
N1 C1 C2 C3 179.0(3) . . . . ?
C1 C2 C3 C4 0.2(6) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 C6 -0.2(6) . . . . ?
C2 C1 C6 C5 0.1(5) . . . . ?
N1 C1 C6 C5 -179.2(3) . . . . ?
C2 C1 C6 P1 179.8(3) . . . . ?
N1 C1 C6 P1 0.5(4) . . . . ?
C4 C5 C6 C1 0.1(6) . . . . ?
C4 C5 C6 P1 -179.5(3) . . . . ?
C18 C13 C14 C15 0.4(5) . . . . ?
N2 C13 C14 C15 -178.7(3) . . . . ?
C13 C14 C15 C16 -0.7(6) . . . . ?
C14 C15 C16 C17 0.5(6) . . . . ?
C15 C16 C17 C18 0.1(6) . . . . ?
C14 C13 C18 C17 0.2(5) . . . . ?
N2 C13 C18 C17 179.3(3) . . . . ?
C14 C13 C18 P2 -179.6(3) . . . . ?
N2 C13 C18 P2 -0.5(4) . . . . ?
C16 C17 C18 C13 -0.5(6) . . . . ?
C16 C17 C18 P2 179.4(3) . . . . ?
C6 C1 N1 C8 118.8(4) . . . . ?
C2 C1 N1 C8 -60.5(4) . . . . ?
C6 C1 N1 C7 -121.6(4) . . . . ?
C2 C1 N1 C7 59.1(4) . . . . ?
C6 C1 N1 Pd1 0.0(4) . . . . ?
C2 C1 N1 Pd1 -179.2(3) . . . . ?
C18 C13 N2 C19 123.5(3) . . . . ?
C14 C13 N2 C19 -57.4(4) . . . . ?
C18 C13 N2 C20 -116.9(3) . . . . ?
C14 C13 N2 C20 62.2(4) . . . . ?
C18 C13 N2 Pd2 1.6(4) . . . . ?
C14 C13 N2 Pd2 -179.3(3) . . . . ?
C1 C6 P1 C11 120.5(3) . . . . ?
C5 C6 P1 C11 -59.8(4) . . . . ?
C1 C6 P1 C9 -125.0(3) . . . . ?
C5 C6 P1 C9 54.7(4) . . . . ?
C1 C6 P1 Pd1 -0.7(3) . . . . ?
C5 C6 P1 Pd1 178.9(3) . . . . ?
C12 C11 P1 C6 -66.6(3) . . . . ?
C12 C11 P1 C9 178.8(3) . . . . ?
C12 C11 P1 Pd1 46.7(3) . . . . ?
C10 C9 P1 C6 54.8(3) . . . . ?
C10 C9 P1 C11 169.4(3) . . . . ?
C10 C9 P1 Pd1 -59.9(3) . . . . ?
C13 C18 P2 C21 120.2(3) . . . . ?
C17 C18 P2 C21 -59.6(3) . . . . ?
C13 C18 P2 C23 -124.5(3) . . . . ?
C17 C18 P2 C23 55.7(4) . . . . ?
C13 C18 P2 Pd2 -0.7(3) . . . . ?
C17 C18 P2 Pd2 179.5(3) . . . . ?
C22 C21 P2 C18 -63.2(3) . . . . ?
C22 C21 P2 C23 -177.9(3) . . . . ?
C22 C21 P2 Pd2 50.0(3) . . . . ?
C24 C23 P2 C18 56.3(3) . . . . ?
C24 C23 P2 C21 171.5(3) . . . . ?
C24 C23 P2 Pd2 -57.9(3) . . . . ?

_refine_diff_density_max         1.278
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.135

####################################################################### 
# 
# 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_dayl190213
_database_code_depnum_ccdc_archive 'CCDC 2163666'
loop_
_audit_author_name
_audit_author_address
'Lydia Karmazin'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-06-27 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_dayl190213          
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: The compound crystallizes in the monoclinic C2 space group, which is chiral. The Flack parameter is 0.171(4), which deviates from zero. This happens because the structure contains significant anomalous scatterers. The absolute configuration was established based on the known absolute configuration of the CD.
;
# Added during the CSD deposition process: Monday 27 June 2022 10:18 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H100 Au Cl N O28 P, C6 H6'
_chemical_formula_sum            'C66 H106 Au Cl N O28 P'
_chemical_formula_weight         1624.90

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'
N N 0.0311 0.0180 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

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

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

_cell_length_a                   38.308(2)
_cell_length_b                   14.1787(8)
_cell_length_c                   15.4860(9)
_cell_angle_alpha                90
_cell_angle_beta                 93.007(2)
_cell_angle_gamma                90
_cell_volume                     8399.7(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9538
_cell_measurement_theta_min      4.35
_cell_measurement_theta_max      66.90

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_F_000             3376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    4.367
_shelx_estimated_absorpt_T_min   0.310
_shelx_estimated_absorpt_T_max   0.560
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4391
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Cu-ImuS Diamond microfocus tube'
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            108770
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.310
_diffrn_reflns_theta_max         67.321
_diffrn_reflns_theta_full        67.321
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             14764
_reflns_number_gt                14501
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_max     0.962
_reflns_Friedel_fraction_full    0.962

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0309P)²+31.8829P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 6564 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.171(4)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         14764
_refine_ls_number_parameters     901
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.1002
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2926(2) 0.9031(6) 0.1999(5) 0.0380(16) Uani 1 1 d . . . . .
H1 H 0.2959 0.9731 0.1995 0.046 Uiso 1 1 calc R U . . .
C2 C 0.2537(2) 0.8816(6) 0.2088(5) 0.0415(17) Uani 1 1 d . . . . .
H2 H 0.2400 0.9165 0.1623 0.050 Uiso 1 1 calc R U . . .
C3 C 0.24619(18) 0.7773(6) 0.1973(5) 0.0379(16) Uani 1 1 d . . . . .
H3 H 0.2561 0.7421 0.2488 0.045 Uiso 1 1 calc R U . . .
C4 C 0.26180(19) 0.7389(6) 0.1162(4) 0.0361(15) Uani 1 1 d . . . . .
H4 H 0.2495 0.7663 0.0635 0.043 Uiso 1 1 calc R U . . .
C5 C 0.30065(19) 0.7650(5) 0.1188(5) 0.0336(15) Uani 1 1 d . . . . .
H5 H 0.3122 0.7389 0.1731 0.040 Uiso 1 1 calc R U . . .
C6 C 0.32181(19) 0.7364(6) 0.0432(5) 0.0388(17) Uani 1 1 d . . . . .
H6A H 0.3166 0.7796 -0.0060 0.047 Uiso 1 1 calc R U . . .
H6B H 0.3153 0.6717 0.0246 0.047 Uiso 1 1 calc R U . . .
C7 C 0.2130(4) 0.9689(13) 0.2822(10) 0.113(6) Uani 1 1 d . . . . .
H7A H 0.2171 1.0246 0.2466 0.169 Uiso 1 1 calc R U . . .
H7B H 0.2067 0.9890 0.3399 0.169 Uiso 1 1 calc R U . . .
H7C H 0.1938 0.9316 0.2551 0.169 Uiso 1 1 calc R U . . .
C8 C 0.1962(2) 0.6988(7) 0.2475(5) 0.049(2) Uani 1 1 d . . . . .
H8A H 0.2063 0.6371 0.2353 0.074 Uiso 1 1 calc R U . . .
H8B H 0.1707 0.6956 0.2388 0.074 Uiso 1 1 calc R U . . .
H8C H 0.2024 0.7166 0.3076 0.074 Uiso 1 1 calc R U . . .
C11 C 0.25112(19) 0.5886(6) 0.0399(4) 0.040(2) Uani 1 1 d . . . . .
H11 H 0.2447 0.6344 -0.0074 0.049 Uiso 1 1 calc R U . . .
C12 C 0.2212(2) 0.5196(6) 0.0489(5) 0.0434(18) Uani 1 1 d . . . . .
H12 H 0.2184 0.4819 -0.0056 0.052 Uiso 1 1 calc R U . . .
C13 C 0.23055(19) 0.4525(6) 0.1233(5) 0.0390(16) Uani 1 1 d . . . . .
H13 H 0.2317 0.4889 0.1787 0.047 Uiso 1 1 calc R U . . .
C14 C 0.2656(2) 0.4065(6) 0.1116(5) 0.0391(16) Uani 1 1 d . . . . .
H14 H 0.2628 0.3557 0.0671 0.047 Uiso 1 1 calc R U . . .
C15 C 0.2939(2) 0.4745(6) 0.0854(5) 0.0401(18) Uani 1 1 d . . . . .
H15 H 0.3014 0.5130 0.1372 0.048 Uiso 1 1 calc R U . . .
C16 C 0.3255(2) 0.4268(7) 0.0529(5) 0.0439(19) Uani 1 1 d . . . . .
H16A H 0.3420 0.4748 0.0328 0.053 Uiso 1 1 calc R U . . .
H16B H 0.3375 0.3905 0.1003 0.053 Uiso 1 1 calc R U . . .
C17 C 0.1685(3) 0.5774(8) -0.0124(7) 0.077(3) Uani 1 1 d . . . . .
H17A H 0.1792 0.6249 -0.0487 0.116 Uiso 1 1 calc R U . . .
H17B H 0.1453 0.5989 0.0025 0.116 Uiso 1 1 calc R U . . .
H17C H 0.1664 0.5177 -0.0440 0.116 Uiso 1 1 calc R U . . .
C18 C 0.1781(2) 0.3994(7) 0.1859(7) 0.058(2) Uani 1 1 d . . . . .
H18A H 0.1885 0.4133 0.2437 0.087 Uiso 1 1 calc R U . . .
H18B H 0.1626 0.3447 0.1890 0.087 Uiso 1 1 calc R U . . .
H18C H 0.1646 0.4541 0.1645 0.087 Uiso 1 1 calc R U . . .
C19 C 0.3440(2) 0.3134(7) -0.0444(6) 0.057(2) Uani 1 1 d . . . . .
H19A H 0.3614 0.3562 -0.0670 0.086 Uiso 1 1 calc R U . . .
H19B H 0.3356 0.2702 -0.0903 0.086 Uiso 1 1 calc R U . . .
H19C H 0.3547 0.2770 0.0039 0.086 Uiso 1 1 calc R U . . .
C21 C 0.2775(2) 0.2675(7) 0.2011(5) 0.0467(19) Uani 1 1 d . . . . .
H21 H 0.2596 0.2420 0.1579 0.056 Uiso 1 1 calc R U . . .
C22 C 0.2661(2) 0.2434(7) 0.2920(6) 0.052(2) Uani 1 1 d . . . . .
H22 H 0.2615 0.1741 0.2944 0.062 Uiso 1 1 calc R U . . .
C23 C 0.2949(2) 0.2667(6) 0.3601(5) 0.0422(17) Uani 1 1 d . . . . .
H23 H 0.2968 0.3369 0.3648 0.051 Uiso 1 1 calc R U . . .
C24 C 0.3300(2) 0.2286(5) 0.3384(5) 0.0375(16) Uani 1 1 d . . . . .
H24 H 0.3304 0.1583 0.3436 0.045 Uiso 1 1 calc R U . . .
C25 C 0.3380(2) 0.2589(5) 0.2453(5) 0.0372(16) Uani 1 1 d . . . . .
H25 H 0.3384 0.3294 0.2432 0.045 Uiso 1 1 calc R U . . .
C26 C 0.3717(2) 0.2234(5) 0.2134(5) 0.0378(16) Uani 1 1 d . . . . .
H26A H 0.3729 0.2389 0.1512 0.045 Uiso 1 1 calc R U . . .
H26B H 0.3914 0.2558 0.2450 0.045 Uiso 1 1 calc R U . . .
C27 C 0.2089(3) 0.2450(11) 0.3469(10) 0.093(4) Uani 1 1 d . . . . .
H27A H 0.2025 0.1879 0.3143 0.139 Uiso 1 1 calc R U . . .
H27B H 0.1886 0.2866 0.3490 0.139 Uiso 1 1 calc R U . . .
H27C H 0.2170 0.2278 0.4059 0.139 Uiso 1 1 calc R U . . .
C28 C 0.2816(3) 0.3007(8) 0.5054(6) 0.060(2) Uani 1 1 d . . . . .
H28A H 0.3048 0.3197 0.5289 0.090 Uiso 1 1 calc R U . . .
H28B H 0.2681 0.2753 0.5521 0.090 Uiso 1 1 calc R U . . .
H28C H 0.2695 0.3557 0.4798 0.090 Uiso 1 1 calc R U . . .
C29 C 0.4093(2) 0.0954(8) 0.2021(6) 0.059(2) Uani 1 1 d . . . . .
H29A H 0.4129 0.1133 0.1421 0.089 Uiso 1 1 calc R U . . .
H29B H 0.4113 0.0268 0.2082 0.089 Uiso 1 1 calc R U . . .
H29C H 0.4270 0.1260 0.2406 0.089 Uiso 1 1 calc R U . . .
C31 C 0.3829(2) 0.2140(5) 0.4337(5) 0.0377(16) Uani 1 1 d . . . . .
H31 H 0.3774 0.1458 0.4237 0.045 Uiso 1 1 calc R U . . .
C32 C 0.3875(2) 0.2327(6) 0.5311(5) 0.0388(16) Uani 1 1 d . . . . .
H32 H 0.4080 0.1952 0.5549 0.047 Uiso 1 1 calc R U . . .
C33 C 0.3949(2) 0.3354(6) 0.5469(5) 0.0385(16) Uani 1 1 d . . . . .
H33 H 0.3734 0.3726 0.5305 0.046 Uiso 1 1 calc R U . . .
C34 C 0.42514(18) 0.3712(5) 0.4943(4) 0.0321(14) Uani 1 1 d . . . . .
H34 H 0.4479 0.3518 0.5237 0.038 Uiso 1 1 calc R U . . .
C35 C 0.4234(2) 0.3342(6) 0.4008(5) 0.0390(17) Uani 1 1 d . . . . .
H35 H 0.4045 0.3695 0.3674 0.047 Uiso 1 1 calc R U . . .
C36 C 0.4570(2) 0.3485(7) 0.3566(6) 0.051(2) Uani 1 1 d . . . . .
H36A H 0.4549 0.3165 0.2998 0.061 Uiso 1 1 calc R U . . .
H36B H 0.4596 0.4168 0.3453 0.061 Uiso 1 1 calc R U . . .
C37 C 0.3553(3) 0.1161(9) 0.5965(7) 0.071(3) Uani 1 1 d . . . . .
H37A H 0.3535 0.0785 0.5434 0.107 Uiso 1 1 calc R U . . .
H37B H 0.3346 0.1060 0.6297 0.107 Uiso 1 1 calc R U . . .
H37C H 0.3762 0.0970 0.6313 0.107 Uiso 1 1 calc R U . . .
C38 C 0.3773(3) 0.3962(9) 0.6816(7) 0.080(4) Uani 1 1 d . . . . .
H38A H 0.3765 0.4634 0.6668 0.120 Uiso 1 1 calc R U . . .
H38B H 0.3824 0.3891 0.7439 0.120 Uiso 1 1 calc R U . . .
H38C H 0.3548 0.3669 0.6655 0.120 Uiso 1 1 calc R U . . .
C39 C 0.4957(4) 0.2236(13) 0.3840(18) 0.160(10) Uani 1 1 d . . . . .
H39A H 0.4767 0.1831 0.4022 0.240 Uiso 1 1 calc R U . . .
H39B H 0.5175 0.2066 0.4163 0.240 Uiso 1 1 calc R U . . .
H39C H 0.4986 0.2150 0.3220 0.240 Uiso 1 1 calc R U . . .
C41 C 0.45327(17) 0.5257(5) 0.5116(5) 0.0331(15) Uani 1 1 d . . . . .
H41 H 0.4719 0.4839 0.5381 0.040 Uiso 1 1 calc R U . . .
C42 C 0.44565(14) 0.6043(9) 0.5749(3) 0.0368(13) Uani 1 1 d . . . . .
H42 H 0.4677 0.6400 0.5892 0.044 Uiso 1 1 calc R U . . .
C43 C 0.41843(17) 0.6721(5) 0.5352(5) 0.0358(16) Uani 1 1 d . . . . .
H43 H 0.3955 0.6388 0.5253 0.043 Uiso 1 1 calc R U . . .
C44 C 0.43115(17) 0.7072(5) 0.4495(5) 0.0323(15) Uani 1 1 d . . . . .
H44 H 0.4525 0.7471 0.4605 0.039 Uiso 1 1 calc R U . . .
C45 C 0.43990(17) 0.6251(5) 0.3908(4) 0.0336(18) Uani 1 1 d . . . . .
H45 H 0.4183 0.5877 0.3761 0.040 Uiso 1 1 calc R U . . .
C46 C 0.45579(18) 0.6579(6) 0.3085(5) 0.0385(16) Uani 1 1 d . . . . .
H46A H 0.4653 0.6032 0.2777 0.046 Uiso 1 1 calc R U . . .
H46B H 0.4376 0.6880 0.2699 0.046 Uiso 1 1 calc R U . . .
C47 C 0.4575(2) 0.5173(8) 0.7041(5) 0.053(2) Uani 1 1 d . . . . .
H47A H 0.4621 0.4574 0.6753 0.079 Uiso 1 1 calc R U . . .
H47B H 0.4486 0.5049 0.7611 0.079 Uiso 1 1 calc R U . . .
H47C H 0.4793 0.5536 0.7109 0.079 Uiso 1 1 calc R U . . .
C48 C 0.3789(2) 0.7648(8) 0.6102(6) 0.062(3) Uani 1 1 d . . . . .
H48A H 0.3650 0.7740 0.5558 0.093 Uiso 1 1 calc R U . . .
H48B H 0.3771 0.8212 0.6464 0.093 Uiso 1 1 calc R U . . .
H48C H 0.3699 0.7101 0.6408 0.093 Uiso 1 1 calc R U . . .
C49 C 0.4973(3) 0.7623(9) 0.2572(10) 0.092(4) Uani 1 1 d . . . . .
H49A H 0.5011 0.7124 0.2149 0.138 Uiso 1 1 calc R U . . .
H49B H 0.5197 0.7921 0.2741 0.138 Uiso 1 1 calc R U . . .
H49C H 0.4813 0.8096 0.2314 0.138 Uiso 1 1 calc R U . . .
C51 C 0.41323(19) 0.8495(5) 0.3707(6) 0.0371(17) Uani 1 1 d . . . . .
H51 H 0.4385 0.8615 0.3866 0.044 Uiso 1 1 calc R U . . .
C52 C 0.3918(2) 0.9305(6) 0.4047(6) 0.0471(19) Uani 1 1 d . . . . .
H52 H 0.3989 0.9905 0.3766 0.057 Uiso 1 1 calc R U . . .
C53 C 0.3535(2) 0.9113(6) 0.3800(6) 0.044(2) Uani 1 1 d . . . . .
H53 H 0.3456 0.8535 0.4103 0.052 Uiso 1 1 calc R U . . .
C54 C 0.34768(19) 0.8993(5) 0.2826(5) 0.0393(17) Uani 1 1 d . . . . .
H54 H 0.3495 0.9622 0.2540 0.047 Uiso 1 1 calc R U . . .
C55 C 0.37317(18) 0.8312(5) 0.2440(5) 0.0359(15) Uani 1 1 d . . . . .
H55 H 0.3661 0.7649 0.2563 0.043 Uiso 1 1 calc R U . . .
C56 C 0.37746(19) 0.8433(5) 0.1455(5) 0.0381(16) Uani 1 1 d . . . . .
H56A H 0.4017 0.8643 0.1375 0.046 Uiso 1 1 calc R U . . .
H56B H 0.3618 0.8951 0.1249 0.046 Uiso 1 1 calc R U . . .
C57 C 0.4295(3) 0.9707(9) 0.5248(9) 0.081(4) Uani 1 1 d . . . . .
H57A H 0.4453 0.9163 0.5265 0.122 Uiso 1 1 calc R U . . .
H57B H 0.4283 0.9971 0.5830 0.122 Uiso 1 1 calc R U . . .
H57C H 0.4382 1.0187 0.4858 0.122 Uiso 1 1 calc R U . . .
C58 C 0.3048(3) 0.9673(8) 0.4530(7) 0.060(2) Uani 1 1 d . . . . .
H58A H 0.2884 0.9288 0.4173 0.090 Uiso 1 1 calc R U . . .
H58B H 0.2930 1.0248 0.4710 0.090 Uiso 1 1 calc R U . . .
H58C H 0.3128 0.9313 0.5043 0.090 Uiso 1 1 calc R U . . .
C60 C 0.3896(2) 0.7750(7) -0.0255(5) 0.048(2) Uani 1 1 d . . . . .
C61 C 0.4033(3) 0.8631(9) -0.0383(7) 0.067(3) Uani 1 1 d . . . . .
H61 H 0.4026 0.9090 0.0062 0.080 Uiso 1 1 calc R U . . .
C62 C 0.4181(3) 0.8858(12) -0.1151(9) 0.091(4) Uani 1 1 d . . . . .
H62 H 0.4282 0.9464 -0.1222 0.110 Uiso 1 1 calc R U . . .
C63 C 0.4184(3) 0.8221(12) -0.1803(8) 0.086(4) Uani 1 1 d . . . . .
H63 H 0.4274 0.8393 -0.2342 0.103 Uiso 1 1 calc R U . . .
C64 C 0.4055(3) 0.7316(10) -0.1684(7) 0.071(3) Uani 1 1 d . . . . .
H64 H 0.4072 0.6854 -0.2124 0.086 Uiso 1 1 calc R U . . .
C65 C 0.3901(2) 0.7088(9) -0.0911(6) 0.057(3) Uani 1 1 d . . . . .
C66 C 0.3454(3) 0.6003(16) -0.1361(5) 0.086(3) Uani 1 1 d . . . . .
H66A H 0.3301 0.6557 -0.1383 0.128 Uiso 1 1 calc R U . . .
H66B H 0.3324 0.5457 -0.1159 0.128 Uiso 1 1 calc R U . . .
H66C H 0.3534 0.5874 -0.1939 0.128 Uiso 1 1 calc R U . . .
C67 C 0.4023(4) 0.5445(11) -0.0760(9) 0.087(4) Uani 1 1 d . . . . .
H67A H 0.4114 0.5388 -0.1337 0.131 Uiso 1 1 calc R U . . .
H67B H 0.3920 0.4842 -0.0594 0.131 Uiso 1 1 calc R U . . .
H67C H 0.4214 0.5611 -0.0342 0.131 Uiso 1 1 calc R U . . .
C68 C 0.3226(3) 0.5465(9) 0.3371(6) 0.073(3) Uani 1 1 d . . . . .
H68 H 0.3361 0.5428 0.2875 0.088 Uiso 1 1 calc R U . . .
C69 C 0.2875(3) 0.5585(9) 0.3278(7) 0.075(3) Uani 1 1 d . . . . .
H69 H 0.2760 0.5546 0.2721 0.090 Uiso 1 1 calc R U . . .
C70 C 0.2683(2) 0.5764(9) 0.3996(8) 0.079(4) Uani 1 1 d . . . . .
H70 H 0.2440 0.5892 0.3929 0.095 Uiso 1 1 calc R U . . .
C71 C 0.2844(3) 0.5754(10) 0.4784(8) 0.088(4) Uani 1 1 d . . . . .
H71 H 0.2717 0.5894 0.5278 0.106 Uiso 1 1 calc R U . . .
C72 C 0.3205(3) 0.5536(11) 0.4882(8) 0.088(4) Uani 1 1 d . . . . .
H72 H 0.3319 0.5486 0.5440 0.105 Uiso 1 1 calc R U . . .
C73 C 0.3382(3) 0.5401(8) 0.4162(7) 0.069(3) Uani 1 1 d . . . . .
H73 H 0.3625 0.5257 0.4219 0.083 Uiso 1 1 calc R U . . .
N1 N 0.3754(2) 0.6183(8) -0.0768(4) 0.061(2) Uani 1 1 d . . . . .
O1 O 0.31198(12) 0.8651(3) 0.2707(3) 0.0340(10) Uani 1 1 d . . . . .
O2 O 0.24316(18) 0.9144(5) 0.2892(5) 0.0586(19) Uani 1 1 d . . . . .
O3 O 0.20933(14) 0.7666(5) 0.1915(4) 0.0499(14) Uani 1 1 d . . . . .
O4 O 0.25670(13) 0.6385(3) 0.1184(3) 0.0377(12) Uani 1 1 d . . . . .
O5 O 0.30296(13) 0.8663(4) 0.1217(3) 0.0362(11) Uani 1 1 d . . . . .
O12 O 0.18939(14) 0.5644(4) 0.0629(4) 0.0504(14) Uani 1 1 d . . . . .
O13 O 0.20504(14) 0.3793(4) 0.1287(4) 0.0452(13) Uani 1 1 d . . . . .
O14 O 0.27819(14) 0.3647(4) 0.1934(3) 0.0419(12) Uani 1 1 d . . . . .
O15 O 0.28099(14) 0.5381(4) 0.0180(3) 0.0422(12) Uani 1 1 d . . . . .
O16 O 0.31566(15) 0.3662(5) -0.0153(4) 0.0569(16) Uani 1 1 d . . . . .
O22 O 0.23512(18) 0.2908(7) 0.3074(5) 0.071(2) Uani 1 1 d . . . . .
O23 O 0.28516(16) 0.2308(5) 0.4412(4) 0.0509(14) Uani 1 1 d . . . . .
O24 O 0.35500(14) 0.2700(4) 0.3988(3) 0.0353(12) Uani 1 1 d . . . . .
O25 O 0.30992(15) 0.2261(4) 0.1860(3) 0.0451(12) Uani 1 1 d . . . . .
O26 O 0.37538(14) 0.1246(4) 0.2246(4) 0.0461(14) Uani 1 1 d . . . . .
O32 O 0.35774(14) 0.2075(4) 0.5762(4) 0.0456(13) Uani 1 1 d . . . . .
O33 O 0.40429(17) 0.3512(5) 0.6356(3) 0.0551(15) Uani 1 1 d . . . . .
O34 O 0.42261(11) 0.4721(4) 0.4950(3) 0.0339(10) Uani 1 1 d . . . . .
O35 O 0.41491(13) 0.2357(4) 0.3972(3) 0.0398(11) Uani 1 1 d . . . . .
O36 O 0.48769(19) 0.3169(6) 0.4001(6) 0.077(2) Uani 1 1 d . . . . .
O42 O 0.43230(13) 0.5699(4) 0.6530(3) 0.0448(14) Uani 1 1 d . . . . .
O43 O 0.41461(14) 0.7491(4) 0.5922(4) 0.0487(14) Uani 1 1 d . . . . .
O44 O 0.40345(12) 0.7642(3) 0.4086(3) 0.0358(11) Uani 1 1 d . . . . .
O45 O 0.46533(11) 0.5661(3) 0.4346(3) 0.0314(10) Uani 1 1 d . . . . .
O46 O 0.48296(15) 0.7236(5) 0.3295(4) 0.0566(15) Uani 1 1 d . . . . .
O52 O 0.39528(17) 0.9412(5) 0.4940(5) 0.0628(18) Uani 1 1 d . . . . .
O53 O 0.33353(15) 0.9914(4) 0.4051(4) 0.0474(13) Uani 1 1 d . . . . .
O55 O 0.40857(12) 0.8476(3) 0.2790(3) 0.0382(11) Uani 1 1 d . . . . .
P1 P 0.36872(5) 0.74074(13) 0.07425(11) 0.0321(4) Uani 1 1 d . . . . .
Cl1 Cl 0.40443(5) 0.46823(13) 0.20004(12) 0.0446(4) Uani 1 1 d . . . . .
Au1 Au 0.38722(2) 0.60697(3) 0.13731(2) 0.03841(9) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O5 1.395(9) . ?
C1 O1 1.400(9) . ?
C1 C2 1.535(11) . ?
C1 H1 1.0000 . ?
C2 O2 1.407(10) . ?
C2 C3 1.514(12) . ?
C2 H2 1.0000 . ?
C3 O3 1.418(9) . ?
C3 C4 1.519(10) . ?
C3 H3 1.0000 . ?
C4 O4 1.438(10) . ?
C4 C5 1.532(10) . ?
C4 H4 1.0000 . ?
C5 O5 1.440(9) . ?
C5 C6 1.514(10) . ?
C5 H5 1.0000 . ?
C6 P1 1.837(8) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 O2 1.391(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 O3 1.406(10) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C11 O15 1.407(9) . ?
C11 O4 1.412(8) . ?
C11 C12 1.519(11) . ?
C11 H11 1.0000 . ?
C12 O12 1.401(10) . ?
C12 C13 1.522(12) . ?
C12 H12 1.0000 . ?
C13 O13 1.431(9) . ?
C13 C14 1.514(11) . ?
C13 H13 1.0000 . ?
C14 O14 1.456(9) . ?
C14 C15 1.520(11) . ?
C14 H14 1.0000 . ?
C15 O15 1.445(10) . ?
C15 C16 1.499(12) . ?
C15 H15 1.0000 . ?
C16 O16 1.397(10) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 O12 1.390(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 O13 1.425(11) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 O16 1.412(10) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C21 O14 1.384(11) . ?
C21 O25 1.406(10) . ?
C21 C22 1.532(12) . ?
C21 H21 1.0000 . ?
C22 O22 1.397(12) . ?
C22 C23 1.520(11) . ?
C22 H22 1.0000 . ?
C23 O23 1.424(9) . ?
C23 C24 1.504(11) . ?
C23 H23 1.0000 . ?
C24 O24 1.429(9) . ?
C24 C25 1.550(10) . ?
C24 H24 1.0000 . ?
C25 O25 1.453(9) . ?
C25 C26 1.495(11) . ?
C25 H25 1.0000 . ?
C26 O26 1.419(9) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O22 1.366(13) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 O23 1.415(12) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 O26 1.424(11) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C31 O35 1.410(9) . ?
C31 O24 1.416(9) . ?
C31 C32 1.533(10) . ?
C31 H31 1.0000 . ?
C32 O32 1.416(9) . ?
C32 C33 1.501(11) . ?
C32 H32 1.0000 . ?
C33 O33 1.419(9) . ?
C33 C34 1.537(10) . ?
C33 H33 1.0000 . ?
C34 O34 1.434(9) . ?
C34 C35 1.538(10) . ?
C34 H34 1.0000 . ?
C35 O35 1.434(10) . ?
C35 C36 1.505(11) . ?
C35 H35 1.0000 . ?
C36 O36 1.397(12) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O32 1.337(14) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 O33 1.435(13) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 O36 1.383(19) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 O34 1.411(8) . ?
C41 O45 1.422(8) . ?
C41 C42 1.524(12) . ?
C41 H41 1.0000 . ?
C42 O42 1.423(8) . ?
C42 C43 1.523(12) . ?
C42 H42 1.0000 . ?
C43 O43 1.417(9) . ?
C43 C44 1.522(11) . ?
C43 H43 1.0000 . ?
C44 O44 1.453(8) . ?
C44 C45 1.524(10) . ?
C44 H44 1.0000 . ?
C45 O45 1.428(8) . ?
C45 C46 1.515(10) . ?
C45 H45 1.0000 . ?
C46 O46 1.422(10) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O42 1.427(10) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O43 1.429(10) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 O46 1.387(13) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C51 O44 1.403(9) . ?
C51 O55 1.422(10) . ?
C51 C52 1.523(10) . ?
C51 H51 1.0000 . ?
C52 O52 1.391(11) . ?
C52 C53 1.520(12) . ?
C52 H52 1.0000 . ?
C53 O53 1.434(10) . ?
C53 C54 1.523(12) . ?
C53 H53 1.0000 . ?
C54 O1 1.454(9) . ?
C54 C55 1.518(10) . ?
C54 H54 1.0000 . ?
C55 O55 1.453(8) . ?
C55 C56 1.551(10) . ?
C55 H55 1.0000 . ?
C56 P1 1.846(8) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O52 1.432(12) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 O53 1.402(12) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C60 C61 1.373(15) . ?
C60 C65 1.384(14) . ?
C60 P1 1.842(8) . ?
C61 C62 1.382(15) . ?
C61 H61 0.9500 . ?
C62 C63 1.36(2) . ?
C62 H62 0.9500 . ?
C63 C64 1.39(2) . ?
C63 H63 0.9500 . ?
C64 C65 1.401(13) . ?
C64 H64 0.9500 . ?
C65 N1 1.423(16) . ?
C66 N1 1.455(13) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 N1 1.469(15) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 C73 1.338(15) . ?
C68 C69 1.358(16) . ?
C68 H68 0.9500 . ?
C69 C70 1.387(16) . ?
C69 H69 0.9500 . ?
C70 C71 1.338(17) . ?
C70 H70 0.9500 . ?
C71 C72 1.415(18) . ?
C71 H71 0.9500 . ?
C72 C73 1.350(16) . ?
C72 H72 0.9500 . ?
C73 H73 0.9500 . ?
P1 Au1 2.2317(18) . ?
Cl1 Au1 2.2763(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 C1 O1 111.8(6) . . ?
O5 C1 C2 109.0(7) . . ?
O1 C1 C2 109.3(6) . . ?
O5 C1 H1 108.9 . . ?
O1 C1 H1 108.9 . . ?
C2 C1 H1 108.9 . . ?
O2 C2 C3 111.5(7) . . ?
O2 C2 C1 109.8(7) . . ?
C3 C2 C1 111.3(6) . . ?
O2 C2 H2 108.1 . . ?
C3 C2 H2 108.1 . . ?
C1 C2 H2 108.1 . . ?
O3 C3 C2 107.1(6) . . ?
O3 C3 C4 110.1(6) . . ?
C2 C3 C4 111.6(6) . . ?
O3 C3 H3 109.4 . . ?
C2 C3 H3 109.4 . . ?
C4 C3 H3 109.4 . . ?
O4 C4 C3 106.0(6) . . ?
O4 C4 C5 111.8(6) . . ?
C3 C4 C5 108.4(6) . . ?
O4 C4 H4 110.2 . . ?
C3 C4 H4 110.2 . . ?
C5 C4 H4 110.2 . . ?
O5 C5 C6 104.9(6) . . ?
O5 C5 C4 107.5(6) . . ?
C6 C5 C4 118.3(6) . . ?
O5 C5 H5 108.6 . . ?
C6 C5 H5 108.6 . . ?
C4 C5 H5 108.6 . . ?
C5 C6 P1 110.2(5) . . ?
C5 C6 H6A 109.6 . . ?
P1 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
P1 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O15 C11 O4 112.0(6) . . ?
O15 C11 C12 108.7(7) . . ?
O4 C11 C12 108.9(6) . . ?
O15 C11 H11 109.1 . . ?
O4 C11 H11 109.1 . . ?
C12 C11 H11 109.1 . . ?
O12 C12 C11 112.9(7) . . ?
O12 C12 C13 109.8(6) . . ?
C11 C12 C13 108.9(6) . . ?
O12 C12 H12 108.4 . . ?
C11 C12 H12 108.4 . . ?
C13 C12 H12 108.4 . . ?
O13 C13 C14 107.9(6) . . ?
O13 C13 C12 111.3(6) . . ?
C14 C13 C12 110.8(6) . . ?
O13 C13 H13 108.9 . . ?
C14 C13 H13 108.9 . . ?
C12 C13 H13 108.9 . . ?
O14 C14 C13 109.1(6) . . ?
O14 C14 C15 106.5(6) . . ?
C13 C14 C15 114.0(7) . . ?
O14 C14 H14 109.1 . . ?
C13 C14 H14 109.1 . . ?
C15 C14 H14 109.1 . . ?
O15 C15 C16 106.9(6) . . ?
O15 C15 C14 111.6(6) . . ?
C16 C15 C14 113.8(7) . . ?
O15 C15 H15 108.1 . . ?
C16 C15 H15 108.1 . . ?
C14 C15 H15 108.1 . . ?
O16 C16 C15 109.9(7) . . ?
O16 C16 H16A 109.7 . . ?
C15 C16 H16A 109.7 . . ?
O16 C16 H16B 109.7 . . ?
C15 C16 H16B 109.7 . . ?
H16A C16 H16B 108.2 . . ?
O12 C17 H17A 109.5 . . ?
O12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O13 C18 H18A 109.5 . . ?
O13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O16 C19 H19A 109.5 . . ?
O16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O14 C21 O25 112.3(7) . . ?
O14 C21 C22 108.1(7) . . ?
O25 C21 C22 110.8(7) . . ?
O14 C21 H21 108.5 . . ?
O25 C21 H21 108.5 . . ?
C22 C21 H21 108.5 . . ?
O22 C22 C23 111.7(8) . . ?
O22 C22 C21 109.5(8) . . ?
C23 C22 C21 111.0(7) . . ?
O22 C22 H22 108.2 . . ?
C23 C22 H22 108.2 . . ?
C21 C22 H22 108.2 . . ?
O23 C23 C24 110.3(7) . . ?
O23 C23 C22 108.7(6) . . ?
C24 C23 C22 113.0(7) . . ?
O23 C23 H23 108.2 . . ?
C24 C23 H23 108.2 . . ?
C22 C23 H23 108.2 . . ?
O24 C24 C23 106.4(6) . . ?
O24 C24 C25 109.7(6) . . ?
C23 C24 C25 109.3(6) . . ?
O24 C24 H24 110.4 . . ?
C23 C24 H24 110.4 . . ?
C25 C24 H24 110.4 . . ?
O25 C25 C26 107.9(6) . . ?
O25 C25 C24 108.9(6) . . ?
C26 C25 C24 115.4(6) . . ?
O25 C25 H25 108.1 . . ?
C26 C25 H25 108.1 . . ?
C24 C25 H25 108.1 . . ?
O26 C26 C25 112.0(6) . . ?
O26 C26 H26A 109.2 . . ?
C25 C26 H26A 109.2 . . ?
O26 C26 H26B 109.2 . . ?
C25 C26 H26B 109.2 . . ?
H26A C26 H26B 107.9 . . ?
O22 C27 H27A 109.5 . . ?
O22 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O22 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O23 C28 H28A 109.5 . . ?
O23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
O23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O26 C29 H29A 109.5 . . ?
O26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O35 C31 O24 112.3(6) . . ?
O35 C31 C32 107.4(6) . . ?
O24 C31 C32 108.9(6) . . ?
O35 C31 H31 109.4 . . ?
O24 C31 H31 109.4 . . ?
C32 C31 H31 109.4 . . ?
O32 C32 C33 108.3(6) . . ?
O32 C32 C31 112.8(6) . . ?
C33 C32 C31 109.8(7) . . ?
O32 C32 H32 108.6 . . ?
C33 C32 H32 108.6 . . ?
C31 C32 H32 108.6 . . ?
O33 C33 C32 110.3(6) . . ?
O33 C33 C34 107.5(6) . . ?
C32 C33 C34 112.0(6) . . ?
O33 C33 H33 109.0 . . ?
C32 C33 H33 109.0 . . ?
C34 C33 H33 109.0 . . ?
O34 C34 C33 105.8(5) . . ?
O34 C34 C35 110.4(6) . . ?
C33 C34 C35 112.9(6) . . ?
O34 C34 H34 109.2 . . ?
C33 C34 H34 109.2 . . ?
C35 C34 H34 109.2 . . ?
O35 C35 C36 108.1(6) . . ?
O35 C35 C34 111.6(6) . . ?
C36 C35 C34 112.6(7) . . ?
O35 C35 H35 108.1 . . ?
C36 C35 H35 108.1 . . ?
C34 C35 H35 108.1 . . ?
O36 C36 C35 117.2(8) . . ?
O36 C36 H36A 108.0 . . ?
C35 C36 H36A 108.0 . . ?
O36 C36 H36B 108.0 . . ?
C35 C36 H36B 108.0 . . ?
H36A C36 H36B 107.2 . . ?
O32 C37 H37A 109.5 . . ?
O32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
O32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O33 C38 H38A 109.5 . . ?
O33 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
O33 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O36 C39 H39A 109.5 . . ?
O36 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
O36 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O34 C41 O45 111.6(5) . . ?
O34 C41 C42 109.0(5) . . ?
O45 C41 C42 109.0(6) . . ?
O34 C41 H41 109.1 . . ?
O45 C41 H41 109.1 . . ?
C42 C41 H41 109.1 . . ?
O42 C42 C43 106.9(5) . . ?
O42 C42 C41 112.6(9) . . ?
C43 C42 C41 110.6(5) . . ?
O42 C42 H42 108.9 . . ?
C43 C42 H42 108.9 . . ?
C41 C42 H42 108.9 . . ?
O43 C43 C44 109.8(6) . . ?
O43 C43 C42 108.9(6) . . ?
C44 C43 C42 108.4(5) . . ?
O43 C43 H43 109.9 . . ?
C44 C43 H43 109.9 . . ?
C42 C43 H43 109.9 . . ?
O44 C44 C43 107.6(5) . . ?
O44 C44 C45 110.1(5) . . ?
C43 C44 C45 111.1(6) . . ?
O44 C44 H44 109.3 . . ?
C43 C44 H44 109.3 . . ?
C45 C44 H44 109.3 . . ?
O45 C45 C46 106.6(5) . . ?
O45 C45 C44 109.3(5) . . ?
C46 C45 C44 112.2(6) . . ?
O45 C45 H45 109.6 . . ?
C46 C45 H45 109.6 . . ?
C44 C45 H45 109.6 . . ?
O46 C46 C45 109.3(6) . . ?
O46 C46 H46A 109.8 . . ?
C45 C46 H46A 109.8 . . ?
O46 C46 H46B 109.8 . . ?
C45 C46 H46B 109.8 . . ?
H46A C46 H46B 108.3 . . ?
O42 C47 H47A 109.5 . . ?
O42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
O42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O43 C48 H48A 109.5 . . ?
O43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
O43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O46 C49 H49A 109.5 . . ?
O46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O44 C51 O55 112.3(6) . . ?
O44 C51 C52 110.1(7) . . ?
O55 C51 C52 108.5(6) . . ?
O44 C51 H51 108.6 . . ?
O55 C51 H51 108.6 . . ?
C52 C51 H51 108.6 . . ?
O52 C52 C53 108.1(7) . . ?
O52 C52 C51 113.6(7) . . ?
C53 C52 C51 108.0(6) . . ?
O52 C52 H52 109.0 . . ?
C53 C52 H52 109.0 . . ?
C51 C52 H52 109.0 . . ?
O53 C53 C52 108.1(7) . . ?
O53 C53 C54 107.7(7) . . ?
C52 C53 C54 111.0(7) . . ?
O53 C53 H53 110.0 . . ?
C52 C53 H53 110.0 . . ?
C54 C53 H53 110.0 . . ?
O1 C54 C55 111.0(6) . . ?
O1 C54 C53 104.5(6) . . ?
C55 C54 C53 113.4(7) . . ?
O1 C54 H54 109.3 . . ?
C55 C54 H54 109.3 . . ?
C53 C54 H54 109.3 . . ?
O55 C55 C54 111.0(6) . . ?
O55 C55 C56 101.8(5) . . ?
C54 C55 C56 114.9(6) . . ?
O55 C55 H55 109.6 . . ?
C54 C55 H55 109.6 . . ?
C56 C55 H55 109.6 . . ?
C55 C56 P1 118.4(5) . . ?
C55 C56 H56A 107.7 . . ?
P1 C56 H56A 107.7 . . ?
C55 C56 H56B 107.7 . . ?
P1 C56 H56B 107.7 . . ?
H56A C56 H56B 107.1 . . ?
O52 C57 H57A 109.5 . . ?
O52 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
O52 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O53 C58 H58A 109.5 . . ?
O53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
O53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C61 C60 C65 119.4(9) . . ?
C61 C60 P1 123.2(8) . . ?
C65 C60 P1 117.4(7) . . ?
C60 C61 C62 120.9(13) . . ?
C60 C61 H61 119.5 . . ?
C62 C61 H61 119.5 . . ?
C63 C62 C61 120.4(13) . . ?
C63 C62 H62 119.8 . . ?
C61 C62 H62 119.8 . . ?
C62 C63 C64 119.9(10) . . ?
C62 C63 H63 120.0 . . ?
C64 C63 H63 120.0 . . ?
C63 C64 C65 119.7(12) . . ?
C63 C64 H64 120.2 . . ?
C65 C64 H64 120.2 . . ?
C60 C65 C64 119.5(11) . . ?
C60 C65 N1 118.5(8) . . ?
C64 C65 N1 121.9(10) . . ?
N1 C66 H66A 109.5 . . ?
N1 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
N1 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N1 C67 H67A 109.5 . . ?
N1 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
N1 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C73 C68 C69 119.8(10) . . ?
C73 C68 H68 120.1 . . ?
C69 C68 H68 120.1 . . ?
C68 C69 C70 120.1(10) . . ?
C68 C69 H69 119.9 . . ?
C70 C69 H69 119.9 . . ?
C71 C70 C69 119.4(9) . . ?
C71 C70 H70 120.3 . . ?
C69 C70 H70 120.3 . . ?
C70 C71 C72 120.0(11) . . ?
C70 C71 H71 120.0 . . ?
C72 C71 H71 120.0 . . ?
C73 C72 C71 118.3(11) . . ?
C73 C72 H72 120.9 . . ?
C71 C72 H72 120.9 . . ?
C68 C73 C72 121.8(11) . . ?
C68 C73 H73 119.1 . . ?
C72 C73 H73 119.1 . . ?
C65 N1 C66 111.4(11) . . ?
C65 N1 C67 111.2(10) . . ?
C66 N1 C67 114.3(12) . . ?
C1 O1 C54 115.3(6) . . ?
C7 O2 C2 113.0(9) . . ?
C8 O3 C3 115.0(6) . . ?
C11 O4 C4 119.4(5) . . ?
C1 O5 C5 112.4(6) . . ?
C17 O12 C12 113.4(7) . . ?
C18 O13 C13 114.2(6) . . ?
C21 O14 C14 118.3(6) . . ?
C11 O15 C15 113.3(5) . . ?
C16 O16 C19 112.7(6) . . ?
C27 O22 C22 119.9(10) . . ?
C28 O23 C23 114.1(7) . . ?
C31 O24 C24 119.1(6) . . ?
C21 O25 C25 113.1(6) . . ?
C26 O26 C29 110.0(7) . . ?
C37 O32 C32 115.3(7) . . ?
C33 O33 C38 113.5(7) . . ?
C41 O34 C34 118.8(5) . . ?
C31 O35 C35 113.4(5) . . ?
C39 O36 C36 114.2(11) . . ?
C42 O42 C47 112.7(6) . . ?
C43 O43 C48 111.9(6) . . ?
C51 O44 C44 117.2(5) . . ?
C41 O45 C45 113.0(5) . . ?
C49 O46 C46 113.0(9) . . ?
C52 O52 C57 113.7(9) . . ?
C58 O53 C53 113.3(7) . . ?
C51 O55 C55 116.2(5) . . ?
C6 P1 C60 104.5(4) . . ?
C6 P1 C56 109.1(4) . . ?
C60 P1 C56 102.7(4) . . ?
C6 P1 Au1 111.7(3) . . ?
C60 P1 Au1 116.7(3) . . ?
C56 P1 Au1 111.4(2) . . ?
P1 Au1 Cl1 178.13(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
O5 C1 C2 O2 177.3(6) . . . . ?
O1 C1 C2 O2 54.8(9) . . . . ?
O5 C1 C2 C3 53.4(8) . . . . ?
O1 C1 C2 C3 -69.1(8) . . . . ?
O2 C2 C3 O3 67.0(7) . . . . ?
C1 C2 C3 O3 -170.0(6) . . . . ?
O2 C2 C3 C4 -172.4(6) . . . . ?
C1 C2 C3 C4 -49.5(8) . . . . ?
O3 C3 C4 O4 -68.2(7) . . . . ?
C2 C3 C4 O4 173.1(5) . . . . ?
O3 C3 C4 C5 171.6(6) . . . . ?
C2 C3 C4 C5 52.9(8) . . . . ?
O4 C4 C5 O5 -176.6(5) . . . . ?
C3 C4 C5 O5 -60.1(7) . . . . ?
O4 C4 C5 C6 65.1(8) . . . . ?
C3 C4 C5 C6 -178.4(7) . . . . ?
O5 C5 C6 P1 78.1(6) . . . . ?
C4 C5 C6 P1 -162.2(6) . . . . ?
O15 C11 C12 O12 -174.4(6) . . . . ?
O4 C11 C12 O12 63.3(8) . . . . ?
O15 C11 C12 C13 63.3(7) . . . . ?
O4 C11 C12 C13 -58.9(8) . . . . ?
O12 C12 C13 O13 62.4(8) . . . . ?
C11 C12 C13 O13 -173.5(6) . . . . ?
O12 C12 C13 C14 -177.5(6) . . . . ?
C11 C12 C13 C14 -53.4(8) . . . . ?
O13 C13 C14 O14 -73.8(7) . . . . ?
C12 C13 C14 O14 164.1(6) . . . . ?
O13 C13 C14 C15 167.3(6) . . . . ?
C12 C13 C14 C15 45.3(8) . . . . ?
O14 C14 C15 O15 -165.0(6) . . . . ?
C13 C14 C15 O15 -44.6(8) . . . . ?
O14 C14 C15 C16 74.0(8) . . . . ?
C13 C14 C15 C16 -165.7(6) . . . . ?
O15 C15 C16 O16 -68.6(9) . . . . ?
C14 C15 C16 O16 55.1(9) . . . . ?
O14 C21 C22 O22 52.5(9) . . . . ?
O25 C21 C22 O22 175.9(7) . . . . ?
O14 C21 C22 C23 -71.3(9) . . . . ?
O25 C21 C22 C23 52.1(10) . . . . ?
O22 C22 C23 O23 65.7(10) . . . . ?
C21 C22 C23 O23 -171.8(7) . . . . ?
O22 C22 C23 C24 -171.4(7) . . . . ?
C21 C22 C23 C24 -48.9(10) . . . . ?
O23 C23 C24 O24 -68.3(8) . . . . ?
C22 C23 C24 O24 169.7(6) . . . . ?
O23 C23 C24 C25 173.3(6) . . . . ?
C22 C23 C24 C25 51.3(9) . . . . ?
O24 C24 C25 O25 -172.9(6) . . . . ?
C23 C24 C25 O25 -56.6(8) . . . . ?
O24 C24 C25 C26 65.6(8) . . . . ?
C23 C24 C25 C26 -178.1(6) . . . . ?
O25 C25 C26 O26 -70.9(7) . . . . ?
C24 C25 C26 O26 51.1(8) . . . . ?
O35 C31 C32 O32 -176.1(6) . . . . ?
O24 C31 C32 O32 62.0(8) . . . . ?
O35 C31 C32 C33 63.0(7) . . . . ?
O24 C31 C32 C33 -58.9(8) . . . . ?
O32 C32 C33 O33 65.0(8) . . . . ?
C31 C32 C33 O33 -171.4(6) . . . . ?
O32 C32 C33 C34 -175.3(6) . . . . ?
C31 C32 C33 C34 -51.7(8) . . . . ?
O33 C33 C34 O34 -75.3(7) . . . . ?
C32 C33 C34 O34 163.4(6) . . . . ?
O33 C33 C34 C35 163.9(6) . . . . ?
C32 C33 C34 C35 42.6(9) . . . . ?
O34 C34 C35 O35 -161.9(5) . . . . ?
C33 C34 C35 O35 -43.7(8) . . . . ?
O34 C34 C35 C36 76.3(8) . . . . ?
C33 C34 C35 C36 -165.5(7) . . . . ?
O35 C35 C36 O36 -72.5(9) . . . . ?
C34 C35 C36 O36 51.2(10) . . . . ?
O34 C41 C42 O42 56.0(7) . . . . ?
O45 C41 C42 O42 178.1(5) . . . . ?
O34 C41 C42 C43 -63.5(8) . . . . ?
O45 C41 C42 C43 58.5(7) . . . . ?
O42 C42 C43 O43 62.9(8) . . . . ?
C41 C42 C43 O43 -174.2(6) . . . . ?
O42 C42 C43 C44 -177.6(6) . . . . ?
C41 C42 C43 C44 -54.7(8) . . . . ?
O43 C43 C44 O44 -66.5(7) . . . . ?
C42 C43 C44 O44 174.5(6) . . . . ?
O43 C43 C44 C45 172.9(5) . . . . ?
C42 C43 C44 C45 53.9(8) . . . . ?
O44 C44 C45 O45 -175.8(5) . . . . ?
C43 C44 C45 O45 -56.7(7) . . . . ?
O44 C44 C45 C46 66.2(7) . . . . ?
C43 C44 C45 C46 -174.7(5) . . . . ?
O45 C45 C46 O46 -71.2(7) . . . . ?
C44 C45 C46 O46 48.4(8) . . . . ?
O44 C51 C52 O52 58.8(9) . . . . ?
O55 C51 C52 O52 -177.9(6) . . . . ?
O44 C51 C52 C53 -61.1(9) . . . . ?
O55 C51 C52 C53 62.2(9) . . . . ?
O52 C52 C53 O53 61.8(9) . . . . ?
C51 C52 C53 O53 -174.9(7) . . . . ?
O52 C52 C53 C54 179.7(7) . . . . ?
C51 C52 C53 C54 -57.0(9) . . . . ?
O53 C53 C54 O1 -71.7(8) . . . . ?
C52 C53 C54 O1 170.1(6) . . . . ?
O53 C53 C54 C55 167.3(7) . . . . ?
C52 C53 C54 C55 49.1(9) . . . . ?
O1 C54 C55 O55 -161.4(6) . . . . ?
C53 C54 C55 O55 -44.1(9) . . . . ?
O1 C54 C55 C56 83.9(8) . . . . ?
C53 C54 C55 C56 -158.9(7) . . . . ?
O55 C55 C56 P1 116.8(5) . . . . ?
C54 C55 C56 P1 -123.2(6) . . . . ?
C65 C60 C61 C62 -1.1(15) . . . . ?
P1 C60 C61 C62 -178.9(8) . . . . ?
C60 C61 C62 C63 2.0(18) . . . . ?
C61 C62 C63 C64 -3.7(19) . . . . ?
C62 C63 C64 C65 4.6(16) . . . . ?
C61 C60 C65 C64 1.9(13) . . . . ?
P1 C60 C65 C64 179.8(7) . . . . ?
C61 C60 C65 N1 -179.4(8) . . . . ?
P1 C60 C65 N1 -1.5(11) . . . . ?
C63 C64 C65 C60 -3.7(14) . . . . ?
C63 C64 C65 N1 177.8(9) . . . . ?
C73 C68 C69 C70 8(2) . . . . ?
C68 C69 C70 C71 -4(2) . . . . ?
C69 C70 C71 C72 -2(2) . . . . ?
C70 C71 C72 C73 4(2) . . . . ?
C69 C68 C73 C72 -6(2) . . . . ?
C71 C72 C73 C68 0(2) . . . . ?
C60 C65 N1 C66 116.6(9) . . . . ?
C64 C65 N1 C66 -64.8(11) . . . . ?
C60 C65 N1 C67 -114.7(9) . . . . ?
C64 C65 N1 C67 63.9(12) . . . . ?
O5 C1 O1 C54 73.9(8) . . . . ?
C2 C1 O1 C54 -165.3(6) . . . . ?
C55 C54 O1 C1 -97.4(7) . . . . ?
C53 C54 O1 C1 140.0(6) . . . . ?
C3 C2 O2 C7 -106.1(12) . . . . ?
C1 C2 O2 C7 130.1(11) . . . . ?
C2 C3 O3 C8 -128.7(7) . . . . ?
C4 C3 O3 C8 109.8(7) . . . . ?
O15 C11 O4 C4 104.5(7) . . . . ?
C12 C11 O4 C4 -135.2(7) . . . . ?
C3 C4 O4 C11 147.5(6) . . . . ?
C5 C4 O4 C11 -94.6(7) . . . . ?
O1 C1 O5 C5 56.6(8) . . . . ?
C2 C1 O5 C5 -64.3(7) . . . . ?
C6 C5 O5 C1 -164.7(6) . . . . ?
C4 C5 O5 C1 68.6(7) . . . . ?
C11 C12 O12 C17 95.8(9) . . . . ?
C13 C12 O12 C17 -142.5(8) . . . . ?
C14 C13 O13 C18 145.1(7) . . . . ?
C12 C13 O13 C18 -93.2(8) . . . . ?
O25 C21 O14 C14 97.0(7) . . . . ?
C22 C21 O14 C14 -140.5(7) . . . . ?
C13 C14 O14 C21 106.9(8) . . . . ?
C15 C14 O14 C21 -129.6(7) . . . . ?
O4 C11 O15 C15 55.2(8) . . . . ?
C12 C11 O15 C15 -65.2(7) . . . . ?
C16 C15 O15 C11 -179.6(6) . . . . ?
C14 C15 O15 C11 55.3(8) . . . . ?
C15 C16 O16 C19 -175.3(8) . . . . ?
C23 C22 O22 C27 -99.3(12) . . . . ?
C21 C22 O22 C27 137.3(11) . . . . ?
C24 C23 O23 C28 116.8(8) . . . . ?
C22 C23 O23 C28 -118.7(8) . . . . ?
O35 C31 O24 C24 105.0(7) . . . . ?
C32 C31 O24 C24 -136.2(7) . . . . ?
C23 C24 O24 C31 140.4(6) . . . . ?
C25 C24 O24 C31 -101.5(7) . . . . ?
O14 C21 O25 C25 59.6(8) . . . . ?
C22 C21 O25 C25 -61.3(9) . . . . ?
C26 C25 O25 C21 -170.3(6) . . . . ?
C24 C25 O25 C21 63.7(8) . . . . ?
C25 C26 O26 C29 -173.8(6) . . . . ?
C33 C32 O32 C37 -155.7(7) . . . . ?
C31 C32 O32 C37 82.6(9) . . . . ?
C32 C33 O33 C38 -106.3(8) . . . . ?
C34 C33 O33 C38 131.3(8) . . . . ?
O45 C41 O34 C34 103.7(7) . . . . ?
C42 C41 O34 C34 -135.8(6) . . . . ?
C33 C34 O34 C41 134.7(6) . . . . ?
C35 C34 O34 C41 -102.9(7) . . . . ?
O24 C31 O35 C35 52.5(8) . . . . ?
C32 C31 O35 C35 -67.2(8) . . . . ?
C36 C35 O35 C31 -177.6(6) . . . . ?
C34 C35 O35 C31 58.0(8) . . . . ?
C35 C36 O36 C39 87.9(16) . . . . ?
C43 C42 O42 C47 -170.6(7) . . . . ?
C41 C42 O42 C47 67.8(7) . . . . ?
C44 C43 O43 C48 113.4(7) . . . . ?
C42 C43 O43 C48 -128.1(7) . . . . ?
O55 C51 O44 C44 111.5(6) . . . . ?
C52 C51 O44 C44 -127.4(6) . . . . ?
C43 C44 O44 C51 136.4(6) . . . . ?
C45 C44 O44 C51 -102.4(7) . . . . ?
O34 C41 O45 C45 57.8(7) . . . . ?
C42 C41 O45 C45 -62.7(7) . . . . ?
C46 C45 O45 C41 -176.9(6) . . . . ?
C44 C45 O45 C41 61.7(7) . . . . ?
C45 C46 O46 C49 -175.8(8) . . . . ?
C53 C52 O52 C57 -173.1(8) . . . . ?
C51 C52 O52 C57 67.1(10) . . . . ?
C52 C53 O53 C58 -130.1(8) . . . . ?
C54 C53 O53 C58 109.9(8) . . . . ?
O44 C51 O55 C55 60.1(7) . . . . ?
C52 C51 O55 C55 -61.9(8) . . . . ?
C54 C55 O55 C51 52.2(8) . . . . ?
C56 C55 O55 C51 174.9(5) . . . . ?
C5 C6 P1 C60 -147.4(6) . . . . ?
C5 C6 P1 C56 -38.1(7) . . . . ?
C5 C6 P1 Au1 85.5(6) . . . . ?
C61 C60 P1 C6 106.7(8) . . . . ?
C65 C60 P1 C6 -71.1(7) . . . . ?
C61 C60 P1 C56 -7.2(9) . . . . ?
C65 C60 P1 C56 175.0(7) . . . . ?
C61 C60 P1 Au1 -129.3(7) . . . . ?
C65 C60 P1 Au1 52.8(7) . . . . ?
C55 C56 P1 C6 86.2(6) . . . . ?
C55 C56 P1 C60 -163.3(6) . . . . ?
C55 C56 P1 Au1 -37.6(6) . . . . ?

_refine_diff_density_max         1.300
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.095

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.184 0.000 741 134 ' '
2 0.500 0.091 1.000 741 134 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
 The residual electron density was assigned to one molecule
 and a half of the benzene solvent [269/4 = 67 e per
 asymmetric unit; 1.5 molecule of C6H6 would give 63e].
;



####################################################################### 
# 
# 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_dayl201124
_database_code_depnum_ccdc_archive 'CCDC 2163663'
loop_
_audit_author_name
_audit_author_address
'Lydia Karmazin'
;University of Strasbourg
France
;
_audit_update_record             
;
2022-03-31 deposited with the CCDC.	2022-06-28 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT987_dayl201124          
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check
RESPONSE: the compound is chiral, hence Flack x >> 0
;
# Added during the CSD deposition process: Thursday 31 March 2022 01:50 PM
# end Validation Reply Form

_audit_creation_date             2021-07-27
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C60 H100 Br2 N Ni O28 P), 5(C6 H6), C5 H12'
_chemical_formula_sum            'C155 H242 Br4 N2 Ni2 O56 P2'
_chemical_formula_weight         3528.49
_chemical_absolute_configuration rmad
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   17.8671(6)
_cell_length_b                   17.8671(6)
_cell_length_c                   53.805(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17176.2(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9398
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.87
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.705
_exptl_absorpt_coefficient_mu    1.252
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             7440
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       -70
_diffrn_reflns_number            277051
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.896
_diffrn_reflns_theta_min         1.895
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω shuterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Mo-ImuS 3.0 microfocus tube'
_reflns_Friedel_coverage         0.792
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15880
_reflns_number_total             20499
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.795
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 
;
 Flack x determined using 5953 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         20499
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      1.040
_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)+(0.0693P)²+18.4409P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1474
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(C57) = Uanis(C57B)
Uanis(C68) = Uanis(C69) = Uanis(C70) = Uanis(C71) = Uanis(C72) = Uanis(C73)
Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(C78) = Uanis(C79)
Uanis(C80) = Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) = Uanis(C85)
Uanis(C86) = Uanis(C87) = Uanis(C88) = Uanis(C89) = Uanis(C90)
2. Others
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C57B(0.5) H57D(0.5)
 H57E(0.5) H57F(0.5) C80(0.5) H80(0.5) C81(0.5) H81(0.5) C82(0.5) H82(0.5)
 C83(0.5) H83(0.5) C84(0.5) H84(0.5) C85(0.5) H85(0.5) C86(0.5) H86A(0.5)
 H86B(0.5) H86C(0.5) C87(0.5) H87A(0.5) H87B(0.5) C88(0.5) H88A(0.5) H88B(0.5)
 C89(0.5) H89A(0.5) H89B(0.5) C90(0.5) H90A(0.5) H90B(0.5) H90C(0.5)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C31(H31),
  C32(H32), C33(H33), C34(H34), C35(H35), C41(H41), C42(H42), C43(H43),
 C44(H44), C45(H45), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C16(H16A,H16B), C26(H26A,H26B), C36(H36A,H36B), C46(H46A,H46B),
 C56(H56A,H56B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B)
3.c Aromatic/amide H refined with riding coordinates:
 C61(H61), C62(H62), C63(H63), C64(H64), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85)
3.d Fitted hexagon refined as free rotating group:
 C68(C69,C70,C71,C72,C73), C74(C75,C76,C77,C78,C79), C80(C81,C82,C83,C84,C85)
3.e Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C57B(H57D,H57E,H57F),
 C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C66(H66A,H66B,H66C), C67(H67A,H67B,
 H67C), C86(H86A,H86B,H86C), C90(H90A,H90B,H90C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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 0.2791(3) 1.1162(3) 0.68629(9) 0.0384(12) Uani 1 1 d . . . . .
H1 H 0.2575 1.1675 0.6846 0.046 Uiso 1 1 calc R U . . .
C2 C 0.2448(3) 1.0662(3) 0.66682(10) 0.0419(13) Uani 1 1 d . . . . .
H2 H 0.2540 1.0882 0.6500 0.050 Uiso 1 1 calc R U . . .
C3 C 0.2795(3) 0.9890(3) 0.66796(9) 0.0368(12) Uani 1 1 d . . . . .
H3 H 0.2675 0.9656 0.6844 0.044 Uiso 1 1 calc R U . . .
C4 C 0.3647(3) 0.9947(3) 0.66505(9) 0.0353(11) Uani 1 1 d . . . . .
H4 H 0.3761 1.0138 0.6480 0.042 Uiso 1 1 calc R U . . .
C5 C 0.3973(3) 1.0490(3) 0.68404(9) 0.0351(11) Uani 1 1 d . . . . .
H5 H 0.3921 1.0285 0.7012 0.042 Uiso 1 1 calc R U . . .
C6 C 0.4784(3) 1.0735(3) 0.67909(9) 0.0377(11) Uani 1 1 d . . . . .
H6A H 0.4767 1.1287 0.6775 0.045 Uiso 1 1 calc R U . . .
H6B H 0.4909 1.0540 0.6624 0.045 Uiso 1 1 calc R U . . .
C7 C 0.1209(5) 1.0775(7) 0.6514(2) 0.098(3) Uani 1 1 d . . . . .
H7A H 0.1393 1.1222 0.6428 0.148 Uiso 1 1 calc R U . . .
H7B H 0.0698 1.0864 0.6573 0.148 Uiso 1 1 calc R U . . .
H7C H 0.1210 1.0350 0.6399 0.148 Uiso 1 1 calc R U . . .
C8 C 0.2245(4) 0.8728(4) 0.65611(12) 0.0510(15) Uani 1 1 d . . . . .
H8A H 0.2678 0.8424 0.6608 0.076 Uiso 1 1 calc R U . . .
H8B H 0.1978 0.8484 0.6424 0.076 Uiso 1 1 calc R U . . .
H8C H 0.1908 0.8778 0.6704 0.076 Uiso 1 1 calc R U . . .
C11 C 0.4524(3) 0.9004(3) 0.65210(9) 0.0341(11) Uani 1 1 d . . . . .
H11 H 0.4461 0.9230 0.6352 0.041 Uiso 1 1 calc R U . . .
C12 C 0.4599(3) 0.8156(3) 0.64952(9) 0.0356(11) Uani 1 1 d . . . . .
H12 H 0.5002 0.8052 0.6371 0.043 Uiso 1 1 calc R U . . .
C13 C 0.4825(3) 0.7785(3) 0.67411(9) 0.0343(11) Uani 1 1 d . . . . .
H13 H 0.4372 0.7746 0.6850 0.041 Uiso 1 1 calc R U . . .
C14 C 0.5436(3) 0.8200(3) 0.68827(9) 0.0364(11) Uani 1 1 d . . . . .
H14 H 0.5931 0.8104 0.6802 0.044 Uiso 1 1 calc R U . . .
C15 C 0.5276(3) 0.9041(3) 0.68832(9) 0.0366(11) Uani 1 1 d . . . . .
H15 H 0.4796 0.9138 0.6973 0.044 Uiso 1 1 calc R U . . .
C16 C 0.5875(3) 0.9540(3) 0.69851(9) 0.0403(12) Uani 1 1 d . . . . .
H16A H 0.6334 0.9478 0.6884 0.048 Uiso 1 1 calc R U . . .
H16B H 0.5993 0.9382 0.7157 0.048 Uiso 1 1 calc R U . . .
C17 C 0.3742(4) 0.7981(4) 0.61656(10) 0.0539(17) Uani 1 1 d . . . . .
H17A H 0.3499 0.8473 0.6163 0.081 Uiso 1 1 calc R U . . .
H17B H 0.3396 0.7604 0.6100 0.081 Uiso 1 1 calc R U . . .
H17C H 0.4194 0.7994 0.6062 0.081 Uiso 1 1 calc R U . . .
C18 C 0.4601(4) 0.6476(4) 0.67628(14) 0.0583(18) Uani 1 1 d . . . . .
H18A H 0.4477 0.6534 0.6939 0.087 Uiso 1 1 calc R U . . .
H18B H 0.4841 0.5989 0.6737 0.087 Uiso 1 1 calc R U . . .
H18C H 0.4143 0.6505 0.6663 0.087 Uiso 1 1 calc R U . . .
C21 C 0.6132(3) 0.7663(3) 0.72323(9) 0.0348(11) Uani 1 1 d . . . . .
H21 H 0.6480 0.7520 0.7095 0.042 Uiso 1 1 calc R U . . .
C22 C 0.6000(3) 0.6987(3) 0.73978(9) 0.0359(11) Uani 1 1 d . . . . .
H22 H 0.6493 0.6803 0.7461 0.043 Uiso 1 1 calc R U . . .
C23 C 0.5504(3) 0.7194(3) 0.76176(9) 0.0351(11) Uani 1 1 d . . . . .
H23 H 0.4993 0.7334 0.7558 0.042 Uiso 1 1 calc R U . . .
C24 C 0.5853(3) 0.7851(3) 0.77581(9) 0.0342(11) Uani 1 1 d . . . . .
H24 H 0.6329 0.7687 0.7839 0.041 Uiso 1 1 calc R U . . .
C25 C 0.6013(3) 0.8504(3) 0.75791(9) 0.0351(11) Uani 1 1 d . . . . .
H25 H 0.5527 0.8701 0.7514 0.042 Uiso 1 1 calc R U . . .
C26 C 0.6432(3) 0.9129(4) 0.76997(10) 0.0449(13) Uani 1 1 d . . . . .
H26A H 0.6592 0.9494 0.7572 0.054 Uiso 1 1 calc R U . . .
H26B H 0.6102 0.9390 0.7819 0.054 Uiso 1 1 calc R U . . .
C27 C 0.5930(4) 0.5683(3) 0.73097(11) 0.0534(16) Uani 1 1 d . . . . .
H27A H 0.6478 0.5680 0.7304 0.080 Uiso 1 1 calc R U . . .
H27B H 0.5734 0.5328 0.7187 0.080 Uiso 1 1 calc R U . . .
H27C H 0.5761 0.5538 0.7476 0.080 Uiso 1 1 calc R U . . .
C28 C 0.4709(4) 0.6289(4) 0.78104(12) 0.0553(16) Uani 1 1 d . . . . .
H28A H 0.4397 0.6666 0.7893 0.083 Uiso 1 1 calc R U . . .
H28B H 0.4720 0.5833 0.7911 0.083 Uiso 1 1 calc R U . . .
H28C H 0.4500 0.6174 0.7646 0.083 Uiso 1 1 calc R U . . .
C29 C 0.7418(4) 0.9432(5) 0.79601(13) 0.071(2) Uani 1 1 d . . . . .
H29A H 0.7625 0.9800 0.7844 0.106 Uiso 1 1 calc R U . . .
H29B H 0.7823 0.9222 0.8061 0.106 Uiso 1 1 calc R U . . .
H29C H 0.7051 0.9676 0.8069 0.106 Uiso 1 1 calc R U . . .
C31 C 0.5595(3) 0.8202(3) 0.81865(8) 0.0338(11) Uani 1 1 d . . . . .
H31 H 0.6069 0.7911 0.8209 0.041 Uiso 1 1 calc R U . . .
C32 C 0.5017(3) 0.7924(3) 0.83764(9) 0.0357(11) Uani 1 1 d . . . . .
H32 H 0.5239 0.7972 0.8546 0.043 Uiso 1 1 calc R U . . .
C33 C 0.4315(3) 0.8388(3) 0.83673(9) 0.0330(11) Uani 1 1 d . . . . .
H33 H 0.4042 0.8289 0.8208 0.040 Uiso 1 1 calc R U . . .
C34 C 0.4489(3) 0.9214(3) 0.83876(9) 0.0319(10) Uani 1 1 d . . . . .
H34 H 0.4653 0.9333 0.8561 0.038 Uiso 1 1 calc R U . . .
C35 C 0.5103(3) 0.9445(3) 0.82041(8) 0.0334(10) Uani 1 1 d . . . . .
H35 H 0.4909 0.9392 0.8031 0.040 Uiso 1 1 calc R U . . .
C36 C 0.5383(3) 1.0232(3) 0.82411(9) 0.0351(11) Uani 1 1 d . . . . .
H36A H 0.5816 1.0325 0.8131 0.042 Uiso 1 1 calc R U . . .
H36B H 0.4983 1.0592 0.8197 0.042 Uiso 1 1 calc R U . . .
C37 C 0.5369(4) 0.6642(3) 0.84100(11) 0.0478(14) Uani 1 1 d . . . . .
H37A H 0.5805 0.6692 0.8301 0.072 Uiso 1 1 calc R U . . .
H37B H 0.5167 0.6133 0.8397 0.072 Uiso 1 1 calc R U . . .
H37C H 0.5520 0.6738 0.8582 0.072 Uiso 1 1 calc R U . . .
C38 C 0.3215(4) 0.7763(4) 0.85106(13) 0.0523(15) Uani 1 1 d . . . . .
H38A H 0.2884 0.8053 0.8402 0.078 Uiso 1 1 calc R U . . .
H38B H 0.2946 0.7625 0.8662 0.078 Uiso 1 1 calc R U . . .
H38C H 0.3378 0.7308 0.8424 0.078 Uiso 1 1 calc R U . . .
C39 C 0.5772(4) 1.1101(3) 0.85426(11) 0.0505(15) Uani 1 1 d . . . . .
H39A H 0.6170 1.1266 0.8430 0.076 Uiso 1 1 calc R U . . .
H39B H 0.5940 1.1154 0.8715 0.076 Uiso 1 1 calc R U . . .
H39C H 0.5325 1.1408 0.8516 0.076 Uiso 1 1 calc R U . . .
C41 C 0.3581(3) 1.0171(3) 0.85020(9) 0.0332(11) Uani 1 1 d . . . . .
H41 H 0.3805 1.0060 0.8668 0.040 Uiso 1 1 calc R U . . .
C42 C 0.2732(3) 1.0156(3) 0.85251(9) 0.0342(11) Uani 1 1 d . . . . .
H42 H 0.2578 1.0546 0.8648 0.041 Uiso 1 1 calc R U . . .
C43 C 0.2378(3) 1.0347(3) 0.82743(9) 0.0351(11) Uani 1 1 d . . . . .
H43 H 0.2473 0.9928 0.8155 0.042 Uiso 1 1 calc R U . . .
C44 C 0.2693(3) 1.1062(3) 0.81685(9) 0.0354(11) Uani 1 1 d . . . . .
H44 H 0.2468 1.1497 0.8258 0.043 Uiso 1 1 calc R U . . .
C45 C 0.3544(3) 1.1113(3) 0.81859(9) 0.0360(11) Uani 1 1 d . . . . .
H45 H 0.3768 1.0770 0.8059 0.043 Uiso 1 1 calc R U . . .
C46 C 0.3847(4) 1.1895(3) 0.81446(10) 0.0424(13) Uani 1 1 d . . . . .
H46A H 0.4390 1.1906 0.8180 0.051 Uiso 1 1 calc R U . . .
H46B H 0.3769 1.2046 0.7969 0.051 Uiso 1 1 calc R U . . .
C47 C 0.2586(4) 0.9294(4) 0.88576(10) 0.0477(14) Uani 1 1 d . . . . .
H47A H 0.3109 0.9135 0.8875 0.072 Uiso 1 1 calc R U . . .
H47B H 0.2255 0.8890 0.8914 0.072 Uiso 1 1 calc R U . . .
H47C H 0.2499 0.9741 0.8959 0.072 Uiso 1 1 calc R U . . .
C48 C 0.1156(4) 0.9897(4) 0.81729(17) 0.068(2) Uani 1 1 d . . . . .
H48A H 0.1212 0.9983 0.7994 0.103 Uiso 1 1 calc R U . . .
H48B H 0.0629 0.9949 0.8219 0.103 Uiso 1 1 calc R U . . .
H48C H 0.1330 0.9392 0.8214 0.103 Uiso 1 1 calc R U . . .
C49 C 0.3760(5) 1.3128(4) 0.82931(13) 0.0609(19) Uani 1 1 d . . . . .
H49A H 0.4299 1.3110 0.8327 0.091 Uiso 1 1 calc R U . . .
H49B H 0.3514 1.3448 0.8416 0.091 Uiso 1 1 calc R U . . .
H49C H 0.3676 1.3332 0.8126 0.091 Uiso 1 1 calc R U . . .
C51 C 0.2258(3) 1.1771(3) 0.78067(10) 0.0390(12) Uani 1 1 d . . . . .
H51 H 0.2127 1.2132 0.7942 0.047 Uiso 1 1 calc R U . . .
C52 C 0.1582(3) 1.1653(3) 0.76419(10) 0.0432(13) Uani 1 1 d . . . . .
H52 H 0.1433 1.2146 0.7569 0.052 Uiso 1 1 calc R U . . .
C53 C 0.1760(3) 1.1121(3) 0.74315(10) 0.0400(12) Uani 1 1 d . . . . .
H53 H 0.1891 1.0618 0.7500 0.048 Uiso 1 1 calc R U . . .
C54 C 0.2428(3) 1.1438(3) 0.72877(10) 0.0348(11) Uani 1 1 d . . . . .
H54 H 0.2278 1.1915 0.7204 0.042 Uiso 1 1 calc R U . . .
C55 C 0.3082(3) 1.1586(3) 0.74609(9) 0.0354(11) Uani 1 1 d . . . . .
H55 H 0.3250 1.1098 0.7533 0.042 Uiso 1 1 calc R U . . .
C56 C 0.3740(3) 1.1958(3) 0.73413(10) 0.0393(12) Uani 1 1 d . . . . .
H56A H 0.4102 1.2113 0.7471 0.047 Uiso 1 1 calc R U . . .
H56B H 0.3995 1.1599 0.7229 0.047 Uiso 1 1 calc R U . . .
C57 C 0.0282(11) 1.1729(15) 0.7745(4) 0.099(5) Uani 0.5 1 d . . P A 1
H57A H 0.0369 1.2262 0.7713 0.149 Uiso 0.5 1 calc R U P A 1
H57B H -0.0035 1.1673 0.7892 0.149 Uiso 0.5 1 calc R U P A 1
H57C H 0.0032 1.1503 0.7601 0.149 Uiso 0.5 1 calc R U P A 1
C57B C 0.0660(11) 1.1966(14) 0.7927(4) 0.099(5) Uani 0.5 1 d . . P A 2
H57D H 0.0947 1.2028 0.8081 0.149 Uiso 0.5 1 calc R U P A 2
H57E H 0.0138 1.1852 0.7968 0.149 Uiso 0.5 1 calc R U P A 2
H57F H 0.0681 1.2430 0.7830 0.149 Uiso 0.5 1 calc R U P A 2
C58 C 0.0869(5) 1.0321(5) 0.72342(15) 0.078(3) Uani 1 1 d . . . . .
H58A H 0.1270 1.0020 0.7160 0.117 Uiso 1 1 calc R U . . .
H58B H 0.0438 1.0332 0.7122 0.117 Uiso 1 1 calc R U . . .
H58C H 0.0720 1.0101 0.7393 0.117 Uiso 1 1 calc R U . . .
C59 C 0.4127(4) 1.2907(4) 0.70742(13) 0.0570(17) Uani 1 1 d . . . . .
H59A H 0.4513 1.3056 0.7194 0.086 Uiso 1 1 calc R U . . .
H59B H 0.3960 1.3347 0.6981 0.086 Uiso 1 1 calc R U . . .
H59C H 0.4334 1.2535 0.6959 0.086 Uiso 1 1 calc R U . . .
C60 C 0.6301(3) 1.0994(3) 0.67988(10) 0.0417(13) Uani 1 1 d . . . . .
C61 C 0.6464(4) 1.0816(4) 0.65492(10) 0.0493(15) Uani 1 1 d . . . . .
H61 H 0.6223 1.0402 0.6473 0.059 Uiso 1 1 calc R U . . .
C62 C 0.6962(4) 1.1230(5) 0.64169(12) 0.0617(19) Uani 1 1 d . . . . .
H62 H 0.7055 1.1117 0.6247 0.074 Uiso 1 1 calc R U . . .
C63 C 0.7332(5) 1.1817(6) 0.65310(13) 0.074(2) Uani 1 1 d . . . . .
H63 H 0.7687 1.2102 0.6439 0.089 Uiso 1 1 calc R U . . .
C64 C 0.7190(5) 1.1994(5) 0.67778(13) 0.066(2) Uani 1 1 d . . . . .
H64 H 0.7448 1.2397 0.6855 0.079 Uiso 1 1 calc R U . . .
C65 C 0.6670(4) 1.1580(4) 0.69108(11) 0.0537(16) Uani 1 1 d . . . . .
C66 C 0.6324(6) 1.2552(4) 0.72034(16) 0.081(3) Uani 1 1 d . . . . .
H66A H 0.6752 1.2859 0.7153 0.121 Uiso 1 1 calc R U . . .
H66B H 0.6196 1.2661 0.7377 0.121 Uiso 1 1 calc R U . . .
H66C H 0.5894 1.2666 0.7097 0.121 Uiso 1 1 calc R U . . .
C67 C 0.7222(5) 1.1565(5) 0.73195(14) 0.075(2) Uani 1 1 d . . . . .
H67A H 0.7278 1.1021 0.7337 0.113 Uiso 1 1 calc R U . . .
H67B H 0.7193 1.1794 0.7485 0.113 Uiso 1 1 calc R U . . .
H67C H 0.7654 1.1767 0.7230 0.113 Uiso 1 1 calc R U . . .
C68 C 0.3137(7) 0.8957(7) 0.77302(15) 0.184(4) Uani 1 1 d G . . . .
H68 H 0.3177 0.9149 0.7894 0.221 Uiso 1 1 calc R U . . .
C69 C 0.3708(6) 0.8518(8) 0.76324(18) 0.184(4) Uani 1 1 d G . . . .
H69 H 0.4139 0.8411 0.7730 0.221 Uiso 1 1 calc R U . . .
C70 C 0.3649(6) 0.8237(7) 0.73923(19) 0.184(4) Uani 1 1 d G . . . .
H70 H 0.4040 0.7938 0.7325 0.221 Uiso 1 1 calc R U . . .
C71 C 0.3019(7) 0.8395(7) 0.72500(15) 0.184(4) Uani 1 1 d G . . . .
H71 H 0.2979 0.8202 0.7086 0.221 Uiso 1 1 calc R U . . .
C72 C 0.2448(6) 0.8833(8) 0.73479(18) 0.184(4) Uani 1 1 d G . . . .
H72 H 0.2017 0.8940 0.7251 0.221 Uiso 1 1 calc R U . . .
C73 C 0.2507(6) 0.9114(8) 0.75880(19) 0.184(4) Uani 1 1 d G . . . .
H73 H 0.2117 0.9414 0.7655 0.221 Uiso 1 1 calc R U . . .
C74 C 0.5670(6) 0.6642(7) 0.61229(15) 0.158(3) Uani 1 1 d G . . . .
H74 H 0.5537 0.6806 0.6285 0.190 Uiso 1 1 calc R U . . .
C75 C 0.5823(6) 0.5890(6) 0.60802(17) 0.158(3) Uani 1 1 d G . . . .
H75 H 0.5795 0.5541 0.6213 0.190 Uiso 1 1 calc R U . . .
C76 C 0.6017(6) 0.5649(5) 0.5843(2) 0.158(3) Uani 1 1 d G . . . .
H76 H 0.6122 0.5135 0.5814 0.190 Uiso 1 1 calc R U . . .
C77 C 0.6059(6) 0.6160(6) 0.56488(15) 0.158(3) Uani 1 1 d G . . . .
H77 H 0.6191 0.5996 0.5487 0.190 Uiso 1 1 calc R U . . .
C78 C 0.5905(6) 0.6912(6) 0.56915(17) 0.158(3) Uani 1 1 d G . . . .
H78 H 0.5933 0.7261 0.5559 0.190 Uiso 1 1 calc R U . . .
C79 C 0.5711(6) 0.7153(5) 0.5929(2) 0.158(3) Uani 1 1 d G . . . .
H79 H 0.5606 0.7667 0.5958 0.190 Uiso 1 1 calc R U . . .
C80 C 0.0820(9) 0.0600(7) 0.9249(2) 0.088(2) Uani 0.5 1 d G . P B 1
H80 H 0.0744 0.0173 0.9351 0.106 Uiso 0.5 1 calc R U P B 1
C81 C 0.0803(8) 0.1312(8) 0.93525(18) 0.088(2) Uani 0.5 1 d G . P B 1
H81 H 0.0715 0.1372 0.9526 0.106 Uiso 0.5 1 calc R U P B 1
C82 C 0.0915(7) 0.1937(6) 0.9203(2) 0.088(2) Uani 0.5 1 d G . P B 1
H82 H 0.0903 0.2424 0.9274 0.106 Uiso 0.5 1 calc R U P B 1
C83 C 0.1043(8) 0.1851(7) 0.8950(2) 0.088(2) Uani 0.5 1 d G . P B 1
H83 H 0.1120 0.2278 0.8848 0.106 Uiso 0.5 1 calc R U P B 1
C84 C 0.1060(7) 0.1139(8) 0.88463(18) 0.088(2) Uani 0.5 1 d G . P B 1
H84 H 0.1149 0.1079 0.8673 0.106 Uiso 0.5 1 calc R U P B 1
C85 C 0.0949(8) 0.0513(6) 0.8995(3) 0.088(2) Uani 0.5 1 d G . P B 1
H85 H 0.0960 0.0027 0.8924 0.106 Uiso 0.5 1 calc R U P B 1
C86 C 0.1076(11) 0.2362(10) 0.8459(3) 0.074(2) Uani 0.5 1 d . . P C 2
H86A H 0.1051 0.1957 0.8337 0.112 Uiso 0.5 1 calc R U P C 2
H86B H 0.1387 0.2769 0.8394 0.112 Uiso 0.5 1 calc R U P C 2
H86C H 0.0571 0.2549 0.8493 0.112 Uiso 0.5 1 calc R U P C 2
C87 C 0.1419(11) 0.2067(10) 0.8699(3) 0.074(2) Uani 0.5 1 d . . P C 2
H87A H 0.1478 0.2487 0.8817 0.089 Uiso 0.5 1 calc R U P C 2
H87B H 0.1923 0.1865 0.8663 0.089 Uiso 0.5 1 calc R U P C 2
C88 C 0.0943(12) 0.1453(10) 0.8820(3) 0.074(2) Uani 0.5 1 d . . P C 2
H88A H 0.0428 0.1644 0.8845 0.089 Uiso 0.5 1 calc R U P C 2
H88B H 0.0915 0.1019 0.8706 0.089 Uiso 0.5 1 calc R U P C 2
C89 C 0.1248(11) 0.1199(10) 0.9065(3) 0.074(2) Uani 0.5 1 d . . P C 2
H89A H 0.1203 0.1615 0.9185 0.089 Uiso 0.5 1 calc R U P C 2
H89B H 0.1788 0.1088 0.9045 0.089 Uiso 0.5 1 calc R U P C 2
C90 C 0.0862(13) 0.0509(10) 0.9172(3) 0.074(2) Uani 0.5 1 d . . P C 2
H90A H 0.0464 0.0346 0.9059 0.112 Uiso 0.5 1 calc R U P C 2
H90B H 0.0645 0.0634 0.9334 0.112 Uiso 0.5 1 calc R U P C 2
H90C H 0.1228 0.0106 0.9192 0.112 Uiso 0.5 1 calc R U P C 2
N1 N 0.6523(3) 1.1734(3) 0.71782(9) 0.0537(13) Uani 1 1 d . . . . .
O1 O 0.2631(2) 1.0891(2) 0.71018(6) 0.0374(8) Uani 1 1 d . . . . .
O2 O 0.1661(2) 1.0620(3) 0.67109(8) 0.0627(14) Uani 1 1 d . . . . .
O3 O 0.2488(2) 0.9443(2) 0.64852(7) 0.0423(9) Uani 1 1 d . . . . .
O4 O 0.3902(2) 0.9193(2) 0.66687(6) 0.0349(8) Uani 1 1 d . . . . .
O5 O 0.3575(2) 1.1199(2) 0.68174(6) 0.0367(8) Uani 1 1 d . . . . .
O12 O 0.3939(2) 0.7796(2) 0.64128(6) 0.0399(9) Uani 1 1 d . . . . .
O13 O 0.5096(2) 0.7051(2) 0.66901(7) 0.0413(9) Uani 1 1 d . . . . .
O14 O 0.5433(2) 0.7892(2) 0.71280(6) 0.0360(8) Uani 1 1 d . . . . .
O15 O 0.5199(2) 0.9272(2) 0.66275(6) 0.0367(8) Uani 1 1 d . . . . .
O22 O 0.5662(2) 0.6416(2) 0.72539(7) 0.0407(9) Uani 1 1 d . . . . .
O23 O 0.5457(2) 0.6574(2) 0.77822(7) 0.0413(9) Uani 1 1 d . . . . .
O24 O 0.5325(2) 0.8084(2) 0.79440(6) 0.0347(8) Uani 1 1 d . . . . .
O25 O 0.6461(2) 0.8252(2) 0.73731(6) 0.0368(8) Uani 1 1 d . . . . .
O26 O 0.7065(2) 0.8851(3) 0.78252(8) 0.0528(11) Uani 1 1 d . . . . .
O32 O 0.4815(2) 0.7164(2) 0.83386(7) 0.0398(8) Uani 1 1 d . . . . .
O33 O 0.3847(2) 0.8199(2) 0.85732(7) 0.0399(9) Uani 1 1 d . . . . .
O34 O 0.3805(2) 0.9611(2) 0.83329(6) 0.0327(7) Uani 1 1 d . . . . .
O35 O 0.5743(2) 0.8968(2) 0.82352(6) 0.0342(8) Uani 1 1 d . . . . .
O36 O 0.5600(2) 1.0340(2) 0.84944(7) 0.0405(9) Uani 1 1 d . . . . .
O42 O 0.2435(2) 0.9460(2) 0.86023(7) 0.0410(9) Uani 1 1 d . . . . .
O43 O 0.1593(2) 1.0437(2) 0.83064(7) 0.0456(10) Uani 1 1 d . . . . .
O44 O 0.2456(2) 1.1078(2) 0.79140(6) 0.0371(8) Uani 1 1 d . . . . .
O45 O 0.3805(2) 1.0893(2) 0.84284(6) 0.0361(8) Uani 1 1 d . . . . .
O46 O 0.3460(3) 1.2398(2) 0.83070(8) 0.0514(11) Uani 1 1 d . . . . .
O52 O 0.0969(2) 1.1369(3) 0.77851(8) 0.0557(12) Uani 1 1 d . . . . .
O53 O 0.1130(2) 1.1057(3) 0.72736(8) 0.0503(10) Uani 1 1 d . . . . .
O55 O 0.2846(2) 1.2072(2) 0.76621(6) 0.0373(8) Uani 1 1 d . . . . .
O56 O 0.3509(2) 1.2592(2) 0.72035(8) 0.0452(10) Uani 1 1 d . . . . .
P1 P 0.56098(8) 1.05317(8) 0.69872(2) 0.0376(3) Uani 1 1 d . . . . .
Ni1 Ni 0.57137(5) 1.11062(4) 0.73316(2) 0.04362(19) Uani 1 1 d . . . . .
Br1 Br 0.48237(3) 1.02626(3) 0.74655(2) 0.04287(14) Uani 1 1 d . . . . .
Br2 Br 0.57747(6) 1.16970(4) 0.77277(2) 0.0709(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 H1 1.0000 . ?
C1 C2 1.507(8) . ?
C1 O1 1.403(6) . ?
C1 O5 1.424(7) . ?
C2 H2 1.0000 . ?
C2 C3 1.512(8) . ?
C2 O2 1.426(7) . ?
C3 H3 1.0000 . ?
C3 C4 1.534(8) . ?
C3 O3 1.426(6) . ?
C4 H4 1.0000 . ?
C4 C5 1.525(7) . ?
C4 O4 1.426(6) . ?
C5 H5 1.0000 . ?
C5 C6 1.537(8) . ?
C5 O5 1.458(6) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 P1 1.850(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C7 O2 1.362(9) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 O3 1.410(7) . ?
C11 H11 1.0000 . ?
C11 C12 1.528(7) . ?
C11 O4 1.407(6) . ?
C11 O15 1.417(6) . ?
C12 H12 1.0000 . ?
C12 C13 1.533(7) . ?
C12 O12 1.415(7) . ?
C13 H13 1.0000 . ?
C13 C14 1.523(8) . ?
C13 O13 1.426(6) . ?
C14 H14 1.0000 . ?
C14 C15 1.529(8) . ?
C14 O14 1.430(6) . ?
C15 H15 1.0000 . ?
C15 C16 1.498(8) . ?
C15 O15 1.443(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 P1 1.834(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 O12 1.415(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 O13 1.410(8) . ?
C21 H21 1.0000 . ?
C21 C22 1.520(8) . ?
C21 O14 1.428(6) . ?
C21 O25 1.424(7) . ?
C22 H22 1.0000 . ?
C22 C23 1.524(7) . ?
C22 O22 1.415(7) . ?
C23 H23 1.0000 . ?
C23 C24 1.529(8) . ?
C23 O23 1.420(6) . ?
C24 H24 1.0000 . ?
C24 C25 1.539(7) . ?
C24 O24 1.437(6) . ?
C25 H25 1.0000 . ?
C25 C26 1.493(8) . ?
C25 O25 1.439(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 O26 1.407(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C27 O22 1.427(7) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 O23 1.438(8) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 O26 1.415(8) . ?
C31 H31 1.0000 . ?
C31 C32 1.535(7) . ?
C31 O24 1.407(6) . ?
C31 O35 1.418(6) . ?
C32 H32 1.0000 . ?
C32 C33 1.505(8) . ?
C32 O32 1.420(7) . ?
C33 H33 1.0000 . ?
C33 C34 1.512(7) . ?
C33 O33 1.428(6) . ?
C34 H34 1.0000 . ?
C34 C35 1.532(7) . ?
C34 O34 1.443(6) . ?
C35 H35 1.0000 . ?
C35 C36 1.505(8) . ?
C35 O35 1.437(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 O36 1.430(6) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 O32 1.415(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C38 O33 1.412(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 O36 1.417(7) . ?
C41 H41 1.0000 . ?
C41 C42 1.523(7) . ?
C41 O34 1.411(6) . ?
C41 O45 1.407(6) . ?
C42 H42 1.0000 . ?
C42 C43 1.528(7) . ?
C42 O42 1.414(7) . ?
C43 H43 1.0000 . ?
C43 C44 1.508(8) . ?
C43 O43 1.422(7) . ?
C44 H44 1.0000 . ?
C44 C45 1.525(8) . ?
C44 O44 1.434(6) . ?
C45 H45 1.0000 . ?
C45 C46 1.515(8) . ?
C45 O45 1.440(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C46 O46 1.432(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 O42 1.431(6) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 O43 1.433(9) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 O46 1.411(8) . ?
C51 H51 1.0000 . ?
C51 C52 1.513(9) . ?
C51 O44 1.410(6) . ?
C51 O55 1.414(7) . ?
C52 H52 1.0000 . ?
C52 C53 1.512(8) . ?
C52 O52 1.431(7) . ?
C53 H53 1.0000 . ?
C53 C54 1.532(8) . ?
C53 O53 1.415(7) . ?
C54 H54 1.0000 . ?
C54 C55 1.518(8) . ?
C54 O1 1.445(6) . ?
C55 H55 1.0000 . ?
C55 C56 1.496(8) . ?
C55 O55 1.451(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 O56 1.416(7) . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C57 O52 1.40(2) . ?
C57B H57D 0.9800 . ?
C57B H57E 0.9800 . ?
C57B H57F 0.9800 . ?
C57B O52 1.42(2) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C58 O53 1.410(9) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C59 O56 1.421(8) . ?
C60 C61 1.410(8) . ?
C60 C65 1.377(9) . ?
C60 P1 1.798(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.359(10) . ?
C62 H62 0.9500 . ?
C62 C63 1.384(11) . ?
C63 H63 0.9500 . ?
C63 C64 1.389(10) . ?
C64 H64 0.9500 . ?
C64 C65 1.387(10) . ?
C65 N1 1.488(8) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C66 N1 1.511(10) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C67 N1 1.493(10) . ?
C68 H68 0.9500 . ?
C68 C69 1.3900 . ?
C68 C73 1.3900 . ?
C69 H69 0.9500 . ?
C69 C70 1.3900 . ?
C70 H70 0.9500 . ?
C70 C71 1.3900 . ?
C71 H71 0.9500 . ?
C71 C72 1.3900 . ?
C72 H72 0.9500 . ?
C72 C73 1.3900 . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?
C74 C75 1.3900 . ?
C74 C79 1.3900 . ?
C75 H75 0.9500 . ?
C75 C76 1.3900 . ?
C76 H76 0.9500 . ?
C76 C77 1.3900 . ?
C77 H77 0.9500 . ?
C77 C78 1.3900 . ?
C78 H78 0.9500 . ?
C78 C79 1.3900 . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
C80 C81 1.3900 . ?
C80 C85 1.3900 . ?
C81 H81 0.9500 . ?
C81 C82 1.3900 . ?
C82 H82 0.9500 . ?
C82 C83 1.3900 . ?
C83 H83 0.9500 . ?
C83 C84 1.3900 . ?
C84 H84 0.9500 . ?
C84 C85 1.3900 . ?
C85 H85 0.9500 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C86 C87 1.52(2) . ?
C87 H87A 0.9900 . ?
C87 H87B 0.9900 . ?
C87 C88 1.53(3) . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C88 C89 1.50(2) . ?
C89 H89A 0.9900 . ?
C89 H89B 0.9900 . ?
C89 C90 1.53(3) . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
N1 Ni1 2.007(6) . ?
P1 Ni1 2.1263(15) . ?
Ni1 Br1 2.3063(10) . ?
Ni1 Br2 2.3807(9) . ?

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 H1 108.8 . . ?
O1 C1 H1 108.8 . . ?
O1 C1 C2 110.4(5) . . ?
O1 C1 O5 112.0(4) . . ?
O5 C1 H1 108.8 . . ?
O5 C1 C2 108.0(4) . . ?
C1 C2 H2 109.2 . . ?
C1 C2 C3 110.2(4) . . ?
C3 C2 H2 109.2 . . ?
O2 C2 C1 108.7(5) . . ?
O2 C2 H2 109.2 . . ?
O2 C2 C3 110.4(5) . . ?
C2 C3 H3 109.3 . . ?
C2 C3 C4 110.0(5) . . ?
C4 C3 H3 109.3 . . ?
O3 C3 C2 108.9(4) . . ?
O3 C3 H3 109.3 . . ?
O3 C3 C4 110.1(4) . . ?
C3 C4 H4 108.6 . . ?
C5 C4 C3 110.7(4) . . ?
C5 C4 H4 108.6 . . ?
O4 C4 C3 104.4(4) . . ?
O4 C4 H4 108.6 . . ?
O4 C4 C5 115.6(4) . . ?
C4 C5 H5 110.6 . . ?
C4 C5 C6 115.2(4) . . ?
C6 C5 H5 110.6 . . ?
O5 C5 C4 108.0(4) . . ?
O5 C5 H5 110.6 . . ?
O5 C5 C6 101.4(4) . . ?
C5 C6 H6A 105.7 . . ?
C5 C6 H6B 105.7 . . ?
C5 C6 P1 126.6(4) . . ?
H6A C6 H6B 106.1 . . ?
P1 C6 H6A 105.7 . . ?
P1 C6 H6B 105.7 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O2 C7 H7A 109.5 . . ?
O2 C7 H7B 109.5 . . ?
O2 C7 H7C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
C12 C11 H11 109.1 . . ?
O4 C11 H11 109.1 . . ?
O4 C11 C12 111.0(4) . . ?
O4 C11 O15 111.3(4) . . ?
O15 C11 H11 109.1 . . ?
O15 C11 C12 107.2(4) . . ?
C11 C12 H12 107.9 . . ?
C11 C12 C13 111.9(4) . . ?
C13 C12 H12 107.9 . . ?
O12 C12 C11 114.0(4) . . ?
O12 C12 H12 107.9 . . ?
O12 C12 C13 107.1(4) . . ?
C12 C13 H13 108.8 . . ?
C14 C13 C12 114.2(4) . . ?
C14 C13 H13 108.8 . . ?
O13 C13 C12 108.7(4) . . ?
O13 C13 H13 108.8 . . ?
O13 C13 C14 107.5(4) . . ?
C13 C14 H14 109.6 . . ?
C13 C14 C15 110.2(4) . . ?
C15 C14 H14 109.6 . . ?
O14 C14 C13 105.8(4) . . ?
O14 C14 H14 109.6 . . ?
O14 C14 C15 112.1(4) . . ?
C14 C15 H15 109.4 . . ?
C16 C15 C14 116.9(5) . . ?
C16 C15 H15 109.4 . . ?
O15 C15 C14 107.3(4) . . ?
O15 C15 H15 109.4 . . ?
O15 C15 C16 104.3(4) . . ?
C15 C16 H16A 109.0 . . ?
C15 C16 H16B 109.0 . . ?
C15 C16 P1 113.1(4) . . ?
H16A C16 H16B 107.8 . . ?
P1 C16 H16A 109.0 . . ?
P1 C16 H16B 109.0 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O12 C17 H17A 109.5 . . ?
O12 C17 H17B 109.5 . . ?
O12 C17 H17C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O13 C18 H18A 109.5 . . ?
O13 C18 H18B 109.5 . . ?
O13 C18 H18C 109.5 . . ?
C22 C21 H21 109.0 . . ?
O14 C21 H21 109.0 . . ?
O14 C21 C22 108.8(4) . . ?
O25 C21 H21 109.0 . . ?
O25 C21 C22 109.9(4) . . ?
O25 C21 O14 111.0(4) . . ?
C21 C22 H22 109.0 . . ?
C21 C22 C23 110.6(4) . . ?
C23 C22 H22 109.0 . . ?
O22 C22 C21 108.5(4) . . ?
O22 C22 H22 109.0 . . ?
O22 C22 C23 110.6(5) . . ?
C22 C23 H23 109.9 . . ?
C22 C23 C24 109.4(4) . . ?
C24 C23 H23 109.9 . . ?
O23 C23 C22 109.2(4) . . ?
O23 C23 H23 109.9 . . ?
O23 C23 C24 108.4(4) . . ?
C23 C24 H24 109.8 . . ?
C23 C24 C25 110.4(4) . . ?
C25 C24 H24 109.8 . . ?
O24 C24 C23 107.3(4) . . ?
O24 C24 H24 109.8 . . ?
O24 C24 C25 109.7(4) . . ?
C24 C25 H25 108.9 . . ?
C26 C25 C24 112.8(4) . . ?
C26 C25 H25 108.9 . . ?
O25 C25 C24 110.4(4) . . ?
O25 C25 H25 108.9 . . ?
O25 C25 C26 106.8(4) . . ?
C25 C26 H26A 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
O26 C26 C25 110.4(5) . . ?
O26 C26 H26A 109.6 . . ?
O26 C26 H26B 109.6 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O22 C27 H27A 109.5 . . ?
O22 C27 H27B 109.5 . . ?
O22 C27 H27C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O23 C28 H28A 109.5 . . ?
O23 C28 H28B 109.5 . . ?
O23 C28 H28C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O26 C29 H29A 109.5 . . ?
O26 C29 H29B 109.5 . . ?
O26 C29 H29C 109.5 . . ?
C32 C31 H31 108.8 . . ?
O24 C31 H31 108.8 . . ?
O24 C31 C32 109.7(4) . . ?
O24 C31 O35 112.3(4) . . ?
O35 C31 H31 108.8 . . ?
O35 C31 C32 108.4(4) . . ?
C31 C32 H32 108.3 . . ?
C33 C32 C31 111.2(4) . . ?
C33 C32 H32 108.3 . . ?
O32 C32 C31 112.7(4) . . ?
O32 C32 H32 108.3 . . ?
O32 C32 C33 108.0(4) . . ?
C32 C33 H33 109.6 . . ?
C32 C33 C34 111.3(4) . . ?
C34 C33 H33 109.6 . . ?
O33 C33 C32 109.4(4) . . ?
O33 C33 H33 109.6 . . ?
O33 C33 C34 107.2(4) . . ?
C33 C34 H34 109.5 . . ?
C33 C34 C35 111.4(4) . . ?
C35 C34 H34 109.5 . . ?
O34 C34 C33 106.8(4) . . ?
O34 C34 H34 109.5 . . ?
O34 C34 C35 110.0(4) . . ?
C34 C35 H35 109.1 . . ?
C36 C35 C34 113.8(4) . . ?
C36 C35 H35 109.1 . . ?
O35 C35 C34 109.6(4) . . ?
O35 C35 H35 109.1 . . ?
O35 C35 C36 105.9(4) . . ?
C35 C36 H36A 109.6 . . ?
C35 C36 H36B 109.6 . . ?
H36A C36 H36B 108.2 . . ?
O36 C36 C35 110.1(4) . . ?
O36 C36 H36A 109.6 . . ?
O36 C36 H36B 109.6 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O32 C37 H37A 109.5 . . ?
O32 C37 H37B 109.5 . . ?
O32 C37 H37C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O33 C38 H38A 109.5 . . ?
O33 C38 H38B 109.5 . . ?
O33 C38 H38C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O36 C39 H39A 109.5 . . ?
O36 C39 H39B 109.5 . . ?
O36 C39 H39C 109.5 . . ?
C42 C41 H41 108.8 . . ?
O34 C41 H41 108.8 . . ?
O34 C41 C42 108.8(4) . . ?
O45 C41 H41 108.8 . . ?
O45 C41 C42 108.8(4) . . ?
O45 C41 O34 112.8(4) . . ?
C41 C42 H42 108.4 . . ?
C41 C42 C43 109.6(4) . . ?
C43 C42 H42 108.4 . . ?
O42 C42 C41 114.5(4) . . ?
O42 C42 H42 108.4 . . ?
O42 C42 C43 107.5(4) . . ?
C42 C43 H43 109.2 . . ?
C44 C43 C42 111.6(5) . . ?
C44 C43 H43 109.2 . . ?
O43 C43 C42 109.0(4) . . ?
O43 C43 H43 109.2 . . ?
O43 C43 C44 108.5(4) . . ?
C43 C44 H44 109.0 . . ?
C43 C44 C45 113.5(4) . . ?
C45 C44 H44 109.0 . . ?
O44 C44 C43 105.5(4) . . ?
O44 C44 H44 109.0 . . ?
O44 C44 C45 110.6(4) . . ?
C44 C45 H45 108.7 . . ?
C46 C45 C44 113.7(5) . . ?
C46 C45 H45 108.7 . . ?
O45 C45 C44 111.2(4) . . ?
O45 C45 H45 108.7 . . ?
O45 C45 C46 105.6(4) . . ?
C45 C46 H46A 110.0 . . ?
C45 C46 H46B 110.0 . . ?
H46A C46 H46B 108.4 . . ?
O46 C46 C45 108.5(4) . . ?
O46 C46 H46A 110.0 . . ?
O46 C46 H46B 110.0 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O42 C47 H47A 109.5 . . ?
O42 C47 H47B 109.5 . . ?
O42 C47 H47C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O43 C48 H48A 109.5 . . ?
O43 C48 H48B 109.5 . . ?
O43 C48 H48C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O46 C49 H49A 109.5 . . ?
O46 C49 H49B 109.5 . . ?
O46 C49 H49C 109.5 . . ?
C52 C51 H51 109.2 . . ?
O44 C51 H51 109.2 . . ?
O44 C51 C52 108.5(5) . . ?
O44 C51 O55 111.9(4) . . ?
O55 C51 H51 109.2 . . ?
O55 C51 C52 108.9(4) . . ?
C51 C52 H52 108.5 . . ?
C53 C52 C51 111.0(5) . . ?
C53 C52 H52 108.5 . . ?
O52 C52 C51 110.2(4) . . ?
O52 C52 H52 108.5 . . ?
O52 C52 C53 110.0(5) . . ?
C52 C53 H53 109.7 . . ?
C52 C53 C54 108.0(5) . . ?
C54 C53 H53 109.7 . . ?
O53 C53 C52 109.5(5) . . ?
O53 C53 H53 109.7 . . ?
O53 C53 C54 110.3(4) . . ?
C53 C54 H54 109.5 . . ?
C55 C54 C53 110.8(4) . . ?
C55 C54 H54 109.5 . . ?
O1 C54 C53 107.1(4) . . ?
O1 C54 H54 109.5 . . ?
O1 C54 C55 110.5(4) . . ?
C54 C55 H55 108.6 . . ?
C56 C55 C54 114.7(4) . . ?
C56 C55 H55 108.6 . . ?
O55 C55 C54 109.8(4) . . ?
O55 C55 H55 108.6 . . ?
O55 C55 C56 106.4(4) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 108.1 . . ?
O56 C56 C55 110.6(4) . . ?
O56 C56 H56A 109.5 . . ?
O56 C56 H56B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
O52 C57 H57A 109.5 . . ?
O52 C57 H57B 109.5 . . ?
O52 C57 H57C 109.5 . . ?
H57D C57B H57E 109.5 . . ?
H57D C57B H57F 109.5 . . ?
H57E C57B H57F 109.5 . . ?
O52 C57B H57D 109.5 . . ?
O52 C57B H57E 109.5 . . ?
O52 C57B H57F 109.5 . . ?
H58A C58 H58B 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
O53 C58 H58A 109.5 . . ?
O53 C58 H58B 109.5 . . ?
O53 C58 H58C 109.5 . . ?
H59A C59 H59B 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
O56 C59 H59A 109.5 . . ?
O56 C59 H59B 109.5 . . ?
O56 C59 H59C 109.5 . . ?
C61 C60 P1 125.1(5) . . ?
C65 C60 C61 119.3(6) . . ?
C65 C60 P1 115.6(4) . . ?
C60 C61 H61 119.6 . . ?
C62 C61 C60 120.7(6) . . ?
C62 C61 H61 119.6 . . ?
C61 C62 H62 120.2 . . ?
C61 C62 C63 119.6(6) . . ?
C63 C62 H62 120.2 . . ?
C62 C63 H63 119.7 . . ?
C62 C63 C64 120.6(7) . . ?
C64 C63 H63 119.7 . . ?
C63 C64 H64 120.2 . . ?
C65 C64 C63 119.6(7) . . ?
C65 C64 H64 120.2 . . ?
C60 C65 C64 120.1(6) . . ?
C60 C65 N1 118.6(6) . . ?
C64 C65 N1 121.2(6) . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
N1 C66 H66A 109.5 . . ?
N1 C66 H66B 109.5 . . ?
N1 C66 H66C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N1 C67 H67A 109.5 . . ?
N1 C67 H67B 109.5 . . ?
N1 C67 H67C 109.5 . . ?
C69 C68 H68 120.0 . . ?
C69 C68 C73 120.0 . . ?
C73 C68 H68 120.0 . . ?
C68 C69 H69 120.0 . . ?
C68 C69 C70 120.0 . . ?
C70 C69 H69 120.0 . . ?
C69 C70 H70 120.0 . . ?
C71 C70 C69 120.0 . . ?
C71 C70 H70 120.0 . . ?
C70 C71 H71 120.0 . . ?
C70 C71 C72 120.0 . . ?
C72 C71 H71 120.0 . . ?
C71 C72 H72 120.0 . . ?
C73 C72 C71 120.0 . . ?
C73 C72 H72 120.0 . . ?
C68 C73 H73 120.0 . . ?
C72 C73 C68 120.0 . . ?
C72 C73 H73 120.0 . . ?
C75 C74 H74 120.0 . . ?
C75 C74 C79 120.0 . . ?
C79 C74 H74 120.0 . . ?
C74 C75 H75 120.0 . . ?
C76 C75 C74 120.0 . . ?
C76 C75 H75 120.0 . . ?
C75 C76 H76 120.0 . . ?
C75 C76 C77 120.0 . . ?
C77 C76 H76 120.0 . . ?
C76 C77 H77 120.0 . . ?
C78 C77 C76 120.0 . . ?
C78 C77 H77 120.0 . . ?
C77 C78 H78 120.0 . . ?
C77 C78 C79 120.0 . . ?
C79 C78 H78 120.0 . . ?
C74 C79 H79 120.0 . . ?
C78 C79 C74 120.0 . . ?
C78 C79 H79 120.0 . . ?
C81 C80 H80 120.0 . . ?
C81 C80 C85 120.0 . . ?
C85 C80 H80 120.0 . . ?
C80 C81 H81 120.0 . . ?
C80 C81 C82 120.0 . . ?
C82 C81 H81 120.0 . . ?
C81 C82 H82 120.0 . . ?
C83 C82 C81 120.0 . . ?
C83 C82 H82 120.0 . . ?
C82 C83 H83 120.0 . . ?
C82 C83 C84 120.0 . . ?
C84 C83 H83 120.0 . . ?
C83 C84 H84 120.0 . . ?
C83 C84 C85 120.0 . . ?
C85 C84 H84 120.0 . . ?
C80 C85 H85 120.0 . . ?
C84 C85 C80 120.0 . . ?
C84 C85 H85 120.0 . . ?
H86A C86 H86B 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C87 C86 H86A 109.5 . . ?
C87 C86 H86B 109.5 . . ?
C87 C86 H86C 109.5 . . ?
C86 C87 H87A 109.1 . . ?
C86 C87 H87B 109.1 . . ?
C86 C87 C88 112.6(16) . . ?
H87A C87 H87B 107.8 . . ?
C88 C87 H87A 109.1 . . ?
C88 C87 H87B 109.1 . . ?
C87 C88 H88A 109.0 . . ?
C87 C88 H88B 109.0 . . ?
H88A C88 H88B 107.8 . . ?
C89 C88 C87 112.9(17) . . ?
C89 C88 H88A 109.0 . . ?
C89 C88 H88B 109.0 . . ?
C88 C89 H89A 108.7 . . ?
C88 C89 H89B 108.7 . . ?
C88 C89 C90 114.4(17) . . ?
H89A C89 H89B 107.6 . . ?
C90 C89 H89A 108.7 . . ?
C90 C89 H89B 108.7 . . ?
C89 C90 H90A 109.5 . . ?
C89 C90 H90B 109.5 . . ?
C89 C90 H90C 109.5 . . ?
H90A C90 H90B 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
C65 N1 C66 107.9(6) . . ?
C65 N1 C67 107.9(6) . . ?
C65 N1 Ni1 114.9(4) . . ?
C66 N1 Ni1 109.5(5) . . ?
C67 N1 C66 110.3(6) . . ?
C67 N1 Ni1 106.3(5) . . ?
C1 O1 C54 116.8(4) . . ?
C7 O2 C2 116.7(6) . . ?
C8 O3 C3 114.5(4) . . ?
C11 O4 C4 116.2(4) . . ?
C1 O5 C5 115.1(4) . . ?
C12 O12 C17 113.3(4) . . ?
C18 O13 C13 113.9(5) . . ?
C21 O14 C14 118.0(4) . . ?
C11 O15 C15 111.8(4) . . ?
C22 O22 C27 113.8(4) . . ?
C23 O23 C28 113.4(5) . . ?
C31 O24 C24 117.6(4) . . ?
C21 O25 C25 114.3(4) . . ?
C26 O26 C29 110.2(6) . . ?
C37 O32 C32 114.4(5) . . ?
C38 O33 C33 114.4(4) . . ?
C41 O34 C34 117.2(4) . . ?
C31 O35 C35 113.7(4) . . ?
C39 O36 C36 111.3(4) . . ?
C42 O42 C47 113.2(4) . . ?
C43 O43 C48 113.6(5) . . ?
C51 O44 C44 118.8(4) . . ?
C41 O45 C45 114.4(4) . . ?
C49 O46 C46 111.4(5) . . ?
C57 O52 C52 115.1(10) . . ?
C57B O52 C52 108.7(10) . . ?
C58 O53 C53 115.3(6) . . ?
C51 O55 C55 113.5(4) . . ?
C56 O56 C59 110.3(5) . . ?
C6 P1 Ni1 118.18(18) . . ?
C16 P1 C6 113.1(3) . . ?
C16 P1 Ni1 116.70(17) . . ?
C60 P1 C6 97.8(3) . . ?
C60 P1 C16 105.2(3) . . ?
C60 P1 Ni1 102.11(19) . . ?
N1 Ni1 P1 88.53(15) . . ?
N1 Ni1 Br1 171.95(16) . . ?
N1 Ni1 Br2 95.01(15) . . ?
P1 Ni1 Br1 84.06(5) . . ?
P1 Ni1 Br2 176.45(6) . . ?
Br1 Ni1 Br2 92.40(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -56.2(6) . . . . ?
C1 C2 C3 O3 -177.0(4) . . . . ?
C1 C2 O2 C7 127.7(8) . . . . ?
C2 C1 O1 C54 -138.1(5) . . . . ?
C2 C1 O5 C5 -63.2(5) . . . . ?
C2 C3 C4 C5 54.0(5) . . . . ?
C2 C3 C4 O4 179.0(4) . . . . ?
C2 C3 O3 C8 -132.1(5) . . . . ?
C3 C2 O2 C7 -111.3(8) . . . . ?
C3 C4 C5 C6 -166.1(4) . . . . ?
C3 C4 C5 O5 -53.7(5) . . . . ?
C3 C4 O4 C11 145.5(4) . . . . ?
C4 C3 O3 C8 107.2(6) . . . . ?
C4 C5 C6 P1 -115.2(5) . . . . ?
C4 C5 O5 C1 60.6(5) . . . . ?
C5 C4 O4 C11 -92.7(5) . . . . ?
C5 C6 P1 C16 69.0(5) . . . . ?
C5 C6 P1 C60 179.2(5) . . . . ?
C5 C6 P1 Ni1 -72.5(5) . . . . ?
C6 C5 O5 C1 -177.9(4) . . . . ?
C11 C12 C13 C14 -43.1(6) . . . . ?
C11 C12 C13 O13 -163.1(4) . . . . ?
C11 C12 O12 C17 66.9(6) . . . . ?
C12 C11 O4 C4 -162.9(4) . . . . ?
C12 C11 O15 C15 -69.2(5) . . . . ?
C12 C13 C14 C15 44.3(6) . . . . ?
C12 C13 C14 O14 165.6(4) . . . . ?
C12 C13 O13 C18 -107.4(5) . . . . ?
C13 C12 O12 C17 -168.8(5) . . . . ?
C13 C14 C15 C16 -172.0(4) . . . . ?
C13 C14 C15 O15 -55.4(6) . . . . ?
C13 C14 O14 C21 130.9(5) . . . . ?
C14 C13 O13 C18 128.5(5) . . . . ?
C14 C15 C16 P1 -177.9(4) . . . . ?
C14 C15 O15 C11 71.4(5) . . . . ?
C15 C14 O14 C21 -109.0(5) . . . . ?
C15 C16 P1 C6 -15.3(5) . . . . ?
C15 C16 P1 C60 -120.8(4) . . . . ?
C15 C16 P1 Ni1 126.8(3) . . . . ?
C16 C15 O15 C11 -164.0(4) . . . . ?
C21 C22 C23 C24 -55.4(6) . . . . ?
C21 C22 C23 O23 -173.9(4) . . . . ?
C21 C22 O22 C27 140.9(5) . . . . ?
C22 C21 O14 C14 -146.4(4) . . . . ?
C22 C21 O25 C25 -60.0(5) . . . . ?
C22 C23 C24 C25 53.6(5) . . . . ?
C22 C23 C24 O24 173.1(4) . . . . ?
C22 C23 O23 C28 -117.9(5) . . . . ?
C23 C22 O22 C27 -97.6(5) . . . . ?
C23 C24 C25 C26 -173.5(4) . . . . ?
C23 C24 C25 O25 -54.2(6) . . . . ?
C23 C24 O24 C31 132.8(4) . . . . ?
C24 C23 O23 C28 122.9(5) . . . . ?
C24 C25 C26 O26 50.2(6) . . . . ?
C24 C25 O25 C21 58.5(5) . . . . ?
C25 C24 O24 C31 -107.2(5) . . . . ?
C25 C26 O26 C29 -174.1(5) . . . . ?
C26 C25 O25 C21 -178.6(4) . . . . ?
C31 C32 C33 C34 -51.8(5) . . . . ?
C31 C32 C33 O33 -170.1(4) . . . . ?
C31 C32 O32 C37 73.7(6) . . . . ?
C32 C31 O24 C24 -141.7(5) . . . . ?
C32 C31 O35 C35 -63.1(5) . . . . ?
C32 C33 C34 C35 49.9(5) . . . . ?
C32 C33 C34 O34 170.0(4) . . . . ?
C32 C33 O33 C38 -105.7(5) . . . . ?
C33 C32 O32 C37 -163.2(4) . . . . ?
C33 C34 C35 C36 -171.3(4) . . . . ?
C33 C34 C35 O35 -53.0(5) . . . . ?
C33 C34 O34 C41 130.1(4) . . . . ?
C34 C33 O33 C38 133.4(5) . . . . ?
C34 C35 C36 O36 52.6(6) . . . . ?
C34 C35 O35 C31 61.6(5) . . . . ?
C35 C34 O34 C41 -108.9(5) . . . . ?
C35 C36 O36 C39 -172.2(5) . . . . ?
C36 C35 O35 C31 -175.2(4) . . . . ?
C41 C42 C43 C44 -51.8(6) . . . . ?
C41 C42 C43 O43 -171.7(4) . . . . ?
C41 C42 O42 C47 71.2(6) . . . . ?
C42 C41 O34 C34 -142.9(4) . . . . ?
C42 C41 O45 C45 -64.1(5) . . . . ?
C42 C43 C44 C45 45.3(6) . . . . ?
C42 C43 C44 O44 166.6(4) . . . . ?
C42 C43 O43 C48 -116.5(6) . . . . ?
C43 C42 O42 C47 -166.8(4) . . . . ?
C43 C44 C45 C46 -164.8(4) . . . . ?
C43 C44 C45 O45 -45.8(6) . . . . ?
C43 C44 O44 C51 143.2(5) . . . . ?
C44 C43 O43 C48 121.7(5) . . . . ?
C44 C45 C46 O46 52.1(6) . . . . ?
C44 C45 O45 C41 56.4(6) . . . . ?
C45 C44 O44 C51 -93.7(6) . . . . ?
C45 C46 O46 C49 175.0(5) . . . . ?
C46 C45 O45 C41 -179.8(4) . . . . ?
C51 C52 C53 C54 -56.6(6) . . . . ?
C51 C52 C53 O53 -176.7(4) . . . . ?
C51 C52 O52 C57 133.0(12) . . . . ?
C51 C52 O52 C57B 75.8(11) . . . . ?
C52 C51 O44 C44 -140.4(5) . . . . ?
C52 C51 O55 C55 -61.2(5) . . . . ?
C52 C53 C54 C55 54.5(6) . . . . ?
C52 C53 C54 O1 175.0(4) . . . . ?
C52 C53 O53 C58 -124.8(6) . . . . ?
C53 C52 O52 C57 -104.3(12) . . . . ?
C53 C52 O52 C57B -161.6(11) . . . . ?
C53 C54 C55 C56 -175.0(4) . . . . ?
C53 C54 C55 O55 -55.2(6) . . . . ?
C53 C54 O1 C1 136.3(5) . . . . ?
C54 C53 O53 C58 116.4(6) . . . . ?
C54 C55 C56 O56 49.3(6) . . . . ?
C54 C55 O55 C51 59.7(5) . . . . ?
C55 C54 O1 C1 -102.9(5) . . . . ?
C55 C56 O56 C59 -175.3(5) . . . . ?
C56 C55 O55 C51 -175.6(4) . . . . ?
C60 C61 C62 C63 2.2(11) . . . . ?
C60 C65 N1 C66 -128.1(8) . . . . ?
C60 C65 N1 C67 112.7(7) . . . . ?
C60 C65 N1 Ni1 -5.6(9) . . . . ?
C61 C60 C65 C64 0.7(11) . . . . ?
C61 C60 C65 N1 -176.7(6) . . . . ?
C61 C60 P1 C6 -59.4(6) . . . . ?
C61 C60 P1 C16 57.2(6) . . . . ?
C61 C60 P1 Ni1 179.5(5) . . . . ?
C61 C62 C63 C64 -1.1(14) . . . . ?
C62 C63 C64 C65 -0.3(14) . . . . ?
C63 C64 C65 C60 0.4(13) . . . . ?
C63 C64 C65 N1 177.7(8) . . . . ?
C64 C65 N1 C66 54.6(10) . . . . ?
C64 C65 N1 C67 -64.6(9) . . . . ?
C64 C65 N1 Ni1 177.0(6) . . . . ?
C65 C60 C61 C62 -2.1(10) . . . . ?
C65 C60 P1 C6 118.3(5) . . . . ?
C65 C60 P1 C16 -125.1(5) . . . . ?
C65 C60 P1 Ni1 -2.8(5) . . . . ?
C68 C69 C70 C71 0.0 . . . . ?
C69 C68 C73 C72 0.0 . . . . ?
C69 C70 C71 C72 0.0 . . . . ?
C70 C71 C72 C73 0.0 . . . . ?
C71 C72 C73 C68 0.0 . . . . ?
C73 C68 C69 C70 0.0 . . . . ?
C74 C75 C76 C77 0.0 . . . . ?
C75 C74 C79 C78 0.0 . . . . ?
C75 C76 C77 C78 0.0 . . . . ?
C76 C77 C78 C79 0.0 . . . . ?
C77 C78 C79 C74 0.0 . . . . ?
C79 C74 C75 C76 0.0 . . . . ?
C80 C81 C82 C83 0.0 . . . . ?
C81 C80 C85 C84 0.0 . . . . ?
C81 C82 C83 C84 0.0 . . . . ?
C82 C83 C84 C85 0.0 . . . . ?
C83 C84 C85 C80 0.0 . . . . ?
C85 C80 C81 C82 0.0 . . . . ?
C86 C87 C88 C89 -175.9(14) . . . . ?
C87 C88 C89 C90 -171.1(15) . . . . ?
O1 C1 C2 C3 -63.8(6) . . . . ?
O1 C1 C2 O2 57.4(6) . . . . ?
O1 C1 O5 C5 58.6(6) . . . . ?
O1 C54 C55 C56 66.5(6) . . . . ?
O1 C54 C55 O55 -173.7(4) . . . . ?
O2 C2 C3 C4 -176.3(4) . . . . ?
O2 C2 C3 O3 62.9(6) . . . . ?
O3 C3 C4 C5 174.0(4) . . . . ?
O3 C3 C4 O4 -61.0(5) . . . . ?
O4 C4 C5 C6 75.4(6) . . . . ?
O4 C4 C5 O5 -172.1(4) . . . . ?
O4 C11 C12 C13 -69.1(6) . . . . ?
O4 C11 C12 O12 52.6(5) . . . . ?
O4 C11 O15 C15 52.3(5) . . . . ?
O5 C1 C2 C3 59.0(6) . . . . ?
O5 C1 C2 O2 -179.9(4) . . . . ?
O5 C1 O1 C54 101.5(5) . . . . ?
O5 C5 C6 P1 128.5(4) . . . . ?
O12 C12 C13 C14 -168.6(4) . . . . ?
O12 C12 C13 O13 71.3(5) . . . . ?
O13 C13 C14 C15 165.0(4) . . . . ?
O13 C13 C14 O14 -73.7(5) . . . . ?
O14 C14 C15 C16 70.5(6) . . . . ?
O14 C14 C15 O15 -172.9(4) . . . . ?
O14 C21 C22 C23 -64.1(5) . . . . ?
O14 C21 C22 O22 57.3(5) . . . . ?
O14 C21 O25 C25 60.4(5) . . . . ?
O15 C11 C12 C13 52.7(6) . . . . ?
O15 C11 C12 O12 174.3(4) . . . . ?
O15 C11 O4 C4 77.7(5) . . . . ?
O15 C15 C16 P1 63.9(5) . . . . ?
O22 C22 C23 C24 -175.7(4) . . . . ?
O22 C22 C23 O23 65.9(5) . . . . ?
O23 C23 C24 C25 172.5(4) . . . . ?
O23 C23 C24 O24 -67.9(5) . . . . ?
O24 C24 C25 C26 68.4(6) . . . . ?
O24 C24 C25 O25 -172.3(4) . . . . ?
O24 C31 C32 C33 -66.1(5) . . . . ?
O24 C31 C32 O32 55.3(6) . . . . ?
O24 C31 O35 C35 58.3(5) . . . . ?
O25 C21 C22 C23 57.6(6) . . . . ?
O25 C21 C22 O22 179.0(4) . . . . ?
O25 C21 O14 C14 92.6(5) . . . . ?
O25 C25 C26 O26 -71.3(5) . . . . ?
O32 C32 C33 C34 -175.9(4) . . . . ?
O32 C32 C33 O33 65.8(5) . . . . ?
O33 C33 C34 C35 169.5(4) . . . . ?
O33 C33 C34 O34 -70.4(5) . . . . ?
O34 C34 C35 C36 70.4(5) . . . . ?
O34 C34 C35 O35 -171.2(4) . . . . ?
O34 C41 C42 C43 -63.2(5) . . . . ?
O34 C41 C42 O42 57.6(5) . . . . ?
O34 C41 O45 C45 56.8(6) . . . . ?
O35 C31 C32 C33 56.9(5) . . . . ?
O35 C31 C32 O32 178.3(4) . . . . ?
O35 C31 O24 C24 97.6(5) . . . . ?
O35 C35 C36 O36 -67.8(5) . . . . ?
O42 C42 C43 C44 -176.8(4) . . . . ?
O42 C42 C43 O43 63.4(5) . . . . ?
O43 C43 C44 C45 165.5(4) . . . . ?
O43 C43 C44 O44 -73.3(5) . . . . ?
O44 C44 C45 C46 76.9(6) . . . . ?
O44 C44 C45 O45 -164.1(4) . . . . ?
O44 C51 C52 C53 -62.3(6) . . . . ?
O44 C51 C52 O52 59.7(6) . . . . ?
O44 C51 O55 C55 58.8(6) . . . . ?
O45 C41 C42 C43 60.1(5) . . . . ?
O45 C41 C42 O42 -179.1(4) . . . . ?
O45 C41 O34 C34 96.3(5) . . . . ?
O45 C45 C46 O46 -70.1(5) . . . . ?
O52 C52 C53 C54 -178.7(5) . . . . ?
O52 C52 C53 O53 61.1(6) . . . . ?
O53 C53 C54 C55 174.1(4) . . . . ?
O53 C53 C54 O1 -65.4(6) . . . . ?
O55 C51 C52 C53 59.7(6) . . . . ?
O55 C51 C52 O52 -178.2(4) . . . . ?
O55 C51 O44 C44 99.4(5) . . . . ?
O55 C55 C56 O56 -72.3(5) . . . . ?
P1 C60 C61 C62 175.6(6) . . . . ?
P1 C60 C65 C64 -177.1(6) . . . . ?
P1 C60 C65 N1 5.5(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
